Compendium of food additive specifications - fao.org · A consolidated edition of the Compendium for food additive specifications is ... Index by JECFA specifications title, chemical

Compendiumof food additivespecifications

Addendum 9

Pre-print editionfor the 34th session of the Codex Alimentarius

Committee for Food Additives and Contaminants(CCFAC)

Joint FAO/WHO Expert Committeeon Food Additives57th session

Rome, Italy, 5-14 June 2001

© FAO, Rome 2001

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INTRODUCTION

This volume contains specifications of identity and purity prepared at the fifty-seventh meeting ofthe Joint FAO/WHO Expert Committee on Food Additives (JECFA), held in Rome, 5-14 June 2001. Thesespecifications should be considered only in conjunction with the Report of the above meeting which will beprinted in the WHO Technical Report Series. Toxicological monographs of the substances considered at the57th meeting of JECFA will be published in the WHO Food Additives Series as No. 48.

The general principles applied in the elaboration of specifications established at the earlier JECFAsessions have been published in the Principles for the Safety Assessment of Food Additives andContaminants in Food, WHO Environmental Health Criteria, No. 70, 1987. The specifications of identityand purity of food additives established by JECFA are meant to identify the substance that has been subjectto biological testing, to ensure that the substance is of adequate degree of purity for safe use in food, and toreflect and encourage good manufacturing practices. These principles were last reaffirmed by the 39thsession of JECFA in 1992.

The specifications are mainly established for the use of toxicologists and others concerned with theidentity and purity of the substance. As agreed by JECFA at its twenty-sixth meeting, specifications mayalso be established prior to the eventual completion of toxicological evaluation, in certain cases, when theavailable toxicological data are inadequate or incomplete, and do not permit the establishment of full ortemporary acceptable daily intakes (ADIs). References are made in individual specifications to some of thecriteria that may be of interest in commerce, but they do not necessarily include all the requirements ofinterest to the commercial user. These specifications are not more stringent than is necessary to accomplishtheir purpose and should easily be attainable by the producing industries. The report of the twenty-thirdsession gives the reasons why certain specifications are designated as "tentative".

There were a total of 342 specifications (25 food additives, uses other than flavouring agent; 317flavouring agents) prepared at the 57th session of which 193 were new. Thirty-two specifications weredesignated newly as tentative, for ninety-four flavouring agents the tentative status was maintained.

Comments and suggestions regarding this Volume are encouraged. Please send to Chief, FoodQuality and Standards Service, Food and Nutrition Division, FAO, Viale delle Terme di Caracalla, 00100Rome, Italy.

NOTE: Use of (FNP 5) in specifications refers to General Methods (Guide to JECFA Specifications),FAO Food and Nutrition Paper 5/Rev. 2 (1991).

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Notes to the Reader:

On-line edition of the Compendium for food additive specifications

A consolidated edition of the Compendium for food additive specifications is now available at FAO'sJECFA web-site (http://www.fao.org/es/ESN/jecfa/). The edition is divided into two sections: one coveringflavouring agents and the other covering all other food additives. Users can search by additive name ornumber (INS, JECFA No., FEMA, CAS). For additives other than flavouring agents, they can also search byfunctional use and purity criteria. Searches can also be conducted for all specifications designated astentative. The analytical methods for food additives which are published as Guide to JECFA Specifications(FAO Food and Nutrition Paper 5/Rev. 2), can be accessed as well, even with a direct link from the singlespecification.

The FAO Joint Secretariat to JECFA welcomes and encourages any feedback on this new tool andencourages suggestions how the availability of the results of JECFA's work can be improved. Please sendyour comments to [email protected].

New: Index by JECFA specifications title, chemical name, or synonym(s)

The structure of this edition was slightly changed. Following comments from users, the table ofcontents for the flavours sections has been replaced by a comprehensive index listing all names, chemicalnames, and synonyms in one comprehensive index.

Acknowledgement

The Committee and the FAO Joint Secretariat wishes to thank Dr. Atsushi Okiyama, VisitingScientist to FAO, for his assistance and support in preparing the the updated online edition of thiscompendium.

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CONTENTS

Section A: Specifications of certain food additives (uses other than as flavouring agent)

ACESULFAME POTASSIUM 1BLACKCURRANT EXTRACT 3CALCIUM DIHYDROGEN DIPHOSPHATE 7beta-CAROTENE FROM BLAKESLEA TRISPORA 9CARRAGEENAN 13

CURCUMIN 21CURDLAN 25alpha-CYCLODEXTRIN 29DIACETYLTARTARIC AND FATTY ACID ESTERS OF GLYCEROL 33GENERAL SPECIFICATIONS AND CONSIDERATIONS FOR ENZYME PREPARATIONS USED INFOOD PROCESSING 37

HYDROGENATED POLY-1-DECENE 41INVERTASE FROM SACCHAROMYCES CEREVISIAE 45D L-MALIC ACID 49MODIFIED STARCHES 53MONOMAGNESIUM PHOSPHATE 69

NATAMYCIN 71PECTINS 75PROCESSED EUCHEUMA SEAWEED 81QUILLAIA EXTRACTS 89SMOKE FLAVOURINGS 93

SODIUM CALCIUM POLYPHOSPHATE 99SODIUM SULPHATE 101D-TAGATOSE 103TAGETES EXTRACT 105TRISODIUM DIPHOSPHATE 107

Section B: Specifications of certain flavourings 109

Section C: Principles governing the establishment and revision of specifications 190

Index to Section B: Specifications of certain flavourings 196

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ACESULFAME POTASSIUM page 1 (2)

ACESULFAME POTASSIUM

Prepared at the 57th JECFA (2001) and published in FNP 52 Add 9 (2001),superseding specifications prepared at the 46th JECFA (1996) and published in FNP52 Add 4 (1996). An ADI of 0-15 mg/kg body weight was established at the 46thJECFA in 1996.

SYNONYMS Acesulfame K; INS No. 950

DEFINITION

Chemical names Potassium salt of 6-methyl-1,2,3-oxathiazine-4(3H)-one-2,2-dioxide; potassium saltof 3,4-dihydro-6-methyl-1,2,3-oxathiazine-4-one-2,2-dioxide

C.A.S. number 55589-62-3

Chemical formula C4H4KNO4S

Structural formula

NK

SO2

OH3C

O

Formula weight 201.24

Assay Not less than 99.0% and not more than 101.0% on the dried basis

DESCRIPTION Odourless, white crystalline powder

FUNCTIONAL USES Sweetener, flavour enhancer

CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Freely soluble in water, very slightly soluble in ethanol

Spectrophotometry Dissolve 10 mg of the sample in 1,000 ml of water. The solution shows anabsorbance maximum at 227±2 nm

Test for potassium (FNP 5) Passes testTest the residue obtained by igniting 2 g of the sample

Precipitation test Add a few drops of a 10% solution of sodium cobaltinitrite to a solution of 0.2 g of thesample in 2 ml of acetic acid TS and 2 ml of water. A yellow precipitate is produced.

PURITY

Loss on drying (FNP 5) Not more than 1.0% (105o, 2 h)

pH (FNP 5) 5.5 – 7.5 (1% soln)

Organic impurities Passes test for 20 mg/kg of UV active componentsSee description under TESTS

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ACESULFAME POTASSIUM page 2 (2)

Fluoride (FNP 5) Not more than 3 mg/kgMethod III; using an appropriate sample size and appropriate volumes of the standardsolution for construction of the calibration curve.

Lead Not more than 1 mg/kgDetermine using an atomic absorption technique appropriate to the specified level. Theselection of sample size and method of sample preparation may be based on theprinciples of the method described in FNP 5, “Instrumental Methods.”

TESTS

PURITY TESTS

Organic impurities Proceed as directed under the method for Chromatography (High Performance LiquidChromatography, FNP 5) using the following conditions and using 4-hydroxybenzoicacid ethyl ester as the reference substance:

Column: 25 cm x 4.6 mm stainless steelStationary phase: Reversed phase (C18 silica gel, 3 - 5 µm)Elution: IsocraticMobile phase: Acetonitrile/0.01 mol/l tetrabutyl ammonium hydrogen sulfate(TBAHS) in water; 40/60 v/vFlow: About 1 ml/minDetector type: UV or Diode array, 227 nmSample size: 20 µl of a 10 g/l solution of the sample in deionized water

The chromatographic system must be capable of separating acesulfame K and 4-hydroxybenzoic acid ethyl ester with a resolution of 2.

If peaks other than that due to acesulfame K appear within three times the elutiontime of acesulfame K, carry out a second run using 20 µl of a 0.2 mg/l solution of thesample.

The sum of the areas of all peaks eluted in the first run within 3 times the elution timeof acesulfame K elution time, except for the acesulfame K peak, does not exceed thepeak area of acesulfame K in the second run.

METHOD OF ASSAY Dissolve about 0.15 g of the dried sample (dissolution may be slow), accuratelyweighed, in 50.0 ml glacial acetic acid and titrate potentiometrically with 0.1 Nperchloric acid, or add two drops of crystal violet TS and titrate with 0.1 N perchloricacid, to a blue-green end-point which persists for at least 30 sec. Perform a blankdetermination and make any necessary correction. Each ml of 0.1 N perchloric acid isequivalent to 20.12 mg of C4H4KNO4S.

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BLACKCURRANT EXTRACT page 1 (3)

BLACKCURRANT EXTRACT

Prepared at the 57th JECFA (2001) and published in FNP 52 Add 9 (2001),superseding tentative specifications prepared at the 55th JECFA (2000), published inFNP 52 Add 8 (2000).

SYNONYMS INS No. 163 (iii)

DEFINITION Blackcurrant extract is obtained from blackcurrant pomace by aqueous extraction. Themain colouring principles are four anthocyanins (cyanidin 3-rutinoside, delphinidin 3-rutinoside, cyanidin 3-glucoside, delphinidin 3-glucoside). Most of the extracted sugarsare fermented to alcohol and practically all the alcohol is removed during theconcentration of fermented extract by vacuum evaporation. During the extractionprocess, sulfur dioxide is used and residual sulfur dioxide may be present. Commercialproducts may be in the form of a concentrated liquid, a paste, or a spray-dried powder.The spray-dried powder may contain an added carrier such as maltodextrin or glucosesyrup.

Chemical names I. Cyanidin 3-rutinosideII. Delphinidin 3-rutinoside

III. Cyanidin 3-glucosideIV. Delphinidin 3-glucoside

C.A.S. number I. 18719-76-1II. 15674-58-5

III. 7084-24-4IV. 6906-38-3

Chemical formula I. [C27H31O15]+ X-

II. [C27H31O16]+ X-

Where X-= counter ion

III. [C21H21O11]+ X-

IV. [C21H21O12]+ X-

Structural formula

OHO

OH

OR2

OH

OH

R1

I. R1 = H, R2 = rutinoseII. R1 = OH, R2 = rutinoseIII. R1 = H, R2 = glucoseIV. R1 = OH, R2 = glucose

Where X-= counter ion

Assay The colour intensity is not less than declared.

DESCRIPTION Purplish-red liquid, paste or powder having a slight characteristic odour.

FUNCTIONAL USES Colour

CHARACTERISTICS

IDENTIFICATION

X-

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Solubility (FNP 5) Soluble in water and ethanol.

Spectrometry (FNP 5) At pH 3 the absorbance maximum is about 520 nm.

Colour reaction Add 0.1 g of the sample to 50 ml of water and shake thoroughly. Filter if necessary.The solution shows red to purplish-red colour and it turns to blue or dark green on theaddition of sodium hydroxide TS.

Chromatography The retention times for the major two peaks in the chromatogram of sample solutioncorrespond to those for cyanidin 3-rutinoside and delphinidin 3-rutinoside in thechromatogram of reference using the conditions described under TESTS.

PURITY

Sulfur dioxide Not more than 50 mg/kg for each unit of colour intensitySee description under TESTS and METHOD OF ASSAY.

Basic colouring matter Add 1 g of the sample to 100 ml of 1% sodium hydroxide solution and shake well.Extract 30 ml of this solution with 15 ml ether. Extract the ether solution twice with 5ml dilute acetic acid TS. The acetic acid extract is colourless.

Other acidic colouring matters Add 1 ml of ammonia TS and 10 ml of water to 1 g of the sample. Following thedirections in Chromatography (FNP 5) place 2 µl of the solution on thechromatographic sheet and dry it. Use a mixture of pyridine and ammonia TS (2:1 byvolume) as developing solvent and stop the development when the solvent front reachesabout 15 cm height from the point where the sample solution was placed. No spot isobserved in daylight at the solvent front after drying. If any spot is observed, it shouldbe decolourized when sprayed with a solution of 40% stannous chloride in hydrochloricacid.

Lead Not more than 2 mg/kgDetermine using an atomic absorption technique appropriate to the specified level.The selection of sample size and method of sample preparation may be based on theprinciples of the method described on FNP 5, "Instrumental methods".

TESTS

IDENTIFICATION TESTS

Chromatography Determined by liquid chromatography (FNP5) using the following procedure:

Preparation of sample solution: Dissolve 500 mg of sample into 25 ml of 0.3% HCland wash with three volumes of ethyl acetate. Filter througha 0.45 µm filter.

Preparation of reference solution: Dissolve 2 mg of cyanidin 3-rutinoside anddelphinidin 3-rutinoside into 10 ml of 0.3% HCl and filterthrough a 0.45 µm filter.

Apparatus: Liquid chromatograph equipped with a UV or diode array detector and anintegrator.

Conditions:Column: Lichrosorb RP18 (length 25 cm, diameter 4.6 mm, particle

size 5 µm) or equivalentColumn temperature: 35°Mobile phase: Linear gradient from 40% B to 100% B during 20 min

A: Formic acid - water (10:90)B: Formic acid - water - acetonitrile (10:75:15)

Flow rate: 0.8 ml/min

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Injection volume: 10 µlWave length: 520 nm

PURITY TESTS

Sulfur dioxide Distil 10 g of the sample with 100 ml of water and 25 ml of 30% phosphoric acidsolution in a distilling flask with the Wagner tube. In an absorption flask, place 25 ml of2% lead acetate solution previously prepared. Insert the lower end of the condenser intothe lead acetate solution in the absorption flask. Distil until the liquid in the absorptionflask reaches about 100 ml and rinse the end of the condenser with a little amount ofwater. To the distilled solution add 5 ml of hydrochloric acid and 1 ml of starch TS, andtitrate with 0.01 N iodine. Each ml of 0.01 N iodine is equivalent to 0.3203 mg of SO2.

METHOD OF ASSAY Prepare approximately 200 ml of pH 3.0 citric acid - dibasic sodium phosphate buffersolution: Mix 159 volumes of 2.1% citric acid solution and 41 volumes of 0.16%dibasic sodium phosphate solution, and adjust the pH to 3.0, using the citric acidsolution or dibasic sodium phosphate solution.

Weigh accurately an adequate amount of the sample so that the measured absorbanceis between 0.2 and 0.7, and add pH 3.0 citric acid - dibasic sodium phosphate buffersolution to make up a 100-ml solution. Measure the absorbance A of this solution in a1-cm cell at the wavelength of maximum absorption around 520 nm, using pH 3.0citric acid - dibasic sodium phosphate buffer solution as the blank.

Colour intensity = [A x 10]/[weight of sample (g)]

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CALCIUM DIHYDROGEN DIPHOSPHATE page 1 (2)

CALCIUM DIHYDROGEN DIPHOSPHATE

New specifications prepared at the 57th JECFA (2001) and published in FNP 52 Add9 (2001). No ADI, but a group MTDI of 70 mg/kg bw, expressed as phosphorus fromall food sources, was established at the 26th JECFA (1982).

SYNONYMS Acid calcium pyrophosphate, monocalcium dihydrogen pyrophosphate;INS No. 450 (vii)

DEFINITION

Chemical names Monocalcium dihydrogen diphosphate

C.A.S. number 14866-19-4

Chemical formula CaH2P2O7


Assay Not more than 64% expressed as P2 O5 on dried basis.

DESCRIPTION White crystals or powder

FUNCTIONAL USES Stabilizer, leavening agent, emulsifier, nutrient

CHARACTERISTICS

IDENTIFICATION

Test for calcium (FNP 5) Passes test

Test for phosphate (FNP 5) Passes test

PURITY

Loss on drying (FNP 5) Anhydrous: Not more than 1% (105°, 4 h)

Acid insoluble matter (FNP 5) Not more than 0.4%

Fluoride (FNP 5) Not more than 30 mg/kgMethod III; use an appropriate sample size and appropriate volumes of standardsolution for construction of the calibration curve.


Arsenic (FNP 5) Not more than 3 mg/kg

METHOD OF ASSAY Weigh accurately about 200 mg of the sample, dissolve in 25 ml of water and 10 ml ofdiluted nitric acid TS and boil for 30 min. Filter if necessary, and wash any precipitate,then dissolve the precipitate by the addition of 1 ml diluted nitric acid TS. Adjust thetemperature to about 50o , add 75 ml of ammonium molybdate TS, and maintain thetemperature at about 50o for 30 min, stirring occasionally. Allow to stand for 16 h orovernight at room temperature. Decant the supernate, through a filter paper, wash theprecipitate once or twice with water by decantation using 30 to 40 ml each time, andpour the washings through the same filter. Transfer the precipitate to the same filter,and wash with potassium nitrate solution (1 in 100) until the filtrate is no longer acid tolitmus paper. Transfer the precipitate with filter paper to the original precipitation

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CALCIUM DIHYDROGEN DIPHOSPHATE page 2 (2)

vessel, add 50.0 ml of 1N sodium hydroxide, agitate until the precipitate is dissolved,add 3 drops of phenolphthalein TS and titrate the excess alkali with 1N sulfuric acid.Each ml of 1N sodium hydroxide consumed is equivalent to 3.088 mg of P2O5.

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beta-CAROTENE FROM BLAKESLEA TRISPORA page 1 (3)

beta-CAROTENE FROM BLAKESLEA TRISPORA(Tentative)

New specifications prepared at the 57th JECFA (2001) and published in FNP 52 Add9 (2001). A group ADI with synthetic ß-carotene of was established at the 57th

JECFA (2001).

Information required on method of analysis for residual solvents (ethyl acetate andisobutyl acetate).

SYNONYMS CI Food Orange 5; INS No. 160a

DEFINITION Obtained by a fermentation process using the two sexual mating types (+) and (-) of thefungus Blakeslea trispora. The colour is isolated from the biomass by solventextraction and crystallised. The colouring principle consists predominantly of trans β-carotene together with variable amounts of cis isomers of β-carotene. Minor amounts ofother carotenoids of which γ-carotene accounts for the major part may also be present.The only organic solvents used in the extraction and purification are ethanol,isopropanol, ethyl acetate and isobutyl acetate.

The main articles of commerce are suspensions in food grade vegetable/plant oil andwater dispersible powders. This is for ease of the use and to improve stability ascarotenes easily oxidise.

Class Carotenoid

Chemical names β-carotene, β,β-carotene

C.A.S. number 7235-40-7

Chemical formula C40H56

Structural formula C H 3

H 3 C C H 3

C H 3

C H 3

C H 3 C H 3 H 3 C C H 3

H 3 C


Assay Not less than 96.0% of total colouring matter (expressed as β-carotene)

DESCRIPTION Red to brownish-red cyrstals or crystalline powder


CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Insoluble in water; practically insoluble in ethanol, slightly soluble in vegetable oil.

Spectrometry Determine the absorbance of the diluted sample solution used in the Method of Assayat 455 nm and 483 nm. The ratio is between 1.14 and 1.19.

Spectrometry Determine the absorbance of the diluted sample solution used in the Method of Assayat 455 nm and 340 nm. The ratio is not lower than 0.75.

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Test for carotenoid The colour of a solution of the sample in acetone disappears after successive addition ofa 5% solution of sodium nitrite and 0.5 M of sulfuric acid.

PURITY

Sulfated ash (FNP 5) Not more than 0.2%

Carotenoids other than β-carotene

Not more than 3.0% of total colouring mattersSee description under TESTS

Ethanol:Ethyl acetate: } Not more than 0.8% singly or in combination

Isopropanol: Not more than 0.1%

Residual solvent (FNP 5)

Isobutyl acetate: Not more than 1.0%


TESTS

PURITY TESTS

Carotenoids other thanβ-carotene

Determine by liquid chromatography (FNP 5) using the following the followingprocedure:

Apparatus:HPLC system equipped with- UV detector (445 nm)- Column heater (30°)- Refrigerated autosampler (0-10°)- Column: 250 mm x 4.6 mm, Vydac 218 TP54, 5 µm, or equivalent- Solvent system: 99% methanol and 1% tetrahydrofuran containing 50 mg/l of L-ascorbic acid.

Working conditions:- Flow rate: 0.6 ml/min- Injection 10 µl- Run time: approximately 25 min

Sample preparation: Weigh 25 mg of the sample and dissolve in tetrahydrofuran.Make up to 100 ml in a volumetric flask. Dilute 1 ml of the solution to 25 ml in avolumetric flask with a 10% ethanol:tetrahydrofuran solution.

Results: The retention time for β-carotene (all trans isomer) is about 19 minutescorresponding to the largest peak in the chromatogram. The retention time for γ-carotene is about 20 minutes and the peak at about 22 minutes corresponds to the 13-cis isomer.

γ-carotene as a % of total β-carotene equals:

321

1

AAA100A

++

×

where

A1 is the area of the ã-carotene peakA2 is the area of the all-trans β-carotene peak

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A3 is the combined area of the peaks from the isomers of all trans β-carotene

METHOD OF ASSAY Proceed as directed in Colouring matters, Total Content by Spectrophotometry (FNP5), procedure 2 using the following conditions:

W = 0.08 gV1 = V2 = V3 = 100 mlv1 = v2 = 5 mlA1%

1 cm = 2500Amax = about 455 nm

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CARRAGEENAN page 1 (8)

CARRAGEENAN

Prepared at the 57th JECFA (2001) and published in FNP 52 Add 9 (2001),superseding specifications prepared at the 51st JECFA (1998), published in FNP 52Add 6 (1998)). A group ADI “not specified” for carrageenan and processedeucheuma seaweed was established at the 57th JECFA (2001).

SYNONYMS Irish moss gelose (from Chondrus spp.); Eucheuman (from Eucheuma spp.);Iridophycan (from Iridaea spp.); Hypnean (from Hypnea spp.); Furcellaran or Danishagar (from Furcellaria fastigiata); INS No. 407.

DEFINITION A substance with hydrocolloid properties obtained from certain members of the classRhodophyceae (red seaweeds).

The principal commercial sources of carrageenans are the following families andgenera of the class of Rhodophyceae:Furcellariacaea such as FurcellariaGigartinaceae such as Chondrus, Gigartina, IridaeaHypnaeceae such as HypneaPhyllophoraceae such as Phyllophora, Gynmogongrus, AhnfeltiaSolieriaceae such as Eucheuma, Anatheca, Meristotheca.

Carrageenan is a hydrocolloid consisting mainly of the ammonium, calcium,magnesium, potassium and sodium sulfate esters of galactose and 3,6-anhydrogalactosepolysaccharides. These hexoses are alternately linked α-1,3 and β-1,4 in the copolymer.The relative proportions of cations existing in carrageenan may be changed duringprocessing to the extent that one may become predominant.

The prevalent polysaccharides in carrageenan are designated as kappa-, iota-, andlambda-carrageenan. Kappa-carrageenan is mostly the alternating polymer ofD-galactose-4-sulfate and 3,6-anhydro-D-galactose; iota-carrageenan is similar, exceptthat the 3,6-anhydrogalactose is sulfated at carbon 2. Between kappa-carrageenan andiota-carrageenan there is a continuum of intermediate compositions differing in degreeof sulfation at carbon 2. In lambda-carrageenan, the alternating monomeric units aremostly D-galactose-2-sulfate (1,3-linked) and D-galactose-2,6-disulfate (1,4-linked).

Carrageenan is obtained by extraction from seaweed into water or aqueous dilute alkali.Carrageenan may be recovered by alcohol precipitation, by drum drying, or byprecipitation in aqueous potassium chloride and subsequent freezing. The alcohols usedduring recovery and purification are restricted to methanol, ethanol, and isopropanol.Articles of commerce may include sugars for standardization purposes, salts to obtainspecific gelling or thickening characteristics, or emulsifiers carried over from drumdrying processes.

C.A.S. number 9000-07-1

DESCRIPTION Yellowish or tan to white, coarse to fine powder that is practically odourless.

FUNCTIONAL USES Thickener, gelling agent, stabilizer, emulsifier

CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Insoluble in ethanol; soluble in water at a temperature of about 80o, forming a viscousclear or slightly opalescent solution that flows readily; disperses in water morereadily if first moistened with alcohol, glycerol, or a saturated solution of glucose orsucrose in water.

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Test for sulfate Dissolve a 100-mg sample in 20 ml of water (with heating if necessary), and add 3 mlof barium chloride TS and 5 ml of hydrochloric acid, dilute TS; filter if a precipitateforms. Boil the solution or the filtrate for 5 min. A white, crystalline precipitateappears.

Test for galactose andanhydrogalactose

Proceed as directed under Gum Constituents Identification (FNP 5) using thefollowing as reference standards: galactose, rhamnose, galacturonic acid,3,6-anhydrogalactose, mannose, arabinose and xylose. Galactose and3,6-anhydrogalactose should be present.

Identification ofhydrocolloid andpredominant type ofcopolymer

Add 4 g of sample to 200 ml of water, and heat the mixture in a water bath at 80o,with constant stirring, until dissolved. Replace any water lost by evaporation, andallow the solution to cool to room temperature. It becomes viscous and may form agel. To 50 ml of the solution or gel add 200 mg of potassium chloride, then reheat,mix well, and cool. A short-textured ("brittle") gel indicates a carrageenan of apredominantly kappa type, and a compliant ("elastic") gel indicates a predominantlyiota type. If the solution does not gel, the carrageenan is of a predominantly lambdatype.

Infrared absorption Passes testSee description under TESTS

PURITY

Loss on drying (FNP 5) Not more than 12% (105o to constant weight)

pH (FNP 5) Between 8 and 11 (1 in 100 suspension)

Viscosity Not less than 5 cp at 75o (1.5% solution)See description under TESTS

Sulfate Not less than 15% and not more than 40% (as SO42-) on a dry weight basis

See description under TESTS

Total ash Not less than 15% and not more than 40% on a dry weight basisSee description under TESTS.

Acid-insoluble ash (FNP 5) Not more than 1%

Acid-insoluble matter(FNP 5)

Not more than 2%Use 2 g of sample obtained from part (a) of the procedure for sulfate determination.

Residual solvents Not more than 0.1% of ethanol, isopropanol, or methanol, singly or in combinationSee description under TESTS

Microbiological criteria(FNP 5)

Initially prepare a 10-1 dilution by adding a 50-g sample to 450 ml of Butterfield’sphosphate-buffered dilution water and homogenising the mixture in a high-speedblender.Total (aerobic) plate count: Not more than 5000 cfu/gSalmonella spp.: Negative per testE. coli: Negative in 1 g

Arsenic (FNP 5) Not more than 3 mg/kgDetermine by atomic absorption hydride technique using a 3 gram sample.

Lead Not more than 5 mg/kgSee description under TESTS

Cadmium Not more than 2 mg/kgSee description under TESTS

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Mercury Not more than 1 mg/kgSee description under TESTS

TESTS


Infrared absorption Obtain infrared absorption spectra on the gelling and non-gelling fractions of thesample by the following procedure: Disperse 2 g of the sample in 200 ml of 2.5%potassium chloride solution, and stir for 1 h. Let stand overnight, stir again for 1 h,and transfer into a centrifuge tube. (If the transfer cannot be made because thedispersion is too viscous, dilute with up to 200 ml of the potassium chloridesolution.) Centrifuge for 15 min at approximately 1000 x g.

Remove the clear supernatant, resuspend the residue in 200 ml of 2.5% potassiumchloride solution, and centrifuge again. Coagulate the combined supernatants byadding 2 volumes of 85% ethanol or isopropanol (NOTE: Retain the sediment for useas directed below). Recover the coagulum, and wash it with 250 ml of the alcohol.Press the excess liquid from the coagulum, and dry it at 60o for 2 h. The productobtained is the non-gelling fraction (lambda-carrageenan).

Disperse the sediment (retained above) in 250 ml of cold water, heat at 90° for 10min, and cool to 60o. Coagulate the mixture, and then recover, wash, and dry thecoagulum as described above. The product obtained is the gelling fraction (kappa-and iota-carrageenan).

Prepare a 0.2% aqueous solution of each fraction, cast films 0.5 mm thick (when dry)on a suitable non-sticking surface such as Teflon, and obtain the infrared absorptionspectrum of each film. (Alternatively, the spectra may be obtained using films cast onpotassium bromide plates, if care is taken to avoid moisture).

Carrageenan has strong, broad absorption bands, typical of all polysaccharides, in the1000 to 1100 cm-1 region. Absorption maxima are 1065 and 1020 cm-1 for gellingand non-gelling types, respectively. Other characteristic absorption bands and theirintensities relative to the absorbance at 1050 cm-1 are as follows:

Wave number(cm-1)

Molecular Assignment Absorbance relative to 1050 cm-1

Kappa Iota Lambda

1220-1260 ester sulfate 0.2-1.2 1.2-1.6 1.4-2.0928-933 3,6-anhydrogalactose 0.2-0.6 0.2-0.4 0-0.2840-850 galactose-4-sulfate 0.1-0.5 0.2-0.4 -825-830 galactose-2-sulfate - - 0.2-0.4810-820 galactose-6-sulfate - - 0.1-0.3800-805 3,6-anhydrogalactose-2-

sulfate0-0.2 0.2-0.4 -

PURITY TESTS

Sulfate Principle: Hydrolysed sulfate groups are precipitated as barium sulfate.

Procedure:(a) Disperse an accurately weighed 8 g sample of commercial product into 400 ml of60% w/w isopropanol/water at room temperature. Stir gently for 4 h. Filter throughash-free filter paper. Discard the filtrate. Wash the material remaining on the filterpaper with two 10-ml portions of 60% isopropanol/water. Dry the material at 105° toconstant weight.

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Approximately 1 g of the dried matter is to be used for part (b). The remainder shouldbe retained for determination of Total ash and Acid-insoluble matter.

(b) Accurately weigh a 1 g sample (W1 ) obtained from part (a). Transfer the sampleto a 100-ml long-neck round-bottom flask. Add 50 ml of 0.2 N hydrochloric acid. Fita condenser, preferably one with at least 5 condensing bulbs, to the flask and refluxfor 1 h. Add 25 ml of a 10% (by volume) hydrogen peroxide solution and resumerefluxing for about 5 h or until the solution becomes completely clear. Transfer thesolution to a 600-ml beaker, bring to a boil, and add dropwise 10 ml of a 10% bariumchloride solution. Heat the reaction mixture for 2 h on a boiling water bath. Filter themixture through ash-free slow-filtration filter paper. Wash with boiling distilledwater until the filtrate is free from chloride. Dry the filter paper and contents in adrying oven. Gently burn and ash the paper at 800° in a tared porcelain or silicacrucible until the ash is white. Cool in a desiccator.

Weigh the crucible containing the ash. Calculate the percentage sulfate from theweight in g (W2) of the ash (barium sulfate) using the formula:

(W2/W1) x 100 x 0.4116

Total ash Accurately weigh 2 g of the dried sample (W1) obtained from part (a) under theprocedure for sulfate determination above. Transfer to a previously ignited, taredsilica or platinum crucible. Heat the sample with a suitable infrared lamp, increasingthe intensity gradually, until the sample is completely charred; continue heating foran additional 30 min. Transfer the crucible with the charred sample into a mufflefurnace and ignite at about 550º for 1 h. Cool in a desiccator and weigh. Repeat theignition in the muffle furnace until a constant weight (W2) is obtained. If a carbon-free ash is not obtained after the first ignition, moisten the charred spot with a 1-in-10solution of ammonium nitrate and dry under an infrared lamp. Repeat the ignitionstep. Calculate the percentage of total ash of the sample:

(W2/W1) x 100

Retain the ash for the Acid-insoluble ash test.

Viscosity Transfer 7.5 g of the sample into a tared, 600-ml tall-form (Berzelius) beaker, anddisperse with agitation for 10 to 20 min in 450 ml of deionized water. Add sufficientwater to bring the final weight to 500 g, and heat in a water bath with continuousagitation, until a temperature of 80o is reached (20 - 30 min). Add water to adjust forloss by evaporation, cool to 76-77o, and heat in a constant temperature bath at 75o.Pre-heat the bob and guard of a Brookfield LVF or LVT viscometer to approximately75º in water. Dry the bob and guard, and attach them to the viscometer, which shouldbe equipped with a No. 1 spindle (19 mm in diameter, approximately 65 mm inlength) and capable of rotating at 30 rpm. Adjust the height of the bob in the samplesolution, start the viscometer rotating at 30 rpm and, after six complete revolutions ofthe viscometer, take the viscometer reading on the 0-100 scale.

If the viscosity is very low, increased precision may be obtained by using theBrookfield UL (ultra low) adapter or equivalent. (Note. Samples of some types ofcarrageenan may be too viscous to read when a No. 1 spindle is used. Such samplesobviously pass the specification, but if a viscosity reading is desired for otherreasons, use a No. 2 spindle and take the reading on the 0-100 scale or on the 0-500scale.)

Record the results in centipoises, obtained by multiplying the reading on the scale bythe factor given by the Brookfield manufacturer.

Residual solvents Standard Alcohol Solution: Transfer 500 mg each of chromatographic qualitymethanol, ethanol, and isopropanol into a 50 ml volumetric flask, dilute to volumewith water, and mix. Pipet 10 ml of this solution into a 100-ml volumetric flask,dilute to volume with water and mix.

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TBA Standard Solution: Transfer 500 mg of chromatographic quality tertiary-butylalcohol into a 50-ml volumetric flask, dilute to volume with water, and mix. Pipet 10ml of this solution into a 100-ml volumetric flask, dilute to volume with water andmix.

Mixed Standard Solution: Pipet 4 ml each of the Standard Alcohol Solution and ofthe TBA Standard Solution into a 125-ml graduated Erlenmeyer flask, dilute to about100 ml with water, and mix. This solution contains approximately 40 µg of eachalcohol per ml.

Sample Preparation: Disperse 1 ml of a suitable antifoam emulsion, such asDow-Corning G-10 or equivalent, in 200 ml of water contained in a 1000-ml 24/40round-bottom distilling flask. Add about 5 g of the sample, accurately weighed, andshake for 1 h on a wrist-action mechanical shaker. Connect the flask to afractionating column, and distil about 100 ml, adjusting the heat so that foam doesnot enter the column. Add 4.0 ml of TBA Standard Solution to the distillate to obtainthe Sample Preparation.

Procedure: Inject 5 µl of the Mixed Standard Solution into a suitable gaschromatograph equipped with a flame-ionization detector and a 1.8-m x 3.2-mmstainless steel column packed with 80/100-mesh Porapak QS or equivalent. Thecarrier is helium flowing at 80 ml per min. The injection port temperature is 200o; thecolumn temperature is 165o; and the detector temperature is 200o. The retention timeof isopropanol is about 2 min, and that of tertiary-butyl alcohol about 3 min.

Measure the areas of the methanol, ethanol, isopropanol, and TBA peaks. Calculateeach response factor, fi, by the formula Ai /ATBA, in which Ai is the area of eachalcohol peak (I = methanol, ethanol, or isopropanol).

Similarly, inject 5 µl of the Sample Preparation, and measure the peak areas,recording the area of each alcohol peak as Ai, and that of the tertiary-butyl alcoholpeak as ATBA. Calculate each alcohol content, in mg/kg, in the sample taken by theformula:

Ai · 4000 / fi · ATBA · W

where W is the weight of the sample taken (grams).

Lead Principle: The sample is wet-ashed with nitric and perchloric acids and analysedusing flame atomic absorption spectrophotometry (FNP 5).

Equipment: Atomic absorption spectrophotometer

Reagents:Nitric acid, concentrated, Reagent GradePerchloric acid, concentrated, Reagent GradeHydrochloric acid, concentrated, Reagent GradeLead standard solution (certified)

Solutions:1. Stock solution (1 mg/ml): Dilute an appropriate volume of certified reagent lead

standard solution with distilled and deionized water (D/D water) to make oneliter.

2. Intermediate solutions: (a) 100 µg/ml. Pipet 10 ml of the stock solution into a100-ml volumetric flask and dilute to volume with D/D water. (b) 10 µg/ml.Pipet 10 ml of the 100 µg/ml solution into a 100-ml volumetric flask and dilute tovolume with D/D water.

3. Working solutions: Assemble four 100-ml volumetric flasks and transfer to them(pipet), respectively, 1, 5, 10, and 20 ml of intermediate lead solution (b). Diluteto volume with D/D water to make solutions containing 0.1, 0.5, 1, and 2 µgPb/ml.

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Sample preparation:(CAUTION: This procedure employs concentrated oxidizing acids and results inevolution of noxious gases. Perform operations in a fume hood.)Accurately weigh 7.5 grams of a representative dry powdered test sample into a 250-ml Erlenmeyer flask. Set up a reagent blank and carry through the same operationsas performed on the test sample. Wet the test sample with ca. 10 ml of D/D waterand add 25 ml of nitric acid. Heat gently on a hot plate (100o – 150o) until most ofthe dark fumes are evolved (ca. one hour); swirl the flask occasionally. Cool and add5 ml of perchloric acid; particles become visible at this stage. Heat gently (hot plate,100o – 150o) to concentrate until the solution turns yellowish or colourless (ca. onehour). Midway during the heating, if the solution darkens, slowly add 2-3 mlportions of nitric acid as necessary until the desired colour is achieved; do not let thesolution go to dryness. Cool the digest and wash the sides of the flask with ca. 5 mlof D/D water and swirl. Add 2 ml of hydrochloric acid. Heat again until all brownfumes are evolved and the solution is white to yellowish in colour; do not let thesolution go to dryness. Cool the solution and wash the sides of the flask with ca. 10ml of D/D water. Transfer the slightly viscous solution to a 50-ml volumetric flaskand dilute to volume with D/D water. Filter using two layers of filter paper(Whatman no. 5 or equivalent).

Determination:Set the spectrophotometer to previously established optimum conditions at 283.3 nmusing an air/acetylene oxidizing flame. Measure the absorbance of the sample, blank,and working solutions. Prepare a standard curve by plotting absorbance against µgPb/ml for the blank and working solutions. Determine the concentration of lead inthe sample solution from the standard curve. The concentration of lead in the testsample (mg Pb/kg) is:

[Pb] = F x A/B

where A is the concentration of lead in the sample solution (µg/ml), B is the weightof the test sample (grams), and F is the dilution factor (50 ml).

Cadmium Proceed as directed above for the determination of lead, using 228.8 nm as theanalysis wavelength. Intermediate and working solutions are prepared from certifiedreagent cadmium standard solution:

Intermediate solutions: (a) 100 µg/ml. Pipet 10 ml of the stock solution(1mg/ml) into a 100-ml volumetric flask and dilute to volume with distilledand deionized (D/D) water. (b) 10 µg/ml. Pipet 10 ml of solution (a) into a100-ml volumetric flask; dilute to volume with D/D water. (c) 1 µg/ml. Pipet1 ml of solution (a) into a 100-ml volumetric flask; dilute to volume with D/Dwater.Working solutions: Assemble five 50-ml volumetric flasks and transfer tothem (pipet), respectively, 0.5, 2.5, 5.0, 10, and 20 ml of intermediate solution(c). Dilute to volume with D/D water to make solutions containing 0.01,0.05, 0.1, 0.20, and 0.40 µg Cd/ml.

The concentration of cadmium in the test sample (mg Cd/kg) is:

[Cd] = F x A/B

where A is the concentration of cadmium in the sample solution (µg/ml), B is theweight of the test sample (grams), and F is the dilution factor (50 ml).

Mercury Principle: The sample is wet-ashed with nitric and perchloric acids and analysedusing hydride-generation atomic absorption spectrophotometry (FNP 5).

Equipment: Atomic absorption spectrophotometer equipped with a hydride vapourgenerator. Integral to the generator is a reactor tube or coil and a peristaltic pumpwith dual tubing channels: one channel for the sample solution and one for the tworeagent solution tubes. Flow control is determined by tubing size and tubing clamps.Flow rates are measured at the exit of the hydride generator.

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Reagents:Nitric acid, concentrated, Reagent GradePerchloric acid, concentrated, Reagent GradeHydrochloric acid, concentrated, Reagent GradeSodium borohydride, >98%Sodium hydroxide, Reagent gradeMercury standard solution (certified)

Solutions:1. Nitric acid-perchloric acid (1:1): Mix equal volumes of the two acids.2. Hydrochloric acid, 5M: Dilute 417 ml concentrated hydrochloric acid to 1 liter

with deionized water.3. Sodium borohydride solution, 0.4% (Prepare immediately before use.): First,

dissolve 2.5 g sodium hydroxide in deionized water. Then, add and dissolve 2.0g sodium borohydride. Dilute to 500 ml.

4. Stock solution (1 mg/ml): Dilute an appropriate volume of certified reagentmercury standard solution with distilled and deionized water (D/D water) tomake one liter.

5. Intermediate solutions: (a) 10,000 µg/l. Pipet 1 ml of the stock solution into a100-ml volumetric flask and dilute to volume with D/D water. (b) 100 µg/l.Pipet 1 ml of the 10,000 µg/l solution into a 100-ml volumetric flask and dilute tovolume with D/D water.

6. Working solutions: Assemble five 100-ml volumetric flasks and transfer to them(pipet), respectively, 1, 5, 10, 15, and 20 ml of intermediate solution (b). Toeach, add 10 ml of 1:1 nitric acid-perchloric acid and dilute to volume with D/Dwater to make solutions containing 1, 5, 10, 15, and 20 µg Hg/l.

Sample preparation:(CAUTION: This procedure employs concentrated oxidizing acids and results inevolution of noxious gases. Perform operations in a fume hood.)Accurately weigh 5 grams of a representative dry powdered test sample into a 250 mlErlenmeyer flask. Set up a reagent blank and carry through the same operations asperformed on the test sample. Wet the test sample with 5 ml of D/D water and thenadd 10 ml of 1:1 nitric acid-perchloric acid. Heat gently on a hot plate (100o-150o)until all of the dark fumes are evolved and the solution turns yellowish or colourless;swirl the flasks occasionally. Do not let the solution go to dryness. Cool and washthe sides of the flask with a small amount of D/D water. (Some particles may bevisible.) Cover the flask lightly and let the slightly viscous solution stand overnight.Transfer the solution to a 50-ml volumetric flask and dilute to volume with D/Dwater. Filter using 2 layers of Whatman no. 5 (or equivalent) filter paper into a 100-ml Erlenmeyer flask. Immerse the flask in an ultrasonic bath and sonicate it for 10minutes or until bubbles no longer form on the surface of the solution.

Determination:Calibrate (using water) the peristaltic pump to provide a flow rate of the samplesolution of 8 ml/min and a combined flow rate for the two reagent solutions (sodiumborohydride and 5M hydrochloric acid) of 2 ml/min. (The combined flow rate isachieved with a single pump setting.)Set the spectrophotometer to previously established optimum conditions at themercury lamp wavelength of 253.7 nm.Transfer suitable quantities of the two reagent solutions into separate graduatedcylinders. Insert separate aspirator tubing leading from the peristaltic pump into eachreagent solution and into the sample flask.Start the flow of argon carrier gas (tank outlet pressure: 3.2±0.2 kg/cm2) through thehydride vapour generator of the spectrophotometer. Start the pump to initiate flow ofthe three solutions into the hydride generator manifold where they are mixed and passinto the reactor coil to generate atomic mercury, which is carried into the absorbancecell of the spectrophotometer. Measure the absorbance for the sample. Repeat forthe blank solution and each of the working standards.Prepare a standard curve by plotting absorbance against µg Hg/l for the blank and

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working solutions. Determine the concentration of mercury in the sample solutionfrom the standard curve. The concentration of mercury in the test sample (mg Hg/kg)is:

[Hg] = FxA/1000B

where A is the concentration of mercury in the sample solution (µg /l), B is theweight of the test sample (grams), and F is the dilution factor (50 ml).

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CURCUMIN page 1 (3)

CURCUMIN

Prepared at the 57th JECFA (2001) and published in FNP 52 Add 9 (2001),superseding specifications prepared at the 55th JECFA (2000) and publishedin FNP 52 Add 8 (2000). A temporary ADI of 0-1 mg/kg bw was established atthe 44th JECFA (1995) and extended at the 57th JECFA (2001) until 2003.

SYNONYMS Curcumin, Turmeric yellow, Diferuloylmethane, Kurkum, CI Natural Yellow 3,CI (1975) 75300; INS No. 100(i)

DEFINITION Curcumin is obtained by solvent extraction of turmeric i.e., the ground rhizomesof Curcuma longa L. (Curcuma domestica Valeton). In order to obtain aconcentrated curcumin powder, the extract is purified by crystallization. Theproduct consists essentially of curcumins; i.e., the colouring principle (1,7-bis-(4-hydroxy-3-methoxy-phenyl)-hepta-1,6-diene-3,5-dione) and its desmethoxy- andbis-desmethoxy-derivatives in varying proportions. Minor amounts of oils andresins naturally occurring in turmeric may be present.

Only the following solvents may be used in the extraction: acetone, methanol,ethanol, isopropanol, hexane.

Chemical names Principal colouring components:

I. 1,7-Bis-(4-hydroxy-3-methoxyphenyl)-hepta-1,6-diene-3,5-dioneII. 1-(4-Hydroxyphenyl)-7-(4-hydroxy-3-methoxyphenyl)-hepta-

1,6-diene-3,5-dioneIII. 1,7-Bis-(4-hydroxyphenyl)-hepta-1,6-diene-3,5-dione

C.A.S. number I. 458-37-7II. 33171-16-3III. 33171-05-0

Chemical formula I. C21H20O6

II. C20H18O5

III. C19H16O4

Structural formula

O O

R2

OHHO

R1

I. R1 = R2 = OCH3

II. R1 = OCH3, R2 = H R1

III. R1 = R2 = H

Formula weight I. 368.39II. 338.39III. 308.39

Assay Not less than 90 % total colouring matters.

DESCRIPTION Orange-yellow crystalline powder.


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CURCUMIN page 2 (3)

CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Insoluble in water and in diethyl ether; soluble in ethanol and in glacial aceticacid

Colour reactions A solution of the sample in ethanol is characterized by pure yellow colour andlight green fluorescence; if this ethanol extract is added to concentrated sulfuricacid, a deep crimson colour is produced.

Treat an aqueous or dilute ethanolic solution of the sample with hydrochloricacid until a slightly orange colour begins to appear. Divide mixture into 2 partsand add some boric acid powder or crystals to one portion. Marked reddeningwill be quickly apparent, best seen by comparison with portion to which theboric acid has not been added. The test may also be made by dipping pieces offilter paper in ethanolic solution of colouring matter, drying at 100º, and thenmoistening with a weak solution of boric acid to which a few drops ofhydrochloric acid have been added. On drying, a cherry-red colour will develop.

Chromatography Spot 5 µl of test solution (0.01 g of sample in 1 ml of 95% ethanol) on a TLC(Microcrystalline cellulose, 0.1 mm) plate. Develop the plate in a chambercontaining a mixture of 3-methyl-1-butanol/ethanol/ water/ammonia (4:4:2:1) assolvent and allow the solvent front to ascend 10-15 cm. Examine under daylightand under UV-light and observe:− Two or three yellow spots with Rf between 0.2 and 0.4 under daylight and

UV-light− Spots with Rf about 0.6 and 0.8 under UV-lightAll spots show distinct yellow fluorescence under UV-light.

PURITY

Acetone: Not more than 30 mg/kgMethanol: Not more than 50 mg/kgEthanol: Not more than 50 mg/kgIsopropanol: Not more than 50 mg/kg

Residual solvents (FNP 5)

Hexane: Not more than 25 mg/kg

Lead Not more than 2 mg/kgDetermine using an atomic absorption technique appropriate to the specifiedlevel. The selection of sample size and method of sample preparation may bebased on the principles of the method described on FNP 5, "Instrumentalmethods".

METHOD OF ASSAY Accurately weigh about 0.08 g of the sample in a 200-ml volumetric flask anddissolve by shaking with ethanol. Make up to volume with ethanol and mix.Pipet 1.0 ml of solution into a 100-ml volumetric flask and make up to volumewith ethanol.

Determine the absorbance (A) at 425 nm in a 1-cm cell. Calculate the totalcolouring matters content of the sample using the following equation.

% Total Colouring matters:

1607W x 100200A x ×

where

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CURCUMIN page 3 (3)

A = absorbance of sampleW = weight of sample (g)1607 = specific absorbance of the curcumin standard in ethanol

The determination must be performed without delay, because the colour fades.

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CURDLAN page 1 (3)

CURDLAN

Prepared at the 57th JECFA (2001) and published in FNP 52 Add 9 (2001),superseding specifications prepared at the 53rd JECFA (1999) and publishedin FNP 52 Add 7 (1999). An ADI “not specified” was established at the 57thJECFA (2001).

SYNONYMS Beta-1,3-glucan; INS No. 424

DEFINITION Curdlan is a high molecular weight polysaccharide consisting of β-1,3-linkedglucose units, produced by pure-culture fermentation from a non-pathogenic andnon-toxicogenic strain of Agrobacterium biovar 1 (identified as Alcaligenesfaecalis var. myxogenes at the time of discovery) or Agrobacterium radiobacter.Curdlan consists of β-(1,3)-linked glucose residues and has the unusual propertyof forming an elastic gel upon heating its aqueous suspension.

C.A.S. number 54724-00-4

Chemical formula (C6H10O5)n

Structural formula

O

OH

OH

CH2OH

OH

O

OH

OH

CH2OH

O

OH

OH

OH

CH2OH

O O

n

Assay Not less than 80% (calculated as anhydrous glucose)

DESCRIPTION Odourless or almost odourless, white to nearly white powder.

FUNCTIONAL USES Firming agent, gelling agent, stabilizer, thickener.

CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Insoluble in water and ethanol.

Solubility in alkali Passes testSuspend 0.2 g of the sample in 5 ml of water, add 1 ml of 3 N sodiumhydroxide, and shake. The sample dissolves.

Gel formation Heat a 2% aqueous suspension of the sample in a boiling water bath for 10 minand cool. A firm gel forms.

Precipitate formation withcupric tartrate

Passes testSee description under TESTS

PURITY

Gel strength Not less than 600 g/cm² (2% aqueous suspension)See description under TESTS

pH (FNP 5) 6.0 - 7.5 (1% aqueous suspension)

Loss on drying (FNP 5) Not more than 10% (60º for 5 h, in vacuum)

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CURDLAN page 2 (3)

Sulfated ash (FNP 5) Not more than 6%Test 1 g of the sample (Method I)

Nitrogen (FNP 5) Not more than 0.3%Test 1 g of the sample (Method II)

Lead (FNP 5) Not more than 0.5 mg/kgDetermine using an atomic absorption technique appropriate to the specifiedlevel. The selection of sample size and method of sample preparation may bebased on the principles of the method described in FNP 5, “Instrumental

Total plate count: Not more than 1,000 cfu/gMicrobiological criteria(FNP 5) E. coli: Negative in 1 g

TESTS


Precipitate formationwith cupric tartrate

Add 5 ml of sulfuric acid TS to 10 ml of a 2% aqueous suspension of thesample, heat in a boiling water bath for 30 min and cool. Neutralize the mixturewith barium carbonate. Centrifuge the mixture at 900xg for 10 min. Add 1 mlof the supernatant to 5 ml of hot alkaline cupric tartrate TS. A copious redprecipitate of cuprous oxide is formed.

Gel strength Place 200 mg of the sample into the tube of a Potter homogenizer, add 10 ml ofwater and homogenize at about 3,500 rpm for 5 min. Transfer the suspensioninto a 16 mm × 150 mm test tube, deaerate in vacuum for 3 min and heat in aboiling water bath for 10 min to form a gel. Cool the tube under running water,let stand for 30 min, then remove the gel from the tube. Cut the gel accuratelyat distances of 20 mm and 30 mm from the bottom to obtain a piece 10 mmlong. Determine gel strength with a Rheo Meter Model CR-200D (SunScientific Co., Ltd., Japan; Load cell: 1,000 g) or an equivalent instrument,under the following conditions:

Measurement mode: 4Velocity of moving plate: 250 mm/minPlunger: cylindrical type, 0.5 cm diameter

Read the breaking point of the gel (B). Calculate the gel strength using thefollowing formula:

Gel strength (g/cm²) = 1,000B/πr²

wherer = the radius of the plunger (cm)

METHOD OF ASSAY Transfer about 100 mg of the sample, accurately weighed, into a 100-mlvolumetric flask and dissolve in about 90 ml of 0.1 N sodium hydroxide. Add0.1 N sodium hydroxide to volume and mix well. Transfer 5 ml of the solutioninto a 100-ml volumetric flask, add water to volume and mix well.Quantitatively transfer 1 ml of the solution to a small flask or test tube, add 1ml of a 5% (w/v) solution of reagent grade phenol in water and 5 ml of sulfuricacid TS. Shake vigorously and cool in ice-cold water. Prepare a blank and areference standard solution in the same manner, using 0.1 ml of water and 100mg of reagent grade glucose, respectively. Determine the absorbances of thesample solution and the reference standard solution in 1-cm cells at 490 nmwith a suitable spectrophotometer, using the blank solution as the blank.Calculate the content (%) of curdlan in the sample using the following formula:

Curdlan content (%) = (A/AR) × (0.9 × WR/W) × 100

whereA = the absorbance of the sample solution

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CURDLAN page 3 (3)

AR = the absorbance of the reference standard solution0.9 = the molecular weight of anhydrous glucose divided by the

molecular weight of glucoseW = the weight of the sample (mg)WR = the weight of the glucose standard used as reference (mg)

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alpha-CYCLODEXTRIN page 1 (4)

alpha-CYCLODEXTRIN

New specifications prepared at the 57th JECFA (2001) and published in FNP52 Add 9 (2001). An ADI “not specified” was established at the 57th JECFA(2001).

SYNONYMS α-Schardinger dextrin, α-dextrin, cyclohexaamylose, cyclomaltohexaose, α-cycloamylase

DEFINITION A non-reducing cyclic saccharide consisting of six α-1,4-linked D-glucopyranosylunits produced by the action of cyclodextrin glucosyltransferase (CGTase, EC2.4.1.19) on hydrolyzed starch. Recovery and purification of α-cyclodextrin maybe carried out using one of the following procedures: precipitation of a complexof α-cyclodextrin with 1-decanol, dissolution in water at elevated temperature andreprecipitation, steam-stripping of the complexant, and crystallization of α-cyclodextrin from the solution; or chromatography with ion-exchange or gelfiltration followed by crystallization of α-cyclodextrin from the purified motherliquor; or membrane separation methods such as ultra-filtration and reverseosmosis.

Chemical names Cyclohexaamylose

C.A.S. number 10016-20-3

Chemical formula (C6H10O5)6

Structural formula


Assay Not less than 98% (dry basis)

DESCRIPTION Virtually odourless, white or almost white crystalline solid

FUNCTIONAL USES Carrier; encapsulating agent for food additives, flavorings, and vitamins;stabilizer; absorbent

CHARACTERISTICS

IDENTIFICATION

Melting range (FNP 5) Decomposes above 278 o

Solubility (FNP 5) Freely soluble in water; very slightly soluble in ethanol

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Specific rotation (FNP 5) [α]25D: Between +145 o and +151o (1% solution)

Chromatography The retention time for the major peak in a liquid chromatogram of the samplecorresponds to that for α-cyclodextrin in a chromatogram of reference α-cyclodextrin (available from Consortium für Elektrochemische Industrie GmbH,München, Germany or Wacker Biochem Group, Adrian, MI, USA) using theconditions described in the METHOD OF ASSAY.

PURITY

Water (FNP 5) Not more than 11% (Karl Fischer Method)

Residual complexant(1-decanol)

Not more than 20 mg/kgSee description under TESTS

Reducing substances Not more than 0.5% (as dextrose)See description under TESTS

Sulfated ash (FNP 5) Not more than 0.1%

Lead (FNP 5) Not more than 1 mg/kgDetermine using an atomic absorption technique appropriate to the specified level.The selection of sample size and method of sample preparation may be based onthe principles of the method described in FNP 5, “Instrumental Methods.”

TESTS

PURITY TESTS

Residual complexant(1-decanol)

Principle: After enzymatic digestion of the sample followed by solid-phaseextraction, 1-decanol is determined by gas chromatography.

Buffer solution: Dissolve 606 mg Tris-buffer (Sigma-Aldrich, St. Louis,MO,USA) and 430 mg calcium sulfate (dihydrate) in 500 ml of water. AdjustpH with concentrated phosphoric acid to pH 6.5.

Internal standard (IS) solution: Add 50 mg 1-octanol (chromatography grade)to 250 ml tetrahydrofuran (THF).

Reference solution (25 mg/kg 1-decanol): Dissolve 75.0 mg 1-decanol(chromatography grade) in 100 ml IS solution. Transfer 200 :l of this stocksolution into a 20-ml volumetric flask and fill with IS solution to the mark.

Sample solution: Dissolve 750 mg of sample and 50 mg of glucoamylase, EC3.2.1.3, (e.g.,Gluczyme 8000, available from Wacker Chemie, Munich,Germany) in 7 ml of a 10 mM Tris-buffer (pH 6.5). Add 100 :l IS solution and50 :l cyclodextrin glucosyltransferase preparation (500 U/ml) (Wacker Chemie,Munich, Germany). Close tightly, mix and incubate in a shaking water bath at40° for 4 hours.Condition an extraction column (Isolute C18 (10 ml) – ICT, Bad Homburg,Germany - or similar) by washing with methanol (2x10 ml) and water (4x10ml). Pass the incubated solution slowly through the column and wash withwater (2x10 ml). Gently pass nitrogen gas through the column to dry it (10min). Apply 2.5 ml of THF to the column and let stand for 5 minutes. Then,elute the sample solution slowly.

Gas chromatography:Column - Hewlett Packard HP-1 (25 m x 0.32 mm), 0.5:m FDCarrier gas - helium (flow rate: 1 ml/min)Detector - flame ionization

- 31 -


Temperatures - injection port: 265°; column: initial 60° (1 min isotherm);heating rate 20°/min; final 300° (7 min isotherm)Injection volume: 1 µlMeasure the areas of the 1-decanol and 1-octanol peaks in the reference solutionand sample solution.

Calculation: The concentration of 1-decanol (mg/kg) in the sample is:

Cdec = (Cdec)R x (Adec/Aoct)S / (Adec/Aoct)R

where (Cdec)R is the concentration of 1-decanol (mg/kg) of the referencesolution; and (Adec/Aoct)S and (Adec/Aoct)R are the peak area ratios for 1-decanolto 1-octanol in the sample solution and reference solution, respectively.

Reducing substances Note: Reducing substances are determined as dextrose. Dextrose levels areusually lower when determined by the following procedure in the presence of α-cyclodextrin compared to levels determined in its absence. Therefore, α-cyclodextrin reference standard is included in the procedure for the constructionof the calibration curve.

Reagent solution: Weigh 10.0 g 3,5-dinitrosalicylic acid in a 1000-mlvolumetric flask. Add 80 ml water and dissolve the 3,5-dinitrosalicylic acid byheating in a water bath. Prepare a solution of 16.0 g sodium hydroxide in 200ml water and a solution of 300 g sodium potassium tartrate in 500 ml water.Transfer both solutions to the 1000-ml flask. Fill with water to the mark, shakethe flask and let it stand for 24 hours. Filter (paper) the reagent solution prior touse if a precipitate appears.

Reference solution: Weigh accurately 1.0 g dextrose (anhydrous) in a 100-mlvolumetric flask and fill with water to the mark.

Test solution: Weigh accurately 10.0 g of test sample into a 100-ml volumetricflask, add 80-90 ml water and dissolve the test sample (ultra-sonification bath,15 minutes, 30o). Fill with water to the mark.

Calibration solutions: Weigh 1.0 g of reference α-cyclodextrin (available fromConsortium für Elektrochemische Industrie GmbH, München, Germany orWacker Biochem Group, Adrian, MI, USA) into each of eleven 10-mlvolumetric flasks (numbered 0 to 10). Add 0, 0.1, 0.2, ..., 1.0 ml of referencesolution to flasks nos. 0, 1, ... to 10, respectively. Fill all flasks with water to themark.

Calibration curve: Assemble a set of eleven 10-ml volumetric flasks. Transfer 1ml of each of the eleven calibration solutions into the flasks and add 1 ml ofreagent solution to each flask. Heat each flask in the boiling water bath for 10minutes. Cool rapidly to room temperature and fill with water to the mark. Foreach solution, measure the absorbance against water at 545 nm. Plot the data asabsorbance vs dextrose concentration (mg/ml).

Analysis: Prepare a set of six 10-ml volumetric flasks (labeled a through f) andadd 1 ml of the reagent solution to each. Transfer 1 ml of the test solution toflasks a, b, and c. Transfer 1 ml of the calibration solutions numbered 0, 3, and6 to flasks d, e, and f. Thoroughly mix the contents of each flask and place in aboiling water bath for 10 minutes. Then, cool the flasks to room temperature,fill to the mark with water, and measure absorbance of the solutions againstwater at 545 nm.

Evaluation and calculation: The result is only valid if the absorbances of thesolutions in flasks d-f do not deviate more than 5% from the calibration curve.Determine the reducing substance concentrations (mg/ml) of the solutions in

- 32 -


flasks a-c and calculate their mean, CRS.

Then,WRS = 10 CRS

and

% reducing substances = 100 x WRS/0.01WTS

where WRS is the mean weight (mg) of reducing substance (as dextrose),determined from the absorbance readings, and WTS is the weight (mg) of the testsample used to prepare the test solution.

METHOD OF ASSAY Determine by liquid chromatography (FNP 5) using the following conditions:

Sample solution: Weigh accurately about 100 mg of test sample into a 10-mlvolumetric flask and add 8 ml of deionized water. Dissolve the samplecompletely using an ultra-sonification bath (10-15 min) and dilute to the markwith purified deionized water. Filter through a 0.45-micrometer filter.

Reference solution: Weigh accurately about 100 mg of reference α-cyclodextrin into a 10-ml volumetric flask and add 8 ml of deionized water.Dissolve the sample completely using an ultra-sonification bath (10-15 min) anddilute to the mark with purified deionized water.

Chromatography: Liquid chromatograph equipped with a refractive indexdetector and an integrating recorder.Column and packing: Nucleosil-100-NH2 (10 µm) (Machery & Nagel Co.,Düren, Germany) or similar

- length: 250 mm- diameter: 4 mm- temperature: 40°

Mobile phase: acetonitrile/water (67/33, v/v)Flow rate: 2.0 ml/minInjection volume: 10 µl

Procedure: Inject the sample solution into the chromatograph, record thechromatogram, and measure the area of the α-cyclodextrin peak. Repeat for thereference solution. Calculate the percentage of α-cyclodextrin in the testsample as follows:

% α-cyclodextrin (dry basis) = 100 x (AS/AR)(WR/WS)

where:AS and AR are the areas of the peaks due to α-cyclodextrin for the samplesolution and reference solution, respectively.WS and WR are the weights (mg) of the test sample and reference α-cyclodextrin, respectively, after correcting for water content.

- 33 -

DIACETYLTARTARIC AND FATTY ACID ESTERS OF GLYCEROL page 1 (4)

DIACETYLTARTARIC AND FATTY ACID ESTERS OF GLYCEROL

Prepared at the 57th JECFA (2001) and published in FNP 52 Add 9 (2001)superseding specifications prepared at the 51st JECFA and published in FNP52 Add 6 (1998). The ADI of 0-50 mg/kg bw established at the 17th JECFA in1973 was changed to a temporary ADI until 2003 at the 57th JECFA (2001).

These specifications cover the two products Diacetyltartaric and fatty acidesters of glycerol (INS 472e) and Tartaric, acetic and fatty acid esters ofglycerol, mixed (INS 472f), which before 1998 had separate specifications,published in FNP 52 Add 5 (1997). The two specifications were combined atthe 51st JECFA into one single set of specification, published in FNP 52 Add 6(1998) under the name Diacetyltartaric and fatty acid esters of glycerol. Asspecifications no longer exist for Tartaric, acetic and fatty acid esters ofglycerol, mixed, the ADI "not limited" was withdrawn at the 57th JECFA(2001).

SYNONYMS Diacetyltartaric acid esters of mono- and diglycerides, DATEM; INS No. 472e;Tartaric, acetic and fatty acid esters of glycerol, mixed; Mixed acetic andtartaric acid esters of mono and diglycerides of fatty acids; INS No. 472f

DEFINITION The product consists of mixed glycerol esters of mono- and diacetyltartaric acidand fatty acids of food fats. It is made by the interaction of diacetyltartaricanhydride and mono- and diglycerides of fatty acids in the presence of aceticacid, or by interaction of acetic anhydride and mono- and diglycerides of fattyacids in the presence of tartaric acid.

Due to inter-and intramolecular acyl group exchange, both methods of productionlead to the same essential components, the distribution of which depends on therelative proportions of the basic raw materials, on temperature and on reactiontime. The product may contain small amounts of free glycerol, free fatty acids,and free tartaric and acetic acids. The article of commerce may be furtherspecified as to acid value, total tartaric acid content, free acetic acid content,saponification value, iodine value, free fatty acid content, solidification point ofthe free fatty acids.

Structural formula The major components are:

CH2 OR1

CH OR2

CH2 OR3

in which1) one or two of the R groups is a fatty acid moiety2) the other R groups are either

- diacetylated tartaric acid moiety- monoacetylated tartaric acid moiety- tartaric acid moiety- acetic acid moiety- hydrogen

DESCRIPTION From liquid to paste to wax-like solids (flakes or powder)

FUNCTIONAL USES Emulsifier

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CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Dispersible in cold and hot water, soluble in methanol and ethanol.

Test for 1,2-diols To a solution of 500 mg in 10 ml methanol, add dropwise, lead acetate TS. Awhite flocculent, insoluble precipitate is formed.

Test for fatty acids (FNP 5) Passes test

Test for acetic acid (FNP 5) Passes test

Test for tartaric acid (FNP 5) Passes test

Test for glycerol (FNP 5) Passes test

PURITY

Acids (FNP 5) Acids other than acetic, tartaric and fatty acids, shall not be detectable

Sulfated ash (FNP 5) Not more than 0.5% determined at 800±25ºTest 5 g of sample (Method I for solids; Method II for liquids)

Free fatty acids (FNP 5) Not more than #% as oleic acid

Total acetic acid Not less than 8% and not more than 32% after hydrolysisSee description under TESTS

Total tartaric acid Not less than 10% and not more than 40% after saponificationSee description under TESTS

Total glycerol Not less than 11% and not more than 28 % after saponificationSee description under TESTS

Free glycerol (FNP 5) Not more than 2.0%

Lead Not more than 2 mg/kgDetermine using an atomic absorption technique appropriate to the specifiedlevel. The selection of sample size and method of sample preparation may bebased on the principles of the method described on FNP 5, "Instrumentalmethods".

TESTS

PURITY TESTS

Total acetic acid Apparatus: Assemble a modified Hortvet-Sellier distillation apparatus as shownin the figure, using a sufficiently large (approximately 38- x 203-mm) innerSellier tube and large distillation trap.

Procedure: Transfer 4 g of sample, accurately weighed into the inner tube ofthe assembly, and insert the tube in the outer flask containing about 300 ml ofrecently boiled hot water. To the sample add 10 ml of approximately 4Nperchloric acid [35 ml (60 g) of 70% perchloric acid in 100 ml of water], andconnect the inner tube to a water-cooled condenser through the distillation trap.Distil by heating the outer flask so that 100 ml of distillate is collected within 20to 25 min. Collect the distillate in 100-ml portions, add phenolphthalein TS toeach portion, and titrate with 0.5N sodium hydroxide. Continue the distillationuntil a 100-ml portion of the distillate requires no more than 0.5 ml of 0.5N

- 35 -


sodium hydroxide for neutralization. (Caution: Do not distil to dryness.)Calculate the weight, in mg, of volatile acids in the sample taken by the formulaV x e, in which V is the total volume, in ml, of 0.5N sodium hydroxide consumedin the series of titrations and e is the equivalence factor 30.03.

Total tartaric acid Standard Curve: Transfer 100 mg of reagent-grade tartaric acid, accuratelyweighed, into a 100-ml volumetric flask, dissolve it in about 90 ml of water,add water to volume, and mix well. Transfer 3.0-. 4.0-, 5.0-, and 6.0-mlportions into separate 19- x 150-mm matched cuvettes, and add sufficient waterto make 10.0 ml. To each cuvette add 4.0 ml of a freshly prepared 1 in 20solution of sodium metavanadate and 1.0 ml of acetic acid. (Note: Use thesesolutions within 10 min after colour development.) Prepare a blank in the samemanner, using 10 ml of water in place of the tartaric acid solutions. Set theinstrument at zero with the blank, and then determine the absorbance of thefour solutions of tartaric acid at 520 nm with a suitable spectrophotometer or aphotoelectric colorimeter equipped with a 520-nm filter. From the data thusobtained, prepare a curve by plotting the absorbances on the ordinate againstthe corresponding quantities, in mg, of the tartaric acid on the abscissa.

Test Preparation: Transfer about 4 g of the sample, accurately weighed, into a250-ml Erlenmeyer flask, and add 80 ml of approximately 0.5N potassiumhydroxide and 0.5 ml of phenolphthalein TS. Connect an air condenser at least65 cm in length to the flask, and heat the mixture on a hot plate for about 2.5 h.Add to the hot mixture approximately 10% phosphoric acid until it is definitelyacid to congo red test paper. Reconnect the air condenser, and heat until thefatty acids are liquified and clear. Cool and then transfer the mixture into a250-ml separator with the aid of small portions of water and chloroform.Extract the liberated fatty acids with three successive 25-ml portions of water,and add the washings to the separator containing the water layer. Transfer thecontents of the first separator to a 250-ml beaker, heat on a steam bath toremove traces of chloroform, filter through acid-washed, fine-texture filterpaper into a 500-ml volumetric flask, and finally dilute to volume with water(Solution I). Pipet 25.0 ml of this solution into a 100-ml volumetric flask, anddilute to volume with water (Solution II). Retain the rest of Solution I for thedetermination of total glycerol.

Procedure: Transfer 10.0 ml of Solution II prepared under Test Preparation intoa 19- x 150-mm cuvette, and continue as directed under Standard Curve,beginning with "To each cuvette add 4.0 ml of a...". From the standard curvedetermine the weight, in mg, of tartaric acid in the final dilution, multiply thisby 20, and divide the result by the weight of the original sample for obtainingthe percentage of tartaric acid.

Total glycerol Transfer 5.0 ml of Solution I prepared in the test for total Tartaric Acid into a250-ml glass-stoppered Erlenmeyer or iodine flask. Add to the flask 15 ml ofglacial acetic acid and 25.0 ml of periodic acid solution, prepared by dissolving2.7 g of periodic acid (H5IO6) in 50 ml of water, adding 950 ml of glacial aceticacid, and mixing thoroughly; protect this solution from light. Shake themixture for 1 or 2 min, allow it to stand for 15 min, add 15 ml of potassiumiodide solution (15 in 100) and 15 ml of water, swirl, let stand 1 min, and thentitrate the liberated iodine with 0.1N sodium thiosulfate, using starch TS as theindicator. Perform a Residual Blank Titration using water in place of thesample. The corrected volume is the number of ml of 0.1N sodium thiosulfaterequired for the glycerol and the tartaric acid in the sample represented by the 5ml of Solution I. From the percentage determined in the Assay for TartaricAcid calculate the volume of 0.1N sodium thiosulfate required for the tartaricacid in the titration. The difference between the corrected volume and thecalculated volume required for the tartaric acid is the number of ml of 0.1Nsodium thiosulfate consumed due to the glycerol in the sample. One ml of 0.1Nsodium thiosulfate is equivalent to 2.303 mg of glycerol and to 7.505 mg of

- 36 -


tartaric acid.

Modified Hortvet-Sellier Distillation Apparatus

- 37 -

GENERAL SPECIFICATIONS FOR ENZYMES page 1 (3)

GENERAL SPECIFICATIONS AND CONSIDERATIONS FOR ENZYMEPREPARATIONS USED IN FOOD PROCESSING

Specifications prepared at the 57th JECFA (2001) and published in FNP 52(Addendum 9), superseding specifications prepared at the 35th JECFA (1989) andpublished in FNP 49 (1990) and in FNP 52 (1992); the general specificationsprepared at the 25th JECFA (1981) and published in FNP 19 (1981) and FNP 31/2(1984); amendments at the 51st JECFA published in FNP 52 Add 6 (1998);amendments at the 53rd JECFA (1999) and partially published in FNP 52 Add 7(1999).

Enzyme Nomenclature Recommendations (1992) of the Nomenclature Committee of the InternationalUnion of Biochemistry, Academic Press (1992) with later supplements. Enzymepreparations used in food processing are usually named according to the substrate towhich the enzyme is applied, such as protease or amylase. Some traditional namesare also in use, such as malt, pepsin and rennet.

DEFINITION Enzyme preparations consist of biologically active proteins, at times combined withmetals, carbohydrates and/or lipids. They are obtained from animal, plant or microbialsources and may consist of whole cells, parts of cells, or cell-free extracts of the sourceused. They may contain one or more active components as well as carriers, solvents,preservatives, antioxidants and other substances consistent with good manufacturingpractice. They may be liquid, semi-liquid, dry or in an immobilized form (immobilizedenzyme preparations are preparations which have been made insoluble in their intendedfood matrix by physical and/or chemical means). Their colour may vary from virtuallycolourless to dark brown.

ACTIVE COMPONENTS The principal activities are characterized by their systematic names and EnzymeCommission Numbers.

The activities of enzyme preparations are measured according to the reactioncatalyzed by individual enzymes and are usually expressed in activity units perweight of preparation.

SOURCE MATERIALS Animal tissues used for the preparation of enzymes must comply withmeat-inspection requirements and be handled in accordance with good hygienicpractice.

Plant material used in the production of enzyme preparations must consist ofcomponents that leave no residues harmful to health in the processed finished foodunder normal conditions of use.

Microbial sources used in the production of enzyme preparations may be nativestrains or variants of microorganisms, or be derived from native strains or variantsby the processes of selective serial culture or genetic modification. Productionstrains for food enzyme preparations must be nonpathogenic and nontoxigenic. Theevaluation of enzyme preparations from fungal sources for toxigenicity shall includea determination that they do not contain toxicologically significant amounts ofmycotoxins that are known to be synthesised by strains of the production organism’sspecies or of species related to the production microorganism. Sourcemicroorganisms must be discrete and stable strains or variants that have beentaxonomically characterised to enable them to be assigned unique identities as thesources of the enzyme preparations that are the subject of individual specifications.The reference or production strain number may be included in individualspecifications. The production strains must be maintained under conditions thatensure the absence of strain drift and, when used in the production of enzymepreparations, must be subjected to methods and culture conditions that are appliedconsistently and reproducibly from batch to batch. Such conditions must ensure theabsence of toxin production by the source organism and prevent the introduction of

- 38 -


microorganisms that could be the source of toxic materials and other undesirablesubstances. Culture media used for the growth of microbial sources must consist ofcomponents that leave no residues harmful to health in the processed finished foodunder normal conditions of use.

Enzyme preparations are produced in accordance with good food manufacturingpractice. They cause no increase in the total microbial count in the treated food, overthe level considered to be acceptable for the respective food.

CARRIERS AND OTHERADDITIVES ANDINGREDIENTS

The carriers, diluents, excipients, supports and other additives and ingredients(including processing aids) used in the production, distribution and application ofenzyme preparations must be substances that are acceptable for the relevant food usesof the enzyme preparations concerned, or substances which are insoluble in food andremoved from the food material after processing.

In the case of immobilized enzyme preparations, leakage of carriers, immobilizationagents and active enzymes must be kept within acceptable limits as specified in theindividual specifications.

In order to distinguish the proportion of the enzyme preparation derived from thesource material from that contributed by diluents and other additives and ingredients,individual specifications may require a statement of percentage Total Organic Solids(T.O.S.) which is defined as follows:

% T.O.S. = 100 - (A + W + D)

whereA = % ash, W = % water and D = % diluents and/or other additives and ingredients.

PURITY

Lead (FNP 5) Not more than 5 mg/kgDetermine using atomic absorption technique appropriate to the specified level. Theselection of the sample size and the method of sample preparation may be based onthe principles described in FNP 5, "Instrumental Methods”.


Salmonella spp.: Absent in 25 g sampleTotal coliforms: Not more than 30 per gEscherichia coli: Absent in 25 g sample

Antibiotic activity(FNP 5)

Absent in preparations from microbial sources

OTHERCONSIDERATIONS

An overall safety assessment of each enzyme preparation intended for use in food orfood processing must be performed. This assessment should include an evaluationof the safety of the production organism, the enzyme component, side activities, themanufacturing process, and the consideration of dietary exposure. Guidelines forsafety assessments of food enzyme preparations derived from microbial strains havebeen developed (Pariza and Foster, 1983; Pariza and Johnson, 2001; IFBC, 1990;Scientific Committee for Foods, 27th series). Further, several internationallyrecognized scientists and expert groups have prepared guidelines for the safetyassessment of food and food ingredients developed through biotechnology (OECD,1993: Health Canada, 1994; FAO/WHO, 1996; and Jonas et al., 1996) which areapplicable to enzyme preparations derived from recombinant sources. The followingpoints need emphasis when considering the production of enzyme preparations fromgenetically modified microorganisms:

1. The genetic material introduced into and remaining in the productionmicroorganism should be characterized and evaluated for function and safety. Itshould be demonstrated that no unexpected genetic material was introduced into thehost microorganism, e.g., by providing the sequences of the final introduced geneticmaterial and/or molecular analysis of the introduced sequences in the final

- 39 -


production strain. This would include demonstration that the genetic material doesnot contain genes coding for virulence factors, protein toxins, or enzymes that maybe involved in the synthesis of mycotoxins or any other toxic or undesirablesubstances.

2. If the production microorganism is capable of producing proteins that inactivateclinically useful antibiotics, documentation should be provided that the finishedenzyme preparation contains neither antibiotic-inactivating proteins atconcentrations that would interfere with antibiotic treatment nor DNA that is capableof transforming microorganisms, which potentially could lead to the spread ofantibiotic resistance.

3. The need to evaluate the allergenic potential of the potential gene productsencoded by the DNA inserted in the production microorganism should be considered(see FAO/WHO, 2000 and 2001).

References FAO/WHO. Biotechnology and Food Safety, Report of a Joint FAO/WHOConsultation. FAO Food and Nutrition Paper 61. Rome, Italy, 1996.

FAO/WHO. Safety aspects of genetically modified foods of plant origin, Report of aJoint FAO/WHO Expert Consultation on Foods Derived from Biotechnology.Geneva, Switzerland, 2000 (also available at www.who.int/fsf).

FAO/WHO. Evaluation of Allergenicity of Genetically Modified Foods, Report of aJoint FAO/WHO Expert Consultation on Allergenicity of Foods Derived fromBiotechnology. Rome, Italy, 2001 (also available at www.fao.org).

Health Canada, Guidelines for the Safety Assessment of Novel Foods, FoodDirectorate Publication, Health Protection Branch, Health Canada, Ottawa, 1994.

IFBC (International Food Biotechnology Council). Chapter 4: Safety Evaluation ofFoods and Food Ingredients Derived from Microorganisms. In Biotechnologies andFood: Assuring the Safety of Foods Produced by Genetic Modification. RegulatoryToxicology and Pharmacology 12:S1-S196, 1990.

Jonas, D.A., Antignac, E., Antoine, J.M., Classen, H.G., Huggett, A., Knudsen, I.,Mahler, J., Ockhuizen, T., Smith, M., Teuber, M., Walker, R., and de Vogel, P. TheSafety Assessment of Novel Foods, Guidelines prepared by ILSI Europe Novel FoodTask Force. Food Chemical Toxicology 34:931-940, 1996.

Organisation for Economic Cooperation and Development, Safety Evaluation ofFoods Derived by Modern Biotechnology, Paris, 1993.

Pariza, M.W. and Foster, E.M. Determining the Safety of Enzymes Used in FoodProcessing. Journal of Food Protection, 46:5:453-468, 1983.

Pariza, M. W. and Johnson, E. A., Evaluating the Safety of Microbial EnzymePreparations Used in Food Processing: Update for a New Century, RegulatoryToxicology and Pharmacology, 33:173-186, 2001.

Scientific Committee for Food, Report (27th series), Ref. No EUR14181 EN-Guidelines for the presentation of data on food enzymes. P13-22, 1992.

- 41 -

HYDROGENATED POLY-1-DECENE page 1 (3)

HYDROGENATED POLY-1-DECENE

Prepared at the 57th JECFA (2001) and published in FNP 52 Add 9 (2001),superseding specifications prepared at the 53rd JECFA (1999), published in FNP 52Add 7 (1999). An ADI of 0 - 6 mg/kg bw was established at the 57th JECFA (2001).

SYNONYMS Hydrogenated polydec-1-ene, Hydrogenated poly-α-olefin; INS No. 907

DEFINITION Hydrogenated poly-1-decene is a mixture of branched isomeric hydrocarbons, preparedby hydrogenation of mixtures of trimers, tetramers, pentamers and hexamers of 1-decenes. Minor amounts of molecules with carbon number less than 30 may be present.

C.A.S. number 68037-01-4

Chemical formula C10nH20n+2, where n = 3 – 6

Formula weight 560 (average)

Assay Not less than 98.5% of hydrogenated poly-1-decene, having the following oligomerdistribution:

C30: 13 - 37%C40: 35 - 70%C50: 9 - 25%C60: 1 - 7%

DESCRIPTION Colourless, odourless, viscous liquid

FUNCTIONAL USES Glazing agent, release agent

CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Insoluble in water; slightly soluble in ethanol; soluble in toluene

Burning The product burns with bright flame and a paraffin-like characteristic smell

Viscosity 5.7 – 6.1 mm2/sec (100°)See description under TESTS

PURITY

Compounds with carbonnumber less than 30

Not more than 1.5 %See METHOD OF ASSAY

Readily carbonisable substances Passes testSee description under TESTS

Nickel (FNP 5) Not more than 1 mg/kg

Lead (FNP 5) Not more than 1 mg/kgDetermine using an atomic absorption technique appropriate to the specified level. Theselection of sample size and method of sample preparation may be based on theprinciples of the method described on FNP 5, "Instrumental methods".

- 42 -


TESTS

PURITY TESTS

Viscosity, 100o

ASTM D 445

Adapted, with permission,from the Annual Book ofASTM Standards, copyrightAmerican Society for Testingand Materials, 100 HarborDrive, West Conshohocken,PA 19428.

Copies of the complete ASTMstandard may be purchaseddirect from ASTM, phone:610-832-9585, fax: 610-832-9555, e-mail:[email protected], website:http://www.astm.org

Use a viscometer of the glass capillary type, calibrated and capable of measuringkinematic viscosity with a repeatability exceeding 0.35% only in one case in twenty.Immerse the viscometer in a liquid bath at the temperature required for the test ± 0.1°ensuring that at no time of the measurement will any portion of the sample in theviscometer be less than 20 mm below the surface of the bath liquid or less than 20mm above the bottom of the bath. Charge the viscometer with sample in the mannerdictated by the design of the instrument. Allow the sample to remain in the bath forabout 30 min. Where the design of the viscometer requires it, adjust the volume ofsample to the mark. Use pressure to adjust the head level of the sample to a positionin the capillary arm of the instrument about 5 mm ahead of the first mark. With thesample flowing freely, measure, in seconds (±0.2 sec), the time required for themeniscus to pass from the first to the second timing mark. If the time is less than 200s, select a viscometer with a capillary of smaller diameter and repeat the operation.Make a second measurement of the flow time. If two measurements agree within0.2%, use the average for calculating the kinematic viscosity. If the measurements donot agree, repeat the determination after thoroughly cleaning and drying theviscometer.

Viscosity, 100o (mm2/sec) = C x t

whereC = calibration constant of the viscometer (mm2/sec2)t = flow time (sec)

Readily carbonizablesubstances

Place 5g of the sample in a glass-stoppered test tube that has previously been cleanedwith a chromic acid cleaning solution, rinsed with water and dried in an oven (105°,1h). Add 5 ml of sulfuric acid TS, and place in a boiling water bath. After the testtube has been in the bath for 30 sec, remove quickly, and while holding the stopper inplace, give three vigorous vertical shakes over an amplitude of about 10 cm. Repeatevery 30 sec. Do not keep the test tube out of the bath longer than 3 sec for eachshaking period. At the end of 10 min from the time when first placed in the waterbath, remove the test tube. The sample remains unchanged in colour, and the aciddoes not become darker than a very slight straw colour (Matching Fluid E , see FNP5). No black material occurs at the interface between the two layers

METHOD OF ASSAY Hydrogenated poly-1-decene, oligomer distribution and the content of hydrogenateddecene dimer. Determine by gas-liquid chromatography using the following conditions:

Column: Capillary column, 16 m x 0.53 mmColumn film: Nonpolar (polydimethyldisiloxane), thickness 0.1 µm, e.g. OV-1, DB 1Column temperature:- initial: 35°, 1 min- 35° - 50°, 5°/min- 50° - 170°, 12°/ min- 170° - 310°, 10°/min

final: 310°, 45 minCarrier- gas: Helium- flow: 10 ml/minInjector pressure: 1.5 psi at 35°, constant flowDetector: FIDInjection temperature: 35°Sample size: 2 µl

Calibration: Calibrate the instrument using a solution with known compositioncontaining about 1.0 % of n-tetradecane, 1.0% of n-hexadecane and 1.0% of squalane

- 43 -


(2,6,10,15,19,23-hexamethyl tetracosane) in pentane. The differences between peakareas of the compounds should be less than 10.0% and the resolution betweentetradecane and n-hexadecane should be between 2 and 5. Calculate the resolution (R)from the distance between n-tetradecane and n-hexadecane peaks at the peak maxima (d)and the width of the peaks at the baseline (Y): R = [2(d1 - d2)/(Y1 - Y2)].

Sample preparation: Take a small amount of the sample into an automatic pipette. Placea drop of the sample in 1.00 ml of pentane, and mix well. Record the chromatogram forabout 45 min.

Retention times: The retention times for C20, C30, C40, C50 and C60 are usually about 10.5,16, 20, 23 and 26 min.

Calculation: Calculate the oligomer distribution by the method of area percentages (areanormalization).Calculate the percentage of molecules with carbon numbers less than 30 in the sampletaken by the formula:

100*L/T

WhereL = the sum of peak areas eluting before and C30

T = the sum of all peak areas eluting in 45 min

Calculate the percentage of hydrogenated poly-1-decene in the sample taken by theformula:

100*A/T

whereA = the sum of peak areas for C30, C40, C50 and C60

T = the sum of all peak areas eluting in 45 min

- 45 -

INVERTASE FROM SACCHAROMYCES CEREVISIAE page 1 (3)

INVERTASE FROM SACCHAROMYCES CEREVISIAE

New specifications prepared at the 57th JECFA (2001) and published in FNP52 Add 9 (2001); previously prepared at the 15th JECFA (1971) as part of thespecifications for“Carbohydrase from Saccharomyces species”, published inFNP 52. The use of this enzyme was considered to be acceptable by the 57th

JECFA (2001) if limited by Good Manufacturing Practice.

SYNONYMS INS No. 1103

SOURCES Produced by the controlled submerged aerobic fermentation of a non-pathogenicand non-toxigenic strain of Saccharomyces cerevisiae and extracted from theyeast cells after washing and autolysis.

ACTIVE PRINCIPLES β-Fructofuranosidase (synonym: invertase, carbohydrase, saccharase)

SYSTEMATIC NAMESAND NUMBERS

β-Fructofuranosidase (EC 3.2.1.26; C.A.S. No. 9001-57-4)

REACTIONS CATALYSED Hydrolyses sucrose to yield glucose and fructose

DESCRIPTION Typically white to tan amorphous powders or liquids that may be dispersed infood grade diluents and may contain stabilisers; soluble in water and practicallyinsoluble in ethanol and ether.

FUNCTIONAL USES Enzyme preparationUsed in confectionery and pastry applications

GENERALSPECIFICATIONS

Must conform to the General Specifications and Considerations for EnzymePreparations Used in Food Processing (FNP 52, current edition, includingamendments)

CHARACTERISTICS

IDENTIFICATION The sample shows invertase activitySee description under TESTS

TESTS

Invertase activity Principle: Invertase hydrolyses the non-reducing β-D-fructofuranoside residuesof sucrose to yield invert sugar. The invert sugar released is then reacted with3.5 dinitrosalicylic acid (DNS). The colour change produced is proportional tothe amount of invert sugar released, which in turn is proportional to theinvertase activity present in the sample. The absorbance is measured at 540 nmand converted into micromoles of reducing sugar produced using a calibrationcurve. One invertase unit is the amount of enzyme which will produce 1micromole of reducing sugar (expressed as invert sugar) per minute under theconditions specified in this procedure.

Apparatus:Spectrophotometer set at 540 nmWater bath set at 30°±1.0°StopwatchBoiling water bathIce water bathMixer

Reagents and solutions:− 0.05 M Sodium acetate buffer, pH 4.7: Adjust the pH of 200 ml of 0.05 M

sodium acetate (4.1 g of sodium acetate anhydrous in 1000 ml of water) to

- 46 -


pH 4.7 ±0.05 with 0.05M acetic acid (2.85 ml of glacial acid in 1000 ml ofwater).

− 0.3M sucrose (5.13 g sucrose in 50.0 ml of water)− 20 mM Tris HCl buffer, pH 7.0: Dissolve 2.42 g of tris (hydroxymethyl)

aminomethane in about 800 ml of water. Adjust pH to 7.0 using 5%hydrochloric acid (5 ml of conc. hydrochloric acid in 100.0 ml of water).

− DNS solution: Weigh 300 g of potassium sodium tartrate tetrahydrate into aone litre conical flask. Add 16 g of sodium hydroxide and 500 ml of waterand dissolve by heating gently. When the solution is clear, add slowly 10g of 3,5-dinitrosalicylic acid (DNS). Keep covered to protect from lightuntil the DNS is totally dissolved. Cool to room temperature and make upto 1 litre with water. Store in a tightly stoppered dark container. Protectfrom light and carbon dioxide.

− Invert sugar standard (0.01M): Dry glucose to constant weight at 105° anddry fructose to constant weight at 70° under vacuum. Dissolve 0.9 g ofglucose and 0.9 g of fructose in 1000 ml of 0.1% benzoic acid (1 g ofbenzoic acid in 1000 ml of water).

Calibration curve: Prepare a series of test tubes, in duplicate, according to thetable below. The calibration curve must include at least 4 suitable standards.

Tube no. 1 2 3 4 5 6 blankInvert sugarstandard (ml)

0.1 0.3 0.5 0.8 1.0 1.2 0.0

Water (ml) 2.4 2.2 2.0 1.7 1.5 1.3 2.5Acetate buffer (ml) 0.5 0.5 0.5 0.5 0.5 0.5 0.5Content of invertsugar (micromoles)

1.0 3.0 5.0 8.0 10 12 0.0

Reaction and measurement: Mix and incubate for exactly 10 min at 30±0.1°.Add 2.0 ml of DNS solution to each tube, cover tubes and place all tubes in aboiling water bath for exactly 10 min. Cool rapidly in an ice water bath and add15 ml of water to each tube. Mix thoroughly. Measure the absorbance at 540 nmof each sample using the blank to zero the spectrophotometer. Plot theabsorbance against content of invert sugar.

Sample preparation: Accurately weigh about 1 g of the sample and dissolve in10 ml of 20 mM Tris HCl buffer. For powder samples it may be necessary touse a magnetic stirrer for up to 10 min. Dilute the sample with 20 mM Tris HClbuffer to obtain a solution for which the measured absorbance will fall withinthe linear range of 0.14 and 0.30.

Procedure: Into each of a series of 30 ml test tubes, pipette, in quadruplicate, 1.4ml of water, 0.5 ml of acetate buffer and 0.1 ml of diluted enzyme. Equilibratethe tubes in a 30° water bath. Add 1 ml of 0.3 M sucrose solution to 3 of the 4tubes. Use the fourth tube as an enzyme blank, adding 2 ml of DNS solutionbefore adding 1.0 ml of 0.3M sucrose solution. Prepare a reagent blank using0.1ml of water in place of diluted enzyme. Continue as described under'Reaction and measurement'. Read the respective contents of invert sugar fromthe calibration curve.

Calculation: Activity for powders (units/minute/g) =

(CS – CB) x 10 x dilutionW x 10

WhereCS = Content of invert sugar in sample solution (micromoles)CB = Content of invert sugar in enzyme blank solution (micromoles)W = Weight of sample (g)

- 47 -


Activity for liquids (units/minute/ml) =

(CS – CB) x 10 x dilution x S.G.W x 10

WhereCS = Content of invert sugar in sample solution (micromoles)CB = Content of invert sugar in enzyme blank solution (micromoles)W = Weight of sample (g)S.G. = Specific gravity of sample (g/ml)

- 49 -

dl-MALIC ACID page 1 (3)

DL-MALIC ACID

Prepared at the 57th JECFA (1999) and published in FNP 52 Add 9 (2001),superseding specifications prepared at the 53th JECFA (1999), published in FNP 52Add 7 (1999). ADI “not specified”, established at the 13th JECFA in 1969.

SYNONYMS 2-Hydroxybutanedioic acid; INS No. 296

DEFINITION

Chemical names DL-Malic acid, 2-Hydroxybutanedioic acid, Hydroxysuccinic acid

C.A.S. number 617-48-1

Chemical formula C4H6O5

Structural formula COOH

CHOH

CH2

COOH


Assay Not less than 99.0%

DESCRIPTION White or nearly white crystalline powder or granules

FUNCTIONAL USES Acidity regulator, flavouring agent

CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Very soluble in water; freely soluble in ethanol

Melting range (FNP 5) 127 - 132°

Test for malate (FNP 5) Passes testTest 5 ml of a 1 in 20 solution of the sample, neutralized with ammonia TS

PURITY

Sulfated ash (FNP 5) Not more than 0.1%Test 2 g of the sample (Method I)

Fumaric and maleic acid Not more than 1.0% of fumaric acid and not more than 0.05% of maleic acidSee description under TESTS

Lead (FNP 5) Not more than 2 mg/kgPrepare a sample solution as directed for organic compounds in the Limit Test anddetermine the lead content by atomic absorption spectroscopy (FNP 5).

TESTS

- 50 -


PURITY TESTS

Fumaric and maleic acid Buffer solution A: In a 1000-ml volumetric flask dissolve 74.5 g of potassiumchloride in 500 ml of water, add 100 ml of concentrated hydrochloric acid, and diluteto volume with water.Buffer solution B: Dissolve 171.0 g of dipotassium hydrogen phosphate, K2HPO4

. ·H2O, in 1000 ml of water, and add potassium dihydrogen phosphate, KH2PO4, untilthe pH is exactly 7.0.

Maxima suppressor: Dissolve, with the aid of a magnetic stirrer, 1 g of gelatin in 65ml of hot, boiled water. After cooling, add 35 ml of ethanol as a preservative.

Standard solution: Weigh out accurately about 20 g of the sample, 200 mg of fumaricacid and 10 mg of maleic acid, both of the highest purity available, and transfer into a500-ml volumetric flask. Add 300 ml of sodium hydroxide TS, a few drops ofphenolphthalein TS and continue adding sodium hydroxide TS to a faint pink colourthat persists for at least 30 sec. Dilute to volume with water, and mix.

Sample solution: Transfer about 4 g of the sample, accurately weighed, to a 100-mlvolumetric flask and dissolve in 25 ml of water. Add phenolphthalein TS, andneutralize with sodium hydroxide TS as directed for standard solution. Dilute tovolume with water, and mix.

Procedure: Transfer two 25-ml portions of the "Sample solution" into separate 100-ml volumetric flasks. Dilute one flask (Sample A) to volume with "Buffer solutionA". To the other flask (Sample B) add 50 ml of "Buffer solution B" and dilute tovolume with water. Rinse a polarograph cell with a portion of "Sample A", add asuitable volume of the solution to the cell, immerse it in a water bath regulated at24.5-25.5º, add 2 drops of the "Maxima suppressor", and then de-aereate by bubblingnitrogen through the solution for at least 5 min. Insert the dropping mercury electrode(negative polarity) of a suitable polarograph, adjust the current sensitivity asnecessary, and record the polarogram from -0.1 to -0.8 volt at the rate of 0.2 volt permin, using a saturated calomel electrode as the reference electrode. Transfer 25 ml ofthe "Standard solution" into a 100-ml volumetric flask, and dilute to volume with"Buffer solution A". Obtain the polarogram of this solution (Standard A) in the samemanner as directed for "Sample A". In each polarogram, determine the height of themaleic acid plus fumaric acid wave occurring at the half-wave potential near -0.56volt, recording that for sample as iU and that for the standard as iS. In the samemanner, obtain polarograms from "Sample B" and a "Standard B", except record thepolarogram from -1.05 to -1.7 volts at the rate of 0.1 volt per minute. In eachpolarogram, determine the height of the maleic acid wave occurring at the half-wavepotential near -1.33 volts, recording that for the sample as iU'’ and that for thestandard as iS’.

Calculation: Calculate the weight in mg, p, of combined maleic acid and fumaric acidin the sample taken by the formula:

500C x [iU/(iS - iU)]

whereC = the concentration, in mg per ml, of combined maleic acid and fumaric acid in theStandard solution.

Similarly, calculate the weight in mg, q, of maleic acid in the sample taken by theformula:

500C’ x [ iU’/(iS’ - iU’)]

whereC’= the concentration, in mg per ml of maleic acid in the Standard solution.

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Calculate the weight of fumaric acid in mg, r, in the sample taken from the differencein these values, i.e. (r = p - q).

Finally, calculate the percentage of fumaric and maleic acids present by multiplying rand q, respectively, by 0.025.

METHOD OF ASSAY Dissolve about 2 g of the sample, accurately weighed, in 40 ml of recently boiled andcooled water, add 2 drops of phenolphthalein TS and titrate with 1 N sodium hydroxideto the first appearance of a faint pink colour which persists for at least 30 sec. Each mlof 1 N sodium hydroxide is equivalent to 67.04 mg of C4H6O5.

- 53 -

MODIFIED STARCHES page 1 (16)

MODIFIED STARCHES

Prepared at the 57th JECFA (2001) and published in FNP 52 Add 9 (2001)superseding specifications prepared at the 35th JECFA (1989), published in FNP 49(1990) and in FNP 52 Add 5 (1997). An ADI “not specified” was established at the26th JECFA (1982) for all modified starches listed below except for acetylatedoxidized starch for which an ADI "not specified" was established at the 57th JECFA(2001).

Modified starches comprise the following:

Dextrin roasted starch: INS No. 1400Acid treated starch: INS No. 1401Alkaline treated starch: INS No. 1402Bleached starch: INS No. 1403Oxidized starch: INS No. 1404Enzyme-treated starch: INS No. 1405Monostarch phosphate: INS No. 1410Distarch phosphate: INS No. 1412Phosphated distarch phosphate: INS No. 1413Acetylated distarch phosphate: INS No. 1414Starch acetate: INS No. 1420Acetylated distarch adipate: INS No. 1422Hydroxypropyl starch: INS No. 1440Hydroxypropyl distarch phosphate: INS No. 1442Starch sodium octenylsuccinate: INS No. 1450Acetylated oxidized starch: INS No. 1451

DEFINITION Food starches which have one or more of their original characteristics altered bytreatment in accordance with good manufacturing practice by one of the procedureslisted in Table 1. In the case of starches treated with heat in the presence of acid or withalkali, the alteration is a minor fragmentation. When the starch is bleached, the changeis essentially in the colour only. Oxidation involves the deliberate production ofcarboxyl groups. Acetylation results in substitution of hydroxyl groups with acetylesters. Treatment with reagents such as orthophosphoric acid results in partialsubstitution in the 2, 3- or 6- position of the anhydroglucose unit unless the 6-position isoccupied for branching. In cases of cross-linking, where a polyfunctional substitutingagent, such as phosphorus oxychloride, connects two chains, the structure can berepresented by: Starch-O-R-O-Starch, where R = cross-linking group and Starch refersto the linear and/or branched structure. The article of commerce can be specified by theparameter specific for the particular type of modification as indicated in Column 3 ofTable 1, and may also be further specified as to the loss on drying, sulfated ash, proteinand fat.

Starch acetate: 9045-28-7Acetylated distarch adipate: 68130-14-3Hydroxypropyl starch: 9049-76-7Hydroxypropyl distarch phosphate: 53124-00-8

C.A.S. number

Acetylated oxidized starch: 68187-08-6

DESCRIPTION Most modified starches are white or off-white, odourless powders. According to thedrying method these powders can consist of whole granules having the appearance ofthe original native starch, or aggregates consisting of a number of granules (pearlstarch, starch-grits) or, if pregelatinized, of flakes, amorphous powder or coarseparticles.

FUNCTIONAL USES Thickener, stabilizer, binder, emulsifier

- 54 -


CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Insoluble in cold water (if not pregelatinized); forming typical colloidal solutionswith viscous properties in hot water; insoluble in ethanol.

Microscopy Passes testSee description under TESTS

Iodine stain Passes testSee description under TESTS

Copper reduction Passes testSee description under TESTS

Differentiation test Passes test for type of starchSee description under TESTS for:1. Hypochlorite oxidized starch2. Specific reaction for acetyl groups3. Positive test for ester groups

PURITY

Sulfur dioxide Not more than 50 mg/kg for modified cereal starchesNot more than 10 mg/kg for other modified starches unless otherwise specified inTable ISee description under TESTS

Lead Not more than 2 mg/kgDetermine using an atomic absorption technique appropriate to the specified level.The selection of sample size and method of sample preparation may be based on theprinciples of the method described in FNP 5, “Instrumental methods”.

Additional purity specifi-cations for individual chemi-cally modified starches

See column 3 of Table ISee description under TESTS

TESTS


Microscopy Modified starches which have not been pregelatinized retain their granular structureand can be identified as starches by microscopic observation. Shape, size andsometimes striations are characteristics of the botanical origin. In polarized lightunder cross nicol prisms the typical polarization cross will be observed

Iodine stain Add a few drops of 0.1 N potassium tri-iodide to an aqueous suspension of the sample.These starches stain with iodine in the same way as native starches. The colour canrange from dark blue to red

Copper reduction Place about 2.5 g of the sample previously washed with water, in a boiling flask, add 10ml of dilute hydrochloric acid (3%) and 70 ml of water, mix, reflux for about threehours and cool. Add 0.5 ml of the resulting solution to 5 ml of hot alkaline cuprictartrate TS. A copious red precipitate is produced

- 55 -


Differentiation test To differentiate between various treated starches perform the following tests:

1. Test for hypochlorite-oxidized starch (not for slightly oxidized potato starch)

Principle: Because of the carboxyl group content, hypochlorite-oxidized starch hasanionic properties. It can be dyed with positively charged dyes such as methylene blue.

Procedure: 50 mg of the sample are kept in suspension for 5-10 min in 25 ml of a 1%aqueous dye solution and stirred occasionally. After decantation of the excess solution,the starch is washed with distilled water. Microscopic inspection clearly showscolouring, if the sample is hypochlorite-oxidized starch. By this test hypochlorite-oxidized starch is distinguished from native and acid modified starch of the samebotanical origin.

2. Specific reaction of acetyl groups

Principle: Acetate is liberated upon saponification of acetylated starch. Afterconcentration the acetate is converted to acetone by heating with calcium hydroxide.The acetone thus produced stains blue with o-nitrobenzaldehyde.

Procedure: About 10 g of the sample is suspended in 25 ml water to which is added 20ml of 0.4 N NaOH. After shaking for 1 h the starch is filtered off and the filtrateevaporated in an oven at 110º. The residue is dissolved in a few drops of water andtransferred to a test tube. Add calcium hydroxide and heat the tube. If the sample isacetylated starch, acetone vapours are produced. These produce a blue colour on apaper strip soaked in a fresh saturated solution of o-nitrobenzaldehyde in 2 N NaOH.The blue colour is more distinct when the original yellow colour of the reagents isremoved with 1 drop of a 1 in 10 solution of hydrochloric acid.

3. Positive test for ester groups

The infrared spectrum of a thin film gives a typical absorption band at about 1720 cm-1which is an indication for ester groups. The limit of detection is about 0.5% acetyl,adipyl or succinyl groups in the product.

PURITY TESTS

Sulfur dioxide Scope: The method is applicable, with minor modifications, to liquid or solid sampleseven in the presence of other volatile sulfur compounds.

Principle: The sulfur dioxide is released from the sample in a boiling acid mediumand is removed by a stream of carbon dioxide. The separated gas is collected in dilutehydrogen peroxide where it is oxidized to sulfuric acid and titrated with standardalkali. Alternatively, the sulfuric acid may be determined gravimetrically as bariumsulfate.

Apparatus: “Monier-Williams" apparatus for the determination of sulfurous acid,constructed with standard-taper glass connections, can be obtained from any reliablescientific glass apparatus store. It is customary, however, to construct the apparatuswith regular laboratory glassware using stopper connections (see Figure 1).

- 56 -


Figure 1

The assembly consists of a 1000-ml two-neck round-bottom boiling flask to which agas-inlet tube, a 60-ml dropping funnel having a 2-mm bore stopcock, and a slopingAllihn reflux condenser are attached. A delivery tube connects the upper end of thecondenser to the bottom of a 250-ml conical receiving flask, which is followed by aPeligot tube.In operation, carbon dioxide is passed through the scrubber and bubbled through theheated reaction mixture, sweeping sulfur dioxide through the condenser and into thereceivers where it is absorbed quantitatively.

Preparation of solutions: Sodium carbonate solution: Dissolve approximately 15 g ofNa2CO3 or 40 g of Na2CO3·10H2O in distilled water, and dilute to 100 ml.Hydrogen peroxide, 3%: Dilute 10 ml of C.P. (Chemical Purity) neutral 30%hydrogen peroxide (H2O2) with distilled water to 100 ml.

Procedure: Pass carbon dioxide from a generator or cylinder through the sodiumcarbonate scrubber solution to remove chlorine, thence into the gas-inlet tube of theboiling flask. Place 15 ml of the 3% hydrogen peroxide in the receiving flask and 5ml in the Peligot tube. Connect the apparatus and introduce into the boiling flask, bymeans of the dropping funnel, 300 ml of distilled water and 20 ml of concentratedhydrochloric acid. Boil the contents approximately 10 min in a current of carbondioxide. Weigh, to the nearest g, 100 g of the sample and disperse in approximately300 ml of recently-boiled distilled water. Transfer the slurry to the boiling flask bymeans of dropping funnel, regulating the sample addition rate and the gas flow ratethrough the apparatus to prevent drawback of hydrogen peroxide, inclusion of air, orburning of sample. Boil the mixture gently for 1 h in a slow current of carbondioxide. Stop the flow of water in the condenser just before the end of thedistillation. When the delivery tube just above the receiving flask becomes hot,remove the tube from the condenser immediately. Wash the delivery tube and thePeligot tube contents into the receiving flask, and titrate with 0.1 N sodiumhydroxide, using bromphenol blue indicator (see Note).

Perform a blank determination on the reagents, and correct results accordingly.

% sulfur dioxide(S B) 0.0032 100

W=

− × ×

in which

S = ml of 0.1 N sodium hydroxide used for the sampleB = ml of 0.1 N sodium hydroxide used for the blankW = the weight (in grams) of the sample.

Note. A gravimetric determination may be made after titration. Acidify with HCl,

- 57 -


precipitate with BaC12, settle, filter, wash, ignite, and weigh as BaSO4.

Table 1. Additional purity specifications for individual chemically modified starches(All percentages calculated on dry substance)

Modification Process limitations End-product specifications

Dextrin roasted starch Dry heat treatment with hydrochloricacid or ortho-phosphoric acid

Final pH 2.5-7.0

Acid treated starch Treatment with hydrochloric acid orortho-phosphoric acid or sulfuric acid

Final pH 4.8-7.0

Alkaline treated starch Treatment with sodium hydroxide orpotassium hydroxide

Final pH 5.0-7.5

Bleached starch Treatment with peracetic acidand/or hydrogen peroxide, or

sodium hypochlorite or sodiumchlorite, or

sulfur dioxide or alternative permittedforms of sulfites, or

potassium permanganate orammonium persulfate

Added carbonyl group not more than0.1%

No residual reagent

Residual sulfur dioxide not more than50 mg/kg

Residual manganese not more than50 mg/kg

Enzyme-treated starch Treatment in an aqueous solution at atemperature below the gelatinizationpoint with one or more food-gradeamyolytic enzymes


Oxidized starch Treatment with sodium hypochlorite Carboxyl groups not more than 1.1%


Monostarch phosphate Esterification with ortho-phosphoricacid, or sodium or potassium ortho-phosphate, or sodium tripolyphosphate

Phosphate calculated as phosphorusnot more than 0.5% for potato orwheat, and not more than 0.4% forother starches

Distarch phosphate Esterification with sodiumtrimetaphosphate or phosphorusoxychloride

Phosphate calculated as phosphorusnot more than 0.5% for potato andwheat, and not more than 0.4% forother starches

Phosphated distarch phosphate Combination of treatments forMonostarch phosphate and Distarchphosphate

Phosphate calculated as phosphorusnot more than 0.5% for potato andwheat, and not more than 0.4% forother starches

Acetylated distarch phosphate Esterification with sodiumtrimetaphosphate or phosphorusoxychloride combined withesterification with acetic anhydride orvinyl acetate

Acetyl groups not more than 2.5%;phosphate calculated as phosphorusnot more than 0.14% for potato andwheat, and 0.04% for other starches;and vinyl acetate not more than 0.1mg/kg

Starch acetate Esterification with acetic anhydride orvinyl acetate

Acetyl groups not more than 2.5%

Acetylated distarch adipate Esterification with acetic anhydrideand adipic anhydride

Acetyl groups not more than 2.5%and adipate groups not more than0.135%

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Hydroxypropyl starch Esterification with propylene oxide Hydroxypropyl groups not more than7.0%; propylene chlorohydrin notmore than 1 mg/kg

Hydroxypropyl distarch phosphate Esterification with sodiumtrimetaphosphate or phosphorusoxychloride combined withetherification by propylene oxide

Hydroxypropyl groups not more than7.0%; propylene chlorohydrin notmore than 1 mg/kg; and residualphosphate calculated as phosphorusnot more than 0.14% for potato andwheat, and not more than 0.04% forother starches

Starch sodium octenylsuccinate Esterification with octenylsuccinicanhydride

Octenylsuccinyl groups not morethan 3%; and residual octenylsuccinicacid not more than 0.3%

Acetylated oxidized starch Treatment with sodium hypochloritefollowed by esterification with aceticanhydride

Acetyl groups not more than2.5 % and carboxyl groups not morethan 1.1 %

Methods for additional purityspecifications:

pH (FNP 5) As specified in Column 3 of Table 1Suspend 20 g of the sample with 80 ml of water, and agitate continuously at a moderaterate for 5 min (In the case of pregelatinized starches, 3 g should be suspended in 97 mlof water).

Carboxyl groups As specified in Column 3 of Table 1.

Principle: The carboxyl containing starch is equilibrated with mineral acid to convertcarboxyl salts to the acid form. Cations and excess acid are removed by washing withwater. The washed sample is gelatinized in water and titrated with standard alkali.

Note: Native phosphate groups present in potato starch increase the titre found in thismethod (See note 6)

Reagents:Hydrochloric Acid Solution, 0.10 N : Standardization unnecessarySodium Hydroxide Solution, 0.10 N : StandardizedPhenolphthalein Indicator, 1%

Procedure: If necessary, grind sample completely through a laboratory cutting mill to20 mesh or finer, taking precautions to prevent any significant change in moisture, andmix thoroughly.

Weigh accurately a sample containing not more than 0.25 milli-equivalent of carboxyl(Note 1), and transfer quantitatively to a 150-ml beaker. Add 25 ml of 0.1 Nhydrochloric acid and stir occasionally over a period of 30 min. Vacuum filter theslurry through a medium porosity fritted-glass crucible or small funnel, using a finestream of water from a wash bottle to aid quantitative transfer of the sample. Wash thesample with distilled water (300 ml usually sufficient) until the filtrate is free fromchloride determined by silver nitrate test (Note 2).

Transfer the demineralized sample quantitatively to a 600-ml beaker with the aid ofdistilled water, and slurry the sample in 300 ml of distilled water. Heat sampledispersion in a steam bath or boiling water bath (Note 3), stirring continuously until thestarch gelatinizes, and continue heating for 15 min to ensure complete gelatinization(Note 4).

Remove sample from bath and titrate while hot with standard 0.10 N sodium hydroxidesolution to a phenolphthalein end-point. The end-point may be detected

- 59 -


electrometrically at pH 8.3. A blank determination is run on the original sample tocorrect for native acid substances (Note 5). Weigh the same quantity of starch as takenfor carboxyl titration, and slurry in 10 ml of distilled water. Stir at about 5-minintervals for 30 min.

Vacuum filter the slurry quantitativey through a medium porosity fritted-glass crucibleor small funnel, and wash sample with 200 ml of distilled water. Transfer, gelatinize,and titrate the sample with standard 0.10 N sodium hydroxide in the same manner asthe demineralized sample.

Calculation:

Carboxyl groups (%)(ml 0.10N NaOH Blank) 0.0045 100

Sample weight (g)=

− × ×

Notes and Precautions:

1. Sample size should not exceed 5.0 g for a mildly oxidized nor less than 0.15 g fora highly oxidized commercial starch.

2. Add 1 ml of 1% aqueous silver nitrate solution to 5 ml of filtrate. Turbidity orprecipitation occurs within 1 min if chloride is present.

3. Heating on a hot plate or over a Bunsen burner is not recommended. Over-heatingor scorching in amounts too small to be visible will cause sample decompositionand apparent high carboxyl results.

4. Thorough gelatinization facilitates rapid titration and accurate end-point detection.

5. A blank titration is run on a water washed sample to correct for acidic componentswhich are not introduced by oxidation or derivatization. Free fatty acidscomplexed with amylose in common corn starch are the principal contributors tothe blank titer.

6. A correction for phosphate content in potato starch (deduction) should be madeafter determining the phosphorus content of the sample being examined.

The deduction is calculated:

2 45.02 P

30.972.907 P

× ×= ×

where:

P = phosphorus content (%)

- 60 -


Manganese As specified in Column 3 of Table 1.

Instrumentation: Atomic absorption spectrophotometer with manganese hollowcathode lamp.

Preparation of solutions:

− Standard solution: Prepare a solution containing 0.5 mg/l of manganese.

− Sample solution: Transfer 10.000 g of the sample into a 200-ml Kohlrauschvolumetric flask, previously rinsed with 0.5 N hydrochloric acid, add 140 ml of 0.5N hydrochloric acid, and shake vigorously for 15 min, preferably with amechanical shaker. Dilute to volume with 0.5 N hydrochloric acid, and shake.Centrifuge approximately 100 ml of the mixture in a heavy-walled centrifuge tubeor bottle at 650xg for 5 min, and collect the supernatant liquid. This supernatantcomprises the “sample solution”.

Procedure: Follow manufacturer's instructions for operating the atomic absorptionspectrophotometer and aspirate distilled water through the air-acetylene burner for 5min to obtain a base-line reading at 279.5 nm. In the same manner aspirate a portion ofthe "Standard solution" and note the reading. Finally, aspirate the "Sample solution"and compare the reading with the reading for the "Standard solution", and multiply thisvalue by 20 to obtain mg per kg of Mn in the original sample taken for analysis.

Phosphorus As specified in the Column 3 of Table 1.

Reagents:

− Ammonium Molybdate Solution (5%): Dissolve 50 g of ammonium molybdatetetrahydrate, (NH4)6Mo7O24·4H2O, in 900 ml of warm water, cool to roomtemperature, dilute to 1000 ml with water, and mix.

− Ammonium Vanadate Solution (0.25%): Dissolve 2.5 g of ammoniummetavanadate, NH4VO3, in 600 ml of boiling water, cool to 60 - 70o, and add 20ml of nitric acid. Cool to room temperature, dilute to 1000 ml with water, and mix.

− Zinc Acetate Solution (10%): Dissolve 120 g of zinc acetate dihydrate,Zn(C2H3O2)2·2H2O, in 880 ml of water, and filter through Whatman No. 2V orequivalent filter paper before use.

− Nitric Acid Solution (29%): Add 300 ml of nitric acid (sp. gr 1.42) to 600 ml ofwater, and mix.

− Standard Phosphorus Solution: (100 µg P in 1 ml): Dissolve 438.7 mg ofmonobasic potassium phosphate, KH2PO4, in water in a 1000-ml volumetric flask,dilute to volume with water, and mix.

Standard Curve: Pipet 5.0, 10.0, and 15.0 ml of the Standard Phosphorus Solution intoseparate 100-ml volumetric flasks. To each of these flasks, and to a fourth blank flask,add in the order stated 10 ml of Nitric Acid Solution, 10 ml of Ammonium VanadateSolution, and 10 ml of Ammonium Molybdate Solution, mixing thoroughly after eachaddition. Dilute to volume with water, mix, and allow to stand for 10 min. Determinethe absorbance of each standard solution in a 1 cm cell at 460 nm, with a suitablespectrophotometer, using the blank to set the instrument at zero. Prepare a standardcurve by plotting the absorbance of each solution versus its concentration, in mg P per100 ml.

Sample Pretreatment: Place 20 to 25 g of the starch sample in a 250-ml beaker, add 200ml of a 7 to 3 methanol-water mixture, disperse the sample, and agitate mechanicallyfor 15 min. Recover the starch by vacuum filtration in a 150 ml medium-porosityfritted-glass or Buchner funnel, and wash the wet cake with 200 ml of the methanol-water mixture. Reslurry the wet cake in the solvent, and wash it a second time in thesame manner. Dry the filter cake in an air oven at a temperature below 50o, then grind

- 61 -


the sample to 20-mesh or finer, and blend thoroughly. Determine the amount of drysubstance by drying a 5 g portion in a vacuum oven, not exceeding 100 mm of Hg, at120o for 5 h. (NOTE: The treatment outlined above is satisfactory for starch productsthat are insoluble in cold water.For pregelatinized starch and other water-soluble starches, prepare a 1% to 2% aqueouspaste, place it in a cellophane tube, and dialyze against running distilled water for 30 to40 h. Precipitate the starch by pouring the solution into 4 volumes of acetone pervolume of paste, while stirring. Recover the starch by vacuum filtration in a medium-porosity fritted-glass or Buchner funnel, and wash the filter cake with absolute ethanol.Dry the filter cake, and determine the amount of dry substance as directed for water-insoluble starches).

Sample preparation: Transfer about 10 g of the Treated Sample, calculated on the dry-substance and accurately weighed, into a Vycor dish, and add 10 ml of Zinc AcetateSolution in a fine stream, distributing the solution uniformly in the sample. Carefullyevaporate to dryness on a hot plate, then increase the heat, and carbonize the sample onthe hot plate or over a gas flame. Ignite in a muffle furnace at 550o until the ash is freefrom carbon (about 1 to 2 h), and cool. Wet the ash with 15 ml of water and washslowly down the sides of the dish with 5 ml of Nitric Acid Solution. Heat to boiling,cool, and quantitatively transfer the mixture into a 200-ml volumetric flask, rinsing thedish with three 20-ml portions of water and adding the rinsings to the flask. Dilute tovolume with water, and mix. Transfer an accurately measured aliquot (V, in ml) of thissolution, containing not more than 1.5 mg of phosphorus, into a 100-ml volumetricflask and add 10 ml of Nitric Acid Solution, 10 ml of Ammonium Vanadate Solution,and 10 ml of Ammonium Molybdate Solution, mixing thoroughly after each addition.Dilute to volume with water, mix, and allow to stand for 10 min.

Procedure: Determine the absorbance of the Sample Preparation in a 1 cm cell at 460nm, with a suitable spectrophotometer, using the blank to set the instrument at zero.From the Standard Curve, determine the mg of phosphorus in the aliquot taken,recording this value as a. Calculate the amount in mg/kg of Phosphorus (P) in theoriginal sample by the formula:

a 2 0 0 1 0 0 0

V W

× ×

×

in which W is the weight of the sample taken, in g.

Acetyl groups As specified in Column 3 of Table 1.

Accurately weigh about 5 g of the sample and transfer into a 250 ml conical flask.Suspend in 50 ml of water, add a few drops of phenolphthalein TS, and titrate with 0.1N sodium hydroxide to a permanent pink end-point. Add 25.0 ml of 0.45 N sodiumhydroxide, stopper the flask, and shake vigorously for 30 min, preferably with amechanical shaker. (NOTE: the temperature should not exceed 30o or some starchesmay gelatinize). Remove the stopper, wash the stopper and sides of the flask with a fewml of water, and titrate the excess alkali with 0.2 N hydrochloric acid to thedisappearance of the pink colour. Record the volume, in ml of 0.2 N hydrochloric acidrequired as S.

Perform a blank titration on 25.0 ml of 0.45 N sodium hydroxide, and record thevolume, in ml, of 0.2 N hydrochloric acid required as B.

A cetyl g r o u p s ( % )(B S ) N 0 .043 100

W=

− × × ×

where:

N = normality of hydrochloric acid solutionW = weight of sample in grams.

- 62 -


Vinyl acetate Headspace Gas Chromatographic method

Chromatographic system Use a gas chromatograph equipped with a 2 m x 2 mm (i.d.)glass column containing Porapak Q, 80-100 mesh (or equivalent) fitted with a flameionization detector, under the following conditions:

- Carrier gas flow (nitrogen): 20 ml/mininjection port temperature: 200o

- column temperature: 50o

- detector temperature: 200o

Standard preparation: Accurately weigh 150 mg vinyl acetate (reagent grade) into a 100ml volumetric flask. Dissolve and make up to volume with distilled water. Place 1 mlof this solution in a 10-ml volumetric flask and make up to volume with distilled water.Add 1 ml of this dilute solution to 30 g unmodified starch of the same botanical originas the test substance in a 100-ml flask with a septum-liner. Seal the flask immediatelywith the septum-liner. This provides a standard starch preparation with a vinyl acetatecontent of 5 mg/kg

Procedure: Weigh 30 g of the test substance into a 100-ml flask with a septum-liner.Seal the flask. Place the flask containing the test substance and the flask containing thestandard preparation in a constant temperature water bath at 70o for 30 min. Withdraw2.0 ml from the headspace volume of the flask containing the standard preparationusing a gas-tight syringe, inject directly into the injection port of the gas chromatographand record the peak height of the chromatogram. Similarly inject 2.0 ml of theheadspace volume from the flask containing the test substance into the chromatograph.Calculate the content of vinyl acetate in the test substance from a comparison of thepeak hights of the two chromatograms.

Adipate groups As specified in Column 3 of Table 1.

Reagents and Solutions:

− N,N-Bis-trimethylsilyltrifluoroacetamide (BSTFA): Macherey-Nagel, D 5160Dueren, Germany or equivalent.

− Glutaric acid solution: Dissolve 1.00 g of glutaric acid (Merck or equivalent) inwater and dilute to 1000 ml.

− Adipic acid solution: Dissolve 1.00 g of adipic acid (UCB, Brussels, Belgium orequivalent) in 900 ml of warm water, cool to room temperature, dilute to 1000ml and mix.

Apparatus: Chromatograph: Hewlett-Packard Model 7620A gas chromatograph orequivalent equipped with flame ionization detector and Model 3370A integrator.Column parameters: 2-m stainless steel, 1.83 mm id, packed with 5% OV-17 on 80-100 mesh Chromosorb GAW-DMCS (Alltech Europe, Inc., B 9731 Eke, Belgium);precondition column 24 h at 350o with nitrogen carrier gas at 40 ml/min. Operatinggas flow rates (ml/min): nitrogen carrier 30, hydrogen 40, air 400. Temperature:injection 280o, detector 250o, column 140o. Retention times (min): glutaric acid 2.83,adipic acid 4.50.

Calibration: Weigh 1.0 g waxy corn starch into each of four 250-ml Erlenmeyerflasks. To each flask add 50 ml water and 1.0 ml of an aqueous solution containing1.0 mg glutaric acid/ml. Add, to one flask, 0.25 ml of an aqueous solution containing1.0 mg adipic acid per ml; to the other three, add 0.50 ml, 0.75 ml, and 1.0 ml,respectively. Each flask then contains 1.0 mg glutaric acid and, respectively, 0.25,0.50, 0.75 and 1.0 mg adipic acid. Agitate flasks manually to disperse the starchfully and add 50 ml 4N sodium hydroxide. Continue agitation another 5 min, placeeach flask in water bath at ambient temperature, and carefully add 20 ml 12 Nhydrochloric acid to each. When each flask is cool quantitatively transfer contents to

- 63 -


250 ml separatory funnel. Extract with 100 ml reagent grade ethyl acetate. Drainbottom aqueous layer into beaker and collect upper organic layer in 500-mlErlenmeyer flask containing 20 g anhydrous sodium sulphate. Transfer aqueousportion back to separatory funnel and repeat ethyl acetate extraction twice more.Shake flasks periodically during 10 min and then filter contents through WhatmanNo. 1 paper into 1-litre round-bottom flasks. Rinse flasks and insoluble residues infilters twice with 50 ml of ethyl acetate. Under vacuum, (50 mm Hg) at temperaturenot exceeding 40o, evaporate total organic extraction and washings of each flask untilcompletely dry.

The evaporation of ethyl acetate should be effected as quickly as possible becausesome hydrolysis takes place on standing. The products of hydrolysis cause adeterioration in the resolution of adipic acid in the chromatographic separation.

Successively add 2 ml pyridine and 1 ml N,N-bis-trimethylsilyltrifluoro-acetamide tothe dry contents. Close each of the round-bottom flasks with stopper and rinseinternal surfaces thoroughly by swirling. Let flasks stand 1 h; then transfer ca 2 mlfrom each to small glass vials and immediately seal. Inject 4 µl into gaschromatograph.

Calculations: Establish retention times for each acid and determine peak height forglutaric acid and for each level of adipic acid represented. A plot of peak height ratioof adipic acid to glutaric acid against amount of adipic acid is linear. This calibrationcurve may be used, but it is simpler to use a response factor (RF):

R FH W

HI S

S

=×

where:

HS and HI = peak heights of the standard adipic acid and glutaric acid,respectively; and WS = weight of the standard adipic acid.

RF should be verified weekly.

Total adipate: Accurately weigh about 1.0 g of the sample into a 250 ml Erlenmeyerflask, and add 50 ml water and 1.0 ml of an aqueous solution containing 1.0 mgglutaric acid/ml. Proceed as in Calibration, beginning "Agitate flasks manually...".

- 64 -


Free adipic acid Accurately weigh about 5.0 g of the sample into a 250 mlErlenmeyer flask, add 100 ml water and 1.0 ml of the glutaric acid solution. Agitatefor 1 h, filter through a 0.45 µm Millipore filter, add 1 ml concentrated hydrochloricacid to the filtrate and transfer it quantitatively to a 250-ml separating funnel.Proceed as in Calibration, beginning "Extract with 100 ml..."

Calculation: For both preparations ("Total adipate content" and "Free adipic acidcontent") record peak heights for adipic acid and glutaric acid (internal standard).Calculate the amounts of total adipate and free adipic acid, respectively, contained inthe sample as follows:

AH R F

H S 10X

IX

=×

× ×

where:

A = content of total adipate or free adipic acid respectively (%)HX = peak height of adipic acid in the actual sample preparationHIX = peak height of glutaric acid in the actual sample preparationRF = response factor for adipic acidS = weight of sample in the actual preparation (g)

Adipate groups (%) = Content of total adipate (%) - content of free adipic acid (%)

Hydroxypropyl groups As specified in Column 3 of Table 1

Ninhydrin reagent: A 3% solution of 1,2,3,-triketohydrindene crystals in 5% aqueoussodium bisulfite solution.

Procedure: Accurately weigh 50 - 100 mg of the sample into a 100-ml volumetricflask and add 25 ml of 1 N sulfuric acid. Prepare a sample of unmodified starch ofthe same source (i.e. corn or potato) in the same manner. Place the flasks in a boilingwater bath and heat until the samples are in solution. Cool and dilute the contents to100 ml with water. If necessary, dilute the sample further to assure the presence ofno more than 4 mg of hydroxypropyl group per 100 ml, and then dilute the blankstarch in the same proportion. Pipet 1 ml of the solutions into 25-ml graduated testtubes with glass stoppers and, with the tubes immersed in cold water, add dropwise 8ml of concentrated sulfuric acid to each. Mix well and place the tubes in a boilingwater bath for exactly 3 min. Immediately transfer the tubes to an ice bath until thesolution is chilled. Add 0.6 ml of ninhydrin reagent, carefully allowing the reagent torun down the walls of the test tubes. Immediately shake well, and place the tubes in a25o water bath for 100 min. Adjust the volume in each tube to 25 ml withconcentrated sulfuric acid and mix by inverting the tubes several times. (Do notshake). Immediately transfer portions of the solutions to 1-cm cells and after exactly5 min, measure the absorption (A) at 590 nm, using the starch blank as the reference.Prepare a calibration curve with 1-ml aliquots of standard aqueous solutions,containing 10, 20, 30, 40 and 50 µg of propylene glycol per ml.

Calculations:

Hydroxypropyl groups (%)C 0.7763 10 F

W=

× × ×

where:

C = amount of propylene glycol in the sample solution read from the calibrationcurve (µg/ml)F = dilution factor (if a further dilution has been necessary)W = weight of sample (mg)

- 65 -


Propylene chlorhydrin As specified in Column 3 of Table 1.

Apparatus

Gas Chromatograph: Use a Hewlett-Packard Model 5750 or equivalent. A dual-column instrument equipped with a flame-ionization detector is recommended. Anintegrator should be part of the recording system.

− Gas Chromatography column: Use a stainless steel column, 3 m x 3.2 mm (od),packed with 10% Carbowax 20 M on 80/100-mesh Gas Chrom 2, or equivalent.After packing and prior to use, condition the column overnight at 200º, using ahelium flow of 25 ml per min.

− Concentrator: Use a Kuderna-Danish concentrator having a 500-ml flask,available from Kontes Glass Co., Vineland, N.J., USA, (Catalog No. K-57000),or equivalent.

− Pressure Bottles: Use 200-ml pressure bottles, with a Neoprene washer, glassstopper, and attached wire clamp, available from Fisher Scientific Co., Pittsburg,PA, USA (Vitro 400, Catalog No. 3-100), or equivalent.

Reagents:

− Diethyl ether: Use anhydrous, analytical reagent-grade diethyl ether

− Florisil: Use 60/100 mesh material, available from Floridin Co., 3 Penn Center,Pittsburg, PA 15235, USA, or an equivalent product.

− Propylene chlorohydrins: Use Eastman No. P1325 1-Chloro-2-propanolPractical, containing 25% 2-chloro-1-propanol, available from Eastman KodakCo., Rochester, N.Y. 14650, USA or equivalent.

− Standard preparation: Draw 25 µl of mixed propylene chlorohydrin isomerscontaining 75% of 1-chloro-2-propanol and 25% of 2-chloro- 1-propanol) into a50-µl syringe. Accurately weigh the syringe and discharge the contents into a500-ml volumetric flask partially filled with water. Reweigh the syringe, andrecord the weight of the chlorohydrins taken. Dilute to the volume with water,and mix. This solution contains about 27.5 mg of mixed chlorohydrins, or about55 µg per ml. Prepare this solution fresh on the day of use.

Sample Preparation: Transfer a blended representative 50.0 g sample into a PressureBottle, and add 125 ml of 2 N sulfuric acid. Clamp the top in place, and swirl thecontents until the sample is completely dispersed. Place the bottle in a boiling waterbath, heat for 10 min, then swirl the bottle to mix the contents, and heat in the bathfor an additional 15 min. Cool in air to room temperature, then neutralize thehydrolyzed sample to pH 7 with 25% sodium hydroxide solution, and filter throughWhatman No. 1 paper, or equivalent, in a Buchner funnel, using suction. Wash thebottle and filter paper with 25 ml of water, and combine the washings with thefiltrate. Add 30 g of anhydrous sodium sulfate, and stir with a magnetic stirring barfor 5 to 10 min, or until the sodium sulfate is completely dissolved. Transfer thesolution into a 500-ml separator equipped with a teflon plug, rinse the flask with 25ml of water, and combine the washings with the sample solution. Extract with five50 ml portions of diethyl ether, allowing at least 5 min in each extraction foradequate phase separation. Transfer the combined ether extracts in a Concentrator,place the graduated receiver of the concentrator in a water bath maintained at 50 -55o, and concentrate the extract to a volume of 4 ml. (NOTE: Ether extracts ofsamples may contain foreign residues that interfere with the analysis and/or theinterpretation of the chromatograms. These residues are believed to be degradationproducts arising during the hydrolysis treatment. Analytical problems created bytheir presence can be avoided through application of a clean-up treatment performedas follows: Concentrate the ether extract to about 8 ml, instead of 4 ml specifiedabove. Add 10 g of Florisil, previously heated to 130º for 16 h just before use, to a

- 66 -


chromatographic tube of suitable size, then tap gently, and add 1 g of anhydroussodium sulfate to the top of the column. Wet the column with 25 ml of diethyl ether,and quantitatively transfer the concentrated extract to the column with the aid ofsmall portions of the ether. Elute with three 25-ml portions of the ether, collect all ofthe eluate, transfer it to a concentrator, and concentrate to a volume of 4 ml). Coolthe extract to room temperature, transfer it quantitatively to a 5.0-ml volumetric flaskwith the aid of small portions of diethyl ether, dilute to volume with the ether, andmix.

Control Preparations: Transfer 50.0 g portions of unmodified (underivatized) waxycorn starch into five separate pressure bottles, and add 125 ml of 2 N sulfuric acid toeach bottle. Add 0.0, 0.5, 1.0, 2.0, and 5.0 ml of the Standard Preparation to thebottles, respectively, giving propylene chlorohydrin concentrations, on the starchbasis, of 0, 0.5, 1.0, 2.0, and 5.0 mg/kg, respectively. Calculate the exactconcentration in each bottle from the weight of propylene chlorohydrins used inmaking the Standard Preparation. Clamp the tops in place, swirl until the contents ofeach bottle are completely dissolved, and proceed with the hydrolysis, neutralization,filtration, extraction, extract concentration, and final dilution as directed underSample Preparation.

Procedure: The operating conditions may be varied, depending upon the particularinstrument used, but a suitable chromatogram is obtained with the Hewlett-PackardModel 5750 using a column oven temperature of 110o, isothermal; injection porttemperature of 210o; detector temperature of 240o; and hydrogen (30 ml per min),helium (25 ml per min), or air (350 ml per min) as the carrier gas. A 1.0 mV full-scale recorder is recommended; range, attenuation, and chart speed should beselected to optimize signal characteristics. Inject 2.0 µl aliquots of each of theconcentrated extracts, prepared as directed under Control Preparation, allowingsufficient time between injections for signal peaks corresponding to the twochlorohydrin isomers to be recorded (and integrated) and for the column to bepurged. Record and sum the signal areas (integrator outputs) from the twochlorohydrin isomers for each of the controls. Using identical operating conditions,inject a 2.0-µl aliquot of the concentrated extract prepared as directed under SamplePreparation, and record and sum the signal areas (integrator outputs) from thesample.

Calculation: Prepare a calibration plot on linear coordinate graph paper by plottingthe summed signal areas for each of the controls against the calculated propylenechlorohydrin concentrations, in mg/kg, derived from the actual weight ofchlorohydrin isomers used. Using the summed signal areas corresponding to the 1-chloro-2-propanol and 2-chloro-1-propanol from the sample, determine theconcentration of mixed propylene chlorohydrins, in mg/kg, in the sample byreference to the calibration plot derived from the control samples. After gainingexperience with the procedure and demonstrating that the calibration plot derivedfrom the control samples is linear and reproducible, the number of controls can bereduced to one containing about 5 mg/kg of mixed propylene chlorohydrin isomers.The propylene chlorohydrin level in the sample can then be calculated as follows:

Propylene chlorohydrins (mg / kg)C a

A=

×

in which C is the concentration, in mg/kg, of propylene chlorohydrins (sum ofisomers) in the control; a is the sum of signal areas produced by the propylenechlorohydrin isomers in the sample; and A is the sum of the signal areas produced bythe propylene chlorohydrin isomers in the control.

- 67 -


Degree of substitution ofstarch sodium octenylsuccinate

Principle: The degree of substitution is determined by alkali consumed afteracidification and thorough washing of the starch half ester.

Procedure: Weigh out 5.0 g of sample in a 150-ml beaker. Wet out with a few ml ofreagent grade isopropyl alcohol. Add, by pipette 25 ml of 2.5 N hydrochloric acid inisopropanol, allowing the acid to wash down any sample on the sides of the beaker.Stir for 30 min on a magnetic stir plate. Add 100 ml of 90% isopropanol from agraduated cylinder. Stir for 10 min. Filter the sample through a Buchner funnel andwash the filter cake with 90% isopropanol until the filtrate is negative for chlorideions. Use 0.1 N AgNO3 to check for chloride ions. Transfer the filter cake to a 600-ml beaker and rinse the Buchner funnel to wash any starch into the beaker. Bring toa 300-ml volume with distilled water. Place for 10 min in a boiling water bath withstirring. Titrate while hot with 0.1 N NaOH to the phenolphthalein end-point.

Calculation: Calculate as follows:

Degree of substitution (DS)0.162 A

1 0.210 A=

×

− ×

where:A = milliequivalents of sodium hydroxide required per g of starch octenylsuccinate.

Residual octenyl succinicacid in starch sodium octenylsuccinate

Extraction and Preparation of Sample Solution: Extract about 500 mg of starch with 15ml of methanol overnight under constant shaking (weigh starch accurately). Filter theextraction mixture. Wash the starch on the filter with 7 ml of methanol. Repeat threetimes. Combine all filtrates (about 80% of the residuals are extracted by thisprocedure). Add 1 ml of 0.16 N methanolic KOH to the extracts. Dry the extracts witha flash evaporator at 30o. Dissolve the residue in 2 ml methanol. Take 0.5 ml of residuesolution to the reaction vial. Add 0.5 ml derivative reagent (2.8 g of 2-p-dibromoacetophenone and 0.28 g 18-Crown-6 in 50 ml CH3CN) to the reaction vial.Add 2 ml CH3CN to the reaction vial. Cap the reaction vial and heat it at 80o for 30min. Cool the reaction solution to room temperature (use within 24 h).

Liquid Chromatography Analysis:

- Column: Micro-Bondapack C18 (Waters) or equivalent- Mobile Phase: Gradient elution of 70% methanol in water to 80%

methanol in water in - 5 min. Curve 6 (Waters 660 solventprogrammer)

- Flow rate: 1.5 ml/min- Detector: UV at 254 nm, attenuation 0.16 AUFS- Injection volume: 5 µl

Preparation of Calibration Curve: Prepare a 0.5 M solution of sodium octenyl succinate(Solution A). With a syringe take 0.25 ml of Solution A and place into a 25-mlvolumetric flask. Dilute to mark with methanol (Solution B). Prepare three calibrationstandards by taking 0.5, 1 and 2 ml of Solution B and placing into three 50-ml roundbottom flasks. Add to each 1 ml of 0.16 N methanolic KOH. Dry each solution with aflash evaporator at 30o. Dissolve the residue in 2.0 ml of methanol (Solution C1, C2 andC3). Place 0.5 ml of the residue solution in the reaction vial. Add 0.5 ml derivativereagent (2.8 g of 2-p-dibromoacetophenone and 0.28 g of 18-Crown-6 in 50 ml ofCH3CN) to the reaction vial. Add 2 ml of CH3CN to the reaction vial. Cap the vial andheat to 80o for 30 min. Cool the reaction solution to room temperature (the derivativeshould be prepared as needed and used immediately). Inject 5 µl into the LiquidChromatograph. The amount of residuals in each of the 5-µl injections are thefollowing:

for Solution C1 0.2375 µgfor Solution C2 0.4750 µgfor Solution C3 0.9500 µg

- 68 -


Plot peak height from Liquid Chromatograph Chart versus µg of residuals per 5 ml ofsolution.

Calculations: Prepare a calibration curve according to the procedure. Using the peakheight of the unknown sample from the Liquid Cromatograph Chart, determine thelevel of residuals (calculated as octenyl succinic acid) in the injected volume from thecalibration curve.

% R e s i d u a l in S t a r c h3 0 0 V a l u e f r o m G r a p hW e i g h t o f S t a r c h (m g )

=×

Note: The formula is corrected to 100% recovery by dividing by 0.80, so that240/0.80 = 300.

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MONOMAGNESIUM PHOSPHATE page 1 (2)

MONOMAGNESIUM PHOSPHATE(Tentative)


Information required on the loss on drying, loss on ignition, test method for loss onignition and assay method for the dihydrate.

SYNONYMS Monomagnesium orthophosphate, Magnesium dihydrogen phosphate; Magnesiumphosphate, mono basic; Magnesium biphosphate; Acid magnesium phosphate;INS No. 343 (i)

DEFINITION

Chemical names Monomagnesium dihydrogen phosphate

C.A.S. number 13092-66-5 (Anhydrous)15609-87-7 (Dihydrate)

Chemical formula Mg (H2PO4)2 . x H2O (x = 0 to 4)

Formula weight 218.3 (Anhydrous)

Assay Not less than 64% and not more than 66% expressed as P2 O5.

DESCRIPTION White odourless crystalline powder

FUNCTIONAL USES Acidity regulator, nutrient

CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Slightly soluble in water

Test for magnesium (FNP 5) Passes test


PURITY


Fluoride (FNP 5) Not more than 10 mg/kgMethod III; use an appropriate sample size and appropriate volumes of the standardsolution for construction of the calibration curve.

Lead Not more than 4 mg/kgDetermine using an atomic absorption technique appropriate to the specified level. Theselection of sample size and method of sample preparation, may be based on theprinciples of the method described in FNP 5, “ Instrumental Methods”.


METHOD OF ASSAY Weigh accurately between 150 to 200 mg of the sample, dissolve in 25 ml of waterand 10 ml of diluted nitric acid TS and boil for 30 min.. Filter if necessary, and washany precipitate, then dissolve the precipitate by the addition of 1 ml diluted nitric acid

- 70 -

MONOMAGNESIUM PHOSPHATE page 2 (2)

TS. Adjust the temperature to about 50o , add 75 ml of ammonium molybdate TS, andmaintain the temperature at about 50o for 30 min, stirring occasionally. Allow tostand for 16 h or overnight at room temperature. Decant the supernate, through afilter paper, wash the precipitate once or twice with water by decantation using 30 to40 ml each time, and pour the washings through the same filter. Transfer theprecipitate to the same filter, and wash with potassium nitrate solution (1 in 100) untilthe filtrate is no longer acid to litmus paper. Transfer the precipitate with filter paperto the original precipitation vessel, add 50.0 ml of 1N sodium hydroxide, agitate untilthe precipitate is dissolved, add 3 drops of phenolphthalein TS and titrate the excessalkali with 1N sulfuric acid. Each ml of 1N sodium hydroxide consumed isequivalent to 3.088 mg of P2O5 .

- 71 -

NATAMYCIN page 1 (4)

NATAMYCIN(Tentative)

Prepared at the 57th JECFA (2001) and published in FNP52 Add 9 (2001)superseding specifications for pimaricin prepared at the 20th JECFA (1976),published in FNP52 (1992). An ADI 0-0.3mg/kg bw was established at the 20thJECFA (1976).

Information required on level and determination of water content, lead limit, specificrotation, assay value and method of assay for the commercial product. Comments onother aspects of the monograph are invited.

SYNONYMS Pimaricin; INS No. 235

DEFINITION A fungicidal antibiotic of the polyene macrolide group. It is produced by severalspecies of Streptomyces. The commercial product may contain up to three moles ofwater.

Chemical names A stereoisomer of 22-(3-Amino-3,6-dideoxy-β-D-mannopyranosyloxy)-1,3,26-trihydroxy-12-methyl-10-oxo-6,11,28-trioxatricyclo[22.3.1.O5,7]octacosa-8,14,16,18,20-pentaene-25-carboxylic acid

C.A.S. number 7681-93-8

Chemical formula C33H47NO13

Structural formula

O

O

O

Me

O

OH

1 5

OH

O

OH

COOH

10

25

15

O

1'

HO

NH2

OHMe


Assay Not less than 95.0% calculated on the dried basis

DESCRIPTION White to creamy-white, almost odourless, crystalline powder

FUNCTIONAL USES Fungicidal preservative

CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Practically insoluble in water and in lipid and mineral oils; slightly soluble in methanol;soluble in glacial acetic acid and dimethyl-formamide.

Colour reaction On adding a few crystals of the sample, on a spot plate, to a drop of- concentrated hydrochloric acid, a blue colour develops;- concentrated phosphoric acid, a green colour develops, which changes into pale-redafter a few minutes

- 72 -


Infrared absorption The infrared spectrum of a potassium bromide dispersion of the sample correspondswith the reference infrared spectrum in appendix A at the end of these specifications.

Ultraviolet absorption A solution of 5mg/l of the sample in 0.1% glacial acetic acid in methanol hasabsorption maxima at about 290, 303 and 318 nm, a shoulder at about 280 nm andexhibits minima at about 250, 295.5 and 311 nm. See appendix B at the end of thesespecifications.

PURITY

Loss on drying (FNP 5) Not more than 8.0% (60o, over P2O5, pressure less than 5 mm Hg)

Specific rotation (FNP 5) : + 250° to + 295o (1% w/v solution in glacial acetic acid)

pH (FNP 5) 5.5 - 7.5 (1.0% w/v solution in a previously neutralized mixture of 20 partsdimethylformamide and 80 parts of water)

Sulfated ash (FNP 5) Not more than 0.5%Test 2 g of the sample (Method I)

Lead Not more than 2 mg/kgDetermine using an atomic absorption technique appropriate to the specified level.The selection of sample size and method of sample preparation may be based on theprinciples of the method described in FNP 5,"Instrumental Methods"

METHOD OF ASSAY High Performance liquid Chromatography

(Note: Throughout this Assay, protect from direct light all solutions containingnatamycin)

Mobile phase: Dissolve 3.0 g of ammonium acetate and 1.0 g of ammonium chloride in760 ml of water, and mix. Add 5.0 ml of tetrahydrofuran and 240 ml of acetonitrile,mix, and filter through a 0.5-µm or finer porosity filter. Make adjustments if necessaryto meet the system suitability requirements.

Standard preparation: Transfer about 20 mg of natamycin Reference Standard,accurately weighed, to a 100-ml volumetric flask. Add 5.0 ml of tetrahydrofuran, andsonicate for 10 min. Add 60 ml of methanol, and swirl to dissolve. Add 25 ml of water,and mix. Allow to cool to room temperature. Dilute with water to volume, mix, andfilter through a membrane filter of 5-µm or finer porosity.

Resolution solution: Dissolve 20 mg of natamycin in a mixture of 99 ml of methanoland 1 ml of 0.1 N hydrochloric acid, and allow to stand for 2 h.Note: use this solution within 1 h.

Assay preparation: Transfer about 20 mg of natamycin, accurately weighed, to a 100-ml volumetric flask. Proceed as directed under ''Standard preparation'', beginning with''add 5.0 ml of tetrahydrofuran....''

Chromatographic system (see High-Performance Liquid Chromatography, FNP 5):Use a high performance liquid chromatograph equipped with an ultraviolet detectormeasuring at 303 nm and a 4.6-mm x 25-cm column packed with octadecylsilanizedsilica (Supelcosil LC 18 or equivalent). The flow rate is about 3 ml/min.Chromatograph the ''standard preparation'', and record the peak responses: The columnefficiency is not less than 3000 theoretical plates:

N = 5.54 (t/w1/2)2

where: N = number of theoretical platest = retention time of natamycinw1/2 = peak width at half height

20°D

[α]

- 73 -


The tailing factor is between 0.8 and 1.3:

T = W0.05/2f

where: T = tailing factorW0.05 = peak width at 0.05 heightf = distance at W0.05h between peak front and perpendicular line from peakmaximum to baseline.

The relative standard deviation for three replicate injections of the standard preparationis not more than 1.0 %.Chromatograph the ''resolution solution''. The relative retention times are about 0.7 forNatamycin and 1.0 for its methyl ester. The resolution (R) between Natamycin and itsmethyl ester is not less than 2.5:

R = 2(t2-t1)/(W2+W1)

where: t2 and t1 are the retention times of natamycin methyl ester andnatamycin respectivelyW2 and W1 are the width of the corresponding peaks at their basesextrapolated to the baseline.

Procedure: Separately inject about 20 µl for each of the ''standard preparation'' and the''assay preparation'' into the chromatograph, and record the peak areas of the majorpeaks. Calculate the percentage of Natamycin in the portion taken by the formula:

0.1(WsPs/Wu)(ru/rs)

in which Ws is the weight, in mg, of Natamycin Reference Standard taken to prepare the''Standard preparation); Ps is the stated content, in µg/ml, of Natamycin ReferenceStandard; Wu is the weight, in mg, of Natamycin taken to prepare the ''Assaypreparation''; and ru and rs are the peak area responses obtained with the ''Assaypreparation'' and the ''Standard preparation'', respectively.

Appendix A

Reference Infrared Spectrum (1.3 mg solid in 300 mg potassium bromide) for natamycin

- 74 -


Appendix B

Ultraviolet absorption spectrum of natamycinConcentration: 5 µg/ml in methanol/glacial acetic acid mixture

- 75 -

PECTINS page 1 (5)

PECTINS

Prepared at the 57th JECFA (2001) and published in FNP 52 Add 9 (2001),superseding specifications prepared at the 39th JECFA (1992) and published in FNP52 Add 1 (1992). A group ADI “not specified” was established for pectins andamidated pectins, singly or in combination at the 25th JECFA in 1981.

SYNONYMS INS No. 440

DEFINITION Consists mainly of the partial methyl esters of polygalacturonic acid and their sodium,potassium, calcium and ammonium salts; obtained by extraction in an aqueous mediumof appropriate edible plant material, usually citrus fruits or apples; no organicprecipitants shall be used other than methanol, ethanol and isopropanol; in some types aportion of the methyl esters may have been converted to primary amides by treatmentwith ammonia under alkaline conditions. Sulfur dioxide may be added as apreservative.

The commercial product is normally diluted with sugars for standardization purposes.In addition to sugars, pectins may be mixed with suitable food-grade buffer saltsrequired for pH control and desirable setting characteristics. The article of commercemay be further specified as to pH value, gel strength, viscosity, degree of esterification,and setting characteristics.

C.A.S. number 9000-69-5

DESCRIPTION White, yellowish, light greyish or light brownish powder

FUNCTIONAL USES Gelling agent, thickener, stabilizer, emulsifier

CHARACTERISTICS

IDENTIFICATION

Test for pectins Passes testSee description under TESTS

Test for amide group Passes test (amidated pectins only)Add 2 ml of hydrochloric acid and 50 ml of 60% ethanol to 0.5 g of the sample, and stirwell for 20 min. Transfer to a fritted glass filter tube wash with six 10 ml portions ofthe HCl-60% ethanol mixture. Dissolve in 100 ml distilled water; it may be necessaryto add a few drops 0.1 mol/L sodium hydroxide to achieve solution. Transfer 4 ml ofthis solution into a test tube (recommended dimensions 15.5 mm inner diameter and146 mm length). Add 1 ml 5 mol/L sodium hydroxide and mix. The mixture will forma gel. Fill a small glass tube (recommended dimensions 7.8 mm inner diameter and 79mm length) with 2.5 ml boric acid TS and let glide into the test tube. Close withparafilm and incubate overnight at 30o. In case of presence of amide groups theindicator changes its colour from red to green, due to release of ammonia.

PURITY

Loss on drying (FNP 5) Not more than 12% (105o, 2 h)

Sulfur dioxide Not more than 50mg/kgSee description under TESTS

Methanol, ethanol and 2-propanol

Not more than 1% singly or in combinationSee description under TESTS


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PECTINS page 2 (5)

Total insolubles Not more than 3%See description under TESTS

Nitrogen content (FNP 5) Not more than 2.5% oafter washing with acid and ethanol

Galacturonic acid Not less than 65% calculated on the ash-free and dried basisSee description under TESTS

Degree of amidation Not more than 25% of total carboxyl groups of pectinSee description under TESTS

Lead (FNP 5) Not more than 5 mg/kgDetermine using an atomic absorption technique appropriate to the specified level.The selection of sample size and method of sample preparation may be based on theprinciples of the method described in FNP 5, “Instrumental Methods.”

TESTS


Moisten 0.05 g of the sample with 2-propanol. Add 50 ml of water on a magneticstirrer. Adjust pH to 12 using 0.5 mol/L sodium hydroxide and let the solution remainwithout stirring for 15 min. Reduce pH to 7.0 with 0.5 mol/L hydrochloric acid.Adjust to 100.0 ml with water. Make up samples in 1 cm quartz cuvettes as follows:

Buffer pH 7.0 *) Sample soln Water Enzyme soln **)

Enzyme blank 0.5 ml 1.0 ml 1.0 ml -

Sample blank 0.5 ml - 1.5 ml 0.5 ml

Sample 0.5 ml 1.0 ml 0.5 ml 0.5 ml

Test for Pectins

*) Dissolve 6.055 g of tris(hydroxymethyl)aminomethane (e.g. TRIZMA Base,Sigma) and 0.147 g of calcium chloride dihydrate in water to 1 L. Adjust pH to 7.0with 1 mol/L hydrochloric acid**) Dilute pure pectate lyase 1:100 with buffer pH 7.0Shake the solutions well, and measure the absorbance at 235 nm at 0 and 10 min.

Calculations

A0 = absorbance at 0 min = Sample – (enzyme blank + sample blank)A10 = absorbance at 10 min = Sample – (enzyme blank + sample blank)

The amount of unsaturated product produced is proportional to the change inabsorbance (A10 – A0). This value should be greater than 0.023. This distinguishespectins from other gums, which show essentially no change.

PURITY TESTSSulfur dioxide Suspend 100 g of the sample in 500 ml of methanol in a 1000-ml round-bottom flask,

which is provided with a gas inlet tube reaching almost the bottom and connected tothe neck with a reflux condenser. Prepare a glass joint connection from the condenserto an absorption flask or U-tube containing 10 ml of 3% hydrogen peroxide solutionneutralized to methyl red TS. Connect the gas inlet tube with an oxygen-free sourceof carbon dioxide or nitrogen, and maintain a gas stream so as to cause steadybubbling. As soon as the apparatus is flushed free of air, pour 30 ml of hydrochloricacid solution (10 ml conc. HCl + 20 ml H2O) into the reflux condenser, andimmediately connect the absorption flask or U-tube. Heat slowly until methanol startsrefluxing, and reflux gently for 2 h. Disconnect the apparatus and titrate the hydrogenperoxide solution against methyl red TS with 0.01 mol/L sodium hydroxide. Each mlof 0.01 mol/L sodium hydroxide corresponds to 0.32 mg of SO2.

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PECTINS page 3 (5)

Total insolubles Dry a 70 mm glass fiber filter paper (GF/B (Whatman code 1821 070) in an ovenwith fan set at 105º for about 1 h. Transfer the filter paper to a dessiccator containingsilica gel and allow to cool. Weigh the paper (M1). Weigh about 1 g (= S) of thesample into a 250-ml beaker. Add 5 ml of 2-propanol to disperse the sample. Whilestirring magnetically, add 100 ml of 0.03 mol/L sodium hydroxide containing 0.1%(w/w) ethylene diamine tetra-acetic acid (Na salt), which has been filtered throughGF/B paper. Stir for about 30 min at room temperature, then heat to boiling (removeheat if excessive foaming occurs). Filter the hot solution through the glass fiber paperunder vacuum using, e.g. a vacuum filtration kit with 3 piece Hartley funnel (70 cm),with heat resistant plate. Rinse the beaker five times and filter the rinsings with 100ml of warm (about 50º) water that has been filtered through GF/B paper.

Dry the filter paper with the residue at 105º for 1 h. Transfer to desiccator containingsilica gel and leave to cool. Weigh the paper (M2). Calculate the percentage of totalinsolubles from

Total insolubles (%) = [(M2 – M1)/S] x 100

Galacturonic acid andDegree of amidation

Weigh 5 g of the sample to the nearest 0.1 mg, and transfer to a suitable beaker. Stirfor 10 min with a mixture of 5 ml of hydrochloric acid TS, and 100 ml of 60%ethanol. Transfer to a fritted-glass filter tube (30 to 60 ml capacity) and wash with six15-ml portions of the HCl-60% ethanol mixture, followed by 60% ethanol until thefiltrate is free of chlorides. Finally wash with 20 ml of ethanol, dry for 2.5 h in anoven at 105o, cool and weigh. Transfer exactly one-tenth of the total net weight of thedried sample (representing 0.5 g of the original unwashed sample) to a 250-mlconical flask and moisten the sample with 2 ml of ethanol TS. Add 100 ml of recentlyboiled and cooled distilled water, stopper and swirl occasionally until a completesolution is formed. Add 5 drops of phenolphthalein TS, titrate with 0.1 mol/L sodiumhydroxide and record the results as the initial titre (V1).

Add exactly 20 ml of 0.5 mol/L sodium hydroxide TS, stopper, shake vigorously andlet stand for 15 min. Add exactly 20 ml of 0.5 mol/L hydrochloric acid and shakeuntil the pink colour disappears. Titrate with 0.1 mol/L sodium hydroxide to a faintpink colour which persists after vigorous shaking; record this value as thesaponification titre (V2).

Quantitatively transfer the contents of the conical flask into a 500-ml distillation flaskfitted with a Kjeldahl trap and a water-cooled condenser, the delivery tube of whichextends well beneath the surface of a mixture of 150 ml of carbon dioxide-free waterand 20.0 ml of 0.1 mol/L hydrochloric acid in a receiving flask. To the distillationflask add 20 ml of a 1-in-10 sodium hydroxide solution, seal the connections, andthen begin heating carefully to avoid excessive foaming. Continue heating until 80-120 ml of distillate has been collected. Add a few drops of methyl red TS to thereceiving flask, and titrate the excess acid with 0.1 mol/L sodium hydroxiderecording the volume required, in ml, as S. Perform a blank determination on 20.0 mlof 0.1 mol/L hydrochloric acid, and record the volume required, in ml, as B. Theamide titre is (B – S).

Transfer exactly one-tenth of total net weight of the dried sample (representing 0.5 gof the original unwashed sample) and wet with about 2 ml ethanol in a 50-ml beaker.Dissolve the pectin in 25 ml 0.125 mol/L sodium hydroxide. Let the solution standfor 1 h with agitation at room temperature. Transfer quantitatively the saponifiedpectin solution to a 50-ml measuring flask and dilute to the mark with distilled water.Transfer 20.00 ml of the diluted pectin solution to a distillation apparatus and add 20ml of Clark's solution, which consists of 100 g of magnesium sulfate heptahydrateand 0.8 ml of concentrated sulphuric acid and distilled water to a total of 180 ml.This apparatus consists of a steam generator connected to a round-bottom flask towhich a condenser is attached. Both steam generator and round-bottom flask areequipped with heating mantles.

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PECTINS page 4 (5)

Start the distillation by heating the round-bottom flask containing the sample. Collectthe first 15 ml of distillate separately in a measuring cylinder. Then start the steamsupply and continue distillation until 150 ml of distillate have been collected in a200-ml beaker. Add quantitatively the first 15 ml distillate and titrate with 0.05 mol/Lsodium hydroxide to pH 8.5 and record volume required, in ml, as A.

Perform a blank determination on 20 ml distilled water. Record the required volume,in ml, as A0. The acetate ester titre is (A – A0).

Calculate degree of amidation (as % of total carboxyl groups) by the formula:

)()( 0AA- SB + V + V

SB x 100

21 −−

−

Calculate mg of galacturonic acid by the formula:

)]()([ 0AA - SB + V + V x 19.41 21 −−

The mg of galacturonic acid obtained in this way is the content of one-tenth of theweight of the washed and dried sample. To calculate % galacturonic acid on amoisture- and ash-free basis, multiply the number of mg obtained by 1000/x, x beingthe weight in mg of the washed and dried sample.

Note 1: If the pectin is known to be of the nonamidated type, only V1 and V2 need tobe determined and (B – S) may be regarded as zero.

Note 2: For pectins from apple or citrus (A – A0) is usually insignificant incalculating galacturonic acid and degree of amidation.

Note 3: If desired, calculate degree of esterification (as % of total carboxyl groups)by the formula:

)()(

)(

0

0

AA - SB + V + V

AA - V x 10021

2

−−

−

Note 4: If desired, calculate degree of acetate ester (as % of total carboxylic groupsfrom galacturonic acid) by the formula:

)()( 0

0

AA- SB+ V + VAA x 100

21 −−

−

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PECTINS page 5 (5)

Methanol, ethanol and 2-propanol

Weigh 200 mg of urea into a 25-ml amber glass vial (Reacti-flasks, Pierce, Rockford3, USA or equivalent). Purge with nitrogen for 5 min and then add 1 ml of saturatedoxalic acid solution, close with a rubber stopper and swirl. Add 1 ml of a samplesolution (100 mg of sample in 10 ml of water using sodium chloride as a dispersingagent if necessary), 1 ml of internal standard solution (50 mg n-propanol in 1000 mlof water) and simultaneously start a stop watch (T=0). Swirl the vial and recap withan open screw cap fitted with a silicone rubber septum. Swirl until T=30 sec. AtT=45 sec inject through the septum 0.5 ml of an aqueous solution of sodium nitrite(250 g/L). This will convert the alcohols to their corresponding nitrite esters. Swirluntil T=70 sec and, at T=150 sec, withdraw through the septum 1.0 ml of theheadspace using a pressure lock syringe (Precision Sampling Corp., Baton Rouge,Louisiana, USA or equivalent).

Head space gas chromatography: Insert syringe needle in the injection port; pre-compress the sample, then open the syringe and inject the sample. Use the followingconditions:Column:

- length: 90 cm- diameter: 4 mm- material: glass- packing: first 15 cm packed with chrompack (or equivalent) and the

remainder with Porapak R 120-150 mesh (or equivalent)Carrier gas: NitrogenFlow rate: 80 ml/minDetector type: FIDTemperatures- injection port: 250°- column: 150° isothermal

Quantify the methanol, ethanol and 2-propanol present in the sample by comparingthe peak areas with the corresponding peaks obtained by chromatographing theheadspace produced by substituting in the procedure 1 ml of an aqueous solutioncontaining 50 mg/l each of methanol, ethanol and 2-propanol for 1 ml of samplesolution.

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PROCESSED EUCHEUMA SEAWEED page 1 (7)

PROCESSED EUCHEUMA SEAWEED

Prepared at the 57th JECFA (2001) and published in FNP 52 Add 9 (2001),superseding specifications prepared at the 51st JECFA (1998), published in FNP 52Add 6 (1998)). A group ADI “not specified” for carrageenan and processedeucheuma seaweed was established at the 57th JECFA (2001).

SYNONYMS PES, PNG-carrageenan, semi-refined carrageenan; INS No. 407a

DEFINITION A substance with hydrocolloid properties obtained from either Eucheuma cottonii or E.spinosum (from the Rhodophyceae class of red seaweeds). In addition to carrageenanpolysaccharides, processed eucheuma seaweed may contain up to 15% of insolublealgal cellulose and minor amounts of other insoluble matter. Articles of commerce mayinclude sugars for standardization purposes or salts to obtain specific gelling orthickening characteristics. It is distinguished from carrageenan (INS No. 407) by itshigher content of cellulosic matter and by the fact that it is not solubilized andprecipitated during processing.

The functional component of the product obtained from E. cottonii is kappa-carrageenan (a copolymer of D-galactose-4-sulfate and 3,6-anhydro-D-galactose).From E. spinosum it is iota-carrageenan (a copolymer of D-galactose-4-sulfate and 3,6-anhydro-D-galactose-2-sulfate).

Processing consists of soaking the cleaned seaweed in alkali for a short time at elevatedtemperatures. The material is then thoroughly washed with water to remove residualsalts followed by purification, drying, and milling to a powder. Alcohols that may beused during purification are restricted to methanol, ethanol, and isopropanol.

DESCRIPTION Light tan to white coarse to fine powder

FUNCTIONAL USES Thickener, gelling agent, stabilizer, emulsifier

CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Forms cloudy viscous suspensions in water; insoluble in ethanolA 1 g sample disperses and partially dissolves in 100 ml of water at 80o giving acloudy opalescent solution. (The sample disperses in water more readily if firstmoistened with alcohol, glycerol, or a saturated solution of glucose or sucrose inwater).

Test for sulfate Dissolve a 100-mg sample in 20 ml of water. Heat to boiling, cool to roomtemperature, and add 3 ml of barium chloride TS and 5 ml of hydrochloric acid,dilute TS. Filter the mixture. Boil the filtrate for 5 min. A white, crystallineprecipitate appears.

Test for galactose andanhydrogalactose

Proceed as directed under Gum Constituents Identification (FNP 5), using the followingas reference standards: galactose, rhamnose, galacturonic acid, 3,6-anhydrogalactose,mannose, arabinose and xylose. Galactose and 3,6-anhydrogalactose should be present.

Identification of hydrocolloidand predominant type of co-polymer

Add 4 g of sample to 200 ml of water, and heat the mixture in a water bath at 80o, withconstant stirring until dissolved. Replace any water lost by evaporation, and allow thesolution to cool to room temperature. The solution becomes viscous and may form agel. To 50 ml of the solution or gel, add 200 mg of potassium chloride, then reheat, mixwell, and cool. A short-textured ("brittle") gel indicates a carrageenan of apredominantly kappa-type. A compliant ("elastic") gel indicates a predominantly iota-type.

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Infrared absorption Passes testSee description under TESTS

PURITY

Loss on drying (FNP 5) Not more than 12% (105o to constant weight)

pH (FNP 5) Between 8 and 11 (1 in 100 suspension)

Viscosity Not less than 5 cp at 75o (1.5% solution)See description under TESTS

Sulfate Not less than 15% and not more than 40% (as SO42-) on a dry weight basis

See description under TESTS

Total ash Not less than 15% and not more than 30% on a dry weight basisSee description under TESTS


Acid-insoluble matter (FNP 5) Not less than 8% and not more than 15% on a dry weight basisUse 2 g of sample obtained from part (a) of the procedure for sulfate determination

Residual solvents (FNP 5) Not more than 0.1% of ethanol, isopropanol, or methanol, singly or in combinationSee description under TESTS


Initially prepare a 10-1 dilution by adding a 50 g sample to 450 ml of Butterfield'sphosphate-buffered dilution water and homogenizing the mixture in a high speedblender.Total (aerobic) plate count: Not more than 5000 cfu/gSalmonella spp.: Negative per testE. coli: Negative in 1 g

Arsenic (FNP 5) Not more than 3 mg/kgDetermine by atomic absorption hydride technique using a 3 gram sample

Lead Not more than 5 mg/kgSee description under TESTS

Cadmium Not more than 2 mg/kgSee description under TESTS

Mercury Not more than 1 mg/kgSee description under TESTS

TESTS


Infrared absorption Prepare a 0.2% aqueous solution of the sample. Cast films of 0.5 mm thickness(when dry) on a suitable non-sticking surface such as Teflon and obtain the infraredabsorption spectrum of each film. (Alternatively, the spectra may be obtainedusingfilms cast on potassium bromide plates if care is taken to avoid moisture).Iota- and kappa-carrageenan have strong, broad absorption bands, typical of allpolysaccharides, in the 1000 to 1100 cm-1 region. Other characteristic absorptionbands and their intensities relative to the absorbance at 1050 cm-1 are as follows:

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Absorbance Relative to 1050 cm-1Wave number(cm-1)

Molecular Assignment

Kappa Iota

1220-1260928-933840-850800-805

ester sulfate3,6-anhydrogalactose

galactose-4-sulfate3,6-anhydrogalactose-2-

sulfate

0.6-1.00.3-0.60.3-0.50.0-0.2

0.9-1.20.2-0.60.2-0.40.2-0.4

PURITY TESTS

Sulfate Principle: Hydrolysed sulfate groups are precipitated as barium sulfate.

Procedure:(a) Disperse an accurately weighed 8 g sample of commercial product into 400 ml of60% w/w isopropanol/water at room temperature. Stir gently for 4 h. Filter throughash-free filter paper. Discard the filtrate. Wash the material remaining on the filterpaper with two 10-ml portions of 60% isopropanol/water. Dry the material at 105° toconstant weight.

Approximately 1 g of the dried matter is to be used for part (b). The remainder shouldbe retained for determination of Total ash and Acid-insoluble matter.

(b) Accurately weigh a 1 g sample (W1 ) obtained from part (a), Transfer the sampleto a 100-ml long-neck round-bottom flaskand add 50 ml of 0.2 N hydrochloric acid.Fit a condenser, preferably one with at least 5 condensing bulbs, to the flask andreflux for 1 h. Add 25 ml of a 10% (by volume) hydrogen peroxide solution andresume refluxing for about 5 h or until the solution becomes completely clear.Transfer the solution to a 600-ml beaker, bring to a boil, and add dropwise 10 ml of a10% barium chloride solution. Heat the reaction mixture for 2 h on a boiling waterbath. Filter the mixture through ash-free slow-filtration filter paper. Wash withboiling distilled water until the filtrate is free from chloride. Dry the filter paper andcontents in a drying oven. Gently burn and ash the paper at 800° in a tared porcelainor silica crucible until the ash is white. Cool in a desiccator.

Weigh the crucible containing the ash. Calculate the percentage sulfate from theweight in g (W2) of the ash (barium sulfate) using the formula: (W2/W1) x 100 x0.4116.

Total ash Accurately weigh 2 g of the dried sample (W1) obtained from part (a) under theprocedure for Sulfate determination. Transfer to a previously ignited, tared, silica orplatinum crucible. Heat the sample with a suitable infrared lamp, increasing theintensity gradually, until the sample is completely charred; continue heating for anadditional 30 min. Transfer the crucible with charred sample into a muffle furnaceand ignite at about 550o for 1 h. Cool in a desiccator and weigh. Repeat the ignitionin the muffle furnace until a constant weight (W2) is obtained. If a carbon-free ash isnot obtained after the first ignition, moisten the charred spot with a 1 in 10 solution ofammonium nitrate and dry under an infrared lamp. Repeat the ignition step. Calculatethe percentage of total ash of the sample: (W2/W1) x 100.

Retain the ash for the Acid-insoluble ash test.

Viscosity Transfer 7.5 g of the sample into a tared, 600-ml tall-form (Berzelius) beaker, anddisperse with agitation for 10 to 20 min in 450 ml of deionized water. Add sufficientwater to bring the final weight to 500 g and heat in a water bath, with continuousagitation, until a temperature of 80o is reached (20-30 min). Add 7.5 g ofdiatomaceous earth or perlite filter aid.

Stir for two minutes. Add water to adjust for loss by evaporation. Filter the solutionthrough a Büchner funnel (pre-heated with hot water to 80o) equipped with a coarse

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filter paper. Place the filter assembly in a vacuum receiver bottle.

Filter 200 ml of solution. Cool to 76-77o, and heat in a constant temperature bath at75o. Pre-heat the bob and guard of a Brookfield LVF viscometer to approximately75o in water. Dry the bob and guard and attach them to the viscometer, which shouldbe equipped with a No. 1 spindle (19 mm in diameter, approximately 65 mm inlength) and capable of rotating at 30 rpm. Adjust the height of the bob in the samplesolution, start the viscometer rotating at 30 rpm and, after six complete revolutions ofthe viscometer, take the viscometer reading on the 0-100 scale.

If the viscosity is very low, increased precision may be obtained by using theBrookfield UL (ultra low) adapter or equivalent.

Record the results in centipoises, obtained by multiplying the reading on the scale bythe factor given by the Brookfield manufacturer.

Residual solvents Standard Alcohol Solution: Transfer 500 mg each of chromatographic qualitymethanol, ethanol, and isopropanol into a 50 ml volumetric flask. Dilute to volumewith water, and mix. Pipet 10 ml of this solution into a 100-ml volumetric flask.Dilute to volume with water and mix.

TBA Standard Solution: Transfer 500 mg of chromatographic quality tertiary-butylalcohol into a 50-ml volumetric flask. Dilute to volume with water, and mix. Pipet 10ml of this solution into a 100-ml volumetric flask. Dilute to volume with water andmix.

Mixed Standard Solution: Pipet 4 ml each of the Standard Alcohol Solution and ofthe TBA Standard Solution into a 125-ml graduated Erlenmeyer flask. Dilute to about100 ml with water and mix. This solution contains approximately 40 µg of eachalcohol per ml.

Sample Preparation: Disperse 1 ml of a suitable antifoam emulsion, such as Dow-Corning G-10 or equivalent, in 200 ml of water contained in a 1000-ml 24/40 round-bottom distilling flask. Add about 5 g of the sample, accurately weighed, and shakefor 1 h on a wrist-action mechanical shaker. Connect the flask to a fractionatingcolumn, and distil about 100 ml, adjusting the heat so that foam does not enter thecolumn. Add 4.0 ml of TBA Standard Solution to the distillate to obtain the SamplePreparation.

Procedure: Inject 5 µl of the Mixed Standard Solution into a suitable gaschromatograph equipped with a flame-ionization detector and a 1.8-m x 3.2-mmstainless steel column packed with 80-100-mesh Porapak QS or equivalent. Thecarrier is helium flowing at 80 ml per min. The injection port temperature is 200o; thecolumn temperature is 165o; and the detector temperature is 200o. The retention timeof isopropanol is about 2 min, and that of tertiary-butyl alcohol about 3 min.

Measure the areas of the methanol, ethanol, isopropanol, and TBA peaks. Calculateeach response factor, fi, by the formula Ai/ATBA, in which Ai is the area of eachalcohol peak (i=methanol, ethanol, or isopropanol).

Similarly, inject 5 µl of the Sample Preparation, and measure the peak areas,recording the area of each alcohol peak as Ai, and that of the tertiary-butyl alcoholpeak as ATBA. Calculate the concentration of each alcohol (mg/kg) in the sampletaken, by the formula:

Ai · 4000 / fi · ATBA · W

where W is the weight of the sample taken (grams).

Lead Principle: The sample is wet-ashed with nitric and perchloric acids and analysedusing flame atomic absorption spectrophotometry (FNP 5).

Equipment: Atomic absorption spectrophotometer

Reagents:Nitric acid, concentrated, Reagent Grade

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Perchloric acid, concentrated, Reagent GradeHydrochloric acid, concentrated, Reagent GradeLead standard solution (certified)

Solutions:1. Stock solution (1 mg/ml): Dilute an appropriate volume of certified reagent lead

standard solution with distilled and deionized water (D/D water) to make oneliter.

2. Intermediate solutions: (a) 100 µg/ml. Pipet 10 ml of the stock solution into a100-ml volumetric flask and dilute to volume with D/D water. (b) 10 µg/ml.Pipet 10 ml of the 100 µg/ml solution into a 100-ml volumetric flask and diluteto volume with D/D water.

3. Working solutions: Assemble four 100-ml volumetric flasks and transfer tothem (pipet), respectively, 1, 5, 10, and 20 ml of intermediate lead solution (b).Dilute to volume with D/D water to make solutions containing 0.1, 0.5, 1, and 2µg Pb/ml.

Sample preparation: (CAUTION: This procedure employs concentrated oxidizingacids and results in evolution of noxious gases. Perform operations in a fume hood.)

Accurately weigh 7.5 grams of a representative dry powdered test sample into a 250-ml Erlenmeyer flask. Set up a reagent blank and carry through the same operationsas performed on the test sample. Wet the test sample with ca. 10 ml of D/D waterand add 25 ml of nitric acid. Heat gently on a hot plate (100o – 150o) until most ofthe dark fumes are evolved (ca. one hour); swirl the flask occasionally. Cool and add5 ml of perchloric acid; particles become visible at this stage. Heat gently (hot plate,100o – 150o) to concentrate until the solution turns yellowish or colourless (ca. onehour). Midway during the heating, if the solution darkens, slowly add 2-3 mlportions of nitric acid as necessary until the desired colour is achieved; do not let thesolution go to dryness. Cool the digest and wash the sides of the flask with ca. 5 mlof D/D water and swirl. Add 2 ml of hydrochloric acid. Heat again until all brownfumes are evolved and the solution is white to yellowish in colour; do not let thesolution go to dryness. Cool the solution and wash the sides of the flask with ca. 10ml of D/D water. Transfer the slightly viscous solution to a 50-ml volumetric flaskand dilute to volume with D/D water. Filter using two layers of filter paper(Whatman no. 5 or equivalent).

Determination: Set the spectrophotometer to previously established optimumconditions at 283.3 nm using an air/acetylene oxidizing flame. Measure theabsorbance of the sample, blank, and working solutions. Prepare a standard curve byplotting absorbance against :g Pb/ml for the blank and working solutions. Determinethe concentration of lead in the sample solution from the standard curve. Theconcentration of lead in the test sample (mg Pb/kg) is:

[Pb] = FxA/B

where A is the concentration of lead in the sample solution (µg /ml), B is the weightof the test sample (grams), and F is the dilution factor (50 ml).

Cadmium Proceed as directed above for the determination of lead, using 228.8 nm as theanalysis wavelength. Intermediate and working solutions are prepared from certifiedreagent cadmium standard solution as follows:

Intermediate solutions: (a) 100 µg/ml. Pipet 10 ml of the stock solution (1mg/ml)into a 100-ml volumetric flask and dilute to volume with distilled and deionized(D/D) water. (b) 10 µg/ml. Pipet 10 ml of solution (a) into a 100-ml volumetricflask; dilute to volume with D/D water. (c) 1 µg/ml. Pipet 1 ml of solution (a) into a100-ml volumetric flask; dilute to volume with D/D water.

Working solutions: Assemble five 50-ml volumetric flasks and transfer to them(pipet), respectively, 0.5, 2.5, 5.0, 10, and 20 ml of intermediate solution (c). Diluteto volume with D/D water to make solutions containing 0.01, 0.05, 0.1, 0.20, and0.40 µg Cd/ml.

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The concentration of cadmium in the test sample (mg Cd/kg) is:

[Cd] = FxA/B

where A is the concentration of cadmium in the sample solution (µg /ml), B is theweight of the test sample (grams), and F is the dilution factor (50 ml).

Mercury Principle: The sample is wet-ashed with nitric and perchloric acids and analysedusing hydride-generation atomic absorption spectrophotometry (FNP 5).

Equipment:

Atomic absorption spectrophotometer equipped with a hydride vapour generator.Integral to the generator is a reactor tube or coil and a peristaltic pump with dualtubing channels: one channel for the sample solution and one for the two reagentsolution tubes. Flow control is determined by tubing size and tubing clamps. Flowrates are measured at the exit of the hydride generator.

Reagents:Nitric acid, concentrated, Reagent GradePerchloric acid, concentrated, Reagent GradeHydrochloric acid, concentrated, Reagent GradeSodium borohydride, >98%Sodium hydroxide, Reagent gradeMercury standard solution (certified)

Solutions:1. Nitric acid-perchloric acid (1:1): Mix equal volumes of the two acids.2. Hydrochloric acid, 5M: Dilute 417 ml concentrated hydrochloric acid to 1 liter

with deionized water.3. Sodium borohydride solution, 0.4% (Prepare immediately before use.): First,

dissolve 2.5 g sodium hydroxide in deionized water. Then, add and dissolve 2.0g sodium borohydride. Dilute to 500 ml.

4. Stock solution (1 mg/ml): Dilute an appropriate volume of certified reagentmercury standard solution with distilled and deionized water (D/D water) tomake one liter.

5. Intermediate solutions: (a) 10,000 µg/l. Pipet 1 ml of the stock solution into a100-ml volumetric flask and dilute to volume with D/D water. (b) 100 µg/l.Pipet 1 ml of the 10,000 :g/l solution into a 100-ml volumetric flask and dilute tovolume with D/D water.

6. Working solutions: Assemble five 100-ml volumetric flasks and transfer to them(pipet), respectively, 1, 5, 10, 15, and 20 ml of intermediate solution (b). Toeach, add 10 ml of 1:1 nitric acid-perchloric acid and dilute to volume with D/Dwater to make solutions containing 1, 5, 10, 15, and 20 µg Hg/l.

Sample preparation: (CAUTION: This procedure employs concentrated oxidizingacids and results in evolution of noxious gases. Perform operations in a fume hood.)Accurately weigh 5 grams of a representative dry powdered test sample into a 250 mlErlenmeyer flask. Set up a reagent blank and carry through the same operations asperformed on the test sample. Wet the test sample with 5 ml of D/D water and thenadd 10 ml of 1:1 nitric acid-perchloric acid. Heat gently on a hot plate (100o-150o)until all of the dark fumes are evolved and the solution turns yellowish or colourless;swirl the flasks occasionally. Do not let the solution go to dryness. Cool and washthe sides of the flask with a small amount of D/D water. (Some particles may bevisible.) Cover the flask lightly and let the slightly viscous solution stand overnight.Transfer the solution to a 50-ml volumetric flask and dilute to volume with D/Dwater. Filter using 2 layers of Whatman no. 5 (or equivalent) filter paper into a 100-ml Erlenmeyer flask. Immerse the flask in an ultrasonic bath and sonicate it for 10minutes or until bubbles no longer form on the surface of the solution.

Determination: Calibrate (using water) the peristaltic pump to provide a flow rate ofthe sample solution of 8 ml/min and a combined flow rate for the two reagentsolutions (sodium borohydride and 5M hydrochloric acid) of 2 ml/min. (The

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combined flow rate is achieved with a single pump setting.)

Set the spectrophotometer to previously established optimum conditions at themercury lamp wavelength of 253.7 nm.

Transfer suitable quantities of the two reagent solutions into separate graduatedcylinders. Insert separate aspirator tubing leading from the peristaltic pump into eachreagent solution and into the sample flask.

Start the flow of argon carrier gas (tank outlet pressure: 3.2±0.2 kg/cm2) through thehydride vapour generator of the spectrophotometer. Start the pump to initiate flow ofthe three solutions into the hydride generator manifold where they are mixed and passinto the reactor coil to generate atomic mercury, which is carried into the absorbancecell of the spectrophotometer. Measure the absorbance for the sample. Repeat forthe blank solution and each of the working standards.

Prepare a standard curve by plotting absorbance against µg Hg/l for the blank andworking solutions. Determine the concentration of mercury in the sample solutionfrom the standard curve. The concentration of mercury in the test sample (mg Hg/kg)is:

[Hg] = FxA/1000B

where A is the concentration of mercury in the sample solution (µg /l), B is theweight of the test sample (grams), and F is the dilution factor (50 ml).

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QUILLAIA EXTRACTS page 1 (4)

QUILLAIA EXTRACTS(Tentative)

Prepared at the 57th JECFA (2001) and published in FNP 52 Add 9 (2001),superseding specifications prepared at the 55th JECFA (2000) and published in FNP52 Add 8 (2000) . An ADI of 0-5mg/kg bw established at the 29th JECFA (1985)which was made temporary at the 57th JECFA (2001) pending clarification of thespecifications.

Information required on: minimum and maximum percentages of saponins inunpurified extracts and in semi-purified extracts; typical saponin content ofunextracted inner bark; ash content of semi-purified extract; tannins content of semi-purified extract; comments on other sections of the monograph are also invited.

SYNONYMS Quillaja extracts, Soapbark extracts, Quillay bark extracts, Bois de Panama, Panamabark extracts, Quillai extracts; INS No. 999

DEFINITION Obtained by aqueous extraction of the milled inner bark or of the wood of pruned stemsand branches of Quillaja saponaria Molina (family Rosaceae). The unpurified quillaiaextracts (QE) contain over 60 triterpenoid saponins (QS) consisting predominantly ofglycosides of quillaic acid. Polyphenols and tannins are also major components.Some sugars and calcium oxalate will also be present.Quillaic acid (CAS no. 631-01-6) is the aglycone common to all the saponins in QE.Different oligosaccharide substituents are substituted at C-3 and C-28 of the quillaicacid moiety. The first sugar residue of the C-28 oligosaccharide may be acylated. Thesugar residues constituting the oligosaccharides include glucose, glucuronic acid,galactose, fucose, arabinose, rhamnose, and xylose.Freshly prepared unpurified QE contain 190-200 g of QS/kg of solids, whereas freshlyprepared semi-purified QE generally contain 750-800 g of QS/kg of solids. Bothunpurified and semi-purified QE are available commercially as aqueous extracts or asspray-dried powders that may contain carriers such as lactose or maltodextrin. Theliquid extracts are usually preserved with sodium benzoate or ethanol; sulfur dioxidehas also been used. The principal saponin component of commercial unpurified QE isdesignated as QS-18. (“Highly purified” QE, which are not specified by thismonograph, are typically used as adjuvants in human and animal vaccines)

Formula weight Monomeric saponins range from ca. 1800 to ca. 2000, consistent with a triterpenewith 8-10 monosaccharide residues

Assay Information required on minimum and maximum percentages of saponins inunpurified extracts and in semi-purified extracts.

DESCRIPTION Unpurified liquid extract has a red-brownish colour; the powder form is light brownwith a pink tinge. The semi-purified liquid or powder product has a light colour.

FUNCTIONAL USES Emulsifier, foaming agent.

CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Very soluble in water, insoluble in ethanol, acetone, methanol, and butanol

Foam Dissolve 0.5 g of powder extract in 9.5 g of water or 1 ml of liquid extract in 9 ml ofwater. Add 1 ml of this mixture to 350 ml of water in a 1000-ml graduated cylinder.Cover the cylinder, vigorously shake it 30 times, and allow settling. Record the foamlevel (ml) after 30 min. Typical values are 150 ml of foam.

QS-18 Saponin Determine as in Method of Assay. The major peak of the sample is compared to theQS-18 peak of the standard.

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Colour and Turbidity Powder form only: Dissolve 0.5 g in 9.5 g of water. The solution must be free of anyvisible aggregates. Determine the solution absorbance against water, at 520 nm.Maximum acceptable levels are 1.2 absorbance units.

PURITY

Water (FNP 5) Powder form: not more than 6% (Karl Fischer Method)

Loss on drying (FNP 5) Liquid form: 50 to 70% (2 g, 105°, 5 h).

pH (FNP 5) 4.2 –5.5 (4% solution)

Ash (FNP 5) Unpurified extract: not more than 14% on a dried basis (use 1.0 g for powdersamples; for liquid samples, use the residue from loss on drying).

Tannins Not more than 8% on a dried basis. Information required on tannins content of semi-purified extract.See description under TESTS

Lead Not more 2 mg/kg.Determine using atomic absorption technique appropriate to the specified level. Theselection of the sample size and method of sample preparation may be based on theprinciples of the method described in FNP 5, “Instrumental Methods”.

TESTS

PURITY TESTS

Tannins Weigh either 3.0 g of the powder form or an equivalent amount of liquid sample,accounting for solids content determined from loss on drying. Dissolve in 250 ml ofwater. Adjust the pH to 3.5 with acetic acid. Dry 25 ml of this solution at 105° for 5h and determine the weight of the dried solid, in g (Wi). Mix 50 ml of the solutionwith 360 mg of polyvinyl polypyrrolidone. Stir the solution for 30 min at roomtemperature; then centrifuge at 800 x g. Recover the supernatant and dry thissolution at 105o (5 h). Weigh the recovered solid (Wf , in g). The percentage oftannins in the sample is:

% tannins (dry basis) = 100 x (Wi - Wf/2) / Wi

METHOD OF ASSAY Sample preparation:Powders: Weigh 0.5 g of sample and dissolve in 9.5 g of water. Filter through a 0.2µm filter.Aqueous extracts (~ 550 mg solids/ml): Weigh 1 g of sample and dilute with 9 g ofwater. Filter through a 0.2 µm filter.In either case, the sample volume is ca. 10 ml.

Standard preparation:Weigh 1.5 g of purified saponins (SuperSap, Natural Response, Chile; Quil-A,Superfos, Denmark or similar, containing at least 90% saponins by weight) anddissolve in 100 ml of water. Filter through a 0.2 µm filter.

High performance liquid chromatography (HPLC):Reverse phase HPLC conditions:Column: Vydac 214TP54 or similar, 4.6 x 250 mm length, 5 µm poreColumn temperature: room temperaturePump: Linear gradient

Solvent A: 0.15% trifluoroacetic acid in HPLC-grade water.Solvent B: 0.15% trifluoroacetic acid in HPLC–grade acetonitrile.

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Gradient: Time(min) % solvent A % solvent B0 70 3040 55 4545 70 30

Flow rate: 1 ml/minDetection wavelength: 220 nmInjection volume: 20 µl

Calculation:The concentration of saponins, Csap, in mg/ml, in the solution prepared as directedunder sample preparation is:

Csap= (Asample/Astandard)CStandard

where CStandard ( mg/ml) is the saponins concentration of the standard injected (e.g.,CStandard = 13.5 mg/ml if the saponin content of 1.5 g of standard sample is 90 %)and Asample and Astandard are the sums of the peak areas attributed to the saponins in thesample preparation and in the standard preparation, respectively. (Tannins andPolyphenols will elute before the saponins. The peaks due to the saponins willappear after the major peak due to the polyphenols – see figure.)The percentage of saponins in the test sample is:

% Saponins = 100 x Csap/(0.1Wsample)

where Wsample is the weight of the sample (mg) taken for the sample preparation and0.1 is the inverse of the sample volume, 10 ml.

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Example chromatograms:A. Unpurified QE (55 mg solids/ml). The peak labeled QS-18 is the dominantsaponin in QE extract.

B. Chromatogram of highly purified saponins (15 mg/ml)

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SMOKE FLAVOURINGS page 1 (5)

SMOKE FLAVOURINGS

Prepared at the 57th JECFA (2001) and published in FNP 52 Add. 9 (2001),superseding tentative specifications prepared at the 55th JECFA (2000) andpublished in FNP 52 Add. 8 (2000). An ADI of “Provisional acceptance” wasestablished at the 31st JECFA (1987).

SYNONYMS Wood smoke flavour, Smoke condensate

DEFINITION Complex mixtures of components of smoke obtained by subjecting untreatedhardwoods to (a) pyrolysis in a limited and controlled amount of air, (b) dry distillationbetween 200o and 800o, or (c) superheated steam between 300o and 500o. Sourcematerials must not contain detectable amounts of pesticides, wood preservatives, orother extraneous matter that may result in hazardous constituents in the wood smoke.The major flavouring principles of Smoke Flavourings are carboxylic acids,compounds with carbonyl groups and phenolic compounds.

During manufacture, wood smoke is subjected to an aqueous extraction system or todistillation, condensation, and separation for collection of the aqueous phase, whichserves to remove hazardous constituents, such as polycyclic aromatic hydrocarbons.The aqueous smoke fraction containing water-soluble constituents may be diluted withwater or be extracted with an edible vegetable oil to produce a smoke flavouring withhigher levels of non-polar constituents that may be further extracted using food-gradesubstances, such as propylene glycol or aqueous solutions of polysorbates.

Commercial products may also contain additives such as emulsifiers, antifoamingagents, and gums. Smoke flavourings may also be prepared in dry form with theaddition of carriers, such as yeasts, flours, salt, phosphates, carbohydrates, and anti-caking agents.

These specifications apply only to the water-soluble distillates of condensed woodsmoke, their aqueous/vegetable oil or polysorbate extracts and concentrates of these.These specifications do not apply to products derived from the water-insoluble tars, tocommercial products( as described in the previous paragraph), nor to pyroligneous acid,a by-product of the manufacture of charcoal by carbonation of wood in the absence ofair.

Assay Acidity: 2 to 20% (as acetic acid)Carbonyls: 2 to 25% (as heptaldehyde)Phenols: 0.1 to 16% (as 2,6-dimethoxyphenol)

DESCRIPTION Light brown to dark amber liquids; smoky odour

FUNCTIONAL USES Flavouring agent, colour

CHARACTERISTICS

IDENTIFICATION

Appearance and odour Characteristic

PURITY

Benzo(a)pyrene Not more than 2 µg/kgSee description under TESTS

Lead (FNP 5) Not more than 2 mg/kgDetermine using an atomic absorption technique appropriate to the specified level.

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The selection of sample size and method of sample preparation may be based on theprinciples of the method described in FNP 5, “Instrumental Methods.”

TESTS

PURITY TESTS

Benzo(a)pyrene Caution: Benzo(a)pyrene and other polycyclic aromatic hydrocarbons are knowncarcinogens. The analyst must exercise appropriate care in handling them.

Principle: Benzo(a)pyrene (BaP) is one of several polycyclic aromatic hydrocarbons(PAHs) that may occur in liquid smoke flavourings. Its quantitation is used as anindicator for levels of PAHs in liquid smoke flavourings. BaP, as well as other PAHsare isolated from the sample by digestion and liquid extraction, and purified by solidphase extraction. Quantitation is accomplished by high performance liquidchromatography with fluorescence detection (FNP 5).

Apparatus:− Liquid chromatograph with fluorescence detector and reverse-phase column,

such as Vydac 201TP54, 4.6 x 250 mm, thermostated at 30E− Digestion apparatus consisting of 250 ml round-bottom flask, 250 ml heating

mantle, reflux condenser, and variable transformer− Rotary evaporator, equipped with water bath set at 40E− Pear-shaped flasks, 50 ml and 100 ml− 30 ml Buchner funnels with coarse-porosity fritted disks− Silica solid phase extraction (SPE) column, 6 ml capacity, 1000 mg packing,

such as Bakerbond− C18 SPE column, 6 ml capacity, 1000 mg packing, such as Bakerbond− Stopcocks with Luer fitting (for SPE columns)− PTFE syringe filter units, 13 mm diam., 0.45 micrometer porosity

Reagents:− UV- or HPLC-grade hexane, methylene chloride, acetonitrile, and water− Anhydrous ethanol, distilled before use− Sodium sulfate, anhydrous, granular

Solutions:− 0.8 g/ml aqueous potassium hydroxide− Commercial PAH Standard Solution in acetonitrile, such as NIST Standard

Reference Material 1647 (National Institute of Standards and Technology,Gaithersburg, MD 20899, USA)

− PAH working standards: prepare at least 4 working standards in 50%acetonitrile/50% water (in the range of 0.5 to 10 µg/l) from the commercialPAH Standard Solution.

Procedure: Caution: Due to the toxicity of solvents used in this method, the use ofgloves is recommended.

Sample preparation: Weigh 10 g of liquid smoke flavouring into a 250 ml round-bottom flask. Add 20 ml ethanol, 2 ml 0.8 g/ml aqueous KOH solution, and a fewboiling chips. Assemble the digestion apparatus, set the variable transformer to 50%output, and reflux the sample for 2 hr. Let cool about 15 min. Transfer the digest toa 250 ml separatory funnel; rinse the flask with 20 ml water, 10 ml ethanol, and 15ml hexane and add to the separatory funnel; extract by shaking gently for 2 min.Drain the lower layer into a second separatory funnel and repeat the extraction with15 ml hexane. Discard the lower layer. To each retained hexane layer add about 3ml water and swirl. Discard the water washes. Pass each hexane layer through aBuchner funnel containing 25 g sodium sulfate (pre-washed with 15 ml hexane) intoa 100 ml pear-shaped flask. Rinse the sodium sulfate with 15 ml hexane; applygentle pressure to the top of the funnel with heel of hand to force residual solvent

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through the sodium sulfate. Concentrate to about 1 ml on a rotary evaporator.Attach a stopcock to the outlet of the silica SPE column and condition the columnwith 15 ml methylene chloride, followed by 3 ml hexane; close the stopcock. (Ifthere is a delay between column conditioning and charging the column with thesample, close the stopcock, leaving about 1 mm hexane above the head of thecolumn. Just before loading the sample extract onto the column, open the stopcockto drain the excess solvent; then, close the stopcock.) Transfer the concentratedsample extract from the pear-shaped flask to the column, using two 1 ml portions ofhexane to rinse. Open the stopcock and allow the sample to pass onto the columnusing gravity flow only, discarding the eluate. Elute the sample (by gravity) with 5ml of 25% methylene chloride/75% hexane, discarding the first milliliter; collect theeluate in a 50 ml pear-shaped flask. Use pressure from a syringe to force residualsolvent through the column. Add 4 ml acetonitrile and concentrate the sample extractto < 1 ml on a rotary evaporator.

Attach a stopcock to the outlet of the C18 column and condition it with 15 ml ofmethylene chloride, followed by 5 ml acetonitrile. Close the stopcock. Transfer theconcentrated sample extract to the column using two 0.5-ml portions of acetonitrile torinse the flask. Open the stopcock to charge the column with the sample; discard theeluate. Elute the sample with 5 ml of 10% methylene chloride/90% acetonitrile,collecting the eluate in a 50 ml pear-shaped flask. Use a syringe to force residualsolvent through the column. Concentrate the eluate to < 1 ml on a rotary evaporator.Transfer to a 5 ml volumetric flask, using three 0.5 ml portions of acetonitrile torinse. Add 2.5 ml water, and dilute to 5.0 ml with acetonitrile. Filter through a PTFEsyringe filter.

High Performance Liquid Chromatography: Analyse the filtered sample extract andthe PAH working standards for BaP.Chromatographic conditions:− Solvent flow rate: 1.0 ml/min− Solvent program: 3 min hold at 50% acetonitrile/50% water; linear gradient to

100% acetonitrile in 15 min; and 8 min hold at 100% acetonitrile− fluorescence detector: excitation wavelength - 290 nm; emission wavelength -

410 nm− Injection volume: 100 µl

The retention time of BaP is approximately 24 min. Using the peak heights for BaPin the standards, prepare a calibration curve of peak height vs. concentration (µg/l),and determine the slope (S) and the intercept (I). Calculate the concentration of BaP:

BaP (µg/kg) = V(H-I)/(S x W)where

H = the peak height of BaP in the sample extractW = the weight of the sample (10 g)V = the volume of the filtered sample extract (5.0 ml).

METHOD OF ASSAYAcidity Accurately weigh about 1 ml of sample in a 250 ml beaker. Dilute with about 100 ml

of water. Titrate with 0.1 N sodium hydroxide solution to an equivalence point ofpH 8.15, as determined using a pH meter. Calculate acidity as percent by weight ofacetic acid using the factor: 1 ml of 0.1 N sodium hydroxide is equivalent to 60.05mg acetic acid.

Carbonyls Principle: The total carbonyls of Smoke Flavourings are determinedspectrophotometrically by reaction with 2,4-dinitrophenylhydrazine (2,4-DNPH) andexpressed as heptaldehyde. The carbonyls of liquid smoke are converted tohydrazone derivatives by reaction with 2,4-DNPH in acid medium at 60o. A redpigment is formed on adjusting to alkaline pH and the absorbance is read at 430 nm.

Apparatus: Spectrophotometer with 1 cm cuvettes, water bath at 60±5o, 25 ml

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volumetric flasks, miscellaneous glassware.

Reagents:− Toluene− Ethanol (anhydrous): Render carbonyl-free by adding 1% 2,4-DNPH, a few

drops of concentrated HCl, refluxing 3 h and distilling.− 2,4-DNHP: Recrystallize from carbonyl-free methanol.− Potassium hydroxide pellets (KOH)− Heptaldehyde− Trichloroacetic Acid (TCA)

Solutions:1. Saturated 2,4 -DNPH: 0.05% in toluene. Shake for 1 h or prepare 1 day in

advance and allow to settle overnight. Insoluble crystals of 2,4-DNPH should bepresent. Filter the upper layer prior to use. Prepare fresh weekly.

2. KOH solution: 4% w/v in carbonyl-free ethanol. Prepare fresh daily.3. TCA solution: 4% w/v in toluene. Stable at room temperature.4. 0.1% Smoke Flavouring, prepared as follows: 1 ml or 1 gram sample dissolved

or diluted to 50 ml with carbonyl-free alcohol of which 5 ml is diluted to 100 mlwith a 10% carbonyl-free ethanol - 90% toluene solution.

5. Heptaldehyde standard solution: 30 µg/ml in toluene.

Procedure: Place 1 ml of diluted sample (Solution 4) in a 15 ml volumetric flask and1 ml toluene in another flask to serve as the blank.

Add to each volumetric flask:− 1 ml toluene− 2 ml saturated 2,4-DNPH solution (Solution 1)− 2 ml TCA solution (Solution 3)

Cover with glass stoppers and heat for 30 min at 60o. Immediately cool in an ice bath.Add 5 ml of KOH solution (Solution 2) and dilute to 25 ml with carbonyl-freeethanol. Allow colour to develop exactly 10 min after addition of Solution 2, thenread absorbance at 430 nm. Correct absorbance for the blank.

Construct a calibration curve using the standard Heptaldehyde solution (solution 5) inthe range of 1-30 µg/ml plotting absorbance at 430 nm versus concentration.

Calculate % Carbonyls (as heptaldehyde) from the calibration curve, correcting fordilution of the sample.

Phenols Principle: Phenolic compounds can be determined spectrophotometrically afterreacting with 2,6-Dibromo-N-chloro-p-benzoquinoneimine (BQC) in a basic buffer.The method cannot differentiate between phenolic compounds but gives reproducibleresults expressed as 2,6-dimethoxyphenol (2,6-DMP). A solution of sample is reactedwith BQC reagent in a basic borate buffer to form indophenols, which have a bluecolour. The colour developed is quantitated at 610 nm using a standard curveprepared with 2,6-DMP.

Apparatus:− Spectrophotometer with 1 cm cells− 100 ml volumetric flasks− Centrifuge− Assorted glassware

Reagents:− Cupric sulfate (CuSO4⋅5H2O)− Sodium borate (Na2B4O7⋅10H2O)− Sodium hydroxide

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− 2,6-Dibromo-N-chloro-p-benzoquinoneimine− 2,6-Dimethoxyphenol− 1-Butanol− Methanol

Solutions:1. 0.05% w/v CuSO4⋅5H2O in water.2. 24.8 g Na2B407⋅10H2O dissolved in 900 ml water. Adjust pH to 9.8 with sodium

hydroxide TS and add water to 1,000 ml volume.3. 40 mg BQC dissolved in 10 ml methanol. (Prepare fresh daily.)4. 2,6-Dimethoxyphenol in water, 20 µg/ml.5. 0.2% Smoke Flavourings in water.

Procedure: Place 5 ml of diluted sample solution (Solution 5) in one test tube and 5ml of water in another test tube to serve as the blank. Then add to each tube:− 1 ml of cupric sulfate solution (Solution 1)− 5 ml of borate buffer (Solution 2)− 4 drops of BQC reagent (Solution 3)

Cover each tube, shake vigorously, and allow colour development in the dark forexactly 10 min. Add 10 ml of 1-butanol to each test tube, cover and invert 6 to 8times (do not shake). Centrifuge test tubes for 5 min at 700 rpm.

Measure the absorbance of the sample at 610 nm and correct for the blank.Construct a calibration curve using the standard 2,6-DMP solution (Solution 4) in therange of 1-20 µg/ml, plotting absorbance at 610 nm versus concentration.

Calculate percent Phenols Content (as 2,6-DMP) from the calibration curve,correcting for dilution of the sample.

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SODIUM CALCIUM POLYPHOSPHATE page 1 (1)

SODIUM CALCIUM POLYPHOSPHATE


SYNONYMS Sodium calcium polyphosphate, glassy; INS No. 452 (iii)

DEFINITION

Chemical names Sodium calcium polyphosphate

Chemical formula (NaPO3)n ⋅ CaO where n is typically 5

Assay Not less than 61% and not more than 69 % expressed as P2 O5 on dried basis

DESCRIPTION White glassy crystals, spheres


CHARACTERISTICS

IDENTIFICATION

Test for sodium (FNP 5) Passes test

Test for calcium (FNP 5) Passes test


PURITY


Lead (FNP 5) Not more than 4 mg/kgDetermine using an atomic absorption technique appropriate to the specified level.The selection of sample size and method of sample preparation, may be based on theprinciples of the method described in FNP 5, “Instrumental Methods”.

Fluoride (FNP 5) Not more than 10 mg/kgMethod III; use an appropriate sample size and appropriate volumes of standardsolution for construction of the calibration curve.

METHOD OF ASSAY Weigh accurately about 200 mg of the sample, dissolve in 25 ml of water and 10 mlof diluted nitric acid TS and boil for 30 min. Filter if necessary, and wash anyprecipitate, then dissolve the precipitate by the addition of 1 ml diluted nitric acid TS.Adjust the temperature to about 50o , add 75 ml of ammonium molybdate TS, andmaintain the temperature at about 50o for 30 min, stirring occasionally. Allow tostand for 16 h or overnight at room temperature. Decant the supernate, through afilter paper, wash the precipitate once or twice with water by decantation using 30 to40 ml each time, and pour the washings through the same filter. Transfer theprecipitate to the same filter, and wash with potassium nitrate solution (1 in 100) untilthe filtrate is no longer acid to litmus paper. Transfer the precipitate with filter paperto the original precipitation vessel, add 50.0 ml of 1N sodium hydroxide, agitate untilthe precipitate is dissolved, add 3 drops of phenolphthalein TS and titrate the excessalkali with 1N sulfuric acid. Each ml of 1N sodium hydroxide consumed isequivalent to 3.088 mg of P2O5.

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SODIUM SULPHATE page 1 (1)

SODIUM SULPHATE

Prepared at the 55th JECFA (2000), maintained at 57th JECFA and published inFNP 52 Add 9 (2001). ADI“not specified” was established at the 57th JECFA(2001).

SYNONYMS Glauber’s salt (decahydrate from); INS No. 514

DEFINITION

C.A.S. number 7757-82-6 (Anhydrous)7727-73-3 (Decahydrate)

Chemical formula Na2SO4 · xH2O (x = 0 or 10)

Formula weight 142.04 (Anhydrous)322.19 (Decahydrate)

Assay Not less than 99.0 % on the dry basis

DESCRIPTION

FUNCTIONAL USES Colour adjuvant

CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Freely soluble in water; practically insoluble in ethanol

Test for sodium (FNP 5) Passes Test

Test for sulfate (FNP 5) Passes Test

PURITY

Loss on drying (FNP 5) Anhydrous: Not more than 1% (105°, 4 h)Decahydrate: Between 51.0% and 57.0% (105°, 4h)

Lead (FNP 5) Not more than 2 mg/kgDetermine using an atomic absorption technique appropriate to the specified level.The selection of sample size and method of sample preparation, may be based on theprinciples of the method described in FNP 5, “ Instrumental Methods”.

Selenium (FNP 5) Not more than 30 mg/kgTest 0.2 g of the sample as directed in the Limit Test (Method II)

METHOD OF ASSAY Weigh accurately about 0.5 g of the dried sample, dissolve in 200 ml of water, add 1ml of hydrochloric acid and heat to boiling. Gradually add, in small portions andwhile stirring constantly, an excess of hot barium chloride TS (about 10 ml), and heatthe mixture on a steam bath for 1 h. Collect the precipitate on a filter, wash until freefrom chloride, dry, ignite and weigh. The weight of the barium sulfate so obtained,multiplied by 0.6086 corresponds to the equivalent amount of Na2SO4.

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d-TAGATOSE page 1 (2)

D-TAGATOSE

Specifications prepared at the 55th JECFA (2000), maintained at 57th JECFA andpublished in FNP 52 Add 9 (2001). An ADI of 0-80 mg/kg bw was established at the57th JECFA (2001).

SYNONYMS D-lyxo-Hexulose

DEFINITION D-Tagatose is a ketohexose, an epimer of D-fructose inverted at C-4, with a sweet taste.It is obtained from D-galactose by isomerization under alkaline conditions in thepresence of calcium.

Chemical names D-Tagatose

C.A.S. number 87-81-0

Chemical formula C6H12O6

Structural formula CH2OH ||

C = O ||HO−−C−−H ||HO−−C−−H || H−−C−−OH || CH2OH


Assay Not less than 98% on the dry basis

DESCRIPTION Virturally odourless, white or almost white crystals

FUNCTIONAL USES Sweetener, texturizer, stabilizer, humectant, formulation aid

CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Very soluble in water, very slightly soluble in ethanol

Specific rotation (FNP 5) [α]20D : -4 to -5.6° (1% aqueous solution)

Melting rannge (FNP 5) 133 − 137°

Reaction with alkalinecupric tartrate

Proceed as directed for the measurement of reducing sublstances (Method II). Acopious red precipitate of cuprous oxid is formed.

Chromatography The retention time for the major peak in the chromatogram of the sample solutioncorresponds to that for D-tagatose in the chromatogram of reference standard D-tagatose (available from Arla Foods Ingredients amba, Skanderborgvej 277, 8260Viby, Denmark) using the conditions described in the METHOD OF ASSAY.

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d-TAGATOSE page 2 (2)

PURITY

Loss on drying (FNP 5) Not more than 0.5% (102°, 2 h)

Lead (FNP 5) Not more than 1mg/kgDetermine using an atomic absorption technique appropriate to the specified level. Theselection of sample size and method of sample preparation may be based on theprinciples of the method described in FNP 5, “Instrumental methods”.

Total ash (FNP 5) Not more than 0.1%

METHOD OF ASSAY Determined by liquid chromatography (FNP5) using the following procedure.

Preparation of sample solution: Weigh accurately about 50 mg of dry sample into a10-ml volumetric flask and add about 8 ml of purified, deionized water. Bring sampleto complete dissolution and dilute to mark with purified deionized water. Filterthrough a 0.2 µm filter.

Preparation of reference solution: Use dry standard D-tagatose. Prepare a solution ofthe reference material as described for the sample solution.

Apparatus: Liquid chromatograph equipped with a refractive index detector and anintegrator.

Conditions:Column: Biorad Aminex HPX-87C (length 30 cm, diameter 7.8 mm, particle size 9µm) or equivalentColumn temperature: 85°Mobile phase: Deionized water with 50 ppm calcium acetateFlow rate: 0.6 ml/minInjection volume: 20 µl

Procedure: Separately inject equal volumes of the sample solution and the referencesolution into the chromatograph. Record the chromatograms and measure theresponse of D-tagatose peak. Calculate the content of D-tagatose in the samplesolution by the following formula:

% D-Tagatose = 100 (AS/AR) (WR/WS)

WhereAS = Peak area of sample solutionAR = Peak area of reference solutionWS = Weight of dry sample (mg)WR = Weight of dry reference standard (mg)

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TAGETES EXTRACT page 1 (2)

TAGETES EXTRACT

Prepared at the 57th JECFA (2001) and published in FNP 52 Add 9 (2001),superseding tentative specifications prepared at the 55th JECFA (2000) andpublished in FNP 52 Add 8 (2000). No ADI was allocated at the 31st JECFA (1987).

SYNONYMS Xanthophylls

DEFINITION The major colouring principles are lutein and its dipalmitate (helenien), obtained byhexane extraction of dried petals of Tagetes erecta L. with subsequent removal of thesolvent. Other hydroxy derivatives of carotenes may be present together with otheroxyderivatives such as epoxides; may contain fats, oils and waxes naturally occurringin the plant material. Products of commerce are normally further formulated e.g. in orderto standardise the colour content or to obtain water soluble/dispersable products.

Chemical names Lutein: β,ε-Carotene-3,3'-diol,Helenien: Lutein dipalmitate; β,ε-Carotene-3,3'-diol dipalmitate

C.A.S. number 127-40-2 (Lutein)

Chemical formula Lutein: C40H5602

Helenien: C72H11604

Structural formulaCH3

H3C CH3

CH3

CH3

CH3 CH3RO

H3C CH3

ORH3C

Lutein: R = HHelenien: R = CH3(CH2)14CO

Formula weight Lutein: 568.88Helenien: 1045.71

Assay Content of total colouring matter (calculated as lutein) not less than declared

DESCRIPTION Dark yellow-brown liquid


CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Insoluble in water; soluble in hexane

Spectrophotometry An acetone solution of the sample shows maximum absorption at about 444 nm

Positive test for carotenoids The colour of a solution of the sample in acetone disappears after successive additionof a 5% solution of sodium nitrite and 0.5 M of sulfuric acid.

PURITY

Residual solvent (FNP 5) Hexane: not more than 50 mg/kg

Lead (FNP 5) Not more than 2 mg/kgDetermine using an atomic absorption technique appropriate to the specified level.The selection of sample size and method of sample preparation may be based on the

- 106 -

TAGETES EXTRACT page 2 (2)

principles of the method described on FNP 5, "Instrumental methods".

METHOD OF ASSAY Accurately weigh 0.5 – 1.5 g of the sample into a 50 ml volumetric flask. Add about30 ml of a 1:1 mixture of cyclohexane and ethanol (96%) and swirl gently until thesample is dissolved. Fill to the mark with cyclohexane/ethanol mixture and mix well.Pipette 0.200 ml of the solution into a 25 ml volumetric flask. Make up to mark withcyclohexane/ethanol and mix well. Measure the absorbance at maximum of about444 nm using cyclohexane/ethanol mixture as blank. The absorbance should bebetween 0.2 and 0.8, otherwise an appropriate dilution must be prepared.

Calculation:

wv2900

VVAlutein% 21

∗∗

∗∗=

Where

A = absorbanceV1 = Volume of fist volumetric flask (ml)V2 = Volume of second volumetric flask (ml)2900 = specific absorbance for lutein in cyclohexane/ethanol at 444 nmv = volume of pipette (0.200 ml)W = weight of sample (g)

- 107 -

TRISODIUM DIPHOSPHATE page 1 (2)

TRISODIUM DIPHOSPHATE(Tentative)

New specifications prepared at the 57th JECFA (2001) and published in FNP 52 Add9 (2001). No ADI was established, but a group MTDI of 70 mg/kg bw, expressed asphosphorus from all food sources, was established at the 26th JECFA (1982).

Information required on the loss on drying, loss on ignition, test method for loss onignition and assay method for the monohydrate

SYNONYMS Acid trisodium pyrophosphate, trisodium monohydrogen diphosphate;

INS No. 450 (ii)

DEFINITION

Chemical names Trisodium monohydrogen diphosphate

C.A.S. number 14691-80-6 (Anhydrous)26573-04-6 (Monohydrate)

Chemical formula Na3HP2O7 . x H2O (x = 0 or 1)

Formula weight 243.93 (Anhydrous)261.95 (Monohydrate)

Assay Not less than 57% and not more than 59% expressed as P2 O5 .

DESCRIPTION White powder or grains


CHARACTERISTICS

IDENTIFICATION

Solubility (FNP 5) Soluble in water

Test for sodium (FNP 5) Passes test


PURITY


Water insoluble matter(FNP5)

Not more than 0.2%

Fluoride (FNP 5) Not more than 10 mg/kgMethod III; use an appropriate sample size and appropriate volumes of the standardsolution for construction of the calibration curve.

Lead Not more than 4 mg/kgDetermine using an atomic absorption technique appropriate to the specified level.The selection of sample size and method of sample preparation, may be based on theprinciples of the method described in FNP 5, “ Instrumental Methods”.

- 108 -

TRISODIUM DIPHOSPHATE page 2 (2)


METHOD OF ASSAY Weigh accurately about 200 mg of the sample, dissolve in 25 ml of water and 10 mlof diluted nitric acid TS and boil for 30 min. Filter if necessary, and wash anyprecipitate, then dissolve the precipitate by the addition of 1 ml diluted nitric acid TS.Adjust the temperature to about 50o , add 75 ml of ammonium molybdate TS, andmaintain the temperature at about 50o for 30 min, stirring occasionally. Allow tostand for 16 h or overnight at room temperature. Decant the supernate, through afilter paper, wash the precipitate once or twice with water by decantation using 30 to40 ml each time, and pour the washings through the same filter. Transfer theprecipitate to the same filter, and wash with potassium nitrate solution (1 in 100) untilthe filtrate is no longer acid to litmus paper. Transfer the precipitate with filter paperto the original precipitation vessel, add 50.0 ml of 1N sodium hydroxide, agitate untilthe precipitate is dissolved, add 3 drops of phenolphthalein TS and titrate the excessalkali with 1N sulfuric acid. Each ml of 1N sodium hydroxide consumed isequivalent to 3.088 mg of P2O5.

- 109 -

Section B: Specifications of certain flavourings

At its 44th meeting JECFA considered a new approach to the safety evaluation of flavouring agents. Thisapproach incorporates a series of criteria whose use enables the evaluation of a large number of these agents ina consistent and timely manner. At the current session of the Committee specifications of identity and puritywere prepared or revised for 317 flavouring agents*.

Information on specifications is given under the following headings, most of which are self-explanatory:

Name; Chemical name (Systematic name); Synonyms; Flavour and Extract Manufacturers' Association ofthe United States (FEMA) No; Council of Europe (COE) No; Chemical Abstract Service Registry (CAS) No;Molecular weight; Chemical formula; Physical form/odour; Solubility; Solubility in ethanol, Boiling point(information only); Identification test (ID), IR infrared spectrum; Assay min% (see page 199-201: Gaschromatographic (GC) assay of flavouring agents); Acid value max; Refractive index (at 20º, if not otherwisestated); Specific gravity (at 25º, if not otherwise stated); Other requirements, e.g. additional tests; the JECFASession at which the specifications were prepared / the status of the specification. R means "specificationsrevised", S means "existing specifications maintained, S,T means "existing tentative specificationsmaintained”, (further information ), N means "new specifications", and N,T means "new tentativespecifications, (further information required).

Chemical names of the new specifications are systematic names to be in harmony with the substance namesused in the WHO Technical Report Series. When more than one systematic name exists, the systematic namewhich is listed is the closest to the name in the first column.

The last column indicates the data (information) required for the tentative specifications. Abbreviations for"data required" are as follows:

A=assay minimum, A(e)=equivalence factor for assay*, A(m)=details of assay method, BP=boiling point,ID=identity test, Low assay=quantitative information on by-products, RI=refractive index, SG=specificgravity. *A(e) is an equivalence factor to convert an assay obtained by aldehyde / ketone determination, esterdetermination, total alcohols de†termination, or titration determination to the % value which would beobtained if GC had been used for the assay (FNP 5).

The infrared and other spectra, used for identification and comparison purposes, are provided from page 157onwards in two sections (page 157: IR spectra; page 184: other spectra).

The table of contents for the flavours sections has been replaced by a comprehensive index listing all names,chemical names, and synonyms (page 197).

The following IR-spectra were reprinted from Merck FT-IR through courtesy of DrK.G.R. Pachler, Mr. F. Matlock, and Dr. H-U. Gremlich, and VCH Verlagsgesell-schaft, Weinheim, Germany: 260, 302, 388, 410.

The following IR-spectra were reprinted with the permission from the Food ChemicalsCodex, 4th Edition. Copyright 1996 by the National Academy of Sciences, Courtesy ofthe National Academy Press, Washington, DC: 272, 275, 326, 349, 360, 401.

* The Flavouring agent with the JECFA No. 906 had been evaluated previously as No. 736 and is therefore missing inthis list.† Copies for certain spectra may be obtained from the FAO Joint Secretariat or from FEMA, Suite 925, 1620 I Street,N.W., Washington DC, USA.

- 110 -

No Name Chemical name Synonyms FEMA COE CAS Mol Wt Formula Physicalform/odour

Pre-print edition for the 34th session of CCFAC

10 Allyl tiglate 2-Propenyl trans-2-methyl-2-butenoate

Allyl tiglate 2043 2183 7493-71-2 140.18 C8 H12 O2 Colourless to paleyellow liquid with

mild greenfruity/green berry

odour

12 Allyl cyclohexane acetate 2-Propenyl cyclohex-ane acetate

Allyl cyclohexane acetate 2023 2070 4728-82-9 182.26 C11 H18 O2 Colourless liquidwith an intense

sweet long lastingpineapple/peach/a

pricot odour

14 Allyl cyclohexane bu-tyrate

2-Propenyl 4-cyclohexane buta-

noate

Allyl cyclohexyl butyrate 2024 283 7493-65-4 210.31 C13 H22 O2 Colourless liquidwith a fatty

pineapple odour

15 Allyl cyclohexanevalerate

2-Propenyl 5-cyclohexanepentanoate

Allyl cyclohexyl valerate 2027 474 7493-68-7 224.34 C14 H24 O2 Colourless liquidwith a

pineapple/mixedfruity odour

16 Allyl cyclohexanehexanoate

2-Propenyl 6-cyclo-hexane hexanoate

Allyl cyclohexyl caproate 2025 2180 7493-66-5 238.37 C14 H28 O2 Colourless liquidwith a weak fatty

fruity odour

22 Benzaldehyde Benzaldehyde Benzoic aldehyde; Artificialalmond oil;

Benzenecarboxaldehyde;Benzenecarbonal

2127 101 100-52-7 106.12 C7 H6 O colourless toyellow liquid with a

sweet, strongalmond odour

23 Benzyl acetate Benzyl acetate Benzyl ethanoate 2135 2040 140-11-4 150.18 C9 H10 O2 colourless liquidwith a sweet, fruity,

floral (Jasmine)odour

24 Benzyl benzoate Benzyl benzoate Benzyl benzenecarboxylate;Benzyl phenylformate

2138 262 120-51-4 212.25 C14 H12 O2 leaflets or oilyliquid with a faint,sweet, balsamic

odour

25 Benzyl alcohol Benzyl alcohol Phenyl carbinol; Phenyl-methanol; alpha-Hydroxytoluene

2137 58 100-51-6 108.14 C7 H8 O colourless liquidwith a slightlypungent, faintaromatic, fruity

odour

42 Isoamyl formate 3-Methylbutyl formate Isopentyl formate 2069 500 110-45-2 116.16 C6 H12 O2 Colourless liquidwith a plum-like

odour

51 Isoamyl 2-methylbutyrate 3-Methylbutyl 2-methylbutanoate

Isoamyl 2-methyl butanoate 3505 10721 27625-35-0 172.27 C10 H20 O2 colourless liquidwith a fruity odour

58 Geranyl acetate 3,7-Dimethyl-2,6-octadien-1-yl acetate

2509 201 105-87-3 196.29 C12 H20 O2 colourless liquidwith a floral odour

64 Rhodinyl propionate 3,7-Dimethyl-7-octen-1-yl propionate

2986 422 105-89-5 212.26 C13 H24 O2 colourless, oilyliquid with a rose,geranium odour

- 111 -

No Solubility Solubility inethanol

BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity

Other requirements JECFA Datarequired


10 Slightly soluble inwater, ether and most

fixed oils

- 153 IR 98 1.0 1.451 -1.454

0.939 -0.943

57th/R

12 Soluble in ethanol andoils

1ml in 4ml 80%ethanol

60(1 mm Hg)

NMR 96 1.0 1.455 -1.499

0.945 -0.965

57th/R

14 Insoluble in water,soluble in ethanol,essential oils andflavour chemicals

- 104(1 mm Hg)

NMR 98 - 1.4608 at20.5°

0.943-0.949

57th/R

15 Insoluble in water,soluble in ethanol,essential oils and

flavour materials, andpoorly soluble inpropylene glycol

- 119(1mm Hg)

IR 98 - 1.4605 at22°

0.942-0.947

57th/R

16 Soluble in oils andethanol, insoluble in

water

- 128(1.5mm Hg)

NMR 98 - 1.462 0.941-0.947

57th/R

22 very slightly soluble inwater; soluble in

organic solvents, oils

miscible at roomtemperature

178 IR 98 5.0 1.544-1.547

1.040-1.047

Passes test forchlorinatedcompounds

57th/R

23 very slightly soluble inwater, glycerol; soluble

in organic solvents,oils


215 IR 98 1.0 1.500-1.504

1.049-1.059

Passes test forchlorinatedcompounds

57th/R

24 insoluble in water;soluble in organic

solvents, oils


323-324 IR 99 1.0 1.566-1.571

1.113-1.121

mp: 21°; passes testfor chlorinated

compounds

57th/R

25 slightly soluble inwater, soluble in



205 IR 98 0.5 1.536-1.541

1.040-1.050

Passes test forchlorinated

compounds; passestest for peroxides

57th/R

42 Soluble in ethanol,most fixed oils andpropylene glycol,slightly soluble inwater, insoluble in

glycerol

1ml in 40ml 60%ethanol

124° IR 92 3.02 1.396 -1.400

0.881 -0.889

Min 96% isoamylformate + isoamyl

alcohol

57th/R

51 soluble in ethanol andoil, insoluble in water

- 70-71(8 mm Hg)

IR 95 - 1.4124 0.852-0.861

57th/R

58 soluble in alcohol,most fixed oils; slightlysoluble in propyleneglycol; insoluble inglycerine, water

1 ml in 9 ml 70%alcohol

240-245 IR 90 (byester

determination)

- 1.458-1.464

0.900-0.914

(equivalence factor forassay = 98.15)

57th/R

64 soluble in alcohol;practically insoluble in

water

- 255 IR 95 (byester

determination)

- 1.457 0.910(15.5°)


57th/R

- 112 -



70 Geranyl hexanoate trans-3,7-Dimethyl-2,6-octadien-1-yl

hexanoate

Geranyl caproate 2515 317 10032-02-7 252.4 C16 H28 O2 colourless liquidwith a rose-geranium,

pineapple, bananaodour

72 Geranyl isobutyrate 3,7-Dimethyl-2,6-octadienyl-2-methyl

propanoate

2513 3061 2345-26-8 224.34 C14 H24 O2 colourless to paleyellow liquid with a

rose odour

74 Rhodinyl isobutyrate 3,7-Dimethyl-7-octen-1-yl-2-methylpropanoate

2983 297 1338-23-8 226.36 C14 H26 O2 colourless to paleyellow oily liquid

with a fruity, floralodour

77 Rhodinyl isovalerate 3,7-Dimethyl-7-octen-1-yl-3-

methylbutanoate

2987 460 7778-96-3 240.26 C15 H28 O2 colourless, oilyliquid with a rose

odour

78 3,7-Dimethyl-2,6-octadien-1-yl 2-ethylbutanoate

3,7-Dimethyl-2,6-octadien-1-yl 2-ethylbutanoate

Geranyl ethylbutanoate 3339 11667 73019-14-4 252.37 C16 H30 O2 -

95 Heptanal Heptanal Aldehyde C-7; Heptaldehyde 2540 117 111-71-7 114.19 C7 H14 O colourless toslightly yellow

liquid/penetrating,oily odour

101 Nonanal Nonanal Aldehyde C-9; Pelargonicaldehyde

2782 114 124-19-6 142.24 C9 H18 O colourless toyellow liquid/fruity

odour

107 Undecanal Undecanal Aldehyde C-11 undecyclic;n-Undecyl aldehyde

3092 121 112-44-7 170.3 C11 H22 O colourless toslightly yellow

liquid/sweet, fatty,floral odour

111 Lauric acid Dodecanoic acid 2614 12 143-07-7 200.32 C12 H24 O2 white or faintlyyellowish

crystalline solid

113 Myristic acid Tetradecanoic acid 2764 16 544-63-8 228.38 C14 H28 O2 hard, white, orfaintly yellowish,

somewhat glossy,crystalline solid

115 Palmitic acid Hexadecanoic acid 2832 14 57-10-3 256.43 C16 H32 O2 hard, white orfaintly yellowishcrystalline solid

116 Stearic acid Octadecanoic acid 3035 15 57-11-4 284.48 C18 H36 O2 hard, white orfaintly yellowish

crystallinesolid/tallow odour

117 Propyl formate Propyl formate Propyl methanoate 2943 340 110-74-7 88.1 C4 H8 O2 colourless to paleyellow liquid with acharacteristic fruity,

rum-plum odour

119 n-Amyl formate Pentyl formate 2068 497 638-49-3 116.16 C6 H1202 colourless to paleyellow liquid with a

fruit-like odour

- 113 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity



70 - - 240 IR 95 (byester

determination)

- 1.45 0.890(15.5°)


57th/R

72 soluble in mostorganic solvents;insoluble in water


determination)

- 1.451-1.457

0.885-0.893

(d20/4)


57th/R

74 soluble in alcohol;insoluble in water

- 260 MS 95 (byester

determination)

- 1.448-1.453

0.881-0.891

(d20/4)


57th/R

77 soluble in alcohol;practically insoluble in

water


determination)

- 1.447 0.8829(15°)


57th/R

78 - - 287 IR 95 (byester

determination)

- 1.449-1.458

0.889-0.896


57th/R

95 slightly soluble inwater; miscible withalcohol, ether, fixed

oils


153 IR 92 10 1.412-1.420

0.814-0.819

2-Methylhexanal: 3%-8%

57th/R

101 soluble in alcohol,most fixed oils,

propylene glycol;insoluble in glycerin

1 ml in 3 ml of70% alcohol

93(23 mm Hg)

191

IR 92 10 1.422-1.429

0.820-0.830

2-Methyloctanal: 4%-8%

57th/R

107 soluble in most fixedoils, propylene glycol;insoluble in glycerin,

water

1 ml in 5 ml of70% alcohol

223 IR 92 10 1.430-1.435

0.825-0.832

2-Methyldecanal: 3%-8%

57th/R

111 practically insoluble inwater; soluble in

alcohol, chloroform,ether

- n/a IR 98 (byHPLC)

252-287

n/a n/a Saponification Value:253 to 287;

Solidification Pt.: 26°to 44°; UnsaponifiableMatter: < 0.3%; Water:

< 0.2%

57th/R,T A

113 practically insoluble inwater; soluble in

alcohol, chloroform,ether

- n/a IR 97 bytitration

242-249


Solidification Pt.: 48°to 55.5°;

Unsaponifiable Matter:< 1%; Water: < 0.2%

57th/R,T A

115 practically insoluble inwater; soluble inalcohol, ether,

chloroform

- n/a IR 97 byHPLC

204-220


Solidification Pt.: 53.3°to 62°; UnsaponifiableMatter: <1.5%; Water:

<0.2%

57th/R,T A

116 practically insoluble inwater; soluble inalcohol, ether,

chloroform

1 g in 20 mlalcohol

n/a IR 98 (bytitration)

196-211

n/a n/a mp: 64° (minimum);Saponification Value:

197 to 212;Unsaponifiable Matter:< 1.5%; Water: < 0.2%

57th/R,T A

117 miscible with alcohol,ether, most organic

solvents; soluble in 1ml in 45 ml water

- 81-82° IR 94 1.369-1.384

0.895-0.905

Min 97% propylformate + propyl

alcohol

57th/R

119 miscible with alcohol,ether, most organic

solvents

- 128-130° IR 92 5 (addto icesoln)

1.396-1.402

0.881-0.887

Min 96% amyl formate+ amyl alcohol

57th/R

- 114 -



124 Isobutyl formate 2-Methylpropylformate

Tetryl formate 2197 502 542-55-2 102.13 C5 H10 O2 colourless to paleyellow liquid with a

fruity, etherealodour

170 n-Amyl heptanoate Pentyl heptanoate 2073 370 7493-82-5 200.32 C12 H24 O2 colourless to paleyellow liquid with a

fruity, unripebanana odour

172 Isobutyl heptanoate 2-Methylpropylheptanoate

Isobutyl heptoate 2200 364 7779-80-8 186.3 C11 H22 O2 colourless liquidwith a green odour

178 Nonyl octanoate Nonyl octanoate Nonyl caprylate 2790 396 7786-48-3 270.46 C17 H34 O2 colourless, oilyliquid with a sweet,

rose, mushroomodour

180 Methyl laurate Methyl dodecanoate 2715 377 111-82-0 214.35 C13 H26 O2 colourless to paleyellow liquid with afatty, floral, winey

odour

182 Isoamyl laurate 3-Methylbutyldodecanoate

Isopentyl laurate 2077 379 6309-51-9 270.46 C17 H34 O2 colourless, oilyliquid with a faintoily, fatty odour

184 Butyl stearate Butyl octadecanoate 2214 2189 123-95-5 340.59 C22 H44 O2 colourless, waxysolid, odourless orwith a faintly fatty

odour

191 trans-3-Heptenyl 2-methyl propanoate

trans-3-Heptenyl 2-methyl propanoate

3494 10663 67801-45-0 184.28 C11 H20 O2 colourless liquid

205 Methyl 2-methylbutyrate Methyl-2-methylbutanoate

2719 2085 868-57-5 116.16 C6 H12 O2 almost colourlessliquid/sweet, fruity,

apple-like odour

212 2-Methylbutyl 2-methylbutyrate

2-Methylbutyl-2-methylbutanoate

3359 10773 2445-78-5 172.27 C10 H20 O2 colourless to paleyellow lquid

240 omega-6-Hexadecenlactone

6-Hexadecenolide;Oxacycloheptadec-7-

en-2-one

Ambrettolide; Hexadec-6-eno-1,16-lactone

2555 180 7779-50-2 252.39 C16 H28 O2 colourless toslightly yellow

liquid with a strong,musk odour

249 cis-4-Hydroxy-6-dodecenoic acid lactone

Dodeca-6-en-1,4-lactone 3780 625 18679-18-0 196.3 C12 H20 O2 colourless liquid

260 2-Methylpentanal 2-Methylpentanal 2-Methylvaleraldehyde 3413 706 123-15-9 100.15 C6 H12 O colourless to paleyellow liquid

265 2-Methylhexanoic acid 2-Methylhexanoic acid 2-Methylcaproic acid; 2-Butylpropionic acid

3191 582 4536-23-6 130.19 C7 H14 O2 colourless, oilyliquid with a fruity

odour

266 5-Methylhexanoic acid 5-Methylhexanoic acid 3572 10142 628-46-6 130.19 C7 H14 O2 liquid with acheese fermented

odour

- 115 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity



124 miscible with alcohol,ether; soluble inorganic solvents;slightly soluble in

water

- 97-98.2° IR 94 1.383-1.39 0.876-0.886

Min 97% isobutylformate + isobutyl

alcohol

57th/R

170 soluble in mostorganic solvents


240-245° IR 93 1 1.422-1.426

0.859-0.863

Amyl 2-methylhexanoate: 2%-

7%

57th/R

172 soluble in mostorganic solvents

- 209 IR 98 - 1.420-1.425

0.8593(20°)

57th/R


- 315 IR 99 - 1.431-1.435

0.86 57th/R

180 soluble in mostorganic solvents;insoluble in water

- 261-262° IR 94 1.430-1.438

0.863-0.872

Melting Pt.: 5°;Saponification value

>124.3

57th/R


- 190(20 mmHg)

IR 97 - 1.400-1.405 /1.434-1.439

0.853-0.859

57th/R,T RI

184 - - 343; 220-225

(25 mm Hg)

IR 99 (byester

determination)

- n/a 0.855-0.875

mp: 25°; (equivalencefactor for assay =

170.30); Iodine Value:< 1; SaponificationValue: 165 to 180

57th/R


- 85-90(3 mm Hg)

IR 98 - 1.429-1.430

0.881-0.886

57th/R

205 soluble in alcohol,most fixed oils;

insoluble in water

- 115 IR 92 2 1.393-1.397

0.879-0.883

Methyl isovalerate:5%-8%

57th/R

212 - - 184-187 IR 90 1.409-1.509

0.854-0.864

2-methylbutylisovalerate: 5%-10%

57th/R

240 - 1 ml in 9 ml 80%alcohol

185-190(16 mm Hg)

IR 98 - 1.477-1.482

0.949-0.957

57th/S

249 soluble in alcohol andether; insoluble in

water and fat

- 113(0.6 mm

Hg)

NMR 95.5 - 1.466 0.958 57th/R

260 - - 116 IR 97 (byaldehydedetermina

tion)

- 1.412 0.805-0.811


57th/R

265 miscible with alcohol,ether and water

- 105(5 mm Hg)

IR 95 1.419-1.422(20°)

0.914-0.918

(20°/20°)

57th/R

266 soluble in water;miscible with fat

- 216 IR 95 1.422 0.912(24°)

57th/R

- 116 -



270 2-Methyloctanal 2-Methyloctanal Methyl hexyl acetaldehyde 2727 113 7786-29-0 142.24 C9 H18 O colourless, oilyliquid with a rose,

lily-like odour

273 2,6-Dimethyloctanal 2,6-Dimethyloctanal 2,6-Dimethyl octanoicaldehyde; Isodecylaldehyde;

isodecanal

2390 112 1321-89-7 156.26 C10 H20 O colourless liquidwith a powerful,sweet fruit odour

275 2-Methylundecanal 2-Methylundecenal Aldehyde C-12; Methyl n-nonyl acetaldehyde


liquid with a fattyodour

304 Isopropyl formate Isopropyl formate Isopropyl methanoate 2944 503 625-55-8 88.11 C4 H8 O2 colourless liquidwith a fruity, ether-

like odour

306 Isopropyl propionate Isopropyl propionate 2959 404 637-78-5 116.16 C6 H12 O2 liquid

308 Isopropyl hexanoate Isopropyl hexanoate Isopropyl caproate 2950 312 2311-46-8 158.24 C9 H18 O2 colourless liquid

322 cis-5-Octen-1-ol (Z)-Oct-5-en-1-ol 3722 64275-73-6 128.21 C8 H16 O colourless liquid

323 cis-5-Octenal (Z)-Oct-5-enal 3749 41547-22-2 126.2 C8 H14 O colourless liquidwith a fruity odour

325 cis-6-Nonenal (Z)-Non-6-en-1-al 3580 661 2277-19-2 140.23 C9 H16 O colourless to paleyellow liquid with amelon-like odour

326 4-Decenal 4-Decenal 3264 2297 30390-50-2 154.25 C10 H18 O colourless toslightly yellowliquid with an

orange-like, fattyodour

328 9-Decenoic acid Dec-9-enoic acid 3660 10090 14436-32-9 170.25 C10 H18 O2 colourless to paleyellow liquid with a

very waxy,somewhat fruityand milky odour

330 10-Undecenal Undec-10-en-1-al 3095 122 112-45-8 168.28 C11 H20 O colourless to lightyellow liquid with a

fatty, rose-likeodour on dilution

334 Methyl 3-hexenoate Methyl hex-3-enoate 3364 10801 2396-78-3 128.17 C7 H12 O2 colourless liquid

344 Butyl 10-undecenoate Butyl undec-10-enoate Butyl undecylenate 2216 2103 109-42-2 240.39 C15 H28 O2 colourless to paleyellow liquid

- 117 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity



270 soluble in alcohol andmost fixed oils;

insoluble in water

- 82-83(20 mm Hg)

IR 96.5 - 1.423(14°)

0.841 (0°) 57th/R

273 insoluble in water;soluble in alcohol

- 82-84(15 mm Hg)

IR 97 - 1.426 (d-isomer)

0.825 (20°,d-isomer)

57th/R

275 soluble in fixed oils,alcohol, and propyleneglycol (solution may be

turbid); insoluble inglycerol

- 171 IR 97 10 1.431-1.436

0.822-0.830

57th/R

304 slightly soluble inwater; completely

miscible with alcohol,ether, and mostorganic solvents

- 67-70 IR 99 - 1.364-1.370

0.877-0.883(20°)

57th/R

306 completely misciblewith alcohol anddiluted alcohol

- 108-111 IR 98 - 1.384-1.390

0.863-0.869(20°)

57th/R

308 almost insoluble inwater; soluble in

alcohol

- 176 MS 99 - 1.405 0.854-0.860(20°)

57th/R

322 - - 95°(25 mm Hg)

IR 90 1.445-1.451

0.840-0.860(20°)

trans-isomer: 5-10% 57th/R


alcohol and most fixedoils

- 62 IR 85 1.436-1.441

0.845-0.853(20°)


325 soluble in alcohol,essential oils;

insoluble in water

- 86°(11 mm Hg)

IR 90 5 1.438-1.445

0.843-0.855(20°)


326 soluble in alcohol andmost fixed oils;

insoluble in water

- 78-80°(10 mm Hg)

IR 95 (min.90%

trans-isomer)

1.442-1.447

0.843-0.850

57th/R

328 insoluble in water;soluble in alcohol

- 270° IR 90 (min95% totaldecenoic

acids)

1.44-1.46 0.893-0.913(20°)

57th/R

330 soluble in propyleneglycol and most fixed

oils; insoluble inglycerol and water

- 235 IR 90 (min97% totaldecenals)

6 1.441-1.447

0.840-0.850

57th/R

334 - - 156 IR 97 - 1.422-1.428

0.912-0.922(20°)

57th/R

344 - - 125-128 IR 98 - 1.439-1.445

0.872-0.878(20°)

57th/R

- 118 -



347 2-Methyl-3-pentenoicacid

2-Methyl pent-3-enoate

3464 10147 37674-63-8 114.15 C6 H10 O2 clear, colourlessliquid

348 2,6-Dimethyl-6-hepten-1-ol

2,6-Dimethylhept-7-en-1-ol

alpha-Melonol 3663 36806-46-9 142.24 C9 H18 O -

350 Ethyl 2-methyl-3-pentenoate

Ethyl 2-methylpent-3-enoate

3456 10612 1617-23-8 142.2 C8 H14 O2 -

352 Hexyl 2-methyl-3&4-pentenoate (mixture)

3693 58625-95-9 198.31 C12 H22 O2 -

367 Terpinyl formate p-Menth-1-en-8-ylformate

3052 348 2153-26-6 182.26 C11 H18 O2 colourless liquidwith a floral citrusy,

tart, herbaceousodour

370 Terpinyl butyrate p-Menth-1-en-8-ylbutyrate

3049 278 2153-28-8 224.34 C14 H24 O2 clear, colourlessliquid

372 Terpinyl isovalerate p-Menth-1-en-8-ylisovalerate

Terpinyl isopentanoate;Terpinyl isovalerate; p-

Menth-1-en-8-ylisopentanoate; p-Menth-1-en-8-yl 3-methylbutyrate

3054 456 1142-85-4 238.38 C15 H26 O2 colourless oilyliquid with a

peculiar sweet-piney, floral-

incense-like citrusodour

374 p-Menth-8-en-1-ol 4-Isopropenyl-1-methyl-1-cyclohexanol

beta-Terpineol 3564 10254 138-87-4 154.25 C10 H18 O colourless, slightlyviscous liquid witha pungent woody-

earthy odour

388 alpha-Ionone 4-(2,6,6-Trimethyl-2-cyclohexenyl)-3-buten-

2-one

alpha-Cyclocitrylideneacetone

2594 141 127-41-3 192.3 C13 H20 O colourless to pale-yellow liquid with a

warm, woody,violet-floral odour

390 gamma-Ionone 4-(2,2-Dimethyl-6-methylenecyclohexyl)-

3-buten-2-one

3175 79-76-5 192.3 C13 H20 O colourless to paleyellow liquid

401 Allyl-alpha-ionone 1-(2,6,6-Trimethyl-2-cyclohexenyl)-1,6-heptadien-3-one

Allyl Ionone 2033 2040 79-78-7 232.37 C16 H24 O colourless toyellow liquid with afruity, woody odour

404 alpha-iso-Methylionone 4-(2,6,6-Trimethyl-2-cyclohexen-1-yl)-3-

methyl-3-buten-2-one

alpha-Cyclocitrylidenebutanone

2714 169 127-51-5 206.33 C14 H22 O clear, colourless toyellowish liquid

416 5-Hydroxy-4-octanone 5-Hydroxyoctan-4-one 5-Octanol-4-one; Butyroin 2587 2045 496-77-5 144.21 C8 H16 O2 yellowish liquid

424 2-Hydroxy-2-cyclohexen-1-one

2-Hydroxy-2-cyclohexen-1-one

3-Methyl-1,2-cyclohexanedione; 2-Methyl-

3,4-cyclohexanedione

3458 11046 10316-66-2 112.13 C6 H8 O2 -

428 d-Neo-Menthol d-beta-Pulegomenthol 2666 2028 2216-52-6 156.27 C10 H20 O colourless liquid

- 119 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity




alcohol and most fixedoils

- 85(10 mm Hg)

IR 99 (as60/40 mix

ofcis/transisomers)

- 1.433-1.440

0.960-0.966

57th/R

348 insoluble in water,soluble in fixed oils

- 62(1 mm Hg)

IR 90 - 1.451 0.841-0.846

6-methyl-5-hepten-2-one: 5-10%

57th/R

350 insoluble in water - 85-91(50 mm Hg)

IR 98 - 1.419 0.870-0.876

57th/R

352 insoluble in water,soluble in alcohol and

fixed oils

- 57-61(2 mm Hg)

IR 99 - 1.431 0.871-0.876

57th/R

367 very slightly soluble inwater


213-225 IR 95 (byester

determination)

- 1.467-1.473

0.987-0.993

(15.5°)


57th/R

370 insoluble in water;soluble in alcohols and

oils

- 244-246 IR 95 (byester

determination)

- 1.463-1.468

0.962-0.968

(15.5°)


57th/R

372 insoluble in water;soluble in alcohols


determination)

- 1.459-1.469

0.931-0.937


57th/R

374 soluble in water,alcohol, and oils

- 210 IR 96 - 1.482-1.485

0.930-0.936

Congealing point 24° 57th/R

388 soluble in alcohol,propylene glycol, mostfixed oils; insoluble in

glycerol and water

1 ml in 3 ml 70%alcohol; 1 ml in

10 ml 60%alcohol

237 IR 85 (min.95% sum

ofisomers)

1.497-1.502

0.927-0.933

57th/R

390 - - 125(10 mmHg)

[req.] [req.] - 1.496-1.502(25°)

0.932-0.935(20°)

57th/R,T ID, A


1 ml in 1 ml 90%alcohol; 1 ml in 8ml 70% alcohol

265 IR 88 (min.95% sum

ofisomers)

1.502-1.507

0.926-0.935

Allyl alcohol <=0.1% 57th/R

404 - - 238 IR 85 (min.95% sum

ofisomers)

1.498-1.503

0.925-0.934

57th/R

416 almost insoluble inwater; soluble in

alcohol

- 182 IR 95 - 1.426-1.432

0.907-0.923(20°)

57th/R

424 soluble in water,ethanol, fat

- 53(2.2 mm

Hg)

IR 99.3 - n/a n/a Melting range 35-38° 57th/R

428 insoluble in water;soluble in alcohol and

acetone

- 211-213 IR 99 - 1.459-1.460

0.896-0.903(20°)

mp: 22°; OpticalRotation: 20° at 20°C

57th/R

- 120 -



434 p-Menth-1-en-3-ol 3179 10248 491-04-3 154.25 C10 H18 O -

440 2-Ethyl-1,3,3-trimethyl-2-norbornanol

2-Ethyl-1,3,3-trimethylbicyclo[2.2.1]

heptan-2-ol

2-Ethylfenchol 3491 10208 18368-91-7 182.31 C12 H22 O colourless to paleyellow liquid with a

sharp,camphoraceous

odour

442 Methyl 1-acetoxycyclohexyl ketone

1-Acetylcyclohexylacetate

1-Acetoxy-1-acetylcyclohexane

3701 52789-73-8 184.24 C10 H16 O3 colourless, oilyliquid with a sweetfruity, floral, honey

odour

448 1-Ethylhexyl tiglate Octen-3-yl 2-methyl-2-butenoate

1-Ethylhexyl 2-methylcrotonate; 3-Octyl

tiglate

3676 94133-92-3 212.34 C13 H24 O2 -

457 (1-Buten-1-yl) methylsulfide

1-Butenyl methylsulfide

3820 32951-19-2 102.21 C5 H10 S pale yellow liquidwith an unpeasant

odour

461 3-(Methylthio)propanol 3-(Methylthio)propanol 3-Hydroxypropyl methylsulfide; Methionol; Methyl 3-

hydroxypropyl sulfide;(Methylmercapto)propyl

alcohol; 3-(Methylthio)propylalcohol

3415 11554 505-10-2 106.18 C4 H10 OS pale yellowish,mobile liquid;

powerful sweet,soup or meat-like

odour

478 3-(Methylthio)propylacetate

3-(Methylthio)propylacetate

3-Acetoxypropyl methylsulfide; Methionyl acetate

3883 16630-55-0 148.22 C6 H12 O2 S colourless liquidwith fatty, estery

odour

490 Allyl thiopropionate Allyl thiopropionate Propionic acid, thioallyl ester 3329 11436 41820-22-8 130.21 C6 H10 OS

510 2-Propanethiol 2-Propanethiol Isopropyl mercaptan 3897 75-33-2 76.16 C3 H8 S colourless liquidwith onion odour

531 2-Naphthalenethiol 2-Naphthalenethiol 2-Mercaptonaphthalene; 2-Naphthyl mercaptan; 2-

Thionapthol

3314 2330 91-60-1 160.23 C10 H8 S crystals withdisagreeable

mercaptan-likeodour

543 Trithioacetone 2,2,4,4,6,6-Hexamethyl-1,3,5-

trithiane

3475 2334 828-26-2 222.42 C9 H18 S3

562 2,5-Dimethyl-2,5-dihydroxy-1,4-dithiane

2,5-Dimethyl-2,5-dihydroxy-1,4-dithiane

2,5-Dimethyl-2,5-dihdroxy-p-dithiane

3450 2322 55704-78-4 180.28 C6 H12 O2S2

white crystallinesolid

580 2-Methyl-2-(methyldithio)propanal

2-Methyl-2-(methyldithio)propanal

2-(Methydithio)isobutylraldehyde

3866 67952-60-7 150.27 C5 H10 OS2 colourless to paleyellow liquid

581 Ethyl 2-(methyldithio)propionate

Ethyl 2-(methyldi-thio)propionate

3834 23747-43-5 180.28 C6 H12 O2S2

colourless to paleyellow liquid

591 Methyl 2-oxo-3-methylpentanoate

Methyl 3-methyl-2-oxovalerate

Methyl 2-keto-3-methylvalerate

3713 3682-42-6 144.17 C7 H12 O3 liquid

- 121 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity



434 - - 232 NMR 97 - 1.4762(25C)

0.930-0.936

57th/R

440 soluble in alcohol,propylene glycol, mostfixed oils; insoluble in

water

- 232 NMR 99.8 - 1.470-1.491

0.946-0.967

57th/R

442 slightly soluble inwater, soluble inalcohols and oils

- 67(3 mm Hg)

NMR 99 - 1.46 1.04 57th/R

448 completely misciblewith alcohol anddiluted alcohol

- 94-96(60 mm Hg)

IR 95 2.9 1.441-1.447

0.879-0.885

57th/R

457 very soluble in alcohol - 123 NMR 98 - 1.393-1.413

0.943-0.948

57th/R

461 slightly soluble inwater; soluble in

alcohol, propyleneglycol and oils

- 195; 93-94(17mm Hg)

IR 98 - 1.483-1.493

1.027-1.033

57th/R

478 very slightly soluble inwater; soluble inalcohol and oils

- 201-202 IR 97 1.0 1.461-1.467

1.036-1.044

57th/R

490 - - 151 IR 83%+15%diallylsulfide

- 1.475-1.485

0.961-0.960

57th/R,T SG range

510 soluble in oil andalcohol

- 57-60 IR, MS,NMR

98 - 1.428-1.434

0.814-0.819

57th/R

531 slightly soluble inwater; soluble inalcohol and ether

- 210.5(100mm

Hg)

MS 98 - n/a n/a mp: 79-81°;Decomposes at 285°

57th/R

543 insoluble in water;miscible in oils

- 78.5(0.5 mm

Hg)

NMR,IR

99 - 1.537-1.545

1.062-1.068

57th/R


alcohol

- n/a NMR 95 - n/a n/a mp: 183° 57th/R

580 very slightly soluble inwater;soluble inalcohol and oils

- 46(1 mm Hg)

NMR 95 - 1.512-1.522

1.095-1.100

mp: 80-138° 57th/R

581 very slightly soluble inwater; soluble inalcohols and oils

- 105(12 mm Hg)

NMR 98 - 1.490-1.500

1.090-1.120

57th/R

591 slightly soluble inwater; soluble in fat

- 197 IR, MS,NMR

99 - 1.416-1.426

0.988-0.995

57th/R

- 122 -



599 Geranyl acetoacetate 3,7-Dimethylocta-2(trans),6-dienyl 3-

oxobutyrate

trans-3,7-Dimethyl-2,6-octadien-1-yl acetoacetate;Geranyl beta-ketobutyrate;

Geranyl 3-oxobutanoate

2510 243 10032-00-5 238.32 C14 H22 O3 colourless to paleyellow oily liquidwith sweet, fruity,winey, fermentedapple-like odour

604 3-(Hydroxymethyl)-2-heptanone

3-(Hydroxymethyl)-2-heptanone

2-Acetyl-1-hexanol; Methylolmethyl amyl ketone

2804 592 65405-68-7 144.21 C8 H16 O2 colourless liquidwith powerful,

herbaceous, fruity,mildly spicy odour

609 1,4-Nonanediol diacetate 1,4-Nonanedioldiacetate

3579 11927 67715-81-5 244.33 C13 H24 O4

627 Aconitic acid 1,2,3-Propene-tricarboxylic acid

Achelleic acid; 2-Carboxyglutaconic acid; Citridic acid;Equisetic acid; 1-Propene-

1,2,3-tricarboxylic acid

2010 33 499-12-7 174.11 C6 H6 O6 colourless oryellow crystals,

leaves, or plates;pleasant winey

acid taste; almostodourless

642 3-Phenylpropylhexanoate

3-Phenylpropylhexanoate

Hydrocinnamyl caproate; 3-Phenylpropyl caproate

2896 321 6281-40-9 234.34 C15 H22 O2 Colourless liquid,sweet, fruity-green

odour

645 3-Phenylpropionaldehyde 3-Phenylpropanal Benzylacetaldehyde;Hydrocinnamaldehyde;Phenylpropyl aldehyde

2887 2013 104-53-0 134.18 C9 H10 O Colourless toslightly yellowliquid, strongpungent floral

odour of hyacinth

648 Cinnamaldehydeethylene glycol acetal

2-(2-Phenylethylene)-1,3-dioxolane

Cincloval; 2-Styryl-1,3-dioxolane

2287 48 5660-60-6 176.22 C11 H12 O2 Nearly colourlessoily liquid, soft,

spicy, warm, sweetodour

652 Cinnamyl butyrate 3-Phenyl-2-propenylbutyrate

3-Phenylallyl butyrate 2296 279 103-61-7 204.27 C13 H16 O2 Colourless toyellowish liquid,

fruity slightly floralbalsamic odour

656 Cinnamaldehyde 3-Phenyl-2-propenal Cinnamal; Cinnamicaldehyde; beta-Phenylacrolein;

Zimtaldehyde; Cassiaaldehyde; Benzylidene

acetaldehyde

2286 102 104-55-2 132.16 C9 H8 O Yellow liquid,strong cinnamon

odour

660 Propyl cinnamate Propyl 3-phenyl-propenoate

Propyl beta-phenylacrylate 2938 324 7778-83-8 190.24 C12 H14 O2 Colourless viscousliquid, sweet,

slightly floral odour

663 Butyl cinnamate Butyl 3-phenyl-propenoate

Butyl beta-phenylacrylate 2192 326 538-65-8 204.27 C13 H16 O2 Colourless, oily,somewhat viscousliquid, sweet, oily,

balsamic, fruityodour

666 Heptyl cinnamate Heptyl 3-phenyl-propenoate

Heptyl beta-phenylacrylate 2551 2104 10032-08-3 246.35 C16 H22 O2 Colourless or pale-straw coloured

viscous liquid, mild,floral-green,

somewhat bark-likeodour

671 Phenethyl cinnamate Phenethyl 3-phenyl-propenoate

Benzylcarbinyl cinnamate;Benzylcarbinyl 3-

phenylpropenoate; beta-Phenethyl beta-

phenylacrylate; 2-Phenylethyl cinnamate

2863 336 103-53-7 252.31 C17 H16 O2 White crystals,heavy balsamic-like rosy odour

- 123 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity



599 insoluble in water;soluble in alcohol and

oil


127-129(22 mm Hg)

IR 97 - 1.426-1.433

0.958-0.966

57th/R


alcohol

- 94.6(8-9 mm

Hg)

MS 90 - 1.444-1.447

0.945-0.949

1-Hydroxy-3-octanone:5%-10%

57th/R, T Low assay

609 - - 272 [req] [req.] - [req.] 0.970 57th/R,T ID, A, RI

627 soluble in water andalcohol

- n/a IR 98 (onanhy-drousbasis)

- n/a n/a Oxalate: passes test;Tridodecylamine: max.

0.1 mg/kg

57th/R,T MP

642 insoluble in water;soluble in oils

miscible 292 IR 99 1.0 1.482-1.488

0.963-1.010

57th/R,T SG range


miscible 222 IR 95 5.0 1.518-1.528

1.008-1.018


57th/R


miscible 265 NMR 90 - 1.561-1.570

1.095-1.103

57th/R

652 insoluble in water miscible 300 IR 98 1.0 1.525-1.530

1.010-1.020

57th/R

656 insoluble in water;miscible in oils

miscible 248-250 IR 98 (byester

determination)

10.0 1.619-1.625

1.046-1.053


57th/R


miscible 283-284 IR 98 (byester

determination)

1.0 1.547-1.553

1.030-1.040


57th/R

663 slightly soluble toinsoluble in water

miscible 287 IR 98 (byester

determination)

1.0 1.539-1.545

1.008-1.014


57th/R


miscible 185(12 mm Hg)

IR 97 1.0 1.528-1.530

0.982-0.990

57th/R


moderatelysoluble

170(1 mmHg)

IR 98 1.0 n/a n/a mp: 54° (minimum) 57th/R

- 124 -



672 3-Phenylpropylcinnamate

3-Phenylpropyl 3-phenylpropenoate

Hydrocinnamyl cinnamate;Hydrocinnamyl 3-

phenylpropenoate; beta-Phenylpropyl cinnamate; 3-

Phenylpropyl beta-phenylacrylate

2894 338 122-68-9

266.34 C18 H18 O2 Colourless toslightly yellow

liquid, rosybalsamic delicately

fruity odour

673 Cinnamyl cinnamate 3-Phenylprop-2-enyl 3-Phenylpropenoate

Cinnamyl beta-phenylacrylate; 3-Phenylallyl

cinnamate; Phenylallylcinnamate

2298 332 122-69-0

264.32 C18 H16 O2 White or colourlesscrystals, mild,

balsamic, floralodour

676 alpha-Amylcinnamylformate

2-(Phenyl-methylene)heptyl

formate

alpha-Amyl-beta-phenylacrylformate; alpha-

Pentylcinnamyl formate

2066 357 7493-79-0

232.32 C15 H20 O2 Colourless liquid,sweet, oily

herbaceous, andsomewhat green

odour

677 alpha-Amylcinnamylacetate

2-(Phenyl-methylene)heptyl

acetate

alpha-n-Amyl-beta-phenylacryl acetate; alpha-

Pentylcinnamyl acetate

2064 216 7493-78-9

246.35 C16 H22 O2 Colourless oilyliquid, mild, oily,fruity, somewhat

green odour

678 alpha-Amylcinnamylisovalerate

2-(Phenyl-methylene)heptyl 3-

methylbutanoate

alpha-Amyl-beta-phenylacrylisovalerate; alpha-n-Amyl-

beta-phenylacryl 3-methylbutanoate; alpha-

Pentylcinnamyl isovalerate

2067 463 7493-80-3

288.43 C19 H28 O2 Colourless liquid,mild fruity, some-what herbaceoustobacco-like odour

681 alpha-Amylcinnamalde-hyde dimethyl acetal

(2-(Dimethoxymethyl)-1-heptenyl)benzene

alpha-Amyl-beta-phenylacrolein dimethylacetal; 1,1-Dimethoxy-2-

benzylideneheptane; alpha-Pentylcinnamaldehydedimethyl acetal; alpha-Amylcinnamic aldehyde

dimethyl acetal

2062 47 91-87-2

248.36 C16 H24 O2 Almost colourlessto pale yellow,

floral odourreminiscent of

jasmine

698 o-Tolyl acetate 2-Methylphenylacetate

Acetyl o-cresol; o-Cresolacetate; o-Cresylic acetate

3072 2078 533-18-6

150.18 C9 H10 O2 Colourless liquid

711 p-Vinylphenol 4-Vinylphenol p-Ethenylphenol; 4-Hydroxystyrene

3739 11257 2628-17-3

120.15 C8 H8 O White solid, vanillaextract odour

719 Guaiacyl phenylacetate 2-Methoxyphenylphenylacetate

Guaiacol phenylacetate; o-Methylcatechol

phenylacetate; o-Methoxyphenolphenylacetate

2535 238 4112-89-4

242.27 C15 H14 O3 Amber viscousliquid. When pure it

forms colourlesscrystals with

heavy, rather dry,woody,

herbaceous odour

720 Hydroquinone monoethylether

4-Ethoxyphenol 1-Ethoxy-4-hydroxybenzene;p-Ethoxyphenol; p-Hydroxyphenetole

3695 2258 622-62-8

138.17 C8 H10 O2 White or colourlesscrystals, sweet

herbaceous odourreminiscent of

anise and fennel

723 4-Ethyl-2,6-dimethoxyphenol

4-Ethyl-2,6-dimethoxyphenol

2,6-Dimethoxy-4-ethylphenol; 4-Ethylsyringol

3671 11231 14059-92-8

182.22 C10 H14 O3 Water white liquid

724 4-Propyl-2,6-dimethoxyphenol

2,6-Dimethoxy-4-propylphenol

4-Propylsyringol 3729 6766-82-1

196.25 C11 H16 O3 Water white liquid

726 4-Allyl-2,6-dimethoxyphenol

4-Allyl-2,6-dimethoxyphenol

4-Allylsyringol; 2,6-Dimethoxy-4-(2-propenyl)

phenol; 6-Methoxy eugenol

3655 11214 6627-88-9

194.23 C11 H14 O3 Clear pale yellowliquid, roasted

meaty bacon odour

- 125 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity




miscible 190(0.2 mm

Hg)

IR 98 (byester

determination)

1.0 1.583-1.588

1.074-1.080


57th/R


moderatelysoluble

370 IR 95 (byester

determination)

2.0 n/a n/a mp: 42° (minimum);(equivalence factor for

assay = 132.16)

57th/R

676 - miscible 277 IR 85%(97%

total ofthe

formateand theparent

alcohol)

- 1.516-1.526

0.980-0.999

57th/R

677 soluble in oils miscible 291 IR 97 1.0 1.487-1.495

0.953-0.961

57th/R

678 - miscible 171(4 mmHg)

IR 97 - 1.498-1.508

0.939-0.959

57th/R,T SG range

681 slightly soluble inwater

miscible 300 IR 97 1.0 1.504-1.511

0.954-0.963

57th/R


1.046-1.053

57th/R

711 soluble in water;slightly soluble in fat

moderatelysoluble

189 MS 99 - n/a n/a mp: 68° 57th/R

719 insoluble in water very soluble 201(2 mm Hg)

IR 97 1.0 n/a n/a mp: 40-43° 57th/R

720 slightly soluble tosoluble in water;

soluble in oils

moderatelysoluble

246-247 IR 95 - n/a n/a mp: 64° (minimum) 57th/R

723 insoluble in water;soluble in fat

miscible 106(0.2 mm

Hg)

MS 98 - 1.536-1.537

1.075-1.080

57th/R


miscible 115(0.38 mm

Hg)

IR 98 - 1.529-1.530

1.071-1.076

57th/R



IR 98 - 1.548-1.550

1.089-1.095

57th/R

- 126 -



729 Dihydroxyacetophenone Mixture of 1-(x,y-dihydroxyphenyl)

ethanones

1-(x,y-Dihydroxyphenyl)ethanone;

Dioxyacetophenone;Dihydroxyphenyl methyl

ketone

3662 11884 28631-86-9 152.15 C8 H8 O3 Yellow needles orcrystals

732 Vanillylidene acetone 4-(4-Hydroxy-3-methoxyphenyl)but-3-

en-2-one

3738 691 1080-12-2 192.21 C11 H12 O3 Yellowish, needlelike crystals, sweet

warm andtenacious odour

740 Furfuryl propionate Furfuryl propionate Furfuryl propanoate 3346 10646 623-19-8 154.17 C8 H10 O3 Oily liquid whichdarkens on

exposure to light,green banana

odour

741 Furfuryl pentanoate Furfuryl valerate alpha-Furfuryl pentanoate;alpha-Furfuryl valerate

3397 10647 36701-01-6 182.22 C10 H14 O3 Colourless oilyliquid, sweet

overripe fruit odour

742 Furfuryl octanoate Furfuryl octanoate alpha-Furfuryl caprylate;alpha-Furfuryl octanoate

3396 10645 39252-03-4 224.3 C13 H20 O3

743 Furfuryl 3-methylbutanoate

Furfuryl 3-methylbutanoate

Furfuryl isovalerate 3283 10642 13678-60-9 182.22 C10 H14 O3

748 Amyl 2-furoate Pentyl 2-furoate Amyl furan-2-carboxylate;Pentyl furan-2-carboxylate

2072 2109 1334-82-3 182.22 C10 H14 O3 Colourless to paleyellow liquid,

sweet, caramellic,winey, somewhatherbaceous odour

749 Hexyl 2-furoate Hexyl 2-furoate Hexyl furan-2-carboxylate 2571 361 39251-86-0 196.25 C11 H16 O3 Colourless to palestraw coloured

liquid, fruity-earthy,yet sweet pear-like

odour

750 Octyl 2-furoate Octyl 2-furoate Octyl 2-furancarboxylate 3518 10864 39251-88-2 224.3 C13 H20 O3 Colourless to palestraw liquid; sweetfruity heavy odour

752 2-Phenyl-3-carbethoxyfuran

Ethyl 2-phenyl-3-furoate

Phenyl oxaromate 3468 2309 50626-02-3 216.24 C13 H12 O3

759 Furfuryl butyrate Furfuryl butyrate 2-Furylmethyl butanoate 638 623-21-2 168.19 C9 H12 O3 Oily liquid, greenbutyric rancid

odour

760 Cinnamyl benzoate 3-Phenyl-2-propenylbenzoate

743 5320-75-2 238.29 C16 H14 O2 White crystallinepowder, balsamic,

aromatic, spicyodour

761 2-Methylpyrazine Methylpyrazine 2-Methyl-1,4-diazine 3309 2270 109-08-0 94.12 C5 H6 N2 colourless toslightly yellow

liquid with a nutty,cocoa-like odour

762 2-Ethylpyrazine Ethylpyrazine 2-Ethyl-1,4-diazine 3281 2213 13925-00-3 108.14 C6 H8 N2 colourless to paleyellow liquid with a

musty, nutty,peanut butter

odour

- 127 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity



729 (3,4-isomer) insolubleto slightly soluble inwater; (2,5-isomer)slightly soluble in

water; (3,5-isomer)soluble in water

moderatelysoluble

decomposes

IR [req.] - n/a n/a mp: 90° (minimum) 57th/R,T A


moderatelysoluble

decomposes

IR 97 - n/a n/a mp: 129-130° 57th/R


miscible 195-196 IR 98 1.0 1.457-1.464

1.076-1.086

57th/R

741 insoluble in water miscible 228-229 IR 98 (byester

determination)

1.0 1.457-1.462

1.024-1.031


57th/R



IR 98 (byester

determination)

1.0 1.456-1.464

0.980-0.989


57th/R


miscible 97-98(11 mm Hg)

IR 98 (byester

determination)

1.0 1.456-1.464

1.014-1.023


57th/R

748 insoluble in water miscible 95-97(1 mm Hg)

IR 98 1.0 1.469-1.475

1.031-1.038

57th/R


miscible 252 IR 97 1.0 1.468-1.473

1.015-1.020

57th/R

750 insoluble in water;miscible in fat

miscible 126-127(1 mm Hg)

IR 98 1.0 1.466-1.472

0.984-0.990

57th/R


- 148-154(6 mm Hg)

IR 99 1.0 [req.] [req.] 57th/R,T RI, SG


1.051-1.057

57th/R


miscible 335 IR 98 1.0 n/a n/a mp: 31° 57th/R

761 soluble in water andoils


137 IR 98 - 1.501-1.509

1.007-1.033

57th/N

762 soluble in water,organic solvents, oils


152 IR 98 - 1.493-1.508

0.981-1.000

57th/N

- 128 -



763 2-Propylpyrazine Propylpyrazine 2-Propyl-1,4-diazine 3961 11362 18138-03-9 122.17 C7 H10 N2 colourless to lightyellow liquid with a

green vegetableodour

764 2-Isopropylpyrazine Isopropylpyrazine 2-Isopropyl-1,4-diazine 3940 29460-90-0 122.17 C7 H10 N2 colourless to lightyellow liquid with aminty, green, nutty,

honey odour

765 2,3-Dimethylpyrazine 2,3-Dimethylpyrazine 2,3-Dimethyl-1,4-diazine 3271 11323 5910-89-4 108.14 C6 H8 N2 colourless to lightyellow liquid with anutty, cocoa-like

odour

766 2,5-Dimethylpyrazine 2,5-Dimethylpyrazine 2,5-Dimethyl-1,4-diazine;Glycoline; Ketine

3272 2210 123-32-0 108.14 C6 H8 N2 colourless toslightly yellowliquid with an

earthy, potato-likeodour

767 2,6-Dimethylpyrazine 2,6-Dimethylpyrazine 2,6-Dimethyl-1,4-diazine;2,6-Dimethyl-p-diazine

3273 2211 108-50-9 108.14 C6 H8 N2 white to yellowlumpy crystals witha nutty, coffee-like

odour

768 2-Ethyl-3-methylpyrazine 2-Ethyl-3-methylpyrazine

2-Ethyl-3-methyl-1,4-diazine;2-Methyl-3-ethylpyrazine

3155 548 15707-23-0 122.17 C7 H10 N2 colourless toslightly yellow

liquid with a strongraw potato odour


2-Ethyl-6-methyl-1,4-diazine 3919 11331 13925-03-6 122.17 C7 H10 N2 colourless toslightly yellowliquid with a

roasted bakedpotato odour


2-Methyl-5-ethylpyrazine; 2-Ethyl-5-methyl-1,4-diazine


liquid with a nutty,roasted, grassy

odour

771 2,3-Diethylpyrazine 2,3-Diethylpyrazine 2,3-Diethyl-1,4-diazine 3136 534 15707-24-1 136.20 C8 H12 N2 colourless toslightly yellowliquid with anearthy, nutty,

baked potato odour

772 2-Methyl-5-isopropylpyrazine

2-Isopropyl-5-methylpyrazine

5-Isopropyl-2-methylpyrazine; 2-Methyl-5-

isopropyl-1,4-diazine

3554 2268 13925-05-8 136.20 C8 H12 N2 colourless toslightly yellowliquid with a

roasted, coffee,nutty, earthy odour

773 2-Isobutyl-3-methylpyrazine

2-Isobutyl-3-methylpyrazine

2-Methyl-3-isobutylpyrazine;2-(2-Methylpropyl)-3-

methylpyrazine; 2-Isobutyl-3-methyl-1,4-diazine

3133 13925-06-9 150.22 C9 H14 N2 colourless toslightly yellow

liquid with a green,earthy, celery

odour

774 2,3,5-Trimethylpyrazine Trimethylpyrazine 2,3,5-Trimethyl-1,4-diazine 3244 735 14667-55-1 122.17 C7 H10 N2 colourless toslightly yellowliquid with a

roasted nut, bakedpotato odour

775 2-Ethyl-3 (5 or 6)-dimethylpyrazine

Mixture of 2-Ethyl-3,5-Dimethylpyrazine and

3-Ethyl-2,5-Dimethylpyrazine

3149 727 13925-07-0(3,5-);

13360-65-1(3,6-)

136.20 C8 H12 N2 colourless toslightly yellowliquid with atoasted nut,

chocolaty, sweetwoody odour

- 129 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity





65(12 mm Hg)

NMR 98 - 1.492-1.496

0.966-0.970

57th/N



70(20 mm Hg)

IR 98 - 1.486-1.496

0.967-0.972

57th/N



156 IR 95 (sumof 2,3-

2,5- and2,6-

isomers)

- 1.501-1.510

0.997-1.030

57th/N



155 IR 98 (sumof 2,3-

2,5- and2,6-

isomers)

- 1.497-1.503

0.982-1.000

57th/N

767 soluble in water,organic solvents

very soluble 154 IR 98 (sumof 2,3-

2,5- and2,6-

isomers)

- NA NA mp: 48° 57th/N



57(10 mm Hg)

IR 97 (sumof 2,3-

2,5- and2,6-

isomers)

- 1.499-1.509

0.972-0.993

57th/N



80(50 mm Hg)

IR 95 (sumof 2,3-

2,5- and2,6-

isomers)

- 1.487-1.497

0.967-0.980

57th/N



79(66 mm Hg)

IR 95 - 1.491-1.501

0.960-0.970

57th/N

771 soluble in water,soluble in oils, organic

solvents


180 IR 97 - 1.492-1.509

0.956-0.976

57th/N

772 soluble in water,soluble in oils, organic

solvents


190 NMR 97 - 1.492-1.498

0.977-0.984

57th/N

773 soluble in water, oils,organic solvents


199 IR 98 - 1.488-1.498

0.936-0.942

57th/N



171 IR 98 - 1.500-1.509

0.960-0.990

57th/N



180 IR 95 - 1.496-1.506

0.950-0.980

57th/N

- 130 -



776 2-Ethyl-3,5-dimethylpyrazine

2-Ethyl-3,5-dimethylpyrazine

2,6-Dimethyl-3-ethylpyrazine; 3-Ethyl-2,6-

dimethylpyrazine


liquid

777 2,3-Diethyl-5-methylpyrazine

2,3-Diethyl-5-methylpyrazine

2-Methyl-5,6-diethylpyrazine; 2,3-Diethyl-

5-methyl-1,4-diazine

3336 11303 18138-04-0 150.22 C9 H14 N2 colourless to lightyellow liquid with a

nutty, roasted,vegetable odour



2,5-Diethyl-3-methyl-1,4-diazine

3915 11304 32736-91-7 150.22 C9 H14 N2 colourless to lightyellow liquid with atoasted hazelnut,

meaty odour



2-Methyl-3,5-diethyl-1,4-diazine


liquid with a nutty,meaty, vegetable

odour

780 2,3,5,6-Tetramethylpyrazine

Tetramethylpyrazine Tetramethyl-1,4-diazine 3237 734 1124-11-4 136.20 C8 H12 N2 white crystals orpowder with a

musty, fermented,coffee odour

781 5-Methyl-6,7-dihydro-5H-cyclopentapyrazine

6,7-Dihydro-5-methyl-5H-cyclopentapyrazine

(5H)-5-Methyl-6,7-dihydrocyclopenta(b)py-

razine; Maple lactonepyrazine

3306 2314 23747-48-0 134.18 C8 H10 N2 light yellow toamber liquid with a

peanut odour

782 6,7-Dihydro-2,3-dimethyl-5H-cyclopentapyrazine

6,7-Dihydro-2,3-dimethyl-5H-

cyclopentapyrazine

(5H)-2,3-Dimethyl-6,7-dihydrocyclopenta(b)py-

razine

3917 11309 38917-63-4 148.21 C9 H12 N2 low melting solidwith a roasted nut

odour

783 (Cyclohexylmethyl)py-razine

(Cyclohexylmethyl)py-razine

(Pyrazinylmethyl)cyclohexane; 2-

Pyrazinylcyclohexylmethane

3631 28217-92-7 176.26 C11 H16 N2 pale amber liquidwith a nutty, musty

odour

784 2-Acetylpyrazine 2-Acetylpyrazine Acetylpyrazine; Methylpyrazinyl ketone

3126 2286 22047-25-2 122.13 C6 H6 N2 O colourless to paleyellow crystals witha nutty, popcorn,breadcrust odour

785 2-Acetyl-3-ethylpyrazine 2-Acetyl-3-ethylpyrazine

2-Acetyl-3-ethyl-1,4-diazine;3-Ethyl-2-pyrazinyl methyl

ketone

3250 11293 32974-92-8 150.18 C8 H10 N2 O colourless to paleyellow liquid with a

nutty, popcorn,potato chip, meaty

odour

786 2-Acetyl-3,(5 or 6)-dimethylpyrazine

2-Acetyl-3,5-dimethylpyrazine and

3-Acetyl-2,5-dimethylpyrazine

Mixture of 3-Acetyl-2,5-dimethylpyrazine and 3-

Acetyl-2,6-dimethylpyrazine

3327 11294 54300-08-2(3,6); 54300-

09-3 (3,5)

150.18 C8 H10 N2 O colourless to paleyellow liquid with apopcorn, roastedhazelnut odour

787 Methoxypyrazine Methoxypyrazine 2-Methoxy-1,4-diazine; 2-Methoxypyrazine

3302 11447 3149-28-8 110.11 C5 H6 N2 O colourless to lightyellow liquid with anutty, cocoa-like

odour

788 2-Methoxy-(3,5 or 6)-methylpyrazine

Mixture of 2-Methoxy-3-methylpyrazine and

2-Methoxy-5-methylpyrazine and 2-

Methoxy-6-methylpyrazine

2 or 5 or 6-Methoxy-3-methyl-1,4-diazine

3183 2266 2847-30-5(2,3); 2822-22-6 (2,5);2882-21-5

(2,6)

124.14 C6 H8 N2 O colourless to slightyellow liquid with aroasted hazelnut,almond, peanut

odour

- 131 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity





180 IR 95 - 1.496-1.502

0.952-0.961

57th/N

777 moderately soluble inwater; soluble in oils,

organic solvents


203 IR 98 - 1.493-1.505

0.938-0.957

57th/N

778 moderately soluble inwater; soluble in oils,

organic solvents


95(14 mm Hg)

NMR 97 - 1.4922-1.5022

0.944-0.954

57th/N

779 slightly soluble inwater; soluble in oils,

organic solvents


95(14 mm Hg)

NMR 97 - 1.492-1.502

0.944-0.954

57th/N


propylene glycol,organic solvents

very soluble 190 IR 95 - NA NA mp: 85-90° 57th/N


propylene glycol,organic solvents


200 IR 97 - 1.525-1.535

1.048-1.059

57th/N


organic solvents

very soluble 66(2 mm Hg)

NMR 97 - NA NA mp: 25-27° 57th/N

783 slightly soluble inwater; soluble in oils


100(4 mm Hg)

NMR 97 - 1.515-1.520

1.003-1.009

57th/N

784 slightly soluble inwater; soluble inorganic solvents

moderatelysoluble

188 IR 99 - NA NA mp: 74-80° 57th/N



220 IR 98 - 1.509-1.520

1.068-1.079

57th/N



70(7 mm Hg)

IR 97 (sumof

isomers)

- 1.510-1.520

1.070-1.075

57th/N

787 miscible with water,organic solvents;

soluble in oils


61-62(29 mm Hg)

IR 99 - 1.492-1.510

1.109-1.140

57th/N



80-85(10 mm Hg)

IR 97 (sumof

isomers)

- 1.505-1.510

1.060-1.090

57th/N

- 132 -



789 Ethyl-(3,5 or 6)-methoxypyrazine (85%)and 2-Methyl-(3,5 or 6)-methoxypyrazine (13%

Mixture of 2-Ethyl-3-methoxypyrazine and2-Ethyl-5-methoxypy-razine and 2-Ethyl-6-methoxypyrazine and2-Methyl-3-methoxy-

pyrazine and 2-Methyl-5-methoxypyrazine

and 2-Methyl-6-methoxypyrazine

3280 11329 (various) colourless to slightyellow liquid with araw potato, earthy,bell pepper odour

790 2-Methoxy-(3,5 or 6)-isopropylpyrazine

2-Isopropyl-3-methoxypyrazine and

2-Isopropyl-5-methoxypyrazine and

2-Isopropyl-6-methoxypyrazine

Mixture of Methoxy isopropylpyrazines

3358 11344 93905-03-4 152.20 C8 H12 N2 O colourless toslightly yellowliquid with an

earthy, raw potato,bell pepper odour

791 2-Methoxy-3-(1-methylpropyl)pyrazine

2-(1-Methylpropyl)-3-methoxypyrazine

2-Methoxy-3-sec-butylpyrazine; 2-sec-Butyl-3-

methoxypyrazine; 2-(2-Butyl)-3-methoxypyrazine

3433 11300 24168-70-5 166.22 C9 H14 N2 O colourless toslightly yellow

liquid with a bellpepper, galbanum

odour

792 2-Isobutyl-3-methoxypyrazine

2-Isobutyl-3-methoxypyrazine

2-Methoxy-3-isobutylpyrazine

3132 11338 24683-00-9 166.22 C9 H14 N2 O colourless toslightly yellow

liquid with a greenbell pepper, green

pea odour

793 2-Methyl-3(or 5 or 6)-ethoxypyrazine

2-Methyl-3-ethoxypyrazine and 2-

Methyl-5-ethoxypyrazine and 2-

Methyl-6-ethoxypyrazine

2-Ethoxy-3 or 5 or 6-methylpyrazine

3569 11921 32737-14-7(2,3); 67845-34-5 (2,5);53163-97-6

(2,6)

138.17 C7 H10 N2 O colourless to lightyellow liquid with achocolate, roasted

odour

794 2- (Mercapto-methyl)pyrazine

Pyrazinemethanethiol Pyrazinylmethyl mercaptan 3299 11502 59021-02-2 126.18 C5 H6 N2 S colourless toyellow liquid with aroasted, meat-like

odour

795 2-Pyrazinylethanethiol 2-Pyrazinylethanethiol Pyrazinylethyl mercaptan 3230 2285 35250-53-4 140.21 C6 H8 N2 S colourless toyellow liquid with ameaty, cabbage,sulfurous odour

796 Pyrazinyl methyl sulfide 2-(Methylthio)pyrazine Benzalglycerin; Mixture of 2-Phenyl-5-hydroxy-1,3-

dioxane and 2-Phenyl-4-hydroxymethyl-1,3-dioxolane

3231 2288 21948-70-9 126.18 C5 H6 N2 S low melting whitecrystalline solidwith an etherealsulfurous odour

797 (3,5 or 6)-Methylthio-2-methylpyrazine

Mixture of 2-Methyl-3-(methylthio)pyrazine

and 2-Methyl-5-(methylthio)pyrazineet

hylthio)pyrazine

2-Methyl-3,5-or 6-methylthiopyrazine;

Methylpyrazinyl methylsulfides (mixture)

3208 2290 67952-65-2 140.21 C6 H8 N2 S colourless to lightyellow liquid with a

cooked meat,roasted, almond,nutty, vegetable

odour

798 5-Methylquinoxaline 5-Methylquinoxaline 5-Methyl-1,4-benzodiazine 3203 2271 13708-12-8 144.18 C9 H8 N2 colourless to lightyellow liquid with a

burnt, roasted,nutty, coffee odour

799 alpha-Methylbenzylalcohol

1-Phenylethanol 1-Phenylethanol; Phenylmethyl carbinol; Methyl

phenyl carbinol; Styrallylalcohol; alpha-Phenethyl

alcohol

2685 2030 98-85-1 122.17 C8 H10 O colourless to paleyellow liquid or

white solid with amild floral odour

800 alpha-Methylbenzylformate

1-Phenylethyl formate Methyl phenyl carbinylformate; Styrallyl formate

2688 574 7775-38-4 150.18 C9 H10 O2 colourless to paleyellow liquid with astrong green-floral,

woody-balsamicodour

- 133 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity





80-95(10 mm Hg)

IR 99 (sumof 6

namedcom-

pounds)

- 1.497-1.505

1.036-1.052

57th/N



120-125(20 mm Hg)

IR 97 (sumof

isomers)

- 1.492-1.499

1.010-1.022

57th/N



50(1 mm Hg)

IR 99 - 1.478-1.498

0.976-1.002

57th/N



60(2 mm Hg)

IR 95 - 1.487-1.497

0.983-1.003

57th/N



175-176 IR 97 - 1.493-1.497

1.034-1.041

57th/N



94(10 mm Hg)

IR 98 - 1.548-1.560

1.148-1.156

57th/N



105-110(20 mm Hg)

IR 97 - 1.553-1.570

1.147-1.157

57th/N



IR 99 - NA NA mp: 42-47° 57th/N

797 miscible at roomtemperature


85-87(10 mm Hg)

IR 99 (sumof

isomers)

- 1.570-1.590

1.133-1.153

57th/N

798 freely soluble in water,organic solvents, oils


IR 98 - 1.616-1.624

1.102-1.128

mp: 20° 57th/N


solvents, oils


204 IR 99 - 1.524-1.529

1.009-1.014

mp: 19-20° 57th/N


solvents, oils


198 IR 98 totalformate

ester

3.0 1.502-1.508

1.042-1.050

57th/N

- 134 -



801 alpha-Methylbenzylacetate

1-Phenylethyl acetate alpha-Phenethyl acetate;Methyl phenyl carbinylacetate; Phenyl methyl

carbinyl acetate; Styrallylacetate

2684 573 93-92-5 164.20 C10 H12 O2 colourless liquidwith a powerful

green-floral odour

802 alpha-Methylbenzylpropionate

1-Phenylethylpropionate

alpha-Phenylethylpropionate; Methyl phenyl

carbinyl propionate; Styrallylpropionate

2689 425 120-45-6 178.23 C11 H14 O2 colourless liquidwith a fruity, floral,sweet, green odour

803 alpha-Methylbenzylbutyrate

1-Phenylethyl butyrate Methyl phenyl carbinylbutyrate; alpha-Phenylethylbutyrate; Styrallyl butyrate

2686 2083 3460-44-4 192.26 C12 H16 O2 colourless oilyliquid with a fruity,

floral odour

804 alpha-Methylbenzylisobutyrate

1-Phenylethyl 2-methylpropanoate

1-Phenylethyl isobutyrate;Methyl phenyl carbinylisobutyrate; Stryallylisobutyrate; alpha-

Phenethyl-2-methylpropanoate

2687 2088 7775-39-5 192.26 C12 H16 O2 colourless oilyliquid with a sweet,floral-green odour

805 p,alpha-Dimethylbenzylalcohol

1-(4-Methylphenyl)ethanol

1-p-Tolylethanol; p-Tolylmethyl carbinol; Methyl p-

tolyl carbinol

3139 10197 536-50-5 136.19 C9 H12 O colourless oilyliquid with a dry,

menthol-like,camphoraceous

odour

806 Acetophenone Acetophenone Acetylbenzene; Methylphenyl ketone; Phenyl

methyl ketone

2009 138 98-86-2 120.15 C8 H8 O colourless liquidwhich will solidify

at 20°C

807 4-Methylacetophenone 1-(4-Methyl-phenyl)ethanone

p-Methylacetophenone; p-Acetyl toluene; Methyl p-tolyl

ketone; 1-Acetyl-4-methylbenzene

2677 156 122-00-9 134.18 C9 H10 O low meltingcolourless or

opaque crystallinemass (tends to

supercool) with astrong fruity-floral,warm, sweet odour

808 p-Isopropylacetophenone 1-(4-Isopropyl-phenyl)ethanone

Acetocumene; p-Acetylcumene; Methyl p-

isopropylphenyl ketone; p-Isopropylacetylbenzene

2927 651 645-13-6 162.23 C11 H14 O colourless liquidwith a powerfulspicy, woody,

herbaceous odour

809 2,4-Dimethylacetophenone

1-(2,4-Dimethyl-phenyl)ethanone

Acetyl-m-xylene; Methyl 2,4dimethylphenyl ketone

2387 157 89-74-7 148.21 C10 H12 O colourless toslightly yellow oilyliquid with a sweet,floral, woody, minty

odour

810 Acetanisole 1-(4-Methoxy-phenyl)ethanone

4-Acetylanisole; p-Acetylanisole; 4-

Methoxyacetophenone; p-Methoxyacetophenone;Methyl 4-methoxyphenyl

ketone

2005 570 100-06-1 150.18 C9 H10 O2 colourless to paleyellow fused solid

with a floral,powdery, vanillic,balsamic odour

811 Methyl beta-naphthylketone

1-(2-naphthyl)ethanone

beta-Acetylnaphthalene;Methyl 2-naphthyl ketone;

Cetone D; Oranger crystals

2723 147 93-08-3 170.21 C12 H10 O white or nearlywhite crystalline

solid with a floral,orange blossom,

neroli odour

812 4-Acetyl-6-t-butyl-1,1-dimethylindan

4-Acetyl-6-(1,1-dimethylethyl)-1,1-

dimethylindane

ABDI 3653 13171-00-1 244.38 C17 H24 O almost whitecrystals with amusky, sweet,animal odour

813 1- (p-Methoxyphenyl)-2-propanone

1-(4-Methoxyphenyl)-2-propanone

Anisic ketone; Anisyl methylketone; 4-Methoxy-

phenylacetone

2674 11836 122-84-9 164.21 C10 H12 O2 colourless oilyliquid with an anise

type odour

- 135 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity




solvents, oils


214 IR 98 5.0 1.492-1.504

1.020-1.035

57th/N


solvents, oils


91-92(5 mm Hg)

IR 98 1.0 1.487-1.494

1.002-1.009

57th/N


solvents, oils


93-84(3 mm Hg)

IR 98 1.0 1.484-1.490

0.977-0.997

57th/N


solvents, oils


219; 80(3 mm Hg)

IR 98 1.0 1.480-1.486

0.977-0.983

57th/N


solvents, oils


218-219 IR 96 - 1.520-1.524

0.980-0.990

57th/N



miscible above20°

202 IR 98 - 1.530-1.535

1.022-1.028

57th/N


solvents, oils

very soluble 226 IR 95 - 1.530-1.536

0.999-1.010

mp: 22-24° 57th/N


solvents, oils


252 IR 98 (sumof

isomers)

- 1.520-1.527

0.967-0.975

57th/N


solvents, oils


228 IR 96 - 1.532-1.536

0.993-0.999

57th/N


solvents, oils


IR 97 (sumof o,m,p-isomers)

- NA NA mp: 36-38° 57th/N


solvents, oils

soluble 300 IR 97 - NA NA Solidification point =53°

57th/N

812 insoluble in water,soluble in oils

soluble n/a IR 97 - NA NA mp: 68-70° 57th/N

813 insoluble in water;soluble in oils, organic

solvents


260minimum

IR 97 - 1.520-1.530

1.067-1.073

57th/N

- 136 -



814 alpha-Methylphenethylbutyrate

1-Methyl-2-phenylethylbutyrate

1-Phenyl-2-propyl butyrate;Methyl benzyl carbinyl

butyrate

3197 2276 68922-11-2 206.29 C13 H18 O2 colourless oilyliquid

815 4-Phenyl-2-butanol 4-Phenyl-2-butanol Methyl 2-phenylethylcarbinol; Phenylethyl methyl

carbinol

2879 85 2344-70-9 150.22 C10 H14 O colourless oilyliquid with a floral-fruity, herbaceous

odour

816 4-Phenyl-2-butyl acetate 1-Methyl-3-phenylpropyl acetate

Phenylethyl methyl carbinylacetate

2882 671 10415-88-0 192.26 C12 H16 O2 colourless oilyliquid with a mild,green, fruity odour

817 4- (p-Tolyl)-2-butanone 4-(4-Methylphenyl)-2-butanone

p-Methylbenzylacetone 3074 160 7774-79-0 162.23 C11 H14 O colourless oilyliquid with a sweet,fruity-floral odour

818 4- (p-Methoxyphenyl)-2-butanone

4-(4-Methoxyphenyl)-2-butanone

Anisylacetone;Methyloxanone; Brambleketone; Raspberry ketone

methyl ether; p-Methoxybenzylacetone

2672 163 104-20-1 178.23 C11 H14 O2 colourless oilyliquid with a sweet,fruity-floral odour

819 4-Phenyl-3-buten-2-ol 4-Phenyl-3-buten-2-ol Methyl styryl carbinol;Homocinnamyl alcohol

2880 2032 17488-65-2 148.21 C10 H12 O colourless slightlyviscous liquid with

a sweet, mild,fruity, floral,

balsamic odour

820 4-Phenyl-3-buten-2-one 4-Phenyl-3-buten-2-one

Benzylideneacetone; Methylstyryl ketone


crystalline solidwith a sweet,

pungent, creamy,floral odour

821 3-Methyl-4-phenyl-3-buten-2-one

3-Methyl-4-phenyl-3-buten-2-one

3-Benzylidene-2-butanone;Benzylidene methyl ethyl

ketone; Benzylidene methylacetone

2734 161 1901-26-4 160.22 C11 H12 O pale yellowcrystalline solid

with a sweet, fruity,berry, camphor

odour

822 1-Phenyl-1-propanol 1-Phenylpropanol Ethyl phenyl carbinol;Phenyl ethyl carbinol; alpha-

Ethylbenzyl alcohol; 1-Phenylpropyl alcohol

2884 82 93-54-9 136.19 C9 H12 O colourless oilyliquid with a sweet

floral balsamicodour

823 alpha-Ethylbenzylbutyrate

1-Phenylpropylbutyrate

Ethyl phenyl carbinolbutyrate; alpha-Phenylpropyl

butyrate

2424 625 10031-86-4 206.28 C13 H18 O2 colourless liquidwith a strong,

sweet, fruity-floralodour

824 Propiophenone 1-Phenyl-1-propanone Phenyl ethyl ketone;Propionylbenzene; Ethyl

phenyl ketone

3469 599 93-55-0 134.18 C9 H10 O colourless oilyliquid or low

melting crystallinesolid with a

pungent, powerful,floral, herbaceous

odour

825 alpha-Propylphenethylalcohol

1-Phenyl-2-pentanol Benzyl propyl carbinol;Benzylbutyl alcohol; n-Propyl benzyl carbinol

2953 83 705-73-7 164.25 C11 H16 O colourless oilyliquid with a mild,

green, sweet odour

826 1- (p-Methoxyphenyl)-1-penten-3-one

1-(4-Methoxyphenyl)-1-penten-3-one

Ethone; alpha-Methylanisylidene acetone; alpha-

Methylanisalacetone; p-Methoxystyryl ethyl ketone

2673 164 104-27-8 190.24 C12 H14 O2 white to paleyellow crystals with

a sweet, buttery,caramellic odour

827 alpha-Isobutylphenethylalcohol

4-Methyl-1-phenyl-2-pentanol

2-Methyl propyl benzylcarbinol; Benzyl isobutylcarbinol; Isobutyl benzylcarbinol; Benzylisoamyl

acetone

2208 2031 7779-78-4 178.28 C12 H18 O colourless slightlyoily liquid with a

green-floral, fresh,slightly sweet

odour

- 137 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity



814 insoluble in water;soluble in oils, organic

solvents


138-140(10 mm Hg)

NMR 99 2 [req.] [req.] 57th/N,T RI, SG


solvents, oils


229 IR 97 - 1.514-1.518

0.977-0.983

57th/N


solvents, oils


72-74(0.5 mm

Hg)

IR 98 1.0 1.498-1.505

0.975-0.980

57th/N


solvents, oils


251 NMR 96 - [req.] [req.] 57th/N,T RI, SG

818 insoluble in water,soluble in organic

solvents, oils


277; 150-152

(10 mm Hg)

IR 96 - 1.515-1.525

1.041-1.050

57th/N


solvents, oils


140(12 mm Hg)

IR 96 - 1.558-1.567

1.006-1.012

57th/N


solvents, oils



solvents, oils

very soluble 124-125(10 mm Hg)

NMR 97 - NA NA mp: 38-40° 57th/N


solvents, oils


219 IR 97 - 1.517-1.522

0.993-1.000

57th/N


solvents, oils


282 IR 97 2.0 1.486-1.491

0.986-0.992

57th/N


solvents, oils


218 IR 98 - 1.521-1.531

1.004-1.014

mp: 21° 57th/N


solvents, oils


247; 75(0.5 mm

Hg)

IR 96 - 1.508-1.513

0.957-0.964

57th/N


solvents, oils

very soluble 278; 74(10 mm Hg)

IR 98 - NA NA mp: 60° 57th/N


solvents, oils


250 IR 96 - 1.500-1.510

0.940-0.949

57th/N

- 138 -



828 4-Methyl-1-phenyl-2-pentanone

4-Methyl-1-phenyl-2-pentanone

Benzyl isobutyl ketone;Isobutyl benzyl ketone;Benzyl 2-methylpropyl

ketone

2740 159 5349-62-2 176.26 C12 H16 O colourless oilyliquid with a sweet,woody, spicy, burnt

sugar odour

829 1- (4-Methoxyphenyl)-4-methyl-1-penten-3-one

1-(4-Methoxyphenyl)-4-methyl-1-penten-3-

one

alpha-,alpha-Dimethyl-anisalacetone; Isopropyl p-

methoxystyryl ketone;Homoethone


buttery, caramellicodour

830 3-Benzyl-4-heptanone 3-Benzyl-4-heptanone Benzyl dipropyl ketone; 1-Phenyl-2-ethyl-3-hexanone;

Morellone

2146 2140 7492-37-7 204.31 C14 H20 O colourless oilyliquid with a fruity,

berry, woody,raisin odour

831 Benzophenone Benzophenone Diphenyl ketone;Benzoylbenzene; Phenyl

ketone

2134 166 119-61-9 182.22 C13 H10 O white rhombiccrystals or flakes

with a mildpowdery floral

odour

832 1,3-Diphenyl-2-propanone

1,3-Diphenyl-2-propanone

Benzyl ketone; Dibenzylketone; alpha,alpha-

Diphenylacetone

2397 11839 102-04-5 210.28 C15 H14 O white or colourlesscrystals with a

sweet, faint fruity-almond odour

833 1-Phenyl-1,2-propanedione

1-Phenyl-1,2-propanedione

Acetyl benzoyl; Methylphenyl diketone; Methyl

phenyl glyoxal

3226 2275 579-07-7 148.16 C9 H8 O2 yellow oily liquidwith a pungentplastic odour

834 Ethyl benzoylacetate Ethyl 3-phenyl-3-oxopropionate

Benzoyl acetic ester; Ethylbeta-keto-beta-

phenylpropionate

2423 627 94-02-0 192.21 C11 H12 O3 colourless to lightyellow liquid with abrandy-like, woody,

cherry, phenolicodour

835 Ethyl 2-acetyl-3-phenylpropionate

Ethyl 2-acetyl-3-phenylpropionate

Ethyl benzylacetoacetate;Ethyl alpha-

acetylhydrocinnamate; Ethyl2-acetyldihydrocinnamate


balsamic, floral-fruity odour

836 Benzoin 2-Hydroxy-1,2-diphenylethanone

Benzoyl phenyl carbinol; 2-Hydroxy-2-

pheylacetophenone

2132 162 119-53-9 212.25 C14 H12 O2 white to light yellowcrystals with afaint, sweet,

balsamic odour

837 Benzaldehyde dimethylacetal

(Dimethoxymethyl)benzene

alpha-,alpha-Dimethoxytoluene

2128 37 1125-88-8 152.20 C9 H12 O2 colourless liquidwith a sweet, floral-

almond odour

838 Benzaldehyde glycerylacetal

5-Hydroxy-2-phenyl-1,3-dioxane and 4-(Hydroxymethyl)-2-

phenyl-1,3-dioxolane

Benzalglycerin; Mixture of 2-Phenyl-5-hydroxy-1,3-

dioxane and 2-Phenyl-4-hydroxymethyl-1,3-dioxolane

2129 36 1319-88-6 180.21 C10 H12 O3 colourless to paleyellow oily liquid

with a mild almondodour

839 Benzaldehyde propyleneglycol acetal

4-Methyl-2-phenyl-1,3-dioxolane

4-Methyl-2-phenyl-m-dioxolane

2130 2226 2568-25-4 164.20 C10 H12 O2 colourless liquidwith a mild almond-

like odour

840 Benzyl 2-methoxyethylacetal

1-Benzyloxy-1-(2-methoxyethoxy)ethane

Acetaldehyde benzyl 2-methoxyethyl mixed acetal;

1-Benzyloxy-1-(2-methoxyethoxy)ethane

2148 523 7492-39-9 210.27 C12 H18 O3 colourless liquidwith a mild, sweet,green-fruity odour

841 Benzyl formate Benzyl formate Benzyl methanoate 2145 344 104-57-4 136.15 C8 H8 O2 colourless liquidwith an intensepleasant, floral-

fruity odour

842 Benzyl propionate Benzyl propionate Benzyl propanoate 2150 413 122-63-4 164.20 C10 H12 O2 colourless liquidwith a sweet, fruity-

floral odour

- 139 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity




solvents, oils


250-251 IR 98 - 1.500-1.510

0.940-0.949

57th/N


solvents, oils


201(10 mm Hg)

NMR 97 - 1.510-1.515

1.016-1.026

57th/N


solvents, oils


158-160(10 mm Hg)

IR 99 - 1.490-1.495

0.931-0.937

57th/N

831 insoluble in water andglycerol; slightly

soluble in propyleneglycol; soluble in oils

very soluble 305 IR 98 - NA NA mp: 48° 57th/N


solvents, oils



solvents, oils


103-105(14 mm Hg)

IR 97 - 1.526-1.536

1.096-1.116

57th/N


solvents, oils


147(11 mm Hg)

IR 88 2.0 1.524-1.533

1.107-1.120

Combined assay(named cpd + ethyl

benzoate): 96%

57th/N


solvents, oils


276; 164(18 mm Hg)

IR 97 2.0 1.498-1.502

1.033-1.037

57th/N

836 insoluble in water;slightly soluble in hot

water, oils

slightly soluble 194(12 mm Hg)

IR 98 - NA NA mp: 137° 57th/N


solvents, oils


198 IR 96 1.0 1.488-1.496

1.007-1.020

57th/N



185(20 mm Hg)

IR 98 (sumof

isomers)

2.0 1.532-1.542

1.181-1.193

57th/N



83-85(4 mm Hg)

IR 95 1.0 1.506-1.516

1.061-1.071

57th/N


solvents, oils


161-162(10 mm Hg)

IR 98 (sumof namedcpd andstarting

materials)

1.0 1.479-1.489

1.019-1.025

57th/N


solvents, oils


202 IR 95 5.0 1.508-1.518

1.082-1.092

57th/N

842 insoluble in water;poorly soluble in

glycerol, glycols, andmineral oil


222 IR 98 1.0 1.495-1.500

1.028-1.033

57th/N

- 140 -



843 Benzyl butyrate Benzyl butyrate Benzyl butanoate; Benzyl n-butyrate; Aldehyde C-19 (so

called)

2140 277 103-37-7 178.23 C11 H14 O2 colourless liquidwith a heavy fruity-

floral, plum-likeodour

844 Benzyl isobutyrate Benzyl 2-methylpropanoate

Benzyl 2-methylpropanoate;Phenylmethyl isobutyrate;Pineapple aldehyde C-19

2141 301 103-28-6 178.23 C11 H14 O2 colourless liquidwith a fresh, fruity-

floral odour

845 Benzyl isovalerate Benzyl 3-methylbutyrate

Benzyl isovalerianate;Benzyl-3-methylbutyrate;

Benzyl isopentanoate

2152 453 103-38-8 192.26 C12 H16 O2 colourless liquidwith a powerful,

fruity, apple odour

846 Benzyl trans-2-methyl-2-butenoate

Benzyl 2-methyl-trans-2-butenoate

Benzyl tiglate; Benzyl-2-methylcrotonate; Benzyl

trans-2,3-dimethyl-acrylate

3330 2184 37526-88-8 190.24 C12 H14 O2 colourless liquidwith a mushroomodour with rosy

undertone

847 Benzyl 2,3-dimethylcrotonate

Benzyl 2,3-dimethyl-trans-2-butenoate

Benzyl methyltiglate 2143 11868 7492-69-5 204.27 C13 H16 O2 colourless oilyliquid with a

powerful, warm,herbaceous, fruity-

spicy

848 Benzyl acetoacetate Benzyl 3-oxobutyrate Benzyl acetylacetate; Benzylbeta-ketobutyrate; Benzyl 3-

oxobutanoate

2136 244 5396-89-4 192.21 C11 H12 O3 colourless oilyliquid with abalsamic,

herbaceous, fruityodour

849 Benzyl phenylacetate Benzyl phenylacetate Benzyl alpha-toluene;Phenylmethyl phenylacetate

2149 232 102-16-9 226.28 C15 H14 O2 colourless liquidwith a sweet,

honey-floral odour

850 Benzoic acid Benzoic acid Benzenecarboxylic acid;Carboxybenzene; Phenylformic acid; Dracylic acid

2131 21 65-85-0 122.12 C7 H6 O2 white crystal scalesor needles with a

faint urine, almondodour

851 Methyl benzoate Methyl benzoate Methyl benzenecarboxylate;Oil of niobe; Niobe oil

2683 260 93-58-3 136.15 C8 H8 O2 colourless liquidwith a pungent,

heavy, floral odourwith fruity

undertones

852 Ethyl benzoate Ethyl benzoate Ethyl benzenecarboxylate 2422 261 93-89-0 150.18 C9 H10 O2 colourless slightlyoily liquid with awarm, heavy,

floral-fruity odour

853 Propyl benzoate Propyl benzoate n-Propylbenzenecarboxylate

2931 677 2315-68-6 164.21 C10 H12 O2 colourless oilyliquid with a warm,

herbaceous,balsamic, nut-like

odour

854 Hexyl benzoate Hexyl benzoate Agrumat; n-Hexylbenzenecarboxylate


woody, green,piney, balsamic

odour

855 Isopropyl benzoate Isopropyl benzoate 1-Methylethyl benzoate 2932 652 939-48-0 164.21 C10 H12 O2 colourless oilyliquid with a heavy,sweet, fruity-floral

odour

856 Isobutyl benzoate Isobutyl benzoate Isobutylbenzenecarboxylate; 2-Methylpropyl benzoate;

Eglantine

2185 567 120-50-3 178.23 C11 H14 O2 colourless oilyliquid with a green,floral, leafy odour

857 Isoamyl benzoate Isopentyl benzoate 3-Methylbutyl benzoate 2058 2307 94-46-2 192.26 C12 H16 O2 colourless oilyliquid with a mild,sweet, fruity-like

odour

- 141 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity



843 insoluble in water,glycols, glycerol;soluble in organic

solvents, oils


239 IR 98 1.0 1.490-1.500

1.005-1.012

57th/N

844 insoluble in water andglycerin, soluble in



229 IR 97 1.0 1.488-1.492

1.000-1.006

57th/N

845 insoluble in water;poorly soluble in

glycerol, propyleneglycol; soluble in oils


246 IR 98 1.0 1.482-1.490

0.981-0.989

57th/N


solvents, oils


250 IR 95 1.0 1.515-1.526

1.029-1.040

57th/N


solvents, oils


259 NMR 97 1.0 [req.] [req.] 57th/N,T RI, SG


solvents, oils


249 IR 98 3.0 1.498-1.520

1.112-1.120

57th/N


solvents, oils


320 IR 98 1.0 1.552-1.560

1.094-1.100

57th/N

850 insoluble in cold water;moderately soluble inhot water; soluble in

oils and glycerol

very soluble 249 IR 99 - NA NA mp: 122° 57th/N

851 insoluble in water,glycerol; soluble in



198 IR 98 1.0 1.513-1.520

1.082-1.089

57th/N




212 IR 98 1.0 1.502-1.508

1.043-1.050

57th/N


solvents, oils


229 IR 98 1.0 1.498-1.503

1.020-1.026

57th/N




272 IR 98 1.0 1.490-1.500

0.978-0.984

57th/N


solvents, oils


218 IR 98 1.0 1.492-1.497

1.005-1.011

57th/N


solvents, oils


240 IR 98 1.0 1.489-1.496

0.994-0.999

57th/N


solvents, oils


261 IR 98 (sumof

isomers)

1.0 1.491-1.497

0.984-0.992

57th/N

- 142 -



858 cis-3-Hexenyl benzoate cis-3-Hexenylbenzoate

3688 11778 25152-85-6 204.27 C13 H16 O2 colourless oilyslightly viscous

liquid with a green,herbaceous,woody odour

859 Linalyl benzoate 1,5-Dimethyl-1-vinylhex-4-enyl

benzoate

Linalool benzoate; 3,7-Dimethyl-1,6-octadien-3-yl

benzoate

2638 654 126-64-7 258.36 C17 H22 O2 yellowish to amberliquid with a heavy,

floral, balsamic,fruity odour

860 Geranyl benzoate 3,7-Dimethylocta-2(trans),6-dienyl

benzoate

Geraniol benzoate; trans-3,7-Dimethyl-2,6-octadien-1-

yl benzoate

2511 639 94-48-4 258.36 C17 H22 O2 colourless toyellowish oily liquidwith a mild, floral

odour

861 Glyceryl tribenzoate Propanetri-1,2,3-yltribenzoate

Tribenzoin 3398 614-33-5 404.42 C24 H20 O6 white crystallinesolid with little or

no odour

862 Propylene glycoldibenzoate

Propan-1,2-diyldibenzoate

3419 10890 19224-26-1 284.31 C17 H16 O4 colourless liquidwith virtually no

odour

863 Methylbenzyl acetate(mixed o,m,p)

Mixture of o-Methylbenzyl acetateand m-Methylbenzyl

acetate and p-Methylbenzyl acetate

Acetoxymethyl-toluene(o,m,p); Tolubenzyl acetate

(o,m,p); Tolyl carbinylacetate (o,m,p); Tolyl

acetate

3702 29759-11-3 164.20 C10 H12 O2 colourless liquidwith a powerful

sweet floral-fruity,herbaceous odour

864 p-Isopropylbenzyl alcohol 4-Isopropylbenzylalcohol

Cumin alcohol; Cuminol;Cuminyl alcohol; Cuminic

alcohol; p-Cymen-7-ol

2933 88 536-60-7 150.22 C10 H14 O colourless to paleyellow oily liquid

with a spicy,caraway-like odour

865 4-Ethylbenzaldehyde 4-Ethylbenzaldehyde p-Ethylbenzaldehyde 3756 705 4748-78-1 134.18 C9 H10 O colourless to paleyellow liquid with a

sweet, bitter-almond odour

866 Tolualdehydes (mixedo,m,p)

Mixture of o-Methylbenzaldehyde

and m-Methylbenzaldehyde

and p-Methylbenzaldehyde

Toluic aldehyde (mixedo,m,p); Tolyl aldehyde

(mixed o,m,p)

3068 115 1334-78-7 120.15 C8 H8 O colourless oilyliquid with a sweet,herbaceous, bitter-

almond odour

867 Tolualdehyde glycerylacetal (mixed isomers)

2-(2,3and 4-Methylphenyl)-5-

hydroxy-1,3-dioxaneand 2-(2,3 and 4-Methylphenyl)-5-

hydroxymethyl-1,3-dioxolane (mixture)

Tolyl glycerin; Mixture of 2-(o,m,p-Cresyl)-5-hydroxy

dioxane and 2-(o,m,p-Cresyl)-5-

hydroxymethyldioxolane

3067 46 1333-09-1 194.23 C11 H14 O3 colourlesssomewhat viscousliquid with a faint,

bitter-almondodour

868 Cuminaldehyde 4-Isopropylbenz-aldehyde

p-Isopropylbenzaldehyde;Cumaldehyde; Cuminal;

Cuminic aldehyde

2341 111 122-03-2 148.20 C10 H12 O colourless to paleyellow liquid with astrong, pungent,

spicy, green,herbaceous odour

869 2,4-Dimethylbenzal-dehyde

2,4-Dimethylbenza-dehyde

2,4-Xylylaldehyde; 1-Formyl-2,4-dimethylbenzene

3427 15764-16-6 134.18 C9 H10 O colourless liquidwith a mild, sweet,

bitter-almondodour

870 Butyl p-hydroxybenzoate Butyl 4-hydroxy-benzoate

Butyl paraben; Butylparasept; Butyl 4-hydroxybenzoate

2203 525 94-26-8 194.23 C11 H14 O3 white crystals withlittle or no odour

- 143 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity



858 insoluble in water;soluble in organicsolvents, fats, oils


130(5 mm Hg)

IR 95 (sumof

isomers)

2.0 1.503-1.514

0.995-1.004

57th/N


solvents, oils


263 IR 95 bychemicalanalysis

(equivalence =

129.08)

5.0 1.505-1.526

0.978-0.999

57th/N


solvents, oils


305 IR 95 bychemicalanalysis

(equivalence =

129.08)

1.0 1.514-1.521

0.980-0.990

57th/N

861 insoluble in water;some solubility inorganic solvents

slightly soluble atroom temperature

n/a IR 95 1.0 NA NA mp: 68-72° 57th/N,T Function


solvents, oils


232(12 mm Hg)

IR 96 2.0 1.542-1.547

1.157-1.163

57th/N,T Function


solvents, oils


215-222 IR 98 (sumof o,m,p-isomers)

1.0 1.500-1.510

1.024-1.040

57th/N


solvents, oils


248 IR 97 - 1.518-1.525

0.974-0.982

57th/N


solvents, oils


220 IR 97 3.0 1.538-1.542

0.980-1.000

57th/N




198 IR 94 (sumof o,m,p-isomers)

10.0 1.540-1.549

1.013-1.029

57th/N,T Low assay


organic solvents, mostoils


292; 160(10 mm Hg)

IR 95 (sumof o,m,p-isomers)

1.0 1.527-1.537

1.148-1.158

57th/N


solvents, oils


235-236 IR 95 bychemicalanalysis

5.0 1.527-1.534

0.973-0.981


57th/N


solvents, oils


215 NMR 95 2.0 1.548-1.552

0.992-1.017

57th/N

870 insoluble in water;soluble in ether,

acetone and propyleneglycol, slightly soluble

in oils

soluble 156-157(3.5 mm

Hg)

IR 98 1.0 NA NA mp: 67-70° 57th/N,T Function

- 144 -



871 Anisyl alcohol 4-Methoxybenzylalcohol

Anisalcohol; Anise alcohol;Anisic alcohol


liquid or opaquecrystalline mass

with a mild, sweet,floral odour

872 Anisyl formate 4-Methoxybenzylformate

4-Methoxybenzyl formate; p-Methoxybenzyl formate;

Anisyl methanoate


sweet, floral,herbaceous-green

odour

873 Anisyl acetate 4-Methoxybenzylacetate

p-Methoxybenzyl acetate; 1-Methoxy-4-

acetoxymethylbenzene;Cassie ketone


floral, fruity,balsamic odour

874 Anisyl propionate 4-Methoxybenzylpropanoate

p-Methoxybenzylpropionate; Anisyl

propanoate


liquid with a sweet,fruity, floral, vanilla-

like odour

875 Anisyl butyrate 4-Methoxybenzylbutanoate

p-Methoxybenzyl butyrate 2100 286 6963-56-0 208.26 C12 H16 O3 colourless liquidwith a weak, floral,very sweet, plum-

like odour

876 Anisyl phenylacetate 4-Methoxybenzylphenylacetate

Anisyl alpha-toluene; p-Methoxybenzylphenylacetate

3740 233 102-17-0 256.30 C16 H16 O3 colourless oilyliquid with a faint,

honey-like,balsamic-rosy

odour

877 Veratraldehyde 3,4-Dimethoxybenz-aldehyde

Methyl vanillin;Protocatechualdehydedimethyl ether; Vanillinmethyl ether; Veratric

aldehyde

3109 106 120-14-9 166.18 C9 H10 O3 white crystallinesolid

878 p-Methoxybenzaldehyde 4-Methoxybenzal-dehyde

p-Anisaldehyde; Anisicaldehyde; Aubepine

2670 130 123-11-5 136.15 C8 H8 O2 colourless toslightly yellowliquid with a

Intensely sweet,floral odour

879 p-Ethoxybenzaldehyde 4-Ethoxybenzaldehyde Homoanisaldehyde 2413 626 10031-82-0 150.18 C9 H10 O2 colourless liquidwith a sweet, floral,

anise odour

880 Methyl o-methoxybenzoate

Methyl 2-methoxybenzoate

Methyl o-anisate; Methylsalicylate methyl ether;

Dimethyl salicylate

2717 2192 606-45-1 166.18 C9 H10 O3 colourless or paleyellow liquid with awarm, herbaceous,floral, spicy odour

881 2-Methoxybenzoic acid 2-Methoxybenzoicacid

o-Anisic acid; o-Methoxybenzoic acid;

Salicylic acid methyl ether

3943 579-75-9 152.15 C8 H8 O3 white crystallineneedles withpractically no

odour


m-Anisic acid; m-Methoxybenzoic acid;

3944 586-38-9 152.15 C8 H8 O3 white crystals,practicallyodourless


Anisic acid; p-Anisic acid; p-Methoxybenzoic acid;

Draconic acid

3945 10077 100-09-4 152.15 C8 H8 O3 white crystals withpractically no

odour

884 Methyl anisate Methyl 4-methoxybenzoate

Methyl p-methoxybenzoate;Methyl p-anisate

2679 248 121-98-2 166.18 C9 H10 O3 white crystals witha sweet, floral

odour

- 145 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity



871 insoluble in water;poorly soluble inglycols, glycerol;soluble in organic

solvents, oils

miscible above20°

259 IR 97 1.0 1.540-1.547

1.107-1.115

mp: 24-25° 57th/N

872 insoluble in water,glycerol, propyleneglycol; soluble in



220 IR 90 3.0 1.519-1.525

1.136-1.145

57th/N,T Low assay




235 IR 97 1.0 1.511-1.517

1.104-1.111

57th/N




100-103(0.5 mm

Hg)

IR 97 1.0 1.505-1.510

1.070-1.086

57th/N


solvents, oils


270 IR 97 1.0 1.500-1.505

1.047-1.067

57th/N


solvents, oils


370 IR 97 1.0 1.553-1.563

1.125-1.133

57th/N

877 insoluble in cold water;soluble in hot water

oils

soluble 281 IR 95 2.0 NA NA mp: 42-45° 57th/N

878 poorly soluble inwater, glycols,

glycerol; soluble inorganic solvents, oils


248 IR 97 6.0 1.568-1.574

1.115-1.123

57th/N

879 poorly soluble inwater, glycols,

glycerol; soluble inorganic solvents, oils


250(minimum)

IR 97 6.0 1.556-1.564

1.078-1.084

57th/N




246 IR 97 1.0 1.529-1.537

1.144-1.160

57th/N

881 soluble in boilingwater, organic

solvents

freely soluble 200 IR 98 byacid/basetitration

- NA NA mp: 98-99° 57th/N


solvents

freely soluble 170-172 IR 98 byacid/basetitration

- NA NA mp: 107-109° 57th/N


solvents

freely soluble 275-280 IR 98 byacid/basetitration

- NA NA m.p = 184° 57th/N



soluble 255 IR 97 1.0 NA NA mp: 48° 57th/N

- 146 -



885 Ethyl p-anisate Ethyl 4-methoxybenzoate

Ethyl p-methoxybenzoate;Ethyl anisate

2420 249 94-30-4 180.20 C10 H12 O3 colourless oilyliquid with a light,fruity-floral, anise-

like odour

886 Vanillyl alcohol 4-Hydroxy-3-methoxybenzyl alcohol

4-Hydroxy-3-methoxybenzylalcohol

3737 690 498-00-0 154.17 C8 H10 O3 white or colourlesscrystals with amild, sweet,

balsamic, vanilla-like odour

887 Vanillyl ethyl ether 4-(Ethoxymethyl)-2-methoxyphenol

VEE; Ethyl 4-hydroxy-3-methoxybenzyl ether

3815 13184-86-6 182.22 C10 H14 O3 pale amber toyellow liquid with aphenolic, smoky

odour

888 Vanillyl butyl ether 4-(Butoxymethyl)-2-methoxyphenol

3796 82654-98-6 210.27 C12 H18 O3 colourless to paleyellow viscous

liquid with a weak,vanillic, acidic

odour

889 Vanillin 4-Hydroxy-3-methoxybenzaldehyde

Vanillaldehyde; Vanillicaldehyde;

Methylprotocatechuicaldehyde

3107 107 121-33-5 152.15 C8 H8 O3 white or slightlyyellow needles orcrystalline powder

with a sweet,creamy, vanilla

odour

890 Vanillin acetate 4-Acetoxy-3-methoxybenzaldehyde

Acetylvanillin; 3-Methoxy-4-acetoxybenzaldehyde

3108 225 881-68-5 194.19 C10 H10 O4 colourless needlesof plates with amild creamy,

balsamic, vanillaodour

891 Vanillin isobutyrate 4-Formyl-2-methoxyphenyl 2-methylpropanoate

4-Hydroxy-3-methoxybenzaldehyde; 4-

Hydroxy-m-anisaldehyde 2-methyl propionate

3754 20665-85-4 222.24 C12 H14 O4 colourless liquidwith a heavy,

sweet, creamy,vanilla-nutmeg

odour

892 Ethyl vanillin beta-d-glucopyranoside

Glucoethylvanillin 3801 122397-96-0 328.32 C15 H20 O8 white powder witha very slight vanilla

odour

893 Ethyl vanillin 3-Ethoxy-4-hydroxybenzaldehyde

3-Ethoxyprotocatechualdehyde;Bourbonal ethyl protal

2464 108 121-32-4 166.18 C9 H10 O3 colourless orslightly yellow

crystal flakes withan intense vanilla

odour

894 Piperonyl acetate 3,4-Methylene-dioxybenzyl acetate

Heliotropyl acetate;Heliotropin acetate

2912 2068 326-61-4 194.19 C10 H10 O4 colourless oilyliquid with a sweet,

light, floral-fruityodour

895 Piperonyl isobutyrate 3,4-Methylene-dioxybenzylisobutyrate

Heliotropyl 2-methylpropanoate;

2913 305 5461-08-5 222.24 C12 H14 O4 colourless oilyliquid with a mild,fruity, berry-like

odour

896 Piperonal 3,4-Methylene-dioxybenzaldehyde

Heliotropin;Piperonylaldehyde

2911 104 120-57-0 150.13 C8 H6 O3 white or colourlesscrystals with a

sweet, floral, spicyodour

897 Salicyladehyde 2-Hydroxy-benzaldehyde

o-Hydroxybenzaldehyde;Salicylal

3004 605 90-02-8 122.12 C7 H6 O2 colourless to strawcoloured oily liquid

with a pungent,bitter, almond-like

odour

898 2-Hydroxy-4-methylbenzaldehyde

2-Hydroxy-4-methylbenzaldehyde

2,4-Cresotaldehyde; 4-Methylsalicylaldehyde

3697 2130 698-27-1 136.15 C8 H8 O2 colourless to lightstraw crystals with

a strong, bitter-almond, phenolic

odour

- 147 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity




solvents, oils


270 IR 97 1.0 1.522-1.528

1.101-1.105

57th/N

886 soluble in hot water,organic solvents, oils

soluble n/a(decom-poses at

the meltingpoint)

IR 98 - NA NA mp: 115° 57th/N


solvents, oils


212 NMR 98 - 1.528-1.532

1.106-1.113

57th/N


solvents, oils


241 IR 95 - 1.511-1.521

1.048-1.068

57th/N



freely soluble 285 IR 97 - NA NA mp: 80-81° 57th/N



soluble 148(10 mm Hg)

IR 97 1.0 NA NA mp: 77-79° 57th/N


solvents, oils


130-132(2 mm Hg)

IR 98 2.0 1.522-1.526

1.110-1.136

57th/N

892 slightly soluble inwater; insoluble in fats,

oils

slightly soluble n/a(decom-poses onheating)

NMR 99 byHPLC

- NA NA mp: 199-200° 57th/N


solvents, oils

very soluble (1gin 2ml)

285 IR 98 - NA NA mp: 78° 57th/N


solvents, oils


150-151(10 mm Hg)

IR 97 2.0 1.523-1.529

1.227-1.239

57th/N


solvents, oils


91-92(0.005 mm

Hg)

IR 97 1.0 1.506-1.513

1.154-1.160

57th/N



freely soluble 263 IR 98 3.0 NA NA mp: 37° 57th/N




196-197 IR 95 10.0 1.570-1.576

1.159-1.170

57th/N


solvents, oils

freely soluble 207 IR 98 - NA NA mp: 57° 57th/N

- 148 -



899 Methyl salicylate Methyl 2-hydroxybenzoate

Methyl o-hydroxybenzoate;Synthetic wintergreen oil;Synthetic sweet birch oil;

Synthetic teaberry oil

2745 433 119-36-8 152.15 C8 H8 O3 colourless toyellowish liquid

with acharacteristic

wintergreen odour

900 Ethyl salicylate Ethyl 2-hydroxybenzoate

Ethyl o-hydroxybenzoate;Salicylic ether; Sal ether


spicy, anisic,wintergreen-like

odour

901 Butyl salicylate Butyl 2-hydroxybenzoate

n-Butyl o-hydroxybenzoate;Nefolia

3650 614 2052-14-4 194.23 C11 H14 O3 colourless liquidwith a rough,herbaceous,

chemical odourwith trace ofwintergreen

902 Isobutyl salicylate Isobutyl 2-hydroxybenzoate

Isobutyl o-hydroxybenzoate;2-Methylpropyl 2-hydroxybenzoate

2213 434 87-19-4 194.23 C11 H14 O3 colourless to paleyellow liquid with asomewhat harsh,floral, herbaceous

odour

903 Isoamyl salicylate Isopentyl 2-hydroxybenzoate

Isopentyl salicylate; Isoamylo-hydroxybenzoate

2084 435 87-20-7 208.26 C12 H16 O3 colourless oilyliquid with a sweetherbaceous-green,slightly floral odour

904 Benzyl salicylate Benzyl 2-hydroxybenzoate

Benzyl o-hydroxybenzoate 2151 436 118-58-1 228.25 C14 H12 O3 colourless oilyliquid or opaquecrystalline mass

(tendency tosupercool) with afaint, sweet, floral

odour

905 Phenethyl salicylate 2-Phenylethyl 2-hydroxybenzoate

Benzyl carbinyl 2-hydroxybenzoate; 2-Phenylethyl

salicylate

2868 437 87-22-9 242.28 C15 H14 O3 white granularcrystals with afaint, balsamic,

floral odour

907 o-Tolyl salicylate 2-Methylphenyl 2-hydroxybenzoate

o-Cresyl salicylate 3734 617-01-6 228.25 C14 H12 O3 semisolid to solidwith a eucalyptus

odour

908 2,4-Dihydroxybenzoicacid

2,4-Dihydroxybenzoicacid

beta-Resorcylic acid 3798 89-86-1 154.12 C7 H6 O4 hydrated whitecrystals with a faint

phenolic odour

909 Glycerol 1,2,3-Propanetriol Glycerine;Trihydroxypropane; Cristal;

Glyceol

2525 56-81-5 92.09 C3 H8 O3 colourless syrupyliquid, odourless

with a sweet taste

910 3-Oxohexanoic aciddiglyceride

2,3-Dihydroxypropyl 3-oxohexanoate

3770 91052-72-1 316.36 C15 H24 O7 solid fatty flakeswith essentially no

odour

911 3-Oxooctanoic acidglyceride

2,3-Dihydroxypropyl 3-oxooctanoate

3771 91052-68-5 232.28 C11 H20 O5 solid fatty flakeswith a faint fatty

odour

- 149 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity






222 IR 98 2.0 1.534-1.538

1.176-1.185

57th/N

900 slightly soluble inwater, glycerol; soluble

in organic solvents,oils


234 IR 98 3.0 1.518-1.525

1.125-1.131

57th/N




268 NMR 98 1.0 1.508-1.520

1.070-1.080

57th/N




260 IR 98 1.0 1.506-1.570

1.062-1.069

57th/N


solvents, oils


277 IR 98 (sumof

isoamyland amylsalicylate)

1.0 1.504-1.509

1.046-1.055

57th/N



miscible above25°

300 IR 98 1.0 1.573-1.584

1.173-1.183

mp: 24-26° 57th/N

905 insoluble in water,glycerol, glycols;soluble in organic

solvents, oils

soluble (1 g in 20ml of 95%ethanol)

190(5 mm Hg)

IR 98 1.0 NA NA mp: 44° 57th/N

907 insoluble in water;soluble in some oils


NMR 99 1.0 1.576-1.584

1.164-1.174

57th/N

908 soluble in hot water,organic solvents, oils

soluble n/a IR 97 bychemicalanalysis

- NA NA mp: 225°(decomposes, rapid

heating required)

57th/N

909 miscible with water;insoluble in hydrocar-bons, alkyl halides,

some oils

miscible 290; 182(20 mm Hg)

IR 95 bychemicalanalysis

(Naperiodate

proce-dure)

- 1.468-1.478

1.257-1.270

57th/N,T A,Function


slightly soluble n/a NMR 95 byester

determination

2.0 NA NA 57th/N,T MP



determination

2.0 NA NA 57th/N,T MP

- 150 -



912 Heptanal glyceryl acetal(mixed 1,2 and 1,3

acetals)

Mixture of 2-Hexyl-4-hydroxymethyl-1,3-dioxolane and 2-

Hexyl-5-hydroxy-1,3-dioxane

Heptaldehyde glyceryl acetal 2542 2016 1708-35-6 188.27 C10 H20 O3 colourless viscousliquid with a mild,

sweet, mushroom-like odour

913 1,2,3-tris[(1'-Ethoxy)ethoxy]propane

1,2,3-tris([1'-Ethoxy]ethoxy)

propane

Acetaldehyde ethyl glycerylmixed acetal

3593 11930 67715-82-6 308.42 C15 H32 O6 colourless liquidwith a slight, sharp,

fruity odour

914 3-Oxodecanoic acidglyceride

2,3-Dihydroxypropyl 3-oxodecanoate


odour

915 3-Oxododecanoic acidglyceride

2,3-Dihydroxypropyl 3-oxododecanoate


odour

916 3-Oxotetradecanoic acidglyceride

2,3-Dihydroxypropyl 3-oxotetradecanoate


odour

917 3-Oxohexadecanoic acidglyceride

2,3-Dihydroxypropyl 3-oxohexadecanoate


odour

918 Glyceryl monostearate 2,3-Dihydroxypropyloctadecanoate

Monostearin; alpha-Monostearin; 1-Glyceryl

monooctadecanoate

2527 123-94-4 358.55 C21 H42 O4 white to paleyellow wax-likesolid with a mild

fatty odour

919 Glyceryl monooleate 2,3-Dihydroxypropyl 9-octadecenoate

monoolien 2526 111-03-5 356.54 C21 H40 O4 pale yellow viscousoily liquid with afaint fatty odour

920 Triacetin 1,2,3-Triacetoxy-propane

Glyceryl triacetate; Triacetylglycerine; Enzactin

2007 102-76-1 218.21 C9 H14 O6 colourless oilyliquid with a veryslight, ethereal,

fruity odour

921 Glyceryl tripropanoate 1,2,3-Tri(propionyloxy)propane

Tripropionin; Glyceryltripropionate

3286 139-45-7 260.29 C12 H20 O6 colourless to paleyellow liquid with

practically noodour

922 Tributyrin 1,2,3-Tri(butyryloxy)propane

Butyrin; Glyceryl tributyrate 2223 747 60-01-5 302.37 C15 H26 O6 colourless oilyliquid

923 Glycerol 5-hydroxydecanoate

2,3-Dihydroxypropyl 5-hydroxydecanoate

3685 10648 26446-31-1 262.35 C13 H26 O5 colourless to paleyellow viscous

liquid with a mildfatty odour

924 Glycerol 5-hydroxydodecanoate

2,3-Dihydroxypropyl 5-hydroxydodecanoate

3686 10649 26446-32-2 290.40 C15 H30 O5 colourless to paleyellow viscous oilyliquid with a mild

fatty odour

925 Propylene glycol 1,2-Propanediol 1,2-Dihydroxypropane;Methyl glycol

2940 2065 57-55-6 76.10 C3 H8 O2 colourless,hygroscopic

viscous liquid withno odour

- 151 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity






IR 96 Totalof mixedisomers

andunreactedaldehyde

1.0 1.445-1.455

0.990-1.003

57th/N


solvents, oils


NMR 97.5 1.0 1.419-1.425

0.952-0.958

57th/N



determination

2.0 NA NA 57th/N,T MP,Function


- n/a NMR 95 byester

determination




determination




determination

2.0 NA NA 57th/N,T MP.Function

918 insoluble in water;soluble in hot oils,organic solvents

soluble in hotalcohol

n/a NMR [req.] - n/a n/a mp: 56-58° 57th/N,T A,Function

919 insoluble in water;soluble in hot organic

solvents


[req.] NMR [req.] - [req.] [req.] 57th/N,T A, BP, RI,SG,

Function

920 moderately soluble inwater; soluble inorganic solvents

miscible 258 IR 98.5 bychemicalanalysis

1.0 1.424-1.432

1.154-1.159

57th/N,T Function




IR 97 2.0 1.428-1.435

1.065-1.082

57th/N,T Function


solvents, oils

miscible 308 IR 99 5.0 1.431-1.441

1.034-1.037

57th/N,T Function


solvents, oils


100-220(2 mm Hg)

IR 96.5 Totalglycerol,mono-,di- andtri-glyc-erides

10.0 1.465-1.468

1.045-1.051

57th/N,T BP range,Function


solvents, oils


120-250(1-2 mm

Hg)

IR 98 Totalglycerol,mono-,di-, andtri-glyc-erides

10.0 1.464-1.467

1.007-1.013

57th/N,T Function

925 miscible with waterand many organic

solvents


188 IR 99.5 - 1.427-1.437

1.033-1.037

57th/N,T Function

- 152 -



926 Propylene glycol stearate 2-Hydroxypropyloctadecanoate

Propylene glycolmonooctadecanoate

2942 142-75-6 342.56 C21 H42 O3 white beads orflakes with a faint

fatty odour

927 1,2-Di[(1'-ethoxy)ethoxy]propane

1,2-Di((1'-ethoxy)-ethoxy)propane

Acetaldehyde ethylpropylene glycol mixed

acetal

3534 67715-79-1 220.31 C11 H24 O4 colourless to paleyellow liquid with afaint, sharp, fruity

odour

928 4-Methyl-2-pentyl-1,3-dioxolane

4-Methyl-2-pentyl-1,3-dioxolane

Hexanal propylene glycolcyclic acetal

3630 1599-49-1 158.24 C9 H18 O2 colourless to paleyellow liquid with amild , fruity, pear-

like odour

929 2,2,4-Trimethyl-1,3-oxacyclopentane

2,2,4-Trimethyl-1,3-dioxolane

Acetone propylene glycolketal

3441 11423 1193-11-9 116.16 C6 H12 O2 colourless liquidwith a mild, musty,

sweet odour

930 Lactic acid 2-Hydroxypropanoicacid

2-Hydroxy-propionic acid;alpha-Hydroxypropanoic

acid

2611 4 598-82-3 90.08 C3 H6 O3 colourless toyellow hygroscopiccrystals becoming

syrupy liquid;odourless

931 Ethyl lactate Ethyl 2-hydroxypropanoate

Ethyl alpha-hydroxypropionate

2440 371 97-64-3 118.13 C5 H10 O3 colourless liquidwith a light

ethereal, butteryodour

932 Butyl lactate Butyl 2-hydroxypropanoate

n-Butyl alpha-hydroxypropionate

2205 372 138-22-7 146.19 C7 H14 O3 colourless liquidwith a faint, sweet,

buttery odour

933 Potassium 2-(1'-ethoxy)ethoxypropanoate

Potassium 2-(1'-ethoxy)ethoxypropano

ate

Potassium O-(1'ethoxy)ethoxypropanoate;

1-Ethoxyethyl ether ofpotassium lactate

3752 200.28 C7 H13K O4 deliquesentpowder with no

odour

934 cis-3-Hexenyl lactate cis-3-Hexenyl 2-hydroxypropanoate

Leaf lactate 3690 10681 61931-81-5 172.22 C9 H16 O3 colourless liquidwith a fruity, green

odour

935 Butyl butyryllactate Butyl 2-butyryloxypropanoate

Butyl butyrolactate 2190 2107 7492-70-8 216.28 C11 H20 O4 colourless to paleyellow liquid with a

sweet-sour,buttermilk odour

936 Pyruvic acid 2-Oxopropanoic acid 2-Ketopropionic acid;Acetylformic acid;Pyroracemic acid

2970 19 127-17-3 88.06 C3 H4 O3 colourless toamber viscous

liquid with a sourvinegar-like odour

937 Pyruvaldehyde 2-Oxopropanal Methylglyoxal; 2-Ketopropionaldehyde;Acetylformaldehyde

2969 105 78-98-8 72.06 C3 H4 O2 yellow mobilehygroscopic liquidwhich polymerizesreadily; pungentstinging odour

938 Ethyl pyruvate Ethyl 2-oxopropanoate Ethyl acetylformate; Ethylalpha-ketopropionate; Ethyl

pyroracemate

2457 430 617-35-6 116.12 C5 H8 O3 colourless liquidwith a sweet, floral-fruity, warm odour

939 Isoamyl pyruvate 3-Methylbutyl 2-oxopropanoate

Isopentyl pyruvate; Isoamylpyroracemate

2083 431 7779-72-8 158.20 C8 H14 O3 colourless liquidwith a fresh,

caramel-rum odourwith fruity-floral

undertone

940 1,1-Dimethoxyethane 1,1-Dimethoxyethane Acetaldehyde dimethylacetal; Dimethyl acetal;

Ethylidene dimethyl ether

2436 510 534-15-6 90.12 C4 H10 O2 volatile colourlessliquid with a sharp,

green, etherealodour

- 153 -


BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity



926 insoluble in water soluble in alcohol n/a NMR [req.] 4.0 n/a n/a 57th/N,T A, MP,Function

927 slightly soluble inwater; miscible with



NMR 97 1.0 1.408-1.414

0.911-0.925

57th/N




82(18 mm Hg)

IR 97 (sumof

isomers)

1.0 1.418-1.425

0.893-0.901

57th/N

929 soluble in water;organic solvents, oils

miscible 98-99 NMR 98 1.0 1.393-1.398

0.899-0.905

57th/N

930 miscible with water,glycerol, glycols, oils


122(15 mm Hg)

IR 95 bychemicalanalysis

(acid/base

titration)

- 1.413-1.429

1.200-1.209

mp: 17° 57th/N

931 miscible with water;soluble in organic

solvents, oils

miscible 154 IR 97 5.0 1.408-1.422

1.029-1.037

57th/N



miscible 185-187; 76(6 mm Hg)

IR 95 1.0 1.418-1.424

0.974-0.984

57th/N

933 freely soluble in water,solvents, oils

slightly soluble n/a NMR 98 byacid/basetitration

- NA NA 57th/N




96(7 mm Hg)

IR 96 1.0 1.441-1.451

0.968-0.984

57th/N


organic solvents, oils,propylene glycol


90(2 mm Hg)

IR 95 1.0 1.417-1.427

0.966-0.978

57th/N

936 miscible with water;soluble in organic

solvents, oils


164 IR 95 - 1.424-1.435

1.260-1.281

mp: 13° 57th/N

937 miscible with waterand most solvents andoils (yellow solutions)

miscible 72 NMR 95 bychemicalanalysis

10.0 1.399-1.406

1.041-1.048

Polymer dissolves inwater with evolution of

heat, reverting tomonomer; only

available as 40%aqueous solution

57th/N,T A(m), Seenote




144 IR 95 2.0 1.403-1.409

1.044-1.065

57th/N


solvents, oils


185 IR 97 2.0 1.417-1.424

0.972-0.980

57th/N

940 miscible with water,organic solvent, oils

miscible 64 IR 96 1.0 1.365-1.367

0.850-0.860

57th/N

- 154 -



941 Acetal 1,1-Diethoxyethane Acetaldehyde diethyl acetal;Diethylacetal; Ethylidene

diethyl ether

2002 35 105-57-7 118.18 C6 H14 O2 volatile colourlessliquid with arefreshing,

pleasant, fruity-green odour

942 Octanal dimethyl acetal 1,1-Dimethoxyoctane Aldehyde C-8 dimethylacetal; Capryl aldehydedimethyl acetal; Resedyl

acetal

2798 42 10022-28-3 174.28 C10 H22 O2 colourless liquidwith a green,

woody, citrusyodour

943 Acetaldehyde ethyl cis-3-hexenyl acetal

1-Ethoxy-1-(cis-3-hexenyloxy)ethane

Ethyl cis-3-hexenyl acetal;Leaf acetal; Leaf alcohol

ethyl acetal

3775 28069-74-1 172.27 C10 H20 O2 colourless mobileliquid with a

powerful, green,herbaceous odour

944 Citral dimethyl acetal 1,1-Dimethoxy-3,7-dimethyl-2,6-octadiene

3,7-Dimethyl-2,6-octadienyldimethyl acetal

2305 39 7549-37-3 198.31 C12 H22 O2 colourless toyellowish liquid

with a mild, fresh,citrus, herbaceous

odour

945 Decanal dimethyl acetal 1,1-Dimethoxydecane Aldehyde C-10 dimethylacetal; Capraldehyde

dimethyl acetal

2363 43 7779-41-1 202.34 C12 H26 O2 colourless liquidwith a herbaceous,green, citrus-floral

odour

946 2,6-Nonadienal diethylacetal

1,1-Diethoxy-2,6-nonadiene

3378 660 67674-36-6 212.33 C13 H24 O2 colourless oilyliquid with a fresh,green, cucumber

odour

947 Heptanal dimethyl acetal 1,1-Dimethoxyheptane Enanthal dimethyl acetal;Oenanthal dimethyl acetal;

Heptaldehyde dimethylacetal

2541 2015 10032-05-0 160.26 C9 H20 O2 colourless oilyliquid with a green,

herbaceous,somewhat nutty

odour

948 Citral diethyl acetal 1,1-Diethoxy-3,7-dimethyl-2,6-octadiene

Citrathal; 3,7-dimethyl-2,6-octadienal diethyl acetal

2304 38 7492-66-2 226.36 C14 H26 O2 colourless liquidwith a mild, green,

citrusy,herbaceous odour

949 4-Heptenal diethyl acetal 1,1-Diethoxy-4-heptene

3349 10011 18492-65-4 186.29 C11 H22 O2 colourless oilyliquid with a mild,

pleasant,herbaceous, fruit,melon-like odour

950 2-Acetyl-3-methyl-pyrazine

2-Acetyl-3-methylpyrazine

2-Acetyl-3-methyl-1,4-diazine

11296 23787-80-6 136.15 C7 H8 N2 O colourless to lightyellow liquid with a

nutty, roastedgrain, baked potato

odour

951 Pyrazine Pyrazine 1,4-Diazine; Paradiazine 11363 290-37-9 80.09 C4 H4 N2 deliquescentcrystals or wax-like

solid with apungent, sweet,corn-like, nutty

odour

952 5,6,7,8-Tetrahydro-quinoxaline

5,6,7,8-Tetrahydro-quinoxaline

Cyclohexapyrazine 3321 721 34413-35-9 134.18 C8 H10 N2 low melting wax-like colourless tolight yellow solid

953 Ethyl vanillin isobutyrate 2-Ethoxy-4-formylphenylisobutyrate

3837 188417-26-7 236.27 C13 H16 O4 white to light yellowpowder

954 Ethyl vanillin propyleneglycol acetal

2-(3-Ethoxy-4-hydroxyphenyl)-4-

methyl-1,3-dioxolane

3838 68527-76-4 224.26 C12 H16 O4 colourless to paleyellow liquid with afaint vanillic odour

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BoilingPoint (°C)

ID Test Assaymin

Acidvaluemax

Refractiveindex

Specificgravity



941 slightly soluble inwater; miscible with

most organic solvents,oils

miscible 102 IR 95 1.0 1.378-1.386

0.822-0.831

57th/N


solvents, oils


185; 60(15 mm Hg)

IR 95 3.0 1.410-1.420

0.841-0.851

57th/N


solvents, oils


85(7 mm Hg)

IR 97 2.0 1.419-1.443

0.846-0.856

57th/N,T RI range


solvents, oils


105-106(10 mm Hg)

IR 92 (sumof

isomers)

2.0 1.450-1.463

0.881-0.893

Minimum assay (sumof isomers +

hemiacetals + citral):98%

57th/N


solvents, oils


218; 77-79(1 mm Hg)

IR 95 1.0 1.420-1.430

0.830-0.852

57th/N


solvents, oils


125(4 mm Hg)

IR 90 (sumof

isomers)

1.0 1.441-1.448

0.860-0.868

Minimum assay(named cpd. +

"isomers" + 2-nonenaldiethyl acetal): 98%

57th/N


solvents, oils


164-165; 60(1 mm Hg)

IR 98 1.0 1.405-1.415

0.844-0.849

57th/N


solvents, oils


230; 140-142

(15 mm Hg)

IR 92 (sumof cis-and

trans-isomers)

2.0 1.445-1.455

0.864-0.879

Minimum assay (sumof isomers +

hemiacetals + citral):98%

57th/N


solvents, oils


93(15 mm Hg)

IR 97 (sumof cis-and

trans-isomers)

1.0 1.420-1.440

0.840-0.860

57th/N



90(20 mm Hg)

IR 98 - 1.521-1.523

1.105-1.114

57th/N

951 freely soluble in water,organic solvents

very soluble 115-118 IR 98 - NA NA mp: 53° 57th/N

952 moderately soluble inwater; soluble inorganic solvents

soluble 85(3 mm Hg)

IR 98 - NA NA mp: 29-30° 57th/N


solvents, oils

freely soluble n/a IR 98 2.0 NA NA mp: 57° 57th/N


solvents, oils


160(1 mm Hg)

IR 97(namedcpd. +ethyl

vanillin)

- 1.528-1.584

1.161-1.175

57th/N,T RI range

Spectra for certain flavouring agents will be available with the printed edition.

- 190 -

Section C: Principles governing the establishment and revision of specifications

Inclusion of raw materials and manufacturing methods in specifications

With increasing volumes of food additives in international trade, it is becoming increasingly important thatspecifications include raw materials and methods of manufacture in order to provide a full account of theproduct that was evaluated. Without this information, a product could be produced from different materialsby different methods; consequently, impurities might have arisen that were not considered during thetoxicological evaluation of the substance.Principles for the safety assessment of food additives and contaminants in food states that ‘To establish thechemical identities of additives, it is necessary to know the nature of the raw materials, methods ofmanufacture and impurities. This information is used to assess the completeness of analytical data on thecomposition of additives, and to assess the similarity of materials used in biological testing with thosecommercially produced.’Therefore, the specifications other than those for flavouring agents will include brief details of raw materialsand methods of manufacture, excluding proprietary details. The level of detail should be similar to thatalready used in many specifications published by the committee for additives made by fermentation or fromplant materials.

Revision of the Guide to specifications

The Committee strongly reiterated its recommendation at the fifty-fifth meeting for revision of the Guide tospecifications. This revision is urgent so that significant developments in methods of analysis can beincluded.‡

Modified starches

The Committee recommended that the present specification monograph that covers 16 modified starchesshould be divided into smaller monographs because the present document is very long and changes to onespecification requires revision of the entire monograph.

General Specifications and Recommendations for Enzyme Preparations

The Committee has, on many occasions, addressed issues related to specifications for enzyme preparationsused in food processing. The General Specifications in use today for enzymes were first elaborated by theCommittee at its twenty-sixth meeting. Several revisions have been made, including 1) an addendum toaddress issues related to enzymes from genetically modified microorganisms; 2) addition of an appendix todescribe the method for determining antibiotic activity (FNP 19); 3) an amendment to address microbialstrain numbers in the specifications for enzyme preparations; and 4) addition of the general requirement thatsource microorganisms be non-pathogenic and non-toxigenic.

At its fifty-fifth meeting, the Committee requested that the General Specifications for enzymes be reviewedand revised. Special consideration was to be given to updating the specifications in light of recenttechnological advances and to ensure consistency and coherence.

The revised General Specifications require that all new enzyme preparations undergo a general safetyassessment. Many of the requirements previously outlined for enzyme preparations from geneticallymodified microorganisms are appropriate for all preparations, regardless of source, and the presentCommittee revised the General Specifications to reflect those requirements. For enzymes from geneticallymodified sources, focus is now placed on the final microbial strain used as the source organism and thegenetic material introduced into and remaining in the final microbial production strain.

‡ A corresponding project by the FAO Joint Secretariat is currently under preparation. Further information will beavailable at at FAO's JECFA web-site (http://www.fao.org/es/ESN/jecfa/).

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At its fifty-fifth meeting, the Committee noted that the list of mycotoxins contained in the existing GeneralSpecifications was not relevant to all food enzyme preparations from fungal sources. It further agreed that anattempt to list all known mycotoxins of potential concern was impractical and unwarranted. At its presentmeeting, the Committee agreed that enzyme preparations derived from fungal sources be evaluated for thosemycotoxins that are known to be produced by strains of the species used in the production of the enzymepreparation or related species.

With regard to limits on heavy metals, the Committee agreed that the specification for lead contained in theexisting General Specifications should be lowered from 10 mg/kg to 5 mg/kg. The Committee recognizedthat arsenic is not a concern in enzyme preparations, and the limit for this metal was deleted. Moreover, asthere is no traceable source of cadmium or mercury in enzyme preparations, the Committee saw no need toestablish limits for those metals. Such changes are consistent with the Committee’s current policy (Note byjlh: report of the fifty-fifth meeting or specifications should be referenced here? Is a reference necessary?) onheavy metals.

In considering microbiological contamination of enzyme preparations, the Committee agreed that theexisting microbiological criteria (for Salmonella spp., Escherichia coli, and total coliforms) and therequirement that use of preparations not increase the total microbial count in treated food over the levelconsidered to be acceptable for the respective food are sufficient to ensure microbial safety and were thusretained. The Committee noted that the specification for a total viable count of 5 x 104/g contained in theexisting General Specifications is arbitrary and is not an indication of the safety of an enzyme preparation.Therefore, it was eliminated.

In considering allergenic potential, the Committee emphasized that when the source organism of an enzymepreparation is a genetically modified microorganism the need for an evaluation for allergenic potential of thegene products encoded by the inserted DNA should be assessed. The Committee agreed that when the DNAsequence of an enzyme from a genetically modified production microorganism is comparable to that codingfor an enzyme already known to have a history of safe use in food, there would be no need to assess theallergic potential of that enzyme further.

Finally, the Committee recognized that the revised Specifications include many criteria for safety evaluationthat would be more appropriately listed elsewhere. The Committee strongly recommended that Principles forthe safety assessment of food additives and contaminants in food be revised to include the safety assessmentof enzymes intended for use in food and subsequent removal of such guidelines from the GeneralSpecifications

The Committee recognized that the revised General Specifications and Recommendations for EnzymePreparations Used in Food Processing contain many safety evaluation criteria that are more appropriate forelaboration elsewhere. The Committee recommended that the update and consolidation of the principles andmethods for the assessment of chemicals in food includes the safety assessment of enzymes intended for usein food and a subsequent removal of these guidelines from the General Specifications.

Revision of metals limits for food additives

At its fifty-fifth meeting, the Committee began its implementation of a systematic five-year programme toreplace the outdated test for heavy metals (as lead) in all existing food additive specifications withappropriate limits for individual metals of concern. Proposed lead and arsenic limits for 43 emulsifiers wereestablished. As no alternative proposals were received by the Secretariat prior to the deadline for submissionof data for the present meeting, the new published limits were adopted, replacing those published in FNP 52and its addenda 1 to 7.

The second group of substances, considered at the present meeting, included 10 anticaking agents, 17 flavourenhancers, 10 sweetening agents, and 13 thickening agents. In response to the call for data, proposed limitsand supporting data were received for sodium ferrocyanide. Comments and proposals were received only forcalcium silicate, magnesium silicates, silicon dioxide, sodium aluminiumsilicate, monosodium glutamate,

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sorbitol, lactitol, xylitol, ammonium alginate, tara gum, methylcellulose, ethylcellulose,methylethylcellulose, powdered cellulose, hydroxypropylcellulose, and hydroxypropylmethylcellulose. Allcomments, proposals, and supporting data were taken into account. Comments on the Committee’s newproposed limits are invited. Where higher limits are requested, analytical data in support of such limits mustbe provided. If alternative values and supporting data are not received by the deadline for submission of datafor the fifty-ninth meeting, the proposed metal limits will supersede the existing metals limits, replacingthose published in FNP 52 and its addenda 1 to 8.

In summary, the proposed changes to the current limits were as follows:• Limits for arsenic were deleted except for ferrocyanides of calcium, potassium and sodium, for

which a limit of 3 mg/kg was proposed.• Proposed limits for lead for thickening agents and magnesium oxide were 2 mg/kg, for flavour

enhancers and sweetening agents 1 mg/kg, for phosphates 4 mg/kg, and for silicate anticaking 5mg/kg.

• No limits were proposed for cadmium or mercury, as there were no concerns for their presence inany of the substances under review.

• Limits for heavy metals (as lead) were deleted.

The Committee emphasized that, following replacement of the Limit Test for Heavy Metals (as lead) byindividual elements, the absence of a particular metal from a specification means that the level ofcontamination is so low as to be of no concern.

The Committee recommended continuation of its activity to update limits for heavy metals in food additivesand concluded that acidity regulators and colours should be reviewed at its next meeting on food additivesand contaminants.

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Category Additive name INS Sub As Pb Hg Cd OtherElementsAnticaking agent Aluminium silicate 0559 - 5 - -

Anticaking agent Calcium aluminium silicate 0556 - 5 - - F<50Anticaking agent Calcium silicate 0552 - 5 - - F<50Anticaking agent Ferrocyanides of Ca, K & Na 0538 3 5 - - Cu<10, Zn<25Anticaking agent Magnesium oxide 0530 - 2 - -Anticaking agent Magnesium silicates (synthetic) 0553 a - 5 - - F<10Anticaking agent Silicon dioxide (amorphous) 0551 - 5 - -Anticaking agent Sodium aluminosilicate 0554 - 5 - -Anticaking agent Tricalcium phosphate 0341 iii - 4 - - F<50Anticaking agent Trimagnesium phosphate 0342 iii - 4 - - F<5Flavour enhancer Calcium-5’-guanylate 0629 - 1Flavour enhancer Calcium 5’-inosinate 0633 - 1Flavour enhancer Calcium 5'-ribonucleotides 0634 - 1 - -Flavour enhancer Calcium di-L-glutamate 0623 - 1 - -Flavour enhancer Dipotassium-5’-guanylate 0628 - 1 - -Flavour enhancer Dipotassium-5’-inosinate 0632 - 1 - -Flavour enhancer Disodium-5’-guanylate 0627 - 1 - -Flavour enhancer Disodium-5’-inosinate 0631 - 1 - -Flavour enhancer Disodium-5'-ribonucleotides 0635 - 1 - -Flavour enhancer Ethyl maltol 0637 - 1 - -Flavour enhancer L-Glutamic acid 0620 - 1 - -Flavour enhancer 5’-Guanylic acid 0626 - 1 - -Flavour enhancer 5’-Inosinic acid 0630 - 1 - -Flavour enhancer Magnesium di-L-glutamate 0625 - 1 - -Flavour enhancer Monoammonium L-glutamate 0624 - 1 - -Flavour enhancer Monopotassium L-glutamate 0622 - 1 - -Flavour enhancer Monosodium L-glutamate 0621 - 1 - -Sweetening agent Alitame 0956 - 1 - -Sweetening agent Aspartame 0951 - 1 - -Sweetening agent Cyclohexylsulfamic acid 0952 - 1 - - Se<30Sweetening agent Isomalt 0953 - 1 - - Ni<2Sweetening agent Lactitol 0966 - 1 - - Ni<2Sweetening agent Mannitol 0421 - 1 - - Ni<2Sweetening agent Saccharin and its Na, K and Ca salts 0954 - 1 - - Se<30Sweetening agent Sorbitol/ sorbitol syrup 0420 - 1 - - Ni<2Sweetening agent Sucralose 0955 - 1 - -Sweetening agent Xylitol 0967 - 1 - - Ni<2Thickening agent Ammonium alginate 0403 - 2 - -Thickening agent Ethyl cellulose 0462 - 2 - -Thickening agent Gum ghatti 0419 - 2 - -Thickening agent Hydroxypropyl cellulose 0463 - 2 - -Thickening agent Hydroxypropylmethyl cellulose 0464 - 2 - -Thickening agent Karaya gum 0416 - 2 - -Thickening agent Konjac flour 0425 - 2 - -Thickening agent Methylethyl cellulose 0465 - 2 - -Thickening agent Methyl cellulose 0461 - 2 - -Thickening agent Polyvinylpyrrollidone 1201 - 2 - -Thickening agent Powdered cellulose 0460 (ii) - 2 - -Thickening agent Tara gum 0417 - 2 - -Thickening agent Tragacanth gum 0413 - 2 - -

Flavouring agents with minimum assay values less than 95%

At its fifty-third meeting, the Committee announced its intention to re-examine specifications for flavouringagents where the minimum assay values were less than 95%. Specifications for these substances were

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designated tentative. At the present meeting, the Committee considered information on all 62 remainingsubstances in this category concerning the secondary components that may be present in commercialproducts.

This information was sufficient for the Committee to revise the specifications for 27 flavouring agents(including two flavouring agents whose specifications were also revised for other reasons) and to remove thetentative designations. This was done by following the general principle that no more than 5% of anycommercial product should remain undefined after taking account of the flavouring agent and namedsecondary components.

The Committee will review this group of flavouring agents at a future meeting to confirm whether all thenamed secondary components are covered by existing safety evaluations. At the same time, the Committeewill determine the need for further information to complete those specifications that remain tentative.

Flavouring agents with specifications designated as tentative at previous meetings

Prior to the present meeting, 142 flavouring agents had been evaluated for safety at the forty-sixth, forty-ninth, fifty-first, fifty-third, and fifty-fifth meetings for which further information was required in ordercomplete the specifications. At the present meeting the Committee reviewed new data on 95 of theseflavouring agents and revised specifications were established to take account of the new information. For83, the tentative designation was removed; for the remaining 12, the revised specifications were classified astentative.

For the remaining 47 substances, no further data were provided that would permit the elaboration ofsatisfactory specifications, according to the criteria identified by the Committee at its fifty-third meeting. Theflavour industry has indicated that many of these substances are highly noxious sulfur-containing compoundsthat are not routinely handled in the pure form. It is therefore impracticable to provide information such asboiling point or specific gravity. In these cases, the Committee concluded that the additional criteriaidentified at its fifty-third meeting for the establishment of satisfactory specifications should not apply andthat only the basic data relating to chemical identity, minimum assay and identity test were required.

The Committee reiterated that the evaluation of flavourings must rely on adequate information on theidentity and composition of products in commercial use. In future, specifications for flavouring agents willbe withdrawn within two years of publication of the tentative specifications if the necessary information isnot provided.

Tentative specifications for food additives (uses other than as flavouring agents)

β-Carotene from Blakeslea trispora: Information is required on the method of analysis for residual solvents(ethyl acetate and isobutyl acetate). This information is required for evaluation in 2003.

Curcumin: The results of a reproductive toxicity study on a substance complying with the specifications forcurcumin, known to be in progress, is required for evaluation in 2003.

Diacetyltartaric and fatty acid esters of glycerol: The following information relating to the two-year toxicitystudy in rats is required for evaluation in 2003:

• To assess whether some of the adverse effects that were observed were treatment-related, the groupstreated with diacetyltartaric and fatty acid esters of glycerol should be compared with both untreatedand monoglyceride-treated controls and the control groups should be compared with one another.

• Additional information on the incidence of mycocardial fibrosis and adrenal medullary hyperplasiain animals at the low and intermediate doses should be provided.

Monomagnesium phosphate, trisodium diphosphate: Information is required on the loss on drying, loss onignition, test method for loss on ignition and assay method for the hydrates. This information is required forevaluation in 2003.

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Natamycin: Information is required on the level and determination of water content, lead limit, specificrotation, assay value and method of assay for the commercial product. Comments on other aspects of themonograph are invited. This information is required for evaluation in 2003.

Quillaia extracts: The existing specifications for quillaia extracts were revised in order to clarify thedifferences between unpurified and semi-purified extracts Additional information on composition (minimumand maximum percentages of saponins unpurified and semi-purified extracts) is necessary, so thespecifications were designated as tentative. Once the requested information has been received, theCommittee will consider whether separate specifications for unpurified and semi-purified extracts arerequired. This information is required for evaluation in 2003. The ADI was made temporary pendingclarification of the specifications. The temporary ADI is applicable only to the unpurified extract.

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Index to Section B: Specifications of certain flavourings

Name PageABDI (812) 134Acetal (941) 138Acetaldehyde benzyl 2-methoxyethylmixed acetal (840) 138Acetaldehyde diethyl acetal (941) 154Acetaldehyde dimethyl acetal (940) 152Acetaldehyde ethyl glyceryl mixedacetal (913) 150Acetaldehyde ethyl cis-3-hexenylacetal (943) 154Acetaldehyde ethyl propylene glycolmixed acetal (927) 152Acetanisole (810) 134Acetocumene (808) 134Acetone propylene glycol ketal (929) 152Acetophenone (806) 1341-Acetoxy-1-acetylcyclohexane (442) 1204-Acetoxy-3-methoxybenzaldehyde(890) 146Acetoxymethyl-toluene (o,m,p) (863) 1423-Acetoxypropyl methyl sulfide (478) 1204-Acetylanisole (810) 134p-Acetylanisole (810) 134Acetylbenzene (806) 134Acetyl benzoyl (833) 138p-Acetylcumene (808) 1341-Acetylcyclohexyl acetate (442) 1204-Acetyl-6-(1,1-dimethylethyl)-1,1-dimethylindane (812) 1342-Acetyl-3,(5 or 6)-dimethylpyrazine(786) 1303-Acetyl-2,5-dimethylpyrazine (786) 1303-Acetyl-2,6-dimethylpyrazine (786) 1302-Acetyl-3,5-dimethylpyrazine (786) 1302-Acetyl-3-ethyl-1,4-diazine (785) 1302-Acetyl-3-ethylpyrazine (785) 130Acetylformaldehyde (937) 152Acetylformic acid (936) 1522-Acetyl-1-hexanol (604) 1221-Acetyl-4-methylbenzene (807) 1342-Acetyl-3-methyl-1,4-diazine (950) 1542-Acetyl-3-methylpyrazine (950) 154Acetyl-m-xylene (809) 134beta-Acetylnaphthalene (811) 134Acetyl o-cresol (698) 1242-Acetylpyrazine (784) 130Acetylpyrazine (784) 1304-Acetyl-6-t-butyl-1,1-dimethylindan(812) 134p-Acetyl toluene (807) 134Acetylvanillin (890) 146Achelleic acid (627) 122Aconitic acid (627) 122Agrumat (854) 140Aldehyde C-12 (275) 116Aldehyde C-7 (95) 112Aldehyde C-9 (101) 112Aldehyde C-10 dimethyl acetal (945) 154Aldehyde C-8 dimethyl acetal (942) 154Aldehyde C-19 (so called) (843) 140Aldehyde C-11 undecyclic (107) 112Allyl cyclohexane acetate (12) 110Allyl cyclohexane butyrate (14) 110

Name PageAllyl cyclohexane hexanoate (16) 110Allyl cyclohexane valerate (15) 110Allyl cyclohexyl butyrate (14) 110Allyl cyclohexyl caproate (16) 110Allyl cyclohexyl valerate (15) 1104-Allyl-2,6-dimethoxyphenol (726) 124Allyl Ionone (401) 118Allyl-alpha-ionone (401) 1184-Allylsyringol (726) 124Allyl thiopropionate (490) 120Allyl tiglate (10) 110Ambrettolide (240) 114alpha-Amylcinnamaldehyde dimethylacetal (681) 124alpha-Amylcinnamic aldehydedimethyl acetal (681) 124alpha-Amylcinnamyl acetate (677) 124alpha-Amylcinnamyl formate (676) 124alpha-Amylcinnamyl isovalerate(678) 124n-Amyl formate (119) 112Amyl furan-2-carboxylate (748) 126Amyl 2-furoate (748) 126n-Amyl heptanoate (170) 114alpha-Amyl-beta-phenylacroleindimethyl acetal (681) 124alpha-n-Amyl-beta-phenylacrylacetate (677) 124alpha-Amyl-beta-phenylacryl formate(676) 124alpha-Amyl-beta-phenylacrylisovalerate (678) 124alpha-n-Amyl-beta-phenylacryl 3-methylbutanoate (678) 124Anisalcohol (871) 144p-Anisaldehyde (878) 144Anise alcohol (871) 144Anisic acid (883) 144m-Anisic acid (882) 144o-Anisic acid (881) 144p-Anisic acid (883) 144Anisic alcohol (871) 144Anisic aldehyde (878) 144Anisic ketone (813) 134Anisyl acetate (873) 144Anisylacetone (818) 136Anisyl alcohol (871) 144Anisyl butyrate (875) 144Anisyl formate (872) 144Anisyl methanoate (872) 144Anisyl methyl ketone (813) 134Anisyl phenylacetate (876) 144Anisyl propanoate (874) 144Anisyl propionate (874) 144Anisyl alpha-toluene (876) 144Artificial almond oil (22) 110Aubepine (878) 144Benzaldehyde (22) 110Benzaldehyde dimethyl acetal (837) 138Benzaldehyde glyceryl acetal (838) 138Benzaldehyde propylene glycolacetal (839) 138Benzalglycerin (838) 132

Name PageBenzenecarbonal (22) 110Benzenecarboxaldehyde (22) 110Benzenecarboxylic acid (850) 140Benzoic acid (850) 140Benzoic aldehyde (22) 110Benzoin (836) 138Benzophenone (831) 138Benzoyl acetic ester (834) 138Benzoylbenzene (831) 138Benzoyl phenyl carbinol (836) 138Benzylacetaldehyde (645) 122Benzyl acetate (23) 110Benzyl acetoacetate (848) 140Benzyl acetylacetate (848) 140Benzyl alcohol (25) 110Benzyl benzenecarboxylate (24) 110Benzyl benzoate (24) 110Benzyl butanoate (843) 140Benzylbutyl alcohol (825) 136Benzyl butyrate (843) 140Benzylcarbinyl cinnamate (671) 122Benzyl carbinyl 2-hydroxy benzoate(905) 148Benzylcarbinyl 3-phenylpropenoate(671) 122Benzyl trans-2,3-dimethyl-acrylate(846) 140Benzyl 2,3-dimethyl-trans-2-butenoate (847) 140Benzyl 2,3-dimethylcrotonate (847) 140Benzyl dipropyl ketone (830) 138Benzyl ethanoate (23) 110Benzyl formate (841) 1383-Benzyl-4-heptanone (830) 138Benzyl 2-hydroxybenzoate (904) 148Benzylidene acetaldehyde (656) 122Benzylideneacetone (820) 1363-Benzylidene-2-butanone (821) 136Benzylidene methyl acetone (821) 136Benzylidene methyl ethyl ketone(821) 136Benzylisoamyl acetone (827) 136Benzyl isobutyl carbinol (827) 136Benzyl isobutyl ketone (828) 138Benzyl isobutyrate (844) 140Benzyl isopentanoate (845) 140Benzyl isovalerate (845) 140Benzyl isovalerianate (845) 140Benzyl beta-ketobutyrate (848) 140Benzyl ketone (832) 138Benzyl methanoate (841) 138Benzyl 2-methoxyethyl acetal (840) 138Benzyl 2-methyl-trans-2-butenoate(846) 140Benzyl trans-2-methyl-2-butenoate(846) 140Benzyl-3-methylbutyrate (845) 140Benzyl-2-methylcrotonate (846) 140Benzyl 2-methylpropanoate (844) 140Benzyl 2-methylpropyl ketone (828) 138Benzyl methyltiglate (847) 140Benzyl n-butyrate (843) 140Benzyl o-hydroxybenzoate (904) 148

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Name PageBenzyl 3-oxobutanoate (848) 140Benzyl 3-oxobutyrate (848) 1401-Benzyloxy-1-(2-methoxyethoxy)ethane (840) 138Benzyl phenylacetate (849) 140Benzyl phenylformate (24) 110Benzyl propanoate (842) 138Benzyl propionate (842) 138Benzyl propyl carbinol (825) 136Benzyl salicylate (904) 148Benzyl tiglate (846) 140Benzyl alpha-toluene (849) 140Bourbonal ethyl protal (893) 146Bramble ketone (818) 136(1-Buten-1-yl) methyl sulfide (457) 1201-Butenyl methyl sulfide (457) 1204-(Butoxymethyl)-2-methoxyphenol(888) 146Butyl butyrolactate (935) 152Butyl butyryllactate (935) 152Butyl 2-butyryloxypropanoate (935) 152Butyl cinnamate (663) 122Butyl 2-hydroxybenzoate (901) 148Butyl 4-hydroxybenzoate (870) 142Butyl 2-hydroxypropanoate (932) 152n-Butyl alpha-hydroxypropionate(932) 152Butyl lactate (932) 1522-(2-Butyl)-3-methoxypyrazine (791) 132Butyl octadecanoate (184) 114n-Butyl o-hydroxybenzoate (901) 148Butyl paraben (870) 142Butyl parasept (870) 142Butyl beta-phenylacrylate (663) 122Butyl 3-phenylpropenoate (663) 122Butyl p-hydroxybenzoate (870) 1422-Butylpropionic acid (265) 114Butyl salicylate (901) 148Butyl stearate (184) 114Butyl 10-undecenoate (344) 116Butyl undec-10-enoate (344) 116Butyl undecylenate (344) 116Butyrin (922) 150Butyroin (416) 118Capraldehyde dimethyl acetal (945) 154Capryl aldehyde dimethyl acetal(942) 154Carboxybenzene (850) 1402-Carboxy glutaconic acid (627) 122Cassia aldehyde (656) 122Cassie ketone (873) 144Cetone D (811) 134Cincloval (648) 122Cinnamal (656) 122Cinnamaldehyde (656) 122Cinnamaldehyde ethylene glycolacetal (648) 122Cinnamic aldehyde (656) 122Cinnamyl benzoate (760) 126Cinnamyl butyrate (652) 122Cinnamyl cinnamate (673) 124Cinnamyl beta-phenylacrylate (673) 124Citral diethyl acetal (948) 154Citral dimethyl acetal (944) 154Citrathal (948) 154Citridic acid (627) 122o-Cresol acetate (698) 1242,4-Cresotaldehyde (898) 146

Name Page2-(o,m,p-Cresyl)-5-hydroxy dioxane(867) 142 2-(o,m,p-Cresyl)-5-hydroxymethyldioxolane (867) 142o-Cresylic acetate (698) 124o-Cresyl salicylate (907) 148Cristal (909) 148Cumaldehyde (868) 142Cuminal (868) 142Cumin alcohol (864) 142Cuminaldehyde (868) 142Cuminic alcohol (864) 142Cuminic aldehyde (868) 142Cuminol (864) 142Cuminyl alcohol (864) 142alpha-Cyclocitrylideneacetone (388) 118alpha-Cyclocitrylidene butanone(404) 118Cyclohexapyrazine (952) 154(Cyclohexylmethyl)pyrazine (783) 130p-Cymen-7-ol (864) 142Decanal dimethyl acetal (945) 1544-Decenal (326) 1169-Decenoic acid (328) 116Dec-9-enoic acid (328) 1161,4-Diazine (951) 154Dibenzyl ketone (832) 1381,1-Diethoxy-3,7-dimethyl-2,6-octadiene (948) 1541,1-Diethoxyethane (941) 1541,2-Di((1'-ethoxy)-ethoxy)propane(927) 1521,2-Di[(1'-ethoxy)ethoxy]propane(927) 1521,1-Diethoxy-4-heptene (949) 1541,1-Diethoxy-2,6-nonadiene (946) 154Diethylacetal (941) 1542,3-Diethyl-1,4-diazine (771) 1282,3-Diethyl-5-methyl-1,4-diazine(777) 1302,5-Diethyl-3-methyl-1,4-diazine(778) 1302,3-Diethyl-5-methylpyrazine (777) 1302,5-Diethyl-3-methylpyrazine (778) 1303,5-Diethyl-2-methylpyrazine (779) 1302,3-Diethylpyrazine (771) 1286,7-Dihydro-2,3-dimethyl-5H-cyclopentapyrazine (782) 1306,7-Dihydro-5-methyl-5H-cyclopentapyrazine (781) 130Dihydroxyacetophenone (729) 1262,4-Dihydroxybenzoic acid (908) 1481-(x,y-Dihydroxyphenyl) ethanone(729) 126Dihydroxyphenyl methyl ketone(729) 1261,2-Dihydroxypropane (925) 1502,3-Dihydroxypropyl 5-hydroxydecanoate (923) 1502,3-Dihydroxypropyl 5-hydroxydodecanoate (924) 1502,3-Dihydroxypropyl octadecanoate(918) 1502,3-Dihydroxypropyl 9-octadecenoate (919) 1502,3-Dihydroxypropyl 3-oxodecanoate(914) 1502,3-Dihydroxypropyl 3-oxododecanoate (915) 150

Name Page2,3-Dihydroxypropyl 3-oxohexadecanoate (917) 1502,3-Dihydroxypropyl 3-oxohexanoate(910) 1482,3-Dihydroxypropyl 3-oxooctanoate(911) 1482,3-Dihydroxypropyl 3-oxotetradecanoate (916) 1503,4-Dimethoxybenzaldehyde (877) 1441,1-Dimethoxy-2-benzylideneheptane (681) 1241,1-Dimethoxydecane (945) 1541,1-Dimethoxy-3,7-dimethyl-2,6-octadiene (944) 1541,1-Dimethoxyethane (940) 1522,6-Dimethoxy-4-ethylphenol (723) 1241,1-Dimethoxyheptane (947) 154(Dimethoxymethyl)benzene (837) 138(2-(Dimethoxymethyl)-1-heptenyl)benzene (681) 1241,1-Dimethoxyoctane (942) 1542,6-Dimethoxy-4-(2-propenyl) phenol(726) 1242,6-Dimethoxy-4-propylphenol (724) 124alpha-,alpha-Dimethoxytoluene (837) 138Dimethyl acetal (940) 1522,4-Dimethylacetophenone (809) 134alpha-,alpha-Dimethyl-anisalacetone(829) 1382,4-Dimethylbenzaldehyde (869) 142p,alpha-Dimethylbenzyl alcohol (805) 1342,3-Dimethyl-1,4-diazine (765) 1282,5-Dimethyl-1,4-diazine (766) 1282,6-Dimethyl-1,4-diazine (767) 1282,5-Dimethyl-2,5-dihdroxy-p-dithiane(562) 120(5H)-2,3-Dimethyl-6,7-dihydrocyclopenta(b)pyrazine (782) 1302,5-Dimethyl-2,5-dihydroxy-1,4-dithiane (562) 1202,6-Dimethyl-3-ethylpyrazine (776) 1302,6-Dimethyl-6-hepten-1-ol (348) 1182,6-Dimethylhept-7-en-1-ol (348) 1184-(2,2-Dimethyl-6-methylenecyclohexyl)-3-buten-2-one(390) 1183,7-dimethyl-2,6-octadienal diethylacetal (948) 1543,7-Dimethyl-2,6-octadien-1-ylacetate (58) 110trans-3,7-Dimethyl-2,6-octadien-1-ylacetoacetate (599) 1223,7-Dimethyl-1,6-octadien-3-ylbenzoate (859) 1423,7-Dimethylocta-2(trans),6-dienylbenzoate (860) 142trans-3,7-Dimethyl-2,6-octadien-1-ylbenzoate (860) 1423,7-Dimethyl-2,6-octadienyl dimethylacetal (944) 1543,7-Dimethyl-2,6-octadien-1-yl 2-ethylbutanoate (78) 112trans-3,7-Dimethyl-2,6-octadien-1-ylhexanoate (70) 1123,7-Dimethyl-2,6-octadienyl-2-methylpropanoate (72) 1123,7-Dimethylocta-2(trans),6-dienyl 3-oxobutyrate (599) 1222,6-Dimethyloctanal (273) 116

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Name Page2,6-Dimethyl octanoic aldehyde(273) 1163,7-Dimethyl-7-octen-1-yl-3-methylbutanoate (77) 1123,7-Dimethyl-7-octen-1-yl-2-methylpropanoate (74) 1123,7-Dimethyl-7-octen-1-yl propionate(64) 1102,6-Dimethyl-p-diazine (767) 1281-(2,4-Dimethylphenyl)ethanone(809) 1342,3-Dimethylpyrazine (765) 1282,5-Dimethylpyrazine (766) 1282,6-Dimethylpyrazine (767) 128Dimethyl salicylate (880) 1441,5-Dimethyl-1-vinylhex-4-enylbenzoate (859) 142Dioxyacetophenone (729) 126alpha,alpha-Diphenylacetone (832) 138Diphenyl ketone (831) 1381,3-Diphenyl-2-propanone (832) 138Dodeca-6-en-1,4-lactone (249) 114Dodecanoic acid (111) 112Draconic acid (883) 144Dracylic acid (850) 140Eglantine (856) 140Enanthal dimethyl acetal (947) 154Enzactin (920) 150Equisetic acid (627) 122p-Ethenylphenol (711) 124Ethone (826) 1364-Ethoxybenzaldehyde (879) 144p-Ethoxybenzaldehyde (879) 1441,2,3-tris([1'-Ethoxy]ethoxy)propane(913) 1501,2,3-tris[(1'-Ethoxy)ethoxy]propane(913) 1501-Ethoxyethyl ether of potassiumlactate (933) 1522-Ethoxy-4-formylphenyl isobutyrate(953) 1541-Ethoxy-1-(cis-3-hexenyloxy)ethane(943) 1543-Ethoxy-4-hydroxybenzaldehyde(893) 1461-Ethoxy-4-hydroxybenzene (720) 1242-(3-Ethoxy-4-hydroxyphenyl)-4-methyl-1,3-dioxolane (954) 1544-(Ethoxymethyl)-2-methoxyphenol(887) 1462-Ethoxy-3 or 5 or 6-methylpyrazine(793) 1324-Ethoxyphenol (720) 124p-Ethoxyphenol (720) 1243-Ethoxy protocatechualdehyde(893) 146Ethyl 2-acetyldihydrocinnamate(835) 138Ethyl acetylformate (938) 152Ethyl alpha-acetylhydrocinnamate(835) 138Ethyl 2-acetyl-3-phenylpropionate(835) 138Ethyl anisate (885) 1464-Ethylbenzaldehyde (865) 142p-Ethylbenzaldehyde (865) 142Ethyl benzenecarboxylate (852) 140Ethyl benzoate (852) 140Ethyl benzoylacetate (834) 138

Name PageEthyl benzylacetoacetate (835) 138alpha-Ethylbenzyl alcohol (822) 136alpha-Ethylbenzyl butyrate (823) 1362-Ethyl-1,4-diazine (762) 1264-Ethyl-2,6-dimethoxyphenol (723) 1242-Ethyl-3 (5 or 6)-dimethylpyrazine(775) 1282-Ethyl-3,5-dimethylpyrazine (776) 1303-Ethyl-2,6-dimethylpyrazine (776) 1302-Ethylfenchol (440) 120Ethyl cis-3-hexenyl acetal (943) 1541-Ethylhexyl 2-methylcrotonate (448) 1201-Ethylhexyl tiglate (448) 120Ethyl 2-hydroxybenzoate (900) 148Ethyl 4-hydroxy-3-methoxybenzylether (887) 146Ethyl 2-hydroxypropanoate (931) 152Ethyl alpha-hydroxypropionate (931) 152Ethylidene diethyl ether (941) 154Ethylidene dimethyl ether (940) 152Ethyl beta-keto-beta-phenylpropionate (834) 138Ethyl alpha-ketopropionate (938) 152Ethyl lactate (931) 152Ethyl 4-methoxybenzoate (885) 1462-Ethyl-3-methoxypyrazine (789) 1322-Ethyl-5-methoxypyrazine (789) 1322-Ethyl-6-methoxypyrazine (789) 132Ethyl-(3,5 or 6)-methoxypyrazine(789) 132Ethyl-(3,5 or 6)-methoxypyrazine(85%) and 2-Methyl-(3,5 or 6)-methoxypyrazine (13%) (789) 1322-Ethyl-3-methyl-1,4-diazine (768) 1282-Ethyl-5-methyl-1,4-diazine (770) 1282-Ethyl-6-methyl-1,4-diazine (769) 128Ethyl 2-(methyldithio)propionate(581) 120Ethyl 2-methyl-3-pentenoate (350) 118Ethyl 2-methylpent-3-enoate (350) 1182-Ethyl-3-methylpyrazine (768) 1282-Ethyl-5-methylpyrazine (770) 1282-Ethyl-6-methylpyrazine (769) 128Ethyl o-hydroxybenzoate (900) 148Ethyl 2-oxopropanoate (938) 152Ethyl p-anisate (885) 146Ethyl phenyl carbinol (822) 136Ethyl phenyl carbinol butyrate (823) 136Ethyl 2-phenyl-3-furoate (752) 126Ethyl phenyl ketone (824) 136Ethyl 3-phenyl-3-oxopropionate(834) 138Ethyl p-methoxybenzoate (885) 1462-Ethylpyrazine (762) 126Ethylpyrazine (762) 1263-Ethyl-2-pyrazinyl methyl ketone(785) 130Ethyl pyroracemate (938) 152Ethyl pyruvate (938) 152Ethyl salicylate (900) 1484-Ethylsyringol (723) 1242-Ethyl-1,3,3-trimethylbicyclo[2.2.1]heptan-2-ol (440) 1202-Ethyl-1,3,3-trimethyl-2-norbornanol(440) 120Ethyl vanillin (893) 146Ethyl vanillin beta-d-glucopyranoside(892) 146Ethyl vanillin isobutyrate (953) 154

Name PageEthyl vanillin propylene glycol acetal(954) 1541-Formyl-2,4-dimethylbenzene (869) 1424-Formyl-2-methoxyphenyl 2-methylpropanoate (891) 146Furfuryl butyrate (759) 126alpha-Furfuryl caprylate (742) 126Furfuryl isovalerate (743) 126Furfuryl 3-methylbutanoate (743) 126alpha-Furfuryl octanoate (742) 126Furfuryl octanoate (742) 126alpha-Furfuryl pentanoate (741) 126Furfuryl pentanoate (741) 126Furfuryl propanoate (740) 126Furfuryl propionate (740) 126alpha-Furfuryl valerate (741) 126Furfuryl valerate (741) 1262-Furylmethyl butanoate (759) 126Geraniol benzoate (860) 142Geranyl acetate (58) 110Geranyl acetoacetate (599) 122Geranyl benzoate (860) 142Geranyl caproate (70) 112Geranyl ethylbutanoate (78) 112Geranyl hexanoate (70) 112Geranyl isobutyrate (72) 112Geranyl beta-ketobutyrate (599) 122Geranyl 3-oxobutanoate (599) 122Glucoethylvanillin (892) 146Glyceol (909) 148Glycerine (909) 148Glycerol (909) 148Glycerol 5-hydroxydecanoate (923) 150Glycerol 5-hydroxydodecanoate(924) 1501-Glyceryl monooctadecanoate (918) 150Glyceryl monooleate (919) 150Glyceryl monostearate (918) 150Glyceryl triacetate (920) 150Glyceryl tribenzoate (861) 142Glyceryl tributyrate (922) 150Glyceryl tripropanoate (921) 150Glyceryl tripropionate (921) 150Glycoline (766) 128Guaiacol phenylacetate (719) 124Guaiacyl phenylacetate (719) 124Heliotropin (896) 146Heliotropin acetate (894) 146Heliotropyl acetate (894) 146Heliotropyl 2-methyl propanoate;(895) 146Heptaldehyde (95) 112Heptaldehyde dimethyl acetal (947) 154Heptaldehyde glyceryl acetal (912) 150Heptanal (95) 112Heptanal dimethyl acetal (947) 154Heptanal glyceryl acetal (mixed 1,2and 1,3 acetals) (912) 1504-Heptenal diethyl acetal (949) 154trans-3-Heptenyl 2-methylpropanoate (191) 114Heptyl cinnamate (666) 122Heptyl beta-phenylacrylate (666) 122Heptyl 3-phenylpropenoate (666) 122Hexadecanoic acid (115) 112omega-6-Hexadecenlactone (240) 114Hexadec-6-eno-1,16-lactone (240) 1146-Hexadecenolide (240) 114

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Name Page2,2,4,4,6,6-Hexamethyl-1,3,5-trithiane (543) 120Hexanal propylene glycol cyclicacetal (928) 152cis-3-Hexenyl benzoate (858) 142cis-3-Hexenyl 2-hydroxypropanoate(934) 152cis-3-Hexenyl lactate (934) 152n-Hexyl benzenecarboxylate (854) 140Hexyl benzoate (854) 140Hexyl furan-2-carboxylate (749) 126Hexyl 2-furoate (749) 1262-Hexyl-5-hydroxy-1,3-dioxane (912) 1502-Hexyl-4-hydroxymethyl-1,3-dioxolane (912) 150Hexyl 2-methyl-3&4-pentenoate(mixture) (352) 118Homoanisaldehyde (879) 144Homocinnamyl alcohol (819) 136Homoethone (829) 138Hydrocinnamaldehyde (645) 122Hydrocinnamyl caproate (642) 122Hydrocinnamyl cinnamate (672) 124Hydrocinnamyl 3-phenylpropenoate(672) 124Hydroquinone monoethyl ether (720) 1242-Hydroxybenzaldehyde (897) 146o-Hydroxybenzaldehyde (897) 1462-Hydroxy-2-cyclohexen-1-one (424) 1182-Hydroxy-1,2-diphenylethanone(836) 138cis-4-Hydroxy-6-dodecenoic acidlactone (249) 1144-Hydroxy-m-anisaldehyde 2-methylpropionate (891) 1464-Hydroxy-3-methoxybenzaldehyde(889) 1464-Hydroxy-3-methoxybenzyl alcohol(886) 1464-(4-Hydroxy-3-methoxyphenyl)but-3-en-2-one (732) 1262-Hydroxy-4-methyl benzaldehyde(898) 1462-Hydroxy-4-methylbenzaldehyde(898) 1463-(Hydroxymethyl)-2-heptanone(604) 1225-Hydroxy-4-octanone (416) 1185-Hydroxyoctan-4-one (416) 118p-Hydroxyphenetole (720) 1245-Hydroxy-2-phenyl-1,3-dioxane and4-(Hydroxymethyl)-2-phenyl-1,3-dioxolane (838) 1382-Hydroxy-2-pheylacetophenone(836) 1382-Hydroxypropanoic acid (930) 152alpha-Hydroxypropanoic acid (930) 1522-Hydroxy-propionic acid (930) 1523-Hydroxypropyl methyl sulfide (461) 1202-Hydroxypropyl octadecanoate(926) 1524-Hydroxystyrene (711) 124alpha-Hydroxytoluene (25) 110alpha-Ionone (388) 118gamma-Ionone (390) 118Isoamyl benzoate (857) 140Isoamyl formate (42) 110Isoamyl laurate (182) 114Isoamyl 2-methyl butanoate (51) 110

Name PageIsoamyl 2-methylbutyrate (51) 110Isoamyl o-hydroxybenzoate (903) 148Isoamyl pyroracemate (939) 152Isoamyl pyruvate (939) 152Isoamyl salicylate (903) 148Isobutyl benzenecarboxylate (856) 140Isobutyl benzoate (856) 140Isobutyl benzyl carbinol (827) 136Isobutyl benzyl ketone (828) 138Isobutyl formate (124) 114Isobutyl heptanoate (172) 114Isobutyl heptoate (172) 114Isobutyl 2-hydroxybenzoate (902) 1482-Isobutyl-3-methoxypyrazine (792) 1322-Isobutyl-3-methyl-1,4-diazine (773) 1282-Isobutyl-3-methylpyrazine (773) 128Isobutyl o-hydroxybenzoate (902) 148alpha-Isobutylphenethyl alcohol(827) 136Isobutyl salicylate (902) 148isodecanal (273) 116Isodecylaldehyde (273) 116alpha-iso-Methylionone (404) 118Isopentyl benzoate (857) 140Isopentyl formate (42) 110Isopentyl 2-hydroxybenzoate (903) 148Isopentyl laurate (182) 114Isopentyl pyruvate (939) 152Isopentyl salicylate (903) 1484-Isopropenyl-1-methyl-1-cyclohexanol (374) 118p-Isopropylacetophenone (808) 134p-Isopropylacetylbenzene (808) 1344-Isopropylbenzaldehyde (868) 142p-Isopropylbenzaldehyde (868) 142Isopropyl benzoate (855) 1404-Isopropylbenzyl alcohol (864) 142p-Isopropylbenzyl alcohol (864) 142Isopropyl caproate (308) 1162-Isopropyl-1,4-diazine (764) 128Isopropyl formate (304) 116Isopropyl hexanoate (308) 116Isopropyl mercaptan (510) 120Isopropyl methanoate (304) 1162-Isopropyl-3-methoxypyrazine and2-Isopropyl-5-methoxypyrazine and2-Isopropyl-6-methoxypyrazine (790) 1322-Isopropyl-5-methylpyrazine (772) 1285-Isopropyl-2-methylpyrazine (772) 1281-(4-Isopropylphenyl)ethanone (808) 134Isopropyl p-methoxystyryl ketone(829) 138Isopropyl propionate (306) 1162-Isopropylpyrazine (764) 128Isopropylpyrazine (764) 128Ketine (766) 1282-Ketopropionaldehyde (937) 1522-Ketopropionic acid (936) 152Lactic acid (930) 152Lauric acid (111) 112Leaf acetal (943) 154Leaf alcohol ethyl acetal (943) 154Leaf lactate (934) 152Linalool benzoate (859) 142Linalyl benzoate (859) 142Maple lactone pyrazine (781) 130alpha-Melonol (348) 118p-Menth-1-en-3-ol (434) 120p-Menth-8-en-1-ol (374) 118

Name Pagep-Menth-1-en-8-yl butyrate (370) 118p-Menth-1-en-8-yl formate (367) 118p-Menth-1-en-8-yl isopentanoate(372) 118p-Menth-1-en-8-yl isovalerate (372) 118p-Menth-1-en-8-yl 3-methylbutyrate(372) 1182- (Mercaptomethyl)pyrazine (794) 1322-Mercaptonaphthalene (531) 120Methionol (461) 120Methionyl acetate (478) 1204-Methoxyacetophenone (810) 134p-Methoxyacetophenone (810) 1343-Methoxy-4-acetoxybenzaldehyde(890) 1461-Methoxy-4-acetoxymethylbenzene(873) 1444-Methoxybenzaldehyde (878) 144p-Methoxybenzaldehyde (878) 1442-Methoxybenzoic acid (881) 1443-Methoxybenzoic acid (882) 1444-Methoxybenzoic acid (883) 144m-Methoxybenzoic acid; (882) 144o-Methoxybenzoic acid (881) 144p-Methoxybenzoic acid (883) 1444-Methoxybenzyl acetate (873) 144p-Methoxybenzyl acetate (873) 144p-Methoxybenzylacetone (818) 1364-Methoxybenzyl alcohol (871) 1444-Methoxybenzyl butanoate (875) 144p-Methoxybenzyl butyrate (875) 1444-Methoxybenzyl formate (872) 144p-Methoxybenzyl formate (872) 1444-Methoxybenzyl phenylacetate(876) 144p-Methoxybenzyl phenylacetate(876) 1444-Methoxybenzyl propanoate (874) 144p-Methoxybenzyl propionate (874) 1442-Methoxy-1,4-diazine (787) 1306-Methoxy eugenol (726) 1242-Methoxy-3-isobutylpyrazine (792) 1322-Methoxy-(3,5 or 6)-isopropylpyrazine (790) 1322 or 5 or 6-Methoxy-3-methyl-1,4-diazine (788) 1302-Methoxy-3-(1-methylpropyl)pyrazine (791) 1322-Methoxy-(3,5 or 6)-methylpyrazine(788) 1302-Methoxy-3-methylpyrazine (788) 1302-Methoxy-5-methylpyrazine (788) 1302-Methoxy-6-methylpyrazine (788) 130o-Methoxyphenol phenylacetate(719) 1244-Methoxyphenylacetone (813) 1344- (p-Methoxyphenyl)-2-butanone(818) 1364-(4-Methoxyphenyl)-2-butanone(818) 1361-(4-Methoxyphenyl)ethanone (810) 1341- (4-Methoxyphenyl)-4-methyl-1-penten-3-one (829) 1381-(4-Methoxyphenyl)-4-methyl-1-penten-3-one (829) 1381- (p-Methoxyphenyl)-1-penten-3-one (826) 1361-(4-Methoxyphenyl)-1-penten-3-one(826) 136

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Name Page2-Methoxyphenyl phenylacetate(719) 1241- (p-Methoxyphenyl)-2-propanone(813) 1341-(4-Methoxyphenyl)-2-propanone(813) 1342-Methoxypyrazine (787) 130Methoxypyrazine (787) 1302-Methoxy-3-sec-butylpyrazine (791) 132p-Methoxystyryl ethyl ketone (826) 1362-(Methydithio) isobutylraldehyde(580) 1204-Methylacetophenone (807) 134p-Methylacetophenone (807) 134Methyl 1-acetoxycyclohexyl ketone(442) 120alpha-Methylanisalacetone (826) 136Methyl anisate (884) 144Methyl o-anisate (880) 144Methyl p-anisate (884) 144alpha-Methyl anisylidene acetone(826) 136m-Methylbenzaldehyde (866) 142o-Methylbenzaldehyde (866) 142p-Methylbenzaldehyde (866) 142Methyl benzenecarboxylate (851) 140Methyl benzoate (851) 1405-Methyl-1,4-benzodiazine (798) 132alpha-Methylbenzyl acetate (801) 134m-Methylbenzyl acetate (863) 142o-Methylbenzyl acetate (863) 142p-Methylbenzyl acetate (863) 142Methylbenzyl acetate (mixed o,m,p)(863) 142p-Methylbenzylacetone (817) 136alpha-Methylbenzyl alcohol (799) 132alpha-Methylbenzyl butyrate (803) 134Methyl benzyl carbinyl butyrate (814) 136alpha-Methylbenzyl formate (800) 132alpha-Methylbenzyl isobutyrate (804) 134alpha-Methylbenzyl propionate (802) 1343-Methylbutyl benzoate (857) 1403-Methylbutyl dodecanoate (182) 1143-Methylbutyl formate (42) 1102-Methylbutyl-2-methylbutanoate(212) 1143-Methylbutyl 2-methylbutanoate(51) 1102-Methylbutyl 2-methylbutyrate (212) 1143-Methylbutyl 2-oxopropanoate (939) 1522-Methylcaproic acid (265) 114o-Methylcatechol phenylacetate(719) 1242-Methyl-3,4-cyclohexanedione(424) 1183-Methyl-1,2-cyclohexanedione(424) 1182-Methyl-1,4-diazine (761) 1262-Methyl-3,5-diethyl-1,4-diazine(779) 1302-Methyl-5,6-diethylpyrazine (777) 130(5H)-5-Methyl-6,7-dihydrocyclopenta(b)pyrazine (781) 1305-Methyl-6,7-dihydro-5H-cyclopentapyrazine (781) 130Methyl 2,4 dimethylphenyl ketone(809) 134Methyl dodecanoate (180) 114

Name Page3,4-Methylenedioxybenzaldehyde(896) 1463,4-Methylenedioxybenzyl acetate(894) 1463,4-Methylenedioxybenzylisobutyrate (895) 1462-Methyl-3-ethoxypyrazine and 2-Methyl-5-ethoxypyrazine and 2-Methyl-6-ethoxypyrazine (793) 1321-Methylethyl benzoate (855) 1402-Methyl-3-ethylpyrazine (768) 1282-Methyl-5-ethylpyrazine (770) 128Methyl glycol (925) 150Methylglyoxal (937) 1522-Methylhexanoic acid (265) 1145-Methylhexanoic acid (266) 114Methyl 3-hexenoate (334) 116Methyl hex-3-enoate (334) 116Methyl hexyl acetaldehyde (270) 116Methyl 2-hydroxybenzoate (899) 148Methyl o-hydroxybenzoate (899) 148Methyl 3-hydroxypropyl sulfide (461) 1202-Methyl-3-isobutylpyrazine (773) 1282-Methyl-5-isopropyl-1,4-diazine(772) 128Methyl p-isopropylphenyl ketone(808) 1342-Methyl-5-isopropylpyrazine (772) 128Methyl 2-keto-3-methylvalerate (591) 120Methyl laurate (180) 114(Methylmercapto)propyl alcohol(461) 120Methyl 2-methoxybenzoate (880) 144Methyl 4-methoxybenzoate (884) 144Methyl o-methoxybenzoate (880) 144Methyl p-methoxybenzoate (884) 144Methyl 4-methoxyphenyl ketone(810) 134 2-Methyl-(3,5 or 6)-methoxypyrazine(789) 1322-Methyl-3-methoxypyrazine (789) 1322-Methyl-5-methoxypyrazine (789) 1322-Methyl-6-methoxypyrazine (789) 132Methyl-2-methylbutanoate (205) 114Methyl 2-methylbutyrate (205) 1142-Methyl-2-(methyldithio)propanal(580) 120Methyl 3-methyl-2-oxovalerate (591) 1202-Methyl-3-(methylthio)pyrazine(797) 1322-Methyl-5-(methylthio)pyrazineethylthio)pyrazine (797) 132Methyl 2-naphthyl ketone (811) 134Methyl beta-naphthyl ketone (811) 134Methyl n-nonyl acetaldehyde (275) 1162-Methyloctanal (270) 113Methylol methyl amyl ketone (604) 1222-Methyl-3(or 5 or 6)-ethoxypyrazine(793) 1322-Methyl-3,5-or 6-methylthiopyrazine(797) 132Methyloxanone (818) 136Methyl 2-oxo-3-methylpentanoate(591) 1202-Methylpentanal (260) 1142-Methyl pent-3-enoate (347) 1182-Methyl-3-pentenoic acid (347) 118

Name Page4-Methyl-2-pentyl-1,3-dioxolane(928) 152alpha-Methylphenethyl butyrate(814) 1362-Methylphenyl acetate (698) 1244-(4-Methylphenyl)-2-butanone (817) 1363-Methyl-4-phenyl-3-buten-2-one(821) 136Methyl phenyl carbinol (799) 132Methyl phenyl carbinyl acetate (801) 134Methyl phenyl carbinyl butyrate (803) 134Methyl phenyl carbinyl formate (800) 132Methyl phenyl carbinyl isobutyrate(804) 134Methyl phenyl carbinyl propionate(802) 134Methyl phenyl diketone (833) 1384-Methyl-2-phenyl-1,3-dioxolane(839) 1381-(4-Methylphenyl)ethanol (805) 1341-(4-Methylphenyl)ethanone (807) 1341-Methyl-2-phenylethyl butyrate(814) 136Methyl 2-phenylethyl carbinol (815) 136Methyl phenyl glyoxal (833) 1382-Methylphenyl 2-hydroxybenzoate(907) 1482-(2,3and 4-Methylphenyl)-5-hydroxy-1,3-dioxane (867) 1422-(2,3 and 4-Methylphenyl)-5-hydroxy-1,3-dioxane and 2-(2,3 and4-Methylphenyl)-5-hydroxymethyl-1,3-dioxolane (mixture) (867) 1422-(2,3 and 4-Methylphenyl)-5-hydroxymethyl-1,3-dioxolane (867) 142Methyl phenyl ketone (806) 1344-Methyl-2-phenyl-m-dioxolane (839) 1384-Methyl-1-phenyl-2-pentanol (827) 1364-Methyl-1-phenyl-2-pentanone(828) 1381-Methyl-3-phenylpropyl acetate(816) 1362-Methylpropyl benzoate (856) 1402-Methyl propyl benzyl carbinol (827) 1362-Methylpropyl formate (124) 1142-Methylpropyl heptanoate (172) 1142-Methylpropyl 2-hydroxybenzoate(902) 1482-(1-Methylpropyl)-3-methoxypyrazine (791) 1322-(2-Methylpropyl)-3-methylpyrazine(773) 128Methylprotocatechuic aldehyde (889) 1462-Methylpyrazine (761) 126Methylpyrazine (761) 126Methyl pyrazinyl ketone (784) 130Methylpyrazinyl methyl sulfides(mixture) (797) 1325-Methylquinoxaline (798) 1324-Methylsalicylaldehyde (898) 146Methyl salicylate (899) 144Methyl salicylate methyl ether (880) 144Methyl styryl carbinol (819) 136Methyl styryl ketone (820) 136(3,5 or 6)-Methylthio-2-methylpyrazine (797) 1323-(Methylthio)propanol (461) 1203-(Methylthio)propyl acetate (478) 1203-(Methylthio)propyl alcohol (461) 120

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Name Page2-(Methylthio)pyrazine (796) 132Methyl p-tolyl carbinol (805) 134Methyl p-tolyl ketone (807) 1342-Methylundecanal (275) 1162-Methylundecenal (275) 1162-Methylvaleraldehyde (260) 114Methyl vanillin (877) 144Mixture of 3-Acetyl-2,5-dimethylpyrazine and 3-Acetyl-2,6-dimethylpyrazine (786) 130Mixture of 2-(o,m,p-Cresyl)-5-hydroxy dioxane and 2-(o,m,p-Cresyl)-5-hydroxymethyldioxolane(867) 142Mixture of 2-Ethyl-3,5-Dimethylpyrazine and 3-Ethyl-2,5-Dimethylpyrazine (775) 128Mixture of 2-Ethyl-3-methoxypyrazine and 2-Ethyl-5-methoxypyrazine and 2-Ethyl-6-methoxypyrazine and 2-Methyl-3-methoxypyrazine and 2-Methyl-5-methoxypyrazine and 2-Methyl-6-methoxypyrazine (789) 132Mixture of 2-Hexyl-4-hydroxymethyl-1,3-dioxolane and 2-Hexyl-5-hydroxy-1,3-dioxane (912) 150Mixture of Methoxy isopropylpyrazines (790) 132Mixture of 2-Methoxy-3-methylpyrazine and 2-Methoxy-5-methylpyrazine and 2-Methoxy-6-methylpyrazine (788) 130Mixture of o-Methylbenzaldehydeand m-Methylbenzaldehyde and p-Methylbenzaldehyde (866) 142Mixture of o-Methylbenzyl acetateand m-Methylbenzyl acetate and p-Methylbenzyl acetate (863) 142Mixture of 2-Methyl-3-(methylthio)pyrazine and 2-Methyl-5-(methylthio)pyrazineethylthio)pyrazine (797) 132Mixture of 2-Phenyl-5-hydroxy-1,3-dioxane and 2-Phenyl-4-hydroxymethyl-1,3-dioxolane (838) 132Mixture of 1-(x,y-dihydroxyphenyl)ethanones (729) 126monoolien (919) 150alpha-Monostearin (918) 150Monostearin (918) 150Morellone (830) 138Myristic acid (113) 1122-Naphthalenethiol (531) 1201-(2-naphthyl)ethanone (811) 1342-Naphthyl mercaptan (531) 120Nefolia (901) 148d-Neo-Menthol (428) 118Niobe oil (851) 1402,6-Nonadienal diethyl acetal (946) 154Nonanal (101) 1121,4-Nonanediol diacetate (609) 122(Z)-Non-6-en-1-al (325) 116cis-6-Nonenal (325) 116Nonyl caprylate (178) 114Nonyl octanoate (178) 114Octadecanoic acid (116) 112Octanal dimethyl acetal (942) 1545-Octanol-4-one (416) 118

Name Page(Z)-Oct-5-enal (323) 116cis-5-Octenal (323) 116(Z)-Oct-5-en-1-ol (322) 116cis-5-Octen-1-ol (322) 116Octen-3-yl 2-methyl-2-butenoate(448) 120Octyl 2-furancarboxylate (750) 126Octyl 2-furoate (750) 1263-Octyl tiglate (448) 120Oenanthal dimethyl acetal (947) 154Oil of niobe (851) 140Oranger crystals (811) 134Oxacycloheptadec-7-en-2-one (240) 1143-Oxodecanoic acid glyceride (914) 1503-Oxododecanoic acid glyceride(915) 1503-Oxohexadecanoic acid glyceride(917) 1503-Oxohexanoic acid diglyceride(910) 1483-Oxooctanoic acid glyceride (911) 1482-Oxopropanal (937) 1522-Oxopropanoic acid (936) 1523-Oxotetradecanoic acid glyceride(916) 150Palmitic acid (115) 112Paradiazine (951) 154Pelargonic aldehyde (101) 112alpha-Pentylcinnamaldehydedimethyl acetal (681) 124alpha-Pentylcinnamyl acetate (677) 124alpha-Pentylcinnamyl formate (676) 124alpha-Pentylcinnamyl isovalerate(678) 124Pentyl formate (119) 112Pentyl furan-2-carboxylate (748) 126Pentyl 2-furoate (748) 126Pentyl heptanoate (170) 114alpha-Phenethyl acetate (801) 134alpha-Phenethyl alcohol (799) 132Phenethyl cinnamate (671) 122alpha-Phenethyl-2-methylpropanoate(804) 134beta-Phenethyl beta-phenylacrylate(671) 122Phenethyl 3-phenylpropenoate (671) 122Phenethyl salicylate (905) 148beta-Phenylacrolein (656) 1223-Phenylallyl butyrate (652) 1223-Phenylallyl cinnamate (673) 124Phenylallyl cinnamate (673) 1244-Phenyl-2-butanol (815) 1364-Phenyl-3-buten-2-ol (819) 1364-Phenyl-3-buten-2-one (820) 1364-Phenyl-2-butyl acetate (816) 1362-Phenyl-3-carbethoxyfuran (752) 126Phenyl carbinol (25) 1101-Phenylethanol (799) 1321-Phenylethyl acetate (801) 1341-Phenylethyl butyrate (803) 134alpha-Phenylethyl butyrate (803) 134Phenyl ethyl carbinol (822) 1362-Phenylethyl cinnamate (671) 1222-(2-Phenylethylene)-1,3-dioxolane(648) 1221-Phenylethyl formate (800) 1321-Phenyl-2-ethyl-3-hexanone (830) 1382-Phenylethyl 2-hydroxybenzoate(905) 148

Name Page1-Phenylethyl isobutyrate (804) 134Phenyl ethyl ketone (824) 136Phenylethyl methyl carbinol (815) 136Phenylethyl methyl carbinyl acetate(816) 1361-Phenylethyl 2-methylpropanoate(804) 1341-Phenylethyl propionate (802) 134alpha-Phenylethyl propionate (802) 1342-Phenylethyl salicylate (905) 148Phenyl formic acid (850) 1402-Phenyl-5-hydroxy-1,3-dioxane(838) 1322-Phenyl-4-hydroxymethyl-1,3-dioxolane (838) 132Phenyl ketone (831) 138Phenylmethanol (25) 110Phenyl methyl carbinol (799) 132Phenyl methyl carbinyl acetate (801) 1342-(Phenylmethylene)heptyl acetate(677) 1242-(Phenylmethylene)heptyl formate(676) 1242-(Phenylmethylene)heptyl 3-methylbutanoate (678) 124Phenylmethyl isobutyrate (844) 140Phenyl methyl ketone (806) 134Phenylmethyl phenylacetate (849) 140Phenyl oxaromate (752) 1261-Phenyl-2-pentanol (825) 1363-Phenylpropanal (645) 1221-Phenyl-1,2-propanedione (833) 1381-Phenyl-1-propanol (822) 1361-Phenylpropanol (822) 1361-Phenyl-1-propanone (824) 1363-Phenyl-2-propenal (656) 1223-Phenyl-2-propenyl benzoate (760) 1263-Phenyl-2-propenyl butyrate (652) 1223-Phenylprop-2-enyl 3-Phenylpropenoate (673) 1243-Phenylpropionaldehyde (645) 1221-Phenylpropyl alcohol (822) 136Phenylpropyl aldehyde (645) 1221-Phenyl-2-propyl butyrate (814) 1361-Phenylpropyl butyrate (823) 136alpha-Phenylpropyl butyrate (823) 1363-Phenylpropyl caproate (642) 1223-Phenylpropyl cinnamate (672) 124beta-Phenylpropyl cinnamate (672) 1243-Phenylpropyl hexanoate (642) 1223-Phenylpropyl beta-phenylacrylate(672) 1243-Phenylpropyl 3-phenylpropenoate(672) 124Pineapple aldehyde C-19 (844) 140Piperonal (896) 146Piperonyl acetate (894) 146Piperonylaldehyde (896) 146Piperonyl isobutyrate (895) 146Potassium 2-(1'-ethoxy)ethoxypropanoate (933) 152Potassium O-(1'ethoxy)ethoxypropanoate (933) 152Propan-1,2-diyl dibenzoate (862) 1421,2-Propanediol (925) 1502-Propanethiol (510) 1201,2,3-Propanetriol (909) 148Propanetri-1,2,3-yl tribenzoate (861) 1421,2,3-Propenetricarboxylic acid (627) 122

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Name Page1-Propene-1,2,3-tricarboxylic acid(627) 1222-Propenyl cyclohexane acetate (12) 1102-Propenyl 4-cyclohexane butanoate(14) 1102-Propenyl 6-cyclohexanehexanoate (16) 1102-Propenyl 5-cyclohexanepentanoate (15) 1102-Propenyl trans-2-methyl-2-butenoate (10) 110Propionic acid, thioallyl ester (490) 120Propionylbenzene (824) 136Propiophenone (824) 136n-Propyl benzenecarboxylate (853) 140Propyl benzoate (853) 140n-Propyl benzyl carbinol (825) 136Propyl cinnamate (660) 1222-Propyl-1,4-diazine (763) 1284-Propyl-2,6-dimethoxyphenol (724) 124Propylene glycol (925) 142Propylene glycol dibenzoate (862) 142Propylene glycolmonooctadecanoate (926) 152Propylene glycol stearate (926) 152Propyl formate (117) 112Propyl methanoate (117) 112alpha-Propylphenethyl alcohol (825) 136Propyl beta-phenylacrylate (660) 122Propyl 3-phenylpropenoate (660) 1222-Propylpyrazine (763) 128Propylpyrazine (763) 1284-Propylsyringol (724) 124Protocatechualdehyde dimethylether (877) 144d-beta-Pulegomenthol (428) 118Pyrazine (951) 154Pyrazinemethanethiol (794) 1322-Pyrazinylcyclohexylmethane (783) 1302-Pyrazinylethanethiol (795) 132Pyrazinylethyl mercaptan (795) 132(Pyrazinylmethyl) cyclohexane (783) 130Pyrazinylmethyl mercaptan (794) 132Pyrazinyl methyl sulfide (796) 132Pyroracemic acid (936) 152Pyruvaldehyde (937) 152Pyruvic acid (936) 152Raspberry ketone methyl ether (818) 136Resedyl acetal (942) 154beta-Resorcylic acid (908) 148Rhodinyl isobutyrate (74) 112Rhodinyl isovalerate (77) 112Rhodinyl propionate (64) 110Sal ether (900) 148Salicyladehyde (897) 146Salicylal (897) 146Salicylic acid methyl ether (881) 144Salicylic ether (900) 1482-sec-Butyl-3-methoxypyrazine (791) 132Stearic acid (116) 112Stryallyl isobutyrate (804) 134Styrallyl acetate (801) 134Styrallyl alcohol (799) 132Styrallyl butyrate (803) 134Styrallyl formate (800) 132Styrallyl propionate (802) 1342-Styryl-1,3-dioxolane (648) 122Synthetic sweet birch oil (899) 148Synthetic teaberry oil (899) 148

Name PageSynthetic wintergreen oil (899) 148beta-Terpineol (374) 118Terpinyl butyrate (370) 118Terpinyl formate (367) 118Terpinyl isopentanoate (372) 118Terpinyl isovalerate (372) 118Tetradecanoic acid (113) 1125,6,7,8-Tetrahydroquinoxaline (952) 154Tetramethyl-1,4-diazine (780) 1302,3,5,6-Tetramethylpyrazine (780) 130Tetramethylpyrazine (780) 130Tetryl formate (124) 1142-Thionapthol (531) 120Tolualdehyde glyceryl acetal (mixedisomers) (867) 142Tolualdehydes (mixed o,m,p) (866) 142Tolubenzyl acetate (o,m,p) (863) 142Toluic aldehyde (mixed o,m,p) (866) 142o-Tolyl acetate (698) 124Tolyl acetate (863) 142Tolyl aldehyde (mixed o,m,p) (866) 1424- (p-Tolyl)-2-butanone (817) 136Tolyl carbinyl acetate (o,m,p) (863) 1421-p-Tolylethanol (805) 134Tolyl glycerin (867) 142p-Tolyl methyl carbinol (805) 134o-Tolyl salicylate (907) 148Triacetin (920) 1501,2,3-Triacetoxypropane (920) 150Triacetyl glycerine (920) 150Tribenzoin (861) 142Tributyrin (922) 1501,2,3-Tri(butyryloxy)propane (922) 150Trihydroxypropane (909) 1484-(2,6,6-Trimethyl-2-cyclohexenyl)-3-buten-2-one (388) 1181-(2,6,6-Trimethyl-2-cyclohexenyl)-1,6-heptadien-3-one (401) 1184-(2,6,6-Trimethyl-2-cyclohexen-1-yl)-3-methyl-3-buten-2-one (404) 1182,3,5-Trimethyl-1,4-diazine (774) 1282,2,4-Trimethyl-1,3-dioxolane (929) 1522,2,4-Trimethyl-1,3-oxacyclopentane(929) 1522,3,5-Trimethylpyrazine (774) 128Trimethylpyrazine (774) 128Tripropionin (921) 1501,2,3-Tri(propionyloxy)propane (921) 150Trithioacetone (543) 120Undecanal (107) 11210-Undecenal (330) 116Undec-10-en-1-al (330) 116n-Undecyl aldehyde (107) 112Vanillaldehyde (889) 146Vanillic aldehyde (889) 146Vanillin (889) 144Vanillin acetate (890) 146Vanillin isobutyrate (891) 146Vanillin methyl ether (877) 144Vanillyl alcohol (886) 146Vanillyl butyl ether (888) 146Vanillyl ethyl ether (887) 146Vanillylidene acetone (732) 126VEE (887) 146Veratraldehyde (877) 144Veratric aldehyde (877) 1444-Vinylphenol (711) 124p-Vinylphenol (711) 1242,4-Xylylaldehyde (869) 142

Name PageZimtaldehyde (656) 122

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Compendium of food additive specifications - fao.org · A consolidated edition of the Compendium for food additive specifications is ... Index by JECFA specifications title, chemical