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Gas Chromatography + olfactometry
basic principles and use in the food QC + RD
Summer School:
“Food Safety, Quality and Nutrition Course”
21st July 2014 ČZU Praha
Jan Marek – Shimadzu Handels GmbH
GC,GCMS Sales & Support Bohemia
Analytical & Measuring Instruments Division
Gas Chromatography + olfactometry
basic principles and use in the food QC + RD
CONTENTS
Gas Chromatography (GC) basic principles
Columns, Injectors, Detectors
Some special options – sampling, detection
Mass spectrometry (MS) for GC
Multidimensional techniques (MDGC, GCxGC)
GC + GCMS of flavour and fragrance
GC – Olfactometry
Conclusion
2
Gas Chromatography - basic principles
Analytical instrumental
techniques for organic compounds
UV-VIS, FTIR, NMR, MS, …. (titrations, etc.)
MIXTURES → SEPARATION BEFORE DETECTION
And so separation techniques are used,
wide range of combinations +
“multidimensional techniques“
GC (FID,...), GC/MS, LC (HPLC, UHPLC), LC/MS, ELECTROMIGRATION (Electrophoresis, ITP)
Gas Chromatography - basic principles
Introduction - Principle and structure of GC
CHROMATOGRAPHY IS ACTUALLY ONE OF THE MOST
IMPORTANT SEPARATION TECHNIQUE
Gas Chromatography - basic principles
Introduction - Principle and structure of GC
Stationary Phase and Mobile Phase ( carrier gas )
Mobile phase and stationary phase contact through phase boundary
Different compounds have different affinities to stationary phase and mobile phase
Difference of moving velocity results in
separation!
(interactions with MF are not so importent in GC but very much in LC! )
Mobile phase
Stationary phase
Strong Weak
Flow of MF (carrier gas)
Gas Chromatography - basic principles
Introduction - Principle and structure of GC
Chromatography : Analytical method
Chromatograph : Instrument
Chromatogram : Obtained
“picture”
Chromatographer : Analyst
Terminology
Gas Chromatography - why and when ?
Qualitative analysis ・ What components?
Quantitative analysis ・ How much of the component ?
Purpose of GC, GC/MS Analysis
Volatile and/or volatilised compounds only *
* Even other materials are possible - pyrolyse of polymers etc.
Gas Chromatography - basic principles Introduction -
Principle and structure of GC - Analytical method
Gas Chromatography - basic principles Introduction -
Principle and structure of GC - Analytical method
Gas Chromatography - basic principles
Introduction - Principle and structure of GC - Instrument
Heated Injection Port (with innert liner)
Sampling device-
syringe/autosampler
Column oven (thermostat) with a column –
capillary or packed
Gas Chromatography - basic principles
Introduction - Principle and structure of GC - columns
Structure of GC (for capillary column)
MS spectrometer
in case of GC/MS
Split unit manual and/or electronic
Flow controllers manual and/or electronic
Flow controllers manual and/or electronic
(Solenoid valve unit)
Gas Chromatography - basic principles
Introduction - Principle and structure of GC
Detectors
TCD
BID*
Inorganic gases, � Low sensitivity for organic compounds
Inorganic gases, � High sensitivity for organic compounds
FID Organic compounds ( higher sensitivity than TCD and linearity) mostly used detector
ECD Good sensitivity for high electron affinity compounds (halogenated compounds)
FPD Good sensitivity for phosphorous compounds and sulfureted compounds
FTD Good sensitivity for nitrogen compounds
* Barrier discharge Ionisation Detector
FPD data with packed column
Analytical Conditions
Column : ββ’-ODPN 25% on Chrormosorb W
60/80mesh 3.2mmφ×3.1m , Glass
COL.Temp. : 70℃
INJ.,DET.Temp. : 150℃
Carrier gas : N2 , 30mL/min
Detector : FPD S-mode
MeSH : Methyl Mercaptan
DMS : Dimethyl Sulfide
DMDS : Dimethyl Disulfide
5 10 15 m i n
H2S
MeSH DMS
DMDS
0
Standard gas 0.5mL injection
(1mg/L, N2 base)
The example of FPD S mode data acquired with typical packed column
for analyzing bad smell.
Gas Chromatography - basic principles
Introduction - Principle and structure of GC
Detectors
Barrier discharge Ionisation Detector
Gas Chromatography - basic principles
Introduction - Principle and structure of GC
Detectors
Barrier discharge Ionisation Detector Acetaldehyde
Meth
anol
Ethanol
Ace
tic A
cid
Form
ic A
cid
Water
BID
100 ppm concentration each comp. in water, 1:24 split
analysis, 0.5 μL sample volume
FID
Gas Chromatography - basic principles
Introduction - Principle and structure of GC
Injection techniques
Split injection Split vent is open. Only a part of sample is introduced to column. Used for high concentration samples Mostly used
Splitless injection Split vent is closed Almost all amount of sample is introduced to column. Used for low concentration samples
OCI injection Samples are directly injected to column. Used for samples including both low boiling components and high boiling
components. Used for thermally decomposed samples.
PTV injection Low temperature at injection port Solvent is removed at injection port. Used for large volume injections( a few L a few tens – a few hundreds L)
Gas Chromatography - basic principles
Introduction - Principle and structure of GC
Injection techniques
OPTIC-4 Most powerful multimode inlet
LINEX Automated Liner Exchanger
Gas Chromatography - basic principles
Introduction - Principle and structure of GC
Injection techniques
Gas Chromatography - basic principles
Introduction - Principle and structure of GC - Chromatogram
Gas Chromatography - basic principles
Introduction - Principle and structure of GC - Chromatogram
Gas Chromatography - basic principles
Introduction - Principle and structure of GC - Chromatogram
SVOC (Phthalate + Siloxane)
Gas Chromatography - basic principles
Introduction - Principle and structure of GC - Chromatogram
Direct TD – Coffee
Gas Chromatography - basic principles
Introduction - Principle and structure of GC/MS
Ionization Part Ionizes sample molecules
in vacuum
Mass Separation part
Separates ions
according to their
masses
Ion Detection Part Detects ions
Gas Chromatography - basic principles
Introduction - Principle and structure of GC/MS
Gas Chromatography - basic principles
Introduction - Principle and structure of GC/MS
EI ELECTRON IMPACT IONIZATION
EI Mass Spectrum
Gas Chromatography - basic principles
Introduction - Principle and structure of GC/MS
Gas Chromatography - basic principles
Introduction - Principle and structure of GC/MS
UF sensitivity Patented ASSP function
ensures high sensitivity
during high speed
scanning
UF scanning High speed calculation
process enables
20,000 u/sec scan
speeds
UF sweeper
(colision cell) High speed CID cell with
minimum 1 ms dwell
time achieves 600
trans/sec
High-Performance Supported by "UF technologies"
Triple Quadrupole Gas Chromatograph Mass Spectrometer
GCMS-TQ8030/40
Quadrupole mass filters Ion source
Detector
GC-MS/MS operation modes
Q1 Q3 Collision Cell
MRM
CID SIM SIM
Q1 Q3 Collision Cell
Precursor Ion Scan
CID SIM Scan
Q1 Q3 Collision Cell
Q3 Scan
Transfer Transfer Scan
Product Ion Scan
CID Scan SIM
Q1 Q3 Collision Cell
Chromatograms (Flavor and Fragrance)
Volatiles (Potpourri Fragrance Compounds) on SLB-IL60
SLB-IL60 has similar polarity, but employs different interaction mechanisms.
In addition to unique selectivity, the SLB-IL60 allows a faster analysis with the same run conditions.
30 sigma-aldrich.com/il-gc
PEG
SLB-IL60
Chromatograms (Flavor and Fragrance)
Essential Oils (Lemon) on SLB-IL59, 3 ºC/min Ramp Rate
SLB-IL59 employs different interaction mechanisms than a PEG.
This results in unique selectivity compared to PEG.
31 sigma-aldrich.com/il-gc
Chromatograms (Flavor and Fragrance)
Essential Oils (Lemon) on SLB-IL59, 5 ºC/min Ramp Rate
SLB-IL59 employs different interaction mechanisms than a PEG.
This results in unique selectivity compared to PEG.
32 sigma-aldrich.com/il-gc
Chromatograms (Flavor and Fragrance)
Essential Oils (Cold Pressed Lemon) on SLB-IL60
SLB-IL60 has similar polarity, but employs different interaction mechanisms.
In addition to unique selectivity, the SLB-IL60 allows a faster analysis with the same run conditions.
33 sigma-aldrich.com/il-gc
PEG
SLB-IL60
Chromatograms (Flavor and Fragrance)
Essential Oils (Distilled Lime) on SLB-IL60
SLB-IL60 has similar polarity, but employs different interaction mechanisms.
In addition to unique selectivity, the SLB-IL60 allows a faster analysis with the same run conditions.
34 sigma-aldrich.com/il-gc
PEG
SLB-IL60
Chromatograms (Flavor and Fragrance)
Essential Oils (Patchouli) on SLB-IL60
SLB-IL60 has similar polarity, but employs different interaction mechanisms.
In addition to unique selectivity, the SLB-IL60 allows a faster analysis with the same run conditions.
35 sigma-aldrich.com/il-gc
PEG
SLB-IL60
Chromatograms (Flavor and Fragrance)
Essential Oils (Peppermint) on SLB-IL59
SLB-IL59 employs different interaction mechanisms than a PEG.
This results in unique selectivity compared to PEG.
36 sigma-aldrich.com/il-gc
Chromatograms (Flavor and Fragrance)
Essential Oils (Kennewick Peppermint) on SLB-IL60
SLB-IL60 has similar polarity, but employs different interaction mechanisms.
In addition to unique selectivity, the SLB-IL60 allows a faster analysis with the same run conditions.
37 sigma-aldrich.com/il-gc
PEG
SLB-IL60
Chromatograms (Flavor and Fragrance)
Essential Oils (Willamette Peppermint) on SLB-IL60
SLB-IL60 has similar polarity, but employs different interaction mechanisms.
In addition to unique selectivity, the SLB-IL60 allows a faster analysis with the same run conditions.
38 sigma-aldrich.com/il-gc
PEG
SLB-IL60
Chromatograms (Flavor and Fragrance)
Essential Oils (Petitgrain) on SLB-IL60, 50 ºC Initial Oven Temp.
SLB-IL60 has similar polarity, but employs different interaction mechanisms.
In addition to unique selectivity, the SLB-IL60 allows a faster analysis with the same run conditions.
39 sigma-aldrich.com/il-gc
PEG
SLB-IL60
Chromatograms (Flavor and Fragrance)
Essential Oils (Petitgrain) on SLB-IL60, 75 ºC Initial Oven Temp.
SLB-IL60 has similar polarity, but employs different interaction mechanisms.
In addition to unique selectivity, the SLB-IL60 allows a faster analysis with the same run conditions.
40 sigma-aldrich.com/il-gc
PEG
SLB-IL60
Chromatograms (Flavor and Fragrance)
Essential Oils (Spearmint) on SLB-IL59, 50 ºC Initial Oven Temp.
SLB-IL59 employs different interaction mechanisms than a PEG.
This results in unique selectivity compared to PEG.
41 sigma-aldrich.com/il-gc
Chromatograms (Flavor and Fragrance)
Essential Oils (Spearmint) on SLB-IL59, 80 ºC Initial Oven Temp.
SLB-IL59 employs different interaction mechanisms than a PEG.
This results in unique selectivity compared to PEG.
42 sigma-aldrich.com/il-gc
Chromatograms (Flavor and Fragrance)
Essential Oils (Native Spearmint) on SLB-IL60
SLB-IL60 has similar polarity, but employs different interaction mechanisms.
In addition to unique selectivity, the SLB-IL60 allows a faster analysis with the same run conditions.
43 sigma-aldrich.com/il-gc
PEG
SLB-IL60
Chromatograms (Flavor and Fragrance)
Essential Oils (Scotch Spearmint) on SLB-IL60
SLB-IL60 has similar polarity, but employs different interaction mechanisms.
In addition to unique selectivity, the SLB-IL60 allows a faster analysis with the same run conditions.
44 sigma-aldrich.com/il-gc
PEG
SLB-IL60
Gas Chromatography - basic principles
Introduction - Principle and structure of GCxGC,MDGC
How to solve the problem
with
complete separation ?
GCxGC, MDGC
multidimensional separations…
Un
iver
sity
of
Mes
sin
a, It
aly
Comprehensive Two-dimensional GC Workshop
Peter Quinto Tranchida and Luigi Mondello
University of Messina, Italy
e-mail: [email protected]
23-24 February, 2010
Charles University, Prague
Conferences and Seminars:\I:\2010\023) GCxGC workshop Praha\Course
Un
iver
sity
of
Mes
sin
a, It
aly
At present, one-dimensional chromatography is the most commonly applied
method for the separation of real-world samples. It is generally accepted that 1D
chromatography methods provide rewarding analytical results on what can be
defined generically as “low-to-mediumly-complex samples”.
1950s: bergamot
oil and a packed GC column 1990s: bergamot
oil and capillary GC
Conferences and Seminars:\I:\2010\023) GCxGC workshop Praha\Course
The World and Chromatography
Un
iver
sity
of
Mes
sin
a, It
aly
GC x GC is an “on-line” multidimensional technique that enables a bidimensional
analysis of the entire initial sample, through continuous heart-cutting. The leap from
heart-cutting MDGC to comprehensive GC was acheived in 1991 by Liu and Phillips who
developed a new transfer system: the thermal modulator.
IT WAS AN EYE-OPENER FOR MANY ANALYTICAL CHEMISTS
Comprehensive 2D GC
Lui ZY and Phillips JB. J. Chromatogr. Sci. 1991, 29, 227-231
Conferences and Seminars:\I:\2010\023) GCxGC workshop Praha\Course
Un
iver
sity
of
Mes
sin
a, It
aly
DB:0
DB:1 C18:0
sec
min
C15:0
C16:0
C17:0
C19:0
C20:0
C21:0
C22:0
C23:0
C24:0
C25:0
C26:0
C15:1 C16:1w9
GC x GC olive oil result: 24 FAMEs,
some of which totally unexpected
C16:1w7
C17:1w7
C18:1w9tr
C18:1w9c
C18:2w6c,tr
C18:2w6c,c C18:3w3
C19:1 C20:1
Conferences and Seminars:\I:\2010\023) GCxGC workshop Praha\Course
Un
iver
sity
of
Mes
sin
a, It
aly
GC x GC hazelnut oil result: 33
FAMEs
DB:0
DB:1
DB:2
DB:3
s
min
C18:0
C15:0
C16:0 C17:0
C19:0
C20:0
C21:0
C22:0
C23:0
C24:0
C25:0
C26:0
C15:1
C16:1w9 C16:1w7 C16:1w5
C17:1w7
C16:2
C18:1w9tr C18:1w9c
C18:1w7
C17:2
C17:3
C19:1
C18:2w6c,tr
C18:2w6c,c
C20:1
C18:3w3
C20:2
C22:1
C22:2
C24:1
GC x GC hazelnut oil result: 31
FAMEs
Conferences and Seminars:\I:\2010\023) GCxGC workshop Praha\Course
Un
iver
sity
of
Mes
sin
a, It
aly
C16:1w7
C17:0
Extra-virgin
olive oil
Hazelnut
oil
C16:1w7
C17:0
C16:1w5
Conferences and Seminars:\I:\2010\023) GCxGC workshop Praha\Course
Gas Chromatography - basic principles
Introduction - Principle and structure of GCxGC
GCMS-TQ8030 Triple Quadrupole Gas Chromatograph Mass Spectrometer
2. Fastest Speed
Using Fast Q3 Scan and GCGC
Qualitative analysis using mass
spectrum from GCGC/Q3 scan
(20,000 u/sec)
Separate and analyze high matrix samples with GCGC
Switch to GCGC/Q3 MRM mode for trace
quantitative analysis of target components
Data currently being acquired at University of Messina.
To be presented at ISCC (capillary symposium) in May.
l
Gas Chromatography - basic principles
Introduction - Principle and structure of MDGC/MS
Easy setting software
MDGC divertible to normal
GC and GC/GCMS
High Performance
Separation with 2 columns
Hardware achieves perfect switching
MDGC/GCMS-2010
Heart-cut SEPARATION ON 2ND COLUMN
Multi Dean‘s Switching
Multi Dean‘s Switching-Cut Mode
P-ΔP2 < P-ΔP1
Pressure=P-ΔP1
APC Pressure=P
Pressure (ΔP2)
Valve
1st DET 2nd Column 1st Column
Pressure (ΔP1)
Pressure=P-ΔP2
Sample
Gas Chromatography - basic principles
Introduction - Principle and structure of MDGC/MS
Heart cutting
Gas Chromatography - basic principles
Introduction - Principle and structure of MDGC/MS
Heart cutting
Barbara d’Acampora Zellner and Luigi Mondello
Université de Messina
Wil van Egmond
ATAS GL, Veldhoven, The Netherlands
http:/pharma.unime.it/foodchem
Grasse, 7th April 2005
Olfactometric Perception by GC-O of Chiral Compounds
What are Chiral Compounds?
Any carbon atom bonded to four different groups is termed a chiral or an assymetric carbon.
Molecules containing one or more of these carbon centers are considered chiral molecules.
Chiral centers can exist in two forms called enantiomers. These two forms are non superimposable mirror images of each other, but both have similar properties.
Life and Chirality
In extremely simple terms, chirality is "handedness“, that means, the existence of left and right opposition, as the
hands, that are mirror images and therefore "chiral".
“[...] I call any geometrical figure, or group of points, chiral, and say it has chirality, if its image in a plane mirror, ideally realized, cannot be
brought to coincide with itself [...]“
From: Lord Kelvin, Baltimore Lectures on Molecular Dymnamics and the Wave
Theory of Light (1904).
Life and Chirality
Enantiomers may show different behaviour when interacting with living beings.
As the enantiomers of chiral drugs, often characterised by different pharmacological activity, one enantiomer being usually bioactive, whereas the other either inactive or inhibitory.
Chirality and Odour Perception
In the beginning of the 20th century chemists in the Flavour and Fragrance Industry recognized that certain enantiomeric chemicals, such as menthol and carvone presented different and also differentiating organoleptic properties.
In 1961 Rienäcker and Ohloff published the first data regarding the enantioselective perception of (+)-b-Citronellol as having a citronella-like odour, while (-)-b-Citronellol had a geranium-like odour.
(Rienäcker, R. and Ohloff G. Angew. Chemie, 73, 240, 1961)
In the 1960's, a number of processes had been developed for the synthesis of the desired enantiomer, e.g. (-)-menthol from optically active terpenoids.
Chirality and Odour Perception
However, based on erroneous theories of olfaction, the premise that optical enantiomers could have different odours was not generally accepted by various academics until the 1980's.
Prior to GC and other measurements of purification techniques, the purity of the enantiomers used in odour evaluations was not precise. In addition, a high enantiomeric excess is nearly always required in organoleptic evaluations.
Flavour and Fragrance Compounds
Numerous substances presenting different functional groups, and frequently chiral centres.
Enantiomers can differ in:
odour quality odour activity odour intensity
Sensorial Properties of Chiral Compounds
eliciting identical or different odour
sensations
described by value of odour threshold
one of the isomers is odourless
Sensorial Properties of Enantiomers
O
H
H
O
HO
H
(R)-(-)-Linalool
floral, fresh, woody, lavender note
Odor Threshold = 9-11 ppb in air
(S)-(+)-Linalool
herbaceous, musty green, odor
reminiscent of petitgrain
Odor Threshold = 35- 40 ppb in air
(4S)-(+)-Carvone
herbaceous, dill and caraway seeds
Odor Threshold = 85-130 ppb in air
(4R)-(-)-Carvone
herbaceous, spearmint
Odor Threshold = 2 ppb in air
(1S,3S,4R)-(+)-Menthol
Sweet, fresh, minty, strong
(1R,3R,4S)-(-)-Menthol
Dusty, vegetable,
less minty, less fresh
H
OH
OH HO
Why is the Olfactive Investigation of Enantiomers important?
• Continuous demand for new synthetic compounds evoking unusual odour sensations or reproducing those elicited by natural fragrances;
• To establish odour-structure relationship requirement;
• Increasing environmental and health risks associated with massive usage of fragrances in fine and functional perfumery;
• Compounds added to food and beverages are subjected to strict regulations choose the ‘best aromatic’ isomer;
• To optimise the analytical methods to assess the authenticity of natural materials.
The identification of the isomer present as the main odour vector has become an unavoidable task.
Chiral Chromatography in Olfactive Enantiomer Evaluation
Chiral chromatography enables to the separation of enantiomeric compounds.
Common liquid stationary phases do not possess adequate selectivity for enantiomeric separation.
Application of stationary phases with added derivatized cyclodextrin (CD) macromolecules leads to the separation of several enantiomers.
CDs derive from enzymatic degradation of starch polysaccharide by CD glycosiltransferase from Klebsiella pneumonia or Bacillus macerans.
Olfactive Investigation of Enantiomers through GC-O
Gas Chromatography- Olfactometry
• Standard technique to assess odour-active components in
natural products and complex mixtures.
• Unique analytical technique which associates resolution
power of capillary GC with the selectivity and sensitivity of
the human nose.
GC-Olfactometry
GC-2010
Sniffer - Phaser
PHASER – GC-O
ATAS GL Internatiobal BV
Glass Nose Cone
Heated Transfer
Line (300oC)
Dimensions: 35mm
(diameter) x 60cm
(length)
Water Reservoir with bubbling
filter
Aux. Gas: He or N2
Controller
Power, Heater, Temperature Controller, Air Flow
Flexible Arm
GC inserting
part
Split Manager
Major Drawbacks of Olfactometry
Evaluation by more than one panelist
Normalisation of the descriptive olfactive language
Involves time-consuming methods
Obtained results are based on detection thresholds,
not on real intensities
Goal: optimize data obtained in any evaluation
Software
Odour Evaluation Software
Quality Description of Olfactive Impressions
• Voice Recognition Software
• Touchscreen
Intensity Description of Olfactive Impressions
• Magnitude Estimation using a variable resistor with a
pointer moving according to the pressure exerted by the
thumb along a category scale
• Finger Span Method
Considering Pros & Contras Software Prototype
Application: Enantiomeric Evaluation
Rosewood oil x Ho oil Linalool is one of the most important substances for F & F Industries
(R)-(-)-Linalool Licareol
floral, fresh, woody, lavender note Odor Threshold = 9-11 ppb in air
(S)-(+)-Linalool Coriandrol
herbaceous, musty green, odor reminiscent of petitgrain
Odor Threshold = 35- 40 ppb in air
Rosewood oil (Aniba roseodora Ducke)
rich in (S)-(+)-Linalool
Ho oil (Cinnamomum camphora)
rich in (R)-(-)-Linalool
differences in optical properties and odour
Application: Enantiomeric Evaluation of Rosewood oil
Distilled Leaves Oil
Column: DETTBSBTA - l: 25m ; i.d.: 0.25 mm; df: 0.25μm (MEGA, Milano) Inj. temp.: 250°C; mode: split, ratio: 1/50; Det.: FID, temp.: 250°C; Temp. progr.: 45°C- 2°C/min - 200°C
5.0 10.0 15.0 20.0 25.0 30.0 35.0 40.0 45.0 min
0.0
1.0
2.0
3.0
4.0
uV(x10,000)Chromatogram
(+) Linalool (-) Linalool
Application: Enantiomeric Evaluation of Ho oil
Column: DETTBSBTA - l: 25m ; i.d.: 0.25 mm; df: 0.25μm (MEGA, Milano) Inj. temp.: 250°C; mode: split, ratio: 1/50; Det.: FID, temp.: 250°C; Temp. progr.: 45°C- 2°C/min - 200°C
Linalool extracted from Ho oil
10.0 15.0 20.0 25.0 30.0 35.0 40.0 45.0 min
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
uV(x10,000)
0
50
100
150
200
250
300
350
400
CChromatogram
(-) Linalool
(+) Linalool
Application: Enantiomeric Evaluation of Rosewood oil
Distilled Leaves Oil
3- (+)- Terpinen-4-ol
4- (-)- Terpinen-4-ol
5- (-)- a- Terpineol
6- (+)- a- Terpineol
Column: DETTBSBTA - l: 25m ; i.d.: 0.25 mm; df: 0.25μm (MEGA, Milano) Inj. temp.: 250°C; mode: split, ratio: 1/50; Det.: FID, temp.: 250°C; Temp. progr.: 45°C- 2°C/min - 200°C
20.0 22.5 25.0 27.5 min
0.0
0.5
1.0
1.5
2.0
uV(x10,000)Chromatogram
30.0 32.5 35.0 37.5 40.0 42.5 min
2.5
5.0
7.5
10.0
uV(x1,000)Chromatogram
1- (-)- Limonene
2- (+)- Limonene
1
2
3
4
5
6
Application: Enantiomeric Evaluation of Rosemary oil
Column: DETTBSBTA - l: 25m ; i.d.: 0.25 mm; df: 0.25μm (MEGA, Milano)
Inj. temp.: 250°C; mode: split, ratio: 1/50; Det.: FID, temp.: 250°C; Temp. progr.: 45°C- 2°C/min - 200°C
5.0 10.0 15.0 20.0 25.0 30.0 35.0 40.0 45.0 50.0 55.0 min
0.0
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
uV(x10,000)
0
50
100
150
200
250
300
350
400
CChromatogram
(+) Linalool: herbaceous, green, petitgrain
(-) Linalool: floral, fresh, lavender
(+) Limonene: fresh, citrus,
orange-like
(-) Limonene: harsh,
turpentine-like
(+) Terpinen-4-ol: musty, dusty
(-) Terpinen-4-ol: musty
“Il est des parfums frais comme des chairs d’enfants,
Doux comme les hautbois, verts comme les prairies,
et d’autres, corrumpus, riches et triomphants,
ayant l’expansion des choses infinies
Comme l’ambre, le musc, le benjoin et l’encens,
Qui chantent les transports de l’esprit et des sens”
Les Fleurs du Mal
C. Baudelaire
http:/pharma.unime.it/foodchem
Phaser – Hardware Conclusion
Phaser – Hardware Conclusion
MDGCMS - Phaser – Hardware Conclusion
• No cold spot possibility to sniff higher boiling point
compounds • Maximum 300°C on transfer line • Protects your nose from drying by adding moisture air to sniffing port • Easy to connect capillary column to splitter • Sitting down or standing up while sniffing • Compact and easy to use •MDGCMS – detailed separation and identification
Gas Chromatography + olfactometry
basic principles and use in the food QC + RD
85
Some more info on www.shimadzu.eu
Shimadzu Handels GmbH - org.složka
Ocelářská 35, 190 00 Praha
tel.+420 284080221
fax +420 284080225
Thank you for your attention !