Proficiency Test Report Clandestine Laboratory and Unknown ID · This report presents the results of AQA 15-17 – Clandestine Laboratory and Unknown ID. This is a qualitative program

Proficiency Test ReportAQA 15-17Clandestine Laboratory and Unknown ID

February 2016

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ACKNOWLEDGMENTS

This study was conducted by the National Measurement Institute (NMI). Support funding was provided by the Australian Government Department of Industry, Innovation and Science. I would like to thank the management and staff of the participating laboratories for supporting the study. It is only through widespread participation that we can provide an effective service to laboratories.

The assistance of the following NMI staff members in the planning, conduct and reporting of the study is acknowledged.

Raluca Iavetz Helen Salouros

Michael Collins

I would also like to thank Ben Painter member of SMANZFL Specialist Advisory Group (SAG) for assisting NMI in the development of this proficiency testing study and providing comments on this report.

Paul Armishaw Manager, Chemical Reference Values 105 Delhi Rd, Riverside Corporate Park, North Ryde NSW 2113 P O Box 138, North Ryde NSW 1670

Phone: 61-2-9449 0149 Fax: 61-2-9449 0123 [email protected]

Accredited for compliance with ISO/IEC 17043

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TABLE OF CONTENTS SUMMARY 1 1 INTRODUCTION 2

1.1 NMI Proficiency Testing Program 2 1.2 Study Aims 2 1.3 Study Conduct 2

2 STUDY INFORMATION 2 2.1 Study Timetable 2 2.2 Participation 2 2.3 Laboratory Code 2 2.4 Sample Storage, Dispatch and Receipt 2 2.5 Instructions to Participants 3 2.6 Interim Report 3

3 SAMPLE SYNTHESIS AND ANALYSIS FOR S1 AND IDENTIFICATION FOR S2 4 3.1 Sample S1 (white powder): Synthesis 4 3.2 Sample S1 (white powder): Analysis 4 3.3 Sample S1 (white powder): Conclusions 7 3.4 Sample S2 (powder): Identification 7

4 PRESENTATION OF RESULTS 9 4.1 Sample S1 9 4.2 Sample S2 17

5 DISCUSSION OF RESULTS 19 6 REFERENCES 20 APPENDIX 1 – PARTICIPANT LABORATORIES 21 APPENDIX 2 - ACRONYMS AND ABBREVIATIONS 22

AQA 15-17 CLANDESTINE LABORATORY 1

SUMMARY

This report presents the results of AQA 15-17 – Clandestine Laboratory and Unknown ID. This is a qualitative program and involved the analysis of two samples. Sample S1 representing material seized from a hypothetical clandestine laboratory required identification and its possible illegitimate uses. Sample S2 is an unknown substance and had to be identified. Sixteen laboratories participated and fifteen submitted results by the due date. One laboratory requested more than one set of test samples. The additional test sample was analysed independently by a different analyst and the laboratory submitted results for each set of samples. Two test samples were prepared at the NMI laboratory in Sydney. Sample S1 prepared to represent the material found in a hypothetical clandestine laboratory was 1-phenyl-1-chloro-2-methylamino-propane hydrochloride or chloromethylamphetamine, a mixture of chloroephedrine and chloropseudoephedrine. Chloromethylamphetamine can be used illegitimately as an immediate precursor to methylamphetamine. The scenario provided by the study coordinator was indicative of ‘Emde’ method as the method employed by the clandestine lab to produce methylamphetamine. Sample S2 was UR-144 or (1-pentyl-1H-indol-3-yl)(2,2,3,3-tetramethylcyclopropyl) methanone or (1-pentylindol-3-yl)(2,2,3,3-tetramethylcyclopropyl) methanone. The aims of this study were:

assess the ability of the participant laboratories to correctly identify the clandestine laboratory product, its possible illegitimate use and the mechanism to produce the substance based on a scenario provided by the study coordinator;

Laboratory 15 identified incorrectly Sample S1 as Ephedrine and Methylamphetamine and did not address the question of its illegitimate use or the mechanism to produce the controlled drug based on the scenario provided.

Laboratory 7 response regarding the mechanism to produce the substance found in the hypothetical clandestine laboratory is inconsistent with the scenario provided.

to correctly identify an unknown substance labelled. All participants identified correctly Sample S2

.


1 INTRODUCTION 1.1 NMI Proficiency Testing Program

The National Measurement Institute (NMI) is responsible for Australia’s national measurement infrastructure, providing a range of services including a chemical proficiency testing program. Proficiency testing (PT) is: ‘evaluation of participant performance against pre-established criteria by means of interlaboratory comparison.’1 NMI PT studies target chemical testing in areas of high public significance such as trade, environment, law enforcement and food safety. NMI offers studies in:

pesticide residues in fruit and vegetables, soil and water; petroleum hydrocarbons in soil and water; metals in soil, water, food and pharmaceuticals; controlled drug assay; and folic acid in flour.

1.2 Study Aims

The aim of the study were to:

assess the ability of the participant laboratories to correctly identify the clandestine laboratory product and, its possible illegitimate use and the mechanism to produce the controlled drug based on a scenario provided by the study coordinator ; and

to correctly identify an unknown substance. The choice of the test method was left to the participating laboratories. 1.3 Study Conduct

NMI is accredited by the National Association of Testing Authorities, Australia (NATA) to ISO 170431 as a provider of proficiency testing schemes. This clandestine laboratory proficiency test is within the scope of NMI’s accreditation. 2 STUDY INFORMATION 2.1 Study Timetable

The timetable of the study was:

Invitation issued: 18 September 2015 Samples dispatched: 11 November 2015 Results due: 08 January 2016 Interim report issued: 20 January 2016 2.2 Participation

Invited 96 Participated 16 Submitted results 15 A list of participant laboratories is presented in Appendix 1.

One laboratory requested two sets of test samples. The additional test sample was analysed independently by a different analyst and the laboratory submitted results for each set. 2.3 Laboratory Code

Each participant was randomly assigned a confidential laboratory code.

2.4 Sample Storage, Dispatch and Receipt

The samples were securely stored at room temperature before dispatch.


A set of two test samples, S1 white powder 120 mg and S2 powder 120 mg, were dispatched on 11 November 2015. The following items were packaged with the samples:

a covering letter with instructions for participants; and

a faxback form for participants to confirm the receipt of the test samples. An Excel spreadsheet for the electronic reporting of results was e-mailed to participants. 2.5 Instructions to Participants

For Sample S1 participants were provided with the following scenario:

“At the premises of a clan lab investigation the following items were retrieved: bottles of ether, ethanol, methanol, chloroform, some aluminium foil cut into strips, palladium catalyst, mercury, some discarded glass jars labelled “Very Toxic - wash your hands after use”, many large pieces of glassware and heating mantles. Also present was a sealed metal vessel with a number of taps and valves which was attached to an unmarked red gas cylinder. A white powder was also found drying on some filter paper. This white powder (Sample S1) has been submitted for analysis. Participants were asked to analyse this sample using their routine method and return the following information:

What is the white powder?

Can this substance be used for illegitimate purposes? If so, in what way?

For Sample S2 participants were asked to identify an unknown substance.

Reporting Results

Return the completed results sheet by e-mail ([email protected])

Results are to be returned by cob Friday 8 January 2016. Initial submission date for results was Friday 18 December 2015, but some participants received the test samples late and the due date has been extended to 8 January 2016.

2.6 Interim Report

An interim report was e-mailed to all participants on 20 January 2016.


3 SAMPLE SYNTHESIS AND ANALYSIS FOR S1 AND IDENTIFICATION FOR S2 3.1 Sample S1 (white powder): Synthesis

Pseudoephedrine hydrochloride was mixed with chloroform and thionyl chloride for several hours. To the reaction mixture was then added ether, resulting in precipitation of the chloromethylamphetamine hydrochloride. The chloromethylamphetamine was then washed with 50:50 ether:chloroform and the sample was dried.

CH3 CH3

ClH

NHCH3H

SOCl2, CHCl3

OH

NHCH3

Figure 1: The synthetic route used to make Sample S1 chloromethylamphetamine sample from pseudoephedrine

NB Chloromethylamphetamine is used to refer to the chlorinated product of pseudoephedrine, which is a mixture of chloropseudoephedrine and chloroephedrine. 3.2 Sample S1 (white powder): Analysis

Analysis of the Sample S1 by GC-MS revealed the presence of cis- and trans-1,2-dimethyl-3-phenylaziridine (1) and chloromethylamphetamine (2).

N

CH3

CH3

H

H

CH3

HNCH3

Cl

(1) (2)

The GC-MS chromatogram is presented in Figure 2. Mass spectra of these substances are presented in Figures 3 and 4 2-5.

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TIC: aeCpeHS.D\ data.ms

Figure 2: GC-MS chromatogram of Sample S1 – alkaline extract

cis- and trans- 1,2-dimethyl-3-phenylaziridine

chloromethylamphetamine Internal Standard


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Scan 613 (6.228 min): aeCpeHS.D\ data.ms146.1

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132.1

91.177.0 117.0

42.163.151.1

Figure 3: Mass spectrum of cis- and trans-1,2-dimethyl-3-phenylaziridine (cis-isomer)

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Average of 7.615 to 7.631 min.: aeCpeHS.D\ data.ms (-)58.1

117.091.0132.1 148.177.042.0 105.1

168.1 182.0

Figure 4: Mass spectrum of chloromethylamphetamine The sample was derivatised using trifluoroacetic acid (TFAA).2 Analysis of the sample by GC-MS (Figure 5) revealed the presence of chloropseudoephedrine (8.49 min) and chloroephedrine (8.21 min). Mass spectra of the TFAA derivatives of these substances are shown in Figures 6 and 7 respectively.

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Figure 5: GC-MS chromatogram of Sample S1 - TFAA derivatised

Internal Standard

chloropseudoephedrine TFAA derivative

chloroephedrine TFAA derivative


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Average of 8.494 to 8.504 min.: tfCpeHS.D\ data.ms (-)154.0

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42.169.0 91.0

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Figure 6: Mass spectrum of chloropseudoephedrine TFAA derivative

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Average of 8.213 to 8.224 min.: tfCpeHS.D\ data.ms (-)154.0

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244.1210.1173.9

Figure 7: Mass spectrum of chloroephedrine TFAA derivative

The sample was analysed by FTIR and the results (Figure 8) matched the infrared spectrum of chloromethylamphetamine hydrochloride.1

Figure 8: Infrared spectrum of chloromethylamphetamine Sample S1


3.3 Sample S1 (white powder): Conclusions

The white powder Sample S1 was identified as chloromethylamphetamine; a mixture of chloroephedrine and chloropseudoephedrine. Chloromethylamphetamine is an immediate precursor to methylamphetamine. Chloromethylamphetamine can be reduced to methylamphetamine with hydrogen under reduced pressure in the presence of a catalyst, such as palladium on barium sulphate. This method is commonly referred to as the ‘Emde’ method. At the premises the presence of the following items: palladium catalyst, ethanol, ‘red gas cylinder’ (most likely hydrogen) and a sealed metal vessel with a number of taps and valves, supports that this laboratory was equipped to synthesise methylamphetamine from Sample S1 chloromethylamphetamine. 3.4 Sample S2 (powder): Identification

Analysis of the Sample S2 by GC-MS revealed one major component (11.67 min) and another minor component (11.76 min) (Figure 9).

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TIC: SUR2h.D\ data.ms11.677

11.766

12.292

Figure 9: GC-MS chromatogram of sample S2

The mass spectrum of the major component (Figure 10) gave a library match to UR-1444 and the minor component (Figure 11) gave a library match to “UR-144 gc artifact”. The minor component is a thermally reduced rearrangement product of UR-144, an artefact produced due to the high GC injection port temperature.6

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Average of 11.655 to 11.682 min.: SUR2h.D\ data.ms (-)214.2

144.1

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Figure 10: Mass spectrum of UR-144

Internal Standard

UR-144

UR-144 cyclopropyl rearrangement product


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Scan 1657 (11.761 min): SUR2h.D\ data.ms (-1664) (-)214.2

144.0

296.3

43.0172.1

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341.1

Figure 11: Mass spectrum of UR-144 cyclopropyl rearrangement product

The sample was analysed by FTIR and the results (Figure 12) matched the infrared spectrum of UR-144.6

Figure 12: Infrared spectrum of UR-144


4 PRESENTATION OF RESULTS 4.1 Sample S1

Identify the substance. Can this substance be used illegitimately? If so, in what way?

Table 1 Sample Details

Sample S1 Chloromethylamphetamine hydrochloride

or

1-phenyl-1-chloro-2-methylamino-propane hydrochloride

Reasoning Sample S1 can be used for illegitimate purpose as it is an immediate precursor of methylamphetamine. It can be reduced to methylamphetamine with hydrogen under reduced pressure in the presence of a catalyst such as palladium on barium sulphate

NB Chloromethylamphetamine is used to refer to the chlorinated product of pseudoephedrine, which is a mixture of chloropseudoephedrine and chloroephedrine.

Participants’ Result Question 1: Identify the substance

Table 2 Sample S1 identity Lab

Code Results

1 Chloroephedrine hydrochloride

2 (aS, bR)-b-chloro-N,a-dimethyl-benzeneethanamine, hydrochloride (also known as (1R, 2S)-chloroephedrine, hydrochloride).

3 (+/-)-Chloroephedrine

4 Indicated to contain chloropseudoephedrine.

5 Chloroephedrines as the hydrochloride

7 Chloromethylamphetamine (1-phenyl-1-chloro-2-methylamino-propane)

8 1-Chloro-N-methyl-1-phenylpropan-2-amine hydrochloride

10 Chloroephedrine

11 Indicated to contain chloro(pesudo)ephedrine

12 1-phenyl-1-chloro-2-methylaminopropane HCl

13 probably 1-phenyl-1-chloro-2-methylaminopropane (chloroephedrine)

14 1-phenyl-1-chloro-2-methylaminopropane (Chloroephedrine/Chloropseudoephedrine)

15 Ephedrine and Methylamphetamine

16 Probably chloroephedrine and/or chloropseudoephedrine. (And probably cis- and/or trans-1,2-dimethyl-3-phenylaziridine.)

17 Chloroephedrine

NOTE: For the purpose of this PT trial the terms chloromethylamphetamine, chloroephedrine and chloropseudoephedrine are accepted.


Question 2: Can this substance be used illegitimately? If so, in what way? Table 3 Illegitimate uses for Sample S1

Lab Code Reasoning Study coordinator comment

1 Chloroephedrine can be used in the manufacture of methamphetamine via the "Emde" method. The "Emde" method involves chloroephedrine being hydrogenated over a palladium (combined with Barium sulphate) catalyst to form methamphetamine. This is commonly carried out in a hydrogenator or pressure vessel equipped with hydrogen gas.

The response is consistent with the scenario provided

2

Yes. It can be made into (S)-methylamphetamine by hydrogenation. Pressurised hydrogen gas (possible contents of the red cylinder) may be applied to this material in the presence of a catalyst such as palladium on barium sulphate (possible "palladium catalyst"). This process may have been occurring in the sealed metal vessel. This material can also be converted to methylamphetamine using the various hydriodic acid methods such as hypophosphorous acid and iodine (not indicated).


3

Chloroephedrine may be produced from pseudoephedrine (or its isomer, ephedrine) using thionyl chloride (or PCl5, POCl3 or PCl3). The chloroephedrine may then be reduced by catalytic hydrogenation to produce methylamphetamine. This is consistent with the description of the suspected clan lab scene, particularly the presence of palladium and a suspected hydrogen cylinder.


4

Yes. Chloropseudephedrine is an intermediate in the manufacture of methylamphetamine from ephedrine/pseudoephedrine, it can undergo metal catalysed hydrogenation to form methylamphetamine. The most common method for the hydrogenation is the Emde method, this method utilises hydrogen gas and Palladium/Barium Sulfate.


5

The substance (S1) contained a mixture of chloropseudoephedrine and chloroephedrine. This was based on structural elucidation by NMR of in house synthesis of Chloroephedrines and, then comparing these results with the literature and the H-1NMR of the unknown sample (S1). Based on the cylinders colouring, the "red gas cylinder" could contain hydrogen gas. Chloro(pseudo)ephedrine can be reduced to methylamphetamine by catalytic hydrogenation. Catalysts such as palladium in conjunction with hydrogen gas could be used to reduce chloro(pseudo)ephedrine to methylamphetamine. The sealed metal vessel attached to the "red gas cylinder" could be used as a hydrogenator. The chemicals and equipment as listed in this scenario would be suitable for the manufacture of controlled substances, including methylamphetamine.


7 Can be used for the illicit manufacture of methamphetamine via electrolytic reduction The response is inconsistent with the scenario provided

8 The substance (aka chloromethamphetamine or chloro(pseudo)ephedrine) can be reduced to methamphetamine. This can be achieved through catalytic hydrogenolysis. The chemicals (palladium catalyst, hydrogen) and apparatus (metal vessel) described in the scenario can be used in that process.




10 Yes. Chloroephedrine is an intermediate in the synthesis of methamphetamine from ephedrine or pseudoephedrine by the Emde method. Two 1,2-dimethyl-3-phenylaziridine signals, probably the cis and trans isomers, are in correspondance with this pathway.


11 Yes. Chloro(pseudo)ephedrine can be reduced to methylamphetamine using the Emde method. This involves the catalytic hydrogenation of chloro(pseudo)ephedrine by reaction with hydrogen and a palladium catalyst.


12 Yes. Reduction (e.g. catalytic hydrogenation) would yield methylamphetamine. The response is consistent with the scenario provided

13 Yes, it's a route specific marker of methamphetamine synthesized from ephedrine via chloroephedrine.

The response is consistent with the scenario provided, but chloromethylamphetamine is not a 'route specific marker compound', the presence of this compound in methylamphetamine does not necessarily indicate an 'Emde synthesis. It can also be produced during the salting out process of the methylamphetamine. (ie the conversion of the methylamphetamine base to methylamphetamine HCl).

14

Chloroephedrine can be reduced to produce methylamphetamine. Most methods of doing this recommend the use of a palladium catalyst in order to get a higher yield of methylamphetamine. These methods also require the use of solvents such as chloroform, methanol and ether, either for the production of the chloroephedrine, or the conversion of chloroephedrine to methylamphetamine. Palladium catalysts and the other solvents are all mentioned as being present in the scenario provided.


15

Ephedrine is not a controlled drug under existing legislation and it does have many potential legitimate uses. It is used as a decongestant in many cold and flu remidies such as sudafed. However it is also used as a precursor for the production of methylamphetamine which is well documented in scientific literature and in online drug manuals. Methylamphetamine is widely abused around the world and is one of the most commonly abused stimulants in the USA. It is also a class A controlled drug within the provisions of the Misuse of Drugs Act 1971. Any legitimate use of this drug is usually in the form of a tablet which can be used in the treatment of ADHD and narcolepsy.

The response does not address the question about the illegitimate use of the Sample S1 or the mechanism to produce the controlled drug based on the scenario provided.

16 Yes, this substance can be uses illegitimally. Cis- and/or trans-1,2-dimethyl-3-phenylaziridine is made as an impurity in conversion of chloroephedrine/chloropseudoephedrine to methamphetamine. So the sample probably comes from a methlab.

The response is consistent with the scenario



17

Ephedrine / Pseudoephedrine is typically converted to the chloro derivative prior to reduction by catalytic hydrogenation. GC-MS analysis of the substance indicated the presence of cis and trans di methyl phenyl aziridines which could have been present as the aziridine or be breakdown products from ephedrine or haloephedrine. LC-MS analysis indicated that it was the chloro ephedrine M+H of 184 and NMR conformed structure in ratio of 3:1 trans :cis chloroephedrine. The red cylinder indicated Hydrogen and Pd catalyst therefore the deduction made that this was an intermediate product to methamphetamine production.

The response is consistent with the scenario


Table 5 Additional Comments from Participants

Lab Code Additional Comments

1 Indications of 1,2-dimethyl-3-phenylaziridine were also detected during GCMS analysis. This was not reported as 1,2-dimethyl-3-phenylaziridine is known to form during the analysis of chloroephedrine by GCMS.

2

The (1R, 2S)-chloroephedrine hydrochloride can be manufactured from (1S, 2S)-pseudoephedrine hydrochloride using thionyl chloride when a co-solvent such as chlorofom is employed. When a co-solvent is employed for the synthesis the SN2 mechanism predominates resulting in inversion of stereochemical configuration. It is interesting to note that when a co-solvent is not used the SNi mechanism predominates which results in the retention of stereochemical configuration. So (1S, 2S)-pseudoephedrine hydrochloride will give (1S, 2S)-chloropseudoephedrine hydrochloride when there is no co-solvent.

3 Unable to confirm the stereoisomer (+/-)-chloroephedrine. No standard material was available for comparison with the sample. The presence of cis- and trans-1,2-dimethyl-3-phenyl aziridine due to rearrangement of chloroephedrine in the GCMS also supports the determination of (+/-) chloroephedrine.

4 The chloropseudoephedrine could only be indicated as there was no reference standard available. There was insufficient time to get a standard and/or synthesis the product ourselves.

5 NMR analysis of synthesised chloro(pseudo)ephedrines and literature (Allen et al, J Forensic Sci 32 953-962 (1987) and Cayman Chemical product information sheet), indicated the substance (S1) has most likely been produced from the chlorination of pseudoephedrine.

7 Running sample S1 by GCMS causes formation of aziridines in the inlet.

8 A reference standard was not available for direct comparison. A molecular weight of 183/185 with single chlorine distribution was confirmed by ESI MS. Reducible chlorine was confirmed by HI reduction to methamphetamine.

11 We were unable to confirm the presence of chloro(pesudo)ephedrine as we had no refence standard available.

15 Sample was found to contain two components when analysed by GCMS which were identified as Ephedrine and Methylamphetamine.

16

We report the identity of chloroephedrine and/or chloropseudoephedrine as probably because we only got the FTIR result and could not confirm it with GCMS. We also found probably cis- or trans-1,2-dimethyl-3-phenylaziridine But we think this is likely to be formed due to too high temperature in the GC column. We can not determine the sterioisomery of cis/trans.

17

Ephedrine / Pseudoephedrine is typically converted to the chloro derivative prior to reduction by catalytic hydrogenation. GC-MS analysis of the substance indicated the presence of cis and trans di methyl phenyl aziridines which could have been present as the aziridine or be breakdown products from ephedrine or haloephedrine. LC-MS analysis indicated that it was the chloro ephedrine M+H of 184 and NMR conformed structure in ratio of 3:1 trans :cis chloroephedrine. The red cylinder indicated Hydrogen and Pd catalyst therefore the deduction made that this was an intermediate product to methamphetamine production

Table 4 Methods used

Lab Code Color GCMS FTIR LCMS TLC Other

1 Y Y

2 Y Y Y DESI-MSD-Trap, Chemical conversion, Raman

3 Y Y Y GCMS of PFPA deriv.GCIRD

4 Y Y

5 Y Y 1-H NMR

7 Y Y

8 Y Y chemical conversion

10 Y

11 Y Y Y

12 Y Y

13 Y Y Y

14 Y Y

15 Y Y

16 Y Y

17 Y Y Y Y NMR


4.2 Sample S2

Table 6 Sample Details Sample S2 UR-144

or (1-pentyl-1H-indol-3-yl)(2,2,3,3-tetramethylcyclopropyl)methanone or (1-pentylindol-3-yl)(2,2,3,3-tetramethylcyclopropyl)methanone

Participants’ Result Question: Identify the substance

Table 7 Sample S2 identity Lab

Code Results

1 UR-144 (not confirmed)

2 (1-Pentylindol-3-yl)-(2,2,3,3-tetramethylcyclopropyl)methanone (also known as UR-144).

3 (1-pentylindol-3-yl)-(2,2,3,3-tetramethylcyclopropyl)methanone (UR-144)

4 (1-pentyl-1H-indol-3-yl)-(2,2,3,3-tetramethylcyclopropyl)methanone (UR-144)

5 (1-pentyl-1H-indol-3-yl)(2,2,3,3-tetramethylcyclopropyl)methanone UR-144

7 UR-144


10 UR-144

11 (1-pentylindol-3-yl)(2,2,3,3-tetramethylcyclopropyl)methanone (UR-144)

12 UR-144

13 UR-144

14 1-(Pentylindol-3-yl)-(2,2,3,3-tetramethylcyclopropyl)methanone (UR-144)


16 UR-144

17 UR-144


Table 9 Methods used Lab

Code Color GC-MS FTIR LC UV Other

1 Y Y

2 Y Y Y Raman

3 Y Y

4 Y Y

5 Y Y Y

7 Y

8 Y Y

10 Y Y Y

11 Y Y

12 Y Y

13 Y Y Y

14 Y Y

15 Y Y

16 Y Y

17 Y

Table 10 Additional Comments from Participants Lab

Code Additional Comments

1 The identification of UR144 was not confirmed as we currently do not have a standard.

5 UR144 cyclopropyl rearrangement product indicated by MS

7 Synthetic cannabanoid

10 LC and UV as inline (HPLC-DAD) analysis

15 Sample found to contain the cannabinoid receptor agonist UR-144

17 Result indicated by Library match and a breakdown UR-144 product indicated also.


5 DISCUSSION OF RESULTS

Participants were required to identify Sample S1 the substance found in the hypothetical clandestine laboratory, its illegitimate use and the mechanism to produce it based on the scenario provided. For Sample S1 results are presented in Table 11.

Table 11 Summary results for Sample S1 Sample S1

White powder Substance Illegitimate uses and the mechanism to produce it

Correct identification 14/15 13/15

Laboratory 15 identified incorrectly Sample S1 as Ephedrine and Methylamphetamine and did not address the question of its illegitimate use or the mechanism to produce the controlled drug based on the scenario provided. Laboratory 7 response regarding the mechanism to produce the substance is inconsistent with the scenario provided. Whilst an electrolytic reduction may be employed to produce methylamphetamine, it is not possible based on the scenario provided. For Sample S2 results are presented in Table 12.

Table 12 Summary results for Sample S2

Sample S2 Powder

Substance Synthesised

Correct

identification 15/15

All laboratories identified correctly Sample S2.


6 REFERENCES

[1] ISO/IEC 17043:2010, Conformity assessment – General requirements for proficiency testing, ISO, Geneva.

[2] Plotka, J.M., Morrison, C., Adam, D., Biziuk M., Chiral Analysis of Chloro Intermediates of Methylamphetamine by One-Dimensional and Multidimensional NMR and GC/MS, Analytical Chemistry, 2012, 84, 5625-5632.

[3] Lekskulchai, V., Carter, K., Poklis, A., Soine, W., GC-MS Analysis of Methylamphetamine Impurities: Reactivity of (+)- or (-)-Chloroephedrine and cis- or trans-1,2-Dimethyl-3-phenylaziridine, Journal of Analytical Toxicology, 2000, 24, 602-605.

[4] Ko, B.J., Suh, S., Suh, Y.J., In, M.K., Kim,S-H., Kim, J-H., (1S,2S)-1-Methylamino-1-phenyl-2-chloropropane: Route specific marker impurity of methamphetamine synthesised from ephedrine via chloroephedrine, Forensic Science International, 2012, 221, 92-97.

[5] Allen, A.C., Kiser, W.O., Methamphetamine from Ephedrine. I. Chloroephedrines and aziridines, Journal of Forensic Science, 1987, 32, 953-962.

[6] SWGDRUG Monographs: http://www.swgdrug.org/monographs.htm accessed on 1/7/2015.


APPENDIX 1 – PARTICIPANT LABORATORIES

ACT Government Analytical Laboratory, ACT Environmental Science and Research Ltd, NEW ZEALAND

Forensic & Analytical Science Services, NSW Forensic Institute, Odense Syddansk Universitet, DENMARK

Forensic Science Laboratory Garda Headquarters, IRELAND Forensic Science SA

Forensic Science Services Tasmania LGC Forensics, UK

Netherlands Forensic Institute, NETHERLANDS National Criminal Investigation Service/Kripos, NORWAY

National Measurement Institute, NSW Queensland Health Forensic and Scientific Services, QLD

Section of Forensic Chemistry, Department of Forensic Medicine, University of Copenhagen, DENMARK

SPA Forensic Services Glasgow, UK

University of Aarhus, Institut of Forensic Medicine Department of Toxicology and Drug Analysis, DENMARK

Victoria Police Forensic Services Dept. VIC


APPENDIX 2 - ACRONYMS AND ABBREVIATIONS DAD Diode Array Detector

FTIR Fourier Transform Infrared Spectroscopy

GC Gas Chromatography

GC-MS Gas Chromatography Mass Spectrometry

HPLC High Performance Liquid Chromatography

ISO International Standards Organisation

LC Liquid Chromatography

LC-MS Liquid Chromatography Mass Spectrometry

NATA National Association of Testing Authorities

NMI

NMR

National Measurement Institute Australia

Nuclear Magnetic Resonance

PT Proficiency Test

SI

TLC

International System of Units

Thin Layer Chromatography

UV Ultraviolet

Documents

Proficiency Test Report Clandestine Laboratory and Unknown ID · This report presents the results of AQA 15-17 – Clandestine Laboratory and Unknown ID. This is a qualitative program