Iqap) International Collaborative Exercises (Ice

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary Report

SEIZED MATERIALS 2014/1 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Table of contents Introduction Page 3 Comments from the International Panel of Forensic Experts Page 4 NPS reported by ICE participants Page 5 Codes and Abbreviations Page 11 Sample 1 Analysis Page 12 Identified substances Page 12 Statement of findings Page 15 Identification methods Page 23 Summary Page 27 Z-Scores Page 28 Sample 2 Analysis Page 30 Identified substances Page 30 Statement of findings Page 34 Identification methods Page 42 Summary Page 46 Z-Scores Page 47 Sample 3 Analysis Page 49 Identified substances Page 49 Statement of findings Page 53 Identification methods Page 61 Summary Page 65 Z-Scores Page 66 Sample 4 Analysis Page 68 Identified substances Page 68 Statement of findings Page 72 Identification methods Page 73 Summary Page 83 Z-Scores Page 84 Test Samples Information Samples Comments on samples Sample 1 SM-1 was prepared from a seizure containing 40.1% w/w 1-(3-chlorophenyl)piperazine base.The seizure also contained glucose. Trace amounts of codeine and morphine were detected upon analysis of a concentrated solution. If detected, the trace components present need not be considered a false positive result. Sample 2 SM-2 was prepared from a seizure containing 73.6% w/w Metamfetamine base.The samples also contain ed glucose and trace amounts of dimethylsulfone.

Sample 3 SM-3 was prepared from a seizure containing 16.1% w/w Ketamine base. The seizure also contained lactose.

Sample 4 SM-4 was prepared from a seizure containing 75.8% w/w cocaine base and trace amounts of benzoylecgonine and trans-cinnamoylcocaine.

Samples Substances Concentrations Comments on substances Sample 1 1-(3-Chlorophenyl)piperazine 40.1 % sample also contained glucose Sample 2 Metamfetamine 73.6 % sample also contained glucose Sample 3 Ketamine 16.1 % Lactose - Sample 4 Cocaine 75.8 %

This report contains the data received from laboratories participating in the current exercise. The results compiled in this report are not intended to be an overview of the quality of work and cannot be interpreted as such. These comments do not reflect the general state of the art within the profession.

Participant results are reported using a randomly assigned "WebCode". This code maintains participant's anonymity, provides linking of the various report sections, and will change with every report.

2 Introduction

An important element of the UNODC International Quality Assurance Programme (IQAP) is the implementation of the International Collaborative Exercises (ICE). The exercises allow laboratories, from both developing and developed countries, to continuously monitor their performance in drug testing on a truly global scale. This report provides information on analytical results of laboratories participating in the Seized Materials (SM) group. In order to maintain confidentiality, the participating laboratories have been assigned random “Web Codes”, which change every round. Two rounds are offered per year with each round presenting participants with four different test samples for analysis. The analytical results returned by laboratories participating in ICE are evaluated by UNODC and a confidential report is provided to each laboratory on its own performance. The overall analytical results are reviewed by the UNODC’s International Panel of Forensic Experts which oversees the implementation of these exercises, and offers guidance and support in addressing relevant quality issues. The exercises provide an overview of the performance and capacity of participating laboratories and enable UNODC to tailor technical support in the laboratory sector for greatest impact.

Revision of calculation of z-scores in ICE

Following a recommendation from the International Panel of Forensic Experts and in order to allow ICE participants to interpret their z-scores in line with recommendations in ISO 13528:2005 and ISO/IEC guide 43-1:1997(E), UNODC have introduced an revision to the method used to calculate the z-scores. z-score is a statistical parameter used in proficiency tests and collaborative exercises as a measure of performance in quantitative analysis. They are calculated as:

z = (x-X)/ σ̂ where x = result of participant, X = assigned value of component being quantified and σ̂ is the standard deviation for proficiency assessment (SDPA).

One of the methods recommended in ISO 13528:2005 for determining the assigned value X is to use the consensus value from participants. Using this method, the SDPA is also calculated from the standard deviation of the results of participants. Initial estimates of X and σ known as x* and s* are calculated as:

x* = median of xi (i = 1,2,……p) where p = number of participants s* = 1.483 median of │xi-x*│

Using these estimates, an iterative calculation (for details see ISO13528:2005, Annex C) is carried out to determine the final values of the robust average (x*) and robust standard deviation (s*) and the z-scores are calculated as z = (xi-x*)/s*

Consequently z-scores can be interpreted by participants in line with ISO 13528:2005, section 7.4.2 and ISO/IEC guide43-1:1997(E) as follows:

|z| < 2 = satisfactory 2 ≤ |z| ≤ 3 = questionable |z| > 3 = unsatisfactory

According to the recommendations in ISO 13528:2005, an unsatisfactory z-score is considered to give an action signal and a questionable z-score is considered to give a warning signal. A single action signal or warning signals in two successive rounds shall be taken that an anomaly has occurred that requires investigation. UNODC would like to acknowledge the valuable contribution of the Chemical Metrology Laboratory of the Health Sciences Authority, Singapore, for the provision of specific software used for the quantitative statistical calculations in the ICE programme

Comments from the International Panel of Forensic Experts

Participation of Laboratories

In the 2014/1 round of the ICE programme, results were submitted within both the Seized Materials (SM) and Biological Specimens (BS) test groups by 182 laboratories in 59 countries. Within the SM test group, there were 151 participating laboratories from 57 countries, representing a 16% increase from the 2013/2 round. Within the BS test group, results were submitted by 72 laboratories from 38 countries, also corresponding to an increase of 16 % in the number of participants compared to the previous round.

Qualitative Analysis

The most commonly used technique for screening of test samples in the SM test group was the marquis reagent (42% of participants), while GC-MS (89%) was the most commonly used technique for identification/confirmation followed by FTIR (37%). The results for the qualitative identification of the controlled substances were excellent for all test samples in the SM group. 93% and 98% of participants correctly identified the 1-(3-chlorophenyl)piperazine and metamfetamine in SM-1 and SM-2 respectively. It is encouraging to note that 93% of participants identified the 1-(3-chlorophenyl)piperazine (94% identified this substance in 2013/2), indicating a continued excellent level of awareness of participants in the identification of this New Psychoactive Substance (NPS). 97% of participants correctly identified the ketamine in SM-3, an increase from 92% who correctly identified ketamine, when this was last used as a test sample in 2011/2. Finally, 99% of participants identified the cocaine in SM-4.

8 false positive results were reported for the four test samples in the SM group and there were only 7 false negative results. The detection limits of the different analytical techniques were taken into consideration when ascribing false positive results and as such laboratories who detected the trace amounts of Morphine and Codeine in SM-1 need not consider their results as false positives.

Quantitative Analysis

The proportion of participants who carried out quantitative analysis, 48 (32%) for SM-1, 83 (55%) for SM-2, 69 (46%) for SM-3 and 107 (71%) for SM-4 continues to be encouraging, particularly the high percentage of participants who quantified the cocaine in SM-4. 1-(3-chlorophenyl)piperazine is a relatively new substance In the ICE menu and there was a 5% increase in the number of laboratories who performed quantitative analysis for this drug compared to the previous round. It is also encouraging to note that 111 (74%) of participants in the SM test group performed quantitation. Of these, 38% quantified all test samples and 78% of laboratories quantified at least two of the 4 test samples. It is understood that quantitative analysis of controlled substances is often governed by local legislation and the requirements of prosecution. With regard to the analytical techniques used by participants performing quantitation, 50% used GC-FID, 24% used HPLC and 19% used GC-MS

Analysis of the z-scores showed that 94% of participants provided acceptable quantitative results with |z| < 3 for 1-(3-chlorophenyl)piperazine in SM-1, 89% for metamphetamine in SM-2, 87% for ketamine in SM-3 and 87% for cocaine in SM-4. Laboratories are encouraged to carry out quantification as it can improve the quality of laboratory analyses and can be helpful in assessing the significance of the results. z-score values obtained assist participating laboratories in evaluating their performance and should be monitored over time as part of each laboratory’s quality assurance programme. Participants with z-scores outside acceptable limits should review their quantification procedures. Laboratories reporting false positive or false negative results should investigate the reasons for this and corrective actions should be taken in order to continuously improve performance. Participation in the ICE programme also helps in monitoring the effect of corrective actions.

New Psychoactive Substances (NPS) reported by laboratories participating in the 2014/1 round of the ICE programme

During the 2014/1 round of ICE, participating laboratories provided information on NPS that had been identified in their laboratories. In total there were 320 reports of 146 substances. The most commonly reported substances were synthetic cannabinoids followed by synthetic cathinones and phenethylamine group substances as shown in figure 1.

2% 1% 3% 3% 3%

Synthetic cannabinoids 32% Phenethylamines 14% Synthetic cathinones Tryptamines Others Plant-based substances 7% Piperazines Phencyclidine type substances Aminoindanes Unverified

19% 16%

Figure 1. NPS reported by ICE laboratories during the 2014/1 round of ICE

The substances that were most commonly reported by participants are shown in table 1.  25I-NBOMe (1-(4-iodo-2,5-dimethoxyphenyl)-N-[(2-methoxyphenyl)methyl]ethanamine) was the substance most often reported  25C-NBOMe (1-(4-chloro-2,5-dimethoxyphenyl)-N-[(2-methoxyphenyl)methyl]ethanamine) and methylone (2-Methylamino-1-(3,4-methylenedioxyphenyl)propan-1-one) were equally the second most reported substances  The synthetic cannabinoids, APINACA (1-pentyl-N-tricyclo[3.3.1.13,7]dec-1-yl-1H-indazole-3- carboxamide) and MAM-2201 ([1-(5-Fluoropentyl)-1H-indol-3-yl](4-methyl-1-naphthalenyl)- methanone) completed the list.

Table 1. Substances most commonly reported by ICE participants in 2014/1 round of ICE

Substance IUPAC Name Structure

2-(4-Iodo-2,5-dimethoxyphenyl)-N-(2- 25I-NBOMe methoxybenzyl)ethanamine

2-(4-Chloro-2,5-dimethoxyphenyl)-N- 25C- (2-methoxybenzyl)ethanamine NBOMe

1-(1,3-Benzodioxol-5-yl)-2- Methylone (methylamino)propan-1-one

1-Pentyl-N-(tricyclo[3.3.1.13,7]dec-2-yl)- 1H-indazole-3-carboxamide - 1-(1,3- APINACA benzodioxol-5-yl)-2- (methylamino)propan-1-one (1:1)

[1-(5-Fluoropentyl)-1H-indol-3-yl](4- MAM-2201 methylnaphthalen-1-yl)methanone

Table 2 shows the namesand structures of the NPS that were reported for the first time to UNODC during the 2014/1 round of ICE.

Table 2. Substances reported to UNODC for the first time by ICE participants in 2014/1 round of ICE

Common name/ IUPAC name Structure Abbreviation

Methoxphenidine, 1-(1-(2-methoxyphenyl)-2- MXP phenylethyl)piperidine

2-(methylamino)-1-(thiophen-2- bk-MPA yl)propan-1-one

methyl 1-(2-phenylethyl)-4- [phenyl(propanoyl)amino]piperidi Carfentanyl ne-4-carboxylate

7-chloro-5-(2-chlorophenyl)-1- methyl-1,3-dihydro-2H-1,4- Diclazepam benzodiazepin-2-one

8-bromo-1-methyl-6-(pyridin-2- Pyrazolam yl)-4H-[1,2,4]triazolo[4,3- a][1,4]benzodiazepine

2- 1-(2-fluorophenyl)-N- Fluoromethamph methylpropan-2-amine etamine, 2-FMA

7 naphthalen-1-yl(1-pentyl-1H- THJ-018 indazol-3-yl)methanone

methyl N-{[1-(5-fluoropentyl)-1H- 5F-AMB indazol-3-yl]carbonyl}valinate

N-(1-amino-3-methyl-1- oxobutan-2-yl)-1- AB-CHMINACA (cyclohexylmethyl)-1H-indazole- 3-carboxamide

N-(1-amino-3-methyl-1- oxobutan-2-yl)-1-(2- AB-FUBINACA(2- fluorobenzyl)-1H-indazole-3- fluorobenzyl) carboxamide

quinolin-8-yl-1-(4-fluorobenzyl)- FUB-PB-22 1H-indole-3-carboxylate

8 (4-methylpiperazin-1-yl)(1- Mepirapim, pentyl-1H-indol-3-yl)methanone

N-(2-methoxyethyl)-N-{[2-(1- pentyl-1H-indol-3-yl)-1,3-thiazol- PTI-2 4-yl]methyl}propan-2-amine

N-ethyl-N-{[2-(1-pentyl-1H-indol- 3-yl)-1,3-thiazol-4- PTI-1 yl]methyl}ethanamine

1-(5-fluoropentyl)-N- (naphthalen-1-yl)-1H-indazole-3- 5F-NNE1 carboxamide

[1-(5-fluoropentyl)-1H-indazol-3- THJ-2201 yl](naphthalen-1-yl)methanone

9 α- 1-phenyl-2-(pyrrolidin-1- pyrrolidinoheptiop yl)heptan-1-one henone, alpha-

PHpP

1-(3-methylphenyl)-2-(pyrrolidin- 3-MePPP 1-yl)propan-1-one

2-(ethylamino)-1-phenylpentan- 1-one

2-MMC, 2-Methyl- 2-(methylamino)-1-(2- N- methylphenyl)propan-1-one, methylcathinone

3,4- 1-(3,4-dimethylphenyl)-2- Dimethylethcathin (ethylamino)propan-1-one one

2-(ethylamino)-1-(4- methylphenyl)pentan-1-one

2-amino-1-(4-bromo-2,5- bk-2C-B dimethoxyphenyl)ethanone

2-(1H-indol-3-yl)-N- N- methylethanamine methyltryptamine

All laboratories participating in the UNODC International Collaborative Exercises can access the UNODC Early Warning Advisory on New Psychoactive Substances by logging on to their account and selecting the link as shown in the image below

11 Introduction

Revision of calculation of z-scores in ICE

z = (x-X)/ σ̂ where x = result of participant, X = assigned value of component being quantified and σ̂ is the standard deviation for proficiency assessment (SDPA).

x* = median of xi (i = 1,2,……p) where p = number of participants s* = 1.483 median of │xi-x*│

Consequently z-scores can be interpreted by participants in line with ISO 13528:2005, section 7.4.2 and ISO/IEC guide43-1:1997(E) as follows:

|z| < 2 = satisfactory 2 ≤ |z| ≤ 3 = questionable |z| > 3 = unsatisfactory

Comments from the International Panel of Forensic Experts

Participation of Laboratories

Qualitative Analysis

Quantitative Analysis

New Psychoactive Substances (NPS) reported by laboratories participating in the 2014/1 round of the ICE programme

2% 1% 3% 3% 3%

Synthetic cannabinoids 32% Phenethylamines 14% Synthetic cathinones Tryptamines Others Plant-based substances 7% Piperazines Phencyclidine type substances Aminoindanes Unverified

19% 16%

Figure 1. NPS reported by ICE laboratories during the 2014/1 round of ICE

Table 1. Substances most commonly reported by ICE participants in 2014/1 round of ICE

Substance IUPAC Name Structure

2-(4-Iodo-2,5-dimethoxyphenyl)-N-(2- 25I-NBOMe methoxybenzyl)ethanamine

2-(4-Chloro-2,5-dimethoxyphenyl)-N- 25C- (2-methoxybenzyl)ethanamine NBOMe

1-(1,3-Benzodioxol-5-yl)-2- Methylone (methylamino)propan-1-one

1-Pentyl-N-(tricyclo[3.3.1.13,7]dec-2-yl)- 1H-indazole-3-carboxamide - 1-(1,3- APINACA benzodioxol-5-yl)-2- (methylamino)propan-1-one (1:1)

[1-(5-Fluoropentyl)-1H-indol-3-yl](4- MAM-2201 methylnaphthalen-1-yl)methanone

15 Table 2 shows the namesand structures of the NPS that were reported for the first time to UNODC during the 2014/1 round of ICE.

Table 2. Substances reported to UNODC for the first time by ICE participants in 2014/1 round of ICE

Common name/ IUPAC name Structure Abbreviation

Methoxphenidine, 1-(1-(2-methoxyphenyl)-2- MXP phenylethyl)piperidine

2-(methylamino)-1-(thiophen-2- bk-MPA yl)propan-1-one

methyl 1-(2-phenylethyl)-4- [phenyl(propanoyl)amino]piperidi Carfentanyl ne-4-carboxylate

7-chloro-5-(2-chlorophenyl)-1- methyl-1,3-dihydro-2H-1,4- Diclazepam benzodiazepin-2-one

8-bromo-1-methyl-6-(pyridin-2- Pyrazolam yl)-4H-[1,2,4]triazolo[4,3- a][1,4]benzodiazepine

2- 1-(2-fluorophenyl)-N- Fluoromethamph methylpropan-2-amine etamine, 2-FMA

naphthalen-1-yl(1-pentyl-1H- THJ-018 indazol-3-yl)methanone

16 methyl N-{[1-(5-fluoropentyl)-1H- 5F-AMB indazol-3-yl]carbonyl}valinate

N-(1-amino-3-methyl-1- oxobutan-2-yl)-1- AB-CHMINACA (cyclohexylmethyl)-1H-indazole- 3-carboxamide

N-(1-amino-3-methyl-1- oxobutan-2-yl)-1-(2- AB-FUBINACA(2- fluorobenzyl)-1H-indazole-3- fluorobenzyl) carboxamide

quinolin-8-yl-1-(4-fluorobenzyl)- FUB-PB-22 1H-indole-3-carboxylate

(4-methylpiperazin-1-yl)(1- Mepirapim, pentyl-1H-indol-3-yl)methanone

17 N-(2-methoxyethyl)-N-{[2-(1- pentyl-1H-indol-3-yl)-1,3-thiazol- PTI-2 4-yl]methyl}propan-2-amine

N-ethyl-N-{[2-(1-pentyl-1H-indol- 3-yl)-1,3-thiazol-4- PTI-1 yl]methyl}ethanamine

1-(5-fluoropentyl)-N- (naphthalen-1-yl)-1H-indazole-3- 5F-NNE1 carboxamide

[1-(5-fluoropentyl)-1H-indazol-3- THJ-2201 yl](naphthalen-1-yl)methanone

α- 1-phenyl-2-(pyrrolidin-1- pyrrolidinoheptiop yl)heptan-1-one henone, alpha-

PHpP

1-(3-methylphenyl)-2-(pyrrolidin- 3-MePPP 1-yl)propan-1-one

18 2-(ethylamino)-1-phenylpentan- 1-one

2-MMC, 2-Methyl- 2-(methylamino)-1-(2- N- methylphenyl)propan-1-one, methylcathinone

3,4- 1-(3,4-dimethylphenyl)-2- Dimethylethcathin (ethylamino)propan-1-one one

2-(ethylamino)-1-(4- methylphenyl)pentan-1-one

2-amino-1-(4-bromo-2,5- bk-2C-B dimethoxyphenyl)ethanone

2-(1H-indol-3-yl)-N- N- methylethanamine methyltryptamine

19 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Codes and Abbreviations

(+) “positive”: Indicates that the analyte is identified; for presumptive tests (e.g. colour reactions), indicates that a positive reaction was obtained. (-) “negative”: Indicates that the analyte is not identified.

(ANP): Analysis not performed.

Tech Code Name 140 Colorimetric reactions 141 Marquis reagent (sulphuric acid, formaldehyde) 142 Cobalt thiocyanate 150 Thin Layer Chromatography 160 High/Ultra High Performance Liquid Chromatography 161 High Performance Liquid Chromatography with diode array detection 170 Gas Chromatography NPD 171 Gas Chromatography FID 172 Gas Chromatography ECD 180 Gas Chromatography/Mass Spectrometry 190 Fourier Transform Infrared Spectrometry 200 Spectrophotometry (visible, UV) 210 Others (specify) 211 NMR 220 Microcrystal test 230 Liquid chromatography/mass spectrometry 231 Liquid chromatography/tandem mass spectrometry

20 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Sample 1 Analysis

Identified substances for Test Sample 1

Code Identified Substances 0LN2QE 1-(3-chlorophenyl)piperazine 0N05YR 1-(3-chlorophenyl)piperazine 0RE0L0 1-(3-chlorophenyl)piperazine, morphine, glucose 1SAEBM 1-(3-Chlorophenyl)piperazine 20LMZF 1-(3-Chlorophenyl)piperazine 28YACH 1-(3-Chlorophenyl) piperazine, Morphine 3BY3P6 1-(3- Chlorophenyl) piperazine 3MGTTL 1-(3-Chlorophenyl)piperazine 3RV3F7 m-cpp 3UMO3Y mCPP 3V0OFD 1-(3-Chlorophenyl)piperazine 4FA8F0 CPP 555YH5 1-(3-chlorophenyl)piperazine 5V22WM Chlorophenypiperazine 5WSWTT piperazines 5ZW2N9 1-(3-Chlorophenyl)piperazine 6306WG m-CPP 666F66 mCPP, morphine, codeine 7FH7HV Morphine et Méthamphétamine 7K1RKK Chlorophenyl piperazine 7WPIJX 1-(3-Chlorophenyl)piperazine 888Z8S 1-(3-Chlorophenyl)piperazine 8SVPRT 1-(3-chlorophenyl)piperazine 8YSG8M 1-(3-Chlorophenyl)piperazine and morphine AEE5WA mCPP AGNIZI 1-(3-Chlorophenyl)piperazine AIPPIG m-CPP, 1-(3-chlorophenyl)piperazine AJ22ZI 1-(3-chlorophenyl) piperazine AKJ5JY CPP ANHVML CPP and morphine (minor component) BLZZMB mCPP: 1-(3-chlorophenyl)piperazine BPLP0L mCPP C9TTRY 1,3-chlorphenylpiperazine CWGDML 1-(3-clhorophenyl )piperazine CWLQJ1 1-(3-Chlorophenyl)piperazine D5BVEI 1-(3-Chlorophenyl)piperazine D8DHQW 1-(3-Chlorophenyl)piperazine DFCXDG 1-(3-Chlorophenyl)piperazine DLDLOB mCPP DNKLDD 1-(3-Chlorophenyl)piperazine)

21 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances DQMISD m-CPP DYEYYG 1-(3-Chlorophenyl)piperazine EDRLTN 1-(3-Chlorophenyl)piperazine ELN44T 1-(3-Chlorophenyl)piperazine EMZZIW MCPP, Morphine FFFAFF m-Cpp FIKSPK 1-(3-chlorophenyl)piperazine FL6M38 1-(3-clorofenil)-piperazine FO8JOE 1-(3-chlorophenyl)piperazine GCGWXG 1-(3-chlorophenyl)piperazine and Morphine GEZZ2P 1-(3-Chlorophenyl) piperazine GK8FTC 1-(3-chlorophenyl)piperazine H4TJQT codeine H74EH5 m-CPP HCW3AW 1-(3-Chlorophenyl)piperazine HCl HYEPEU 1-(3-Chlorophenyl)piperazine HYRH0O mCPP, Morphine I3W3SW 1-(3-Chlorophenyl)piperazine IJ37J2 1-(3-Chlorophenyl)piperazine IM8WG1 1-(3-chlorophenyl)piperazine IMEQDK Not identified IOP7DS 1-(3-Chlorophenyl)piperazine IRIBPI mCPP IT3XHS 1-3 chloro -phenyl piperizine J1X7S4 mCPP HCl JA3JJQ 1-(3-Chlorophenyl)piperazine JIRDRI 1-(3-Chlorophenyl)piperazine KEANRN 1-(3 Chlorophenyl) piperazine KGJIJS 1-(3-Chlorophenyl)piperazine KN4PSK 1-(3-Chlorophenyl)piperazine KPAKKD 1-(3-chlorophenyl)piperazine KX18KO chlorophenyl piperazine, morphine KYGWUS CHLORO PHENYL PIPERAZINE LG45WT 1-(3-chlorophenyl)piperazine LLLSLL mCPP HCl (1-(3-chlorophenyl)piperazine HCl) LYWXR6 morphine and codeine M1Q1F5 1-(3-Chlorophenyl)piperazine MJHGVG mCPP MRWDWG 1-(3-Chlorophenyl)piperazine NBI4J4 1-(3-Chlorophenyl)piperazine NHY1ZE morphine, codeine, 3-chlorphenylpiperazine NSJNGB 1-(3-Chlorophenyl)piperazine NU06C7 1-(3-Chlorophenyl)piperazine NVENEN 1-(3-Chlorophenyl)piperazine

22 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances O2WSYF meta-chlorophenylpiperazine, traces of morphine and codeine OGLNKI 1-(3-Chlorophenyl)piperazine OLLRLR 1-(3-Chlorophenyl)piperazine ORHNDM m-CPP OW2RIV mCPP PIRHNH 1-(3-Chlorophenyl)piperezine PPHBGP 1,3 CLOROPHENYLPIPERAZINE PSQS7F MORPHINE Q11YO1 1-(3-Chlorophenyl)piperazine Q8ECTW 1-(3-Chlorophenyl)piperazine QIEBZB 1-(3-Chlorophenyl)piperazine QOOCT8 1-(3-Chlorophenyl)piperazine QTTSCI 1-(3-Chlophenyl)piperazine and codein RJXPPP mCPP RV9IZA Piperazine RXKBFM 1-(3-clorofenil)pipirazina S4B5OL 1-(3-Chlorophenyl)piperazine and Lactose SAZ3ZW 1-(3-clorofenil)piperazina SF9898 1-(3-Chlorophenyl)piperazine SUOIOI 1-(3-Chlorophenyl)piperazine TIILNU 1-(3-chlorophenyl)piperazine TLVU3E mCPP U54UUY HEROIN UIIF4G 1-(3-Chlorophenyl)piperazine ULQHBK 1-(3-chlorophenyl)piperazine ULXUTD 1-(3-Chlorophenyl)piperazine V3BKMA 1-(3-Chlorophenyl)piperazine VGVOLX Morphine, 1-(3-Chloro Phenyl)Piperazine and Codeine VJMKCE Morphine, Codeine and Chlorophenylpiperazine VLJXIU 1-(3-chlorophenyl)piperazine VMHH2Y mCPP VXXFXK mCPP (1-(3-chlorophenyl)-piperazine) VZSIJV 1-(3-chlorophenyl)piperazine and morphine W33NYG m- CPP - Hcl; Heroine XGELS2 Morphine and codéine XL5KA0 1-(3-chlorophenyl)piperazine XMAYN4 1-(3-chlorophenyl)piperazine, morphine, codeine XVDW7X candidate molecule: mCPP YVAVK8 mCPP: 1-(3-chlorophenyl)piperazine YWZYAR m-CPP, morphine, codeine YYDEDD Morphine, Codeine, mCPP Z154TB mCPP Z8YS9F 1-(3-Chlorophenyl)piperazine,Codeine,Morphine ZZKXPP 1-(3-Chlorophenyl)piperazine

23 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Statement of findings for Test Sample 1

Code 1-(3-Chlorophenyl) piperazine 0J0PYS + Sample one contains MCPP,HCL (25.2% as base) cut with glucose 0LN2QE + 1-(3-chlorophenyl)piperazine 0N05YR +

0RE0L0 + The sample contains traces of morphine which is scheduled as illicit drug in France. 1-(3- chlorophenyl)piperazine is not scheduled as illicit drug in France. Glucose is a cutting agent. 1SAEBM + Sample contains 37.7± 1.8 % (w/w) 1-(3-Chlorophenyl)piperazine base in HCL salt form. Trace amount of morphine and codeine were also detected by GC/MS. The sample also contains glucose. 20LMZF + One glass bottle containing 0.21 grammes of a powder containing 0.08 grammes of 1-(3- chlorophenyl)piperazine. 28YACH + 1-(3-Chlorophenyl) piperazine, Morphine existed in salt form. We were found Codeine in the sample 2H9171 +

33HOOD + Based on the above analysis, the sample was found to contain 1-(3-Chlorophenyl)piperazine and traces of morphine. 3BY3P6 +

3MGTTL +

3RV3F7 + in the sample is m-cpp who is on the list of drugs in Montenegro 3UMO3Y + white powder, also contain morphine, codeine and glucose 3V0OFD + white powder containing 1-(3-Chlorophenyl)piperazine , not quantified. Contains also glucose. 4FA8F0 + 1-(3-chlorophenyl)piperazine 555YH5 +

5V22WM + The powder was analysed and found to contain Chlorophenylpiperazine. 5WSWTT + after chemical analysis was performed, the sample was found to contain piperazines. 5ZW2N9 + 1-(3-Chlorophenyl)piperazine was detected by GCMS screening 6306WG + Unable to quantify due to lack of analytical standards 666F66 + mCPP, morphine, codeine

24 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 1-(3-Chlorophenyl) piperazine 7FH7HV - Après analyse, l'échantillon 2014/1/SM-1 contient de la morphine et de la méthamphétamine 7K1RKK + A sample of the powder was analysed and found to contain chlorophenyl piperazine , which is a class C controlled substance under the Misuse of Drugs Act 1971 7WPIJX + +lactose 888Z8S + On analysis, I found the substance to contain MCPP 8GORYY + The analysis did not reveal any controlled drug according to french order, decree of February 22nd 1990. 8SVPRT + The result of the IR of test sample was shown same as those of the reference substance of 1-(3- chlorophenyl)piperazine 8YSG8M +

8ZZZO7 + On analysis, I found the substances to contain 1-(3-chlorophenyl)piperazine A3AH32 ANP lactosa AEE5WA +

AGNIZI + mixture of 1-(3-Chlorophenyl)piperazine with lactose AIPPIG + White powder containing mCPP. AJ22ZI + The sample was found to contain 1-(3-chlorophenyl) piperazine AKJ5JY + Sample 2014/1/SM-1, a white, odourless powder, gave a positive result for CPP, a controlled substance under national legislation on drugs. ANHVML + Off-white powder containing (Chlorophenyl)piperazine (CPP) and morphine (as a minor component). Morphine is a Class A controlled drug and CPP is a Class C controlled drug under the provisions of the Misuse of Drugs Act 1971 (as amended). BLZZMB + contamination morphine BPLP0L + This sample is mCPP. C9TTRY +

CWGDML +

CWLQJ1 + The coincidence in the mass fragmentogram between the analyzed sample and a espectral library indicates the 1-(3-Chlorophenyl)piperazine presence. CZV766 ANP Label Non-Conformity: Sample coded "2013/2/SM-1" contrary to above. No test performed.

25 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 1-(3-Chlorophenyl) piperazine D5BVEI + Powder containing 1-(3-Chlorophenyl)piperazine. D8DHQW + 1-(3-Chlorophenyl)piperazine, a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. DFCXDG + The sample contains m-CPP 45.04 %, m/m. DLDLOB + Identified substance:mCPP (1-(3-chlorophenyl)piperazine) the substance identified XXX its chemical structure a piperazine, concentration: approx 36 % as free base DNKLDD +

DQEDDN +

DQMISD + powder with 43,1 % of m-CPP as a active substance and glucose as a adulterant DYEYYG + 1-(3-Chlorophenyl)piperazine and glucose EBQAXY + The sample 2014/1/SM-1 contains mCpp. mCpp is not a controlled substance in France EDRLTN + The exhibit item was found to contain 1-(3-Chlorophenyl)piperazine. ELN44T + On analysis, I found the sample to contain 1-(3-Chlorophenyl)piperazine (also known as mCPP) EMZZIW +

ET1YHT + 47.7 % 1-(3-Chlorophenyl)piperazine FFFAFF + White powder that contains substance under control - m-Cpp. FIKSPK + It has been detecded that tehe subject of study including White colour dust substance was 1-(3- chlorophenyl)piperazine. This is a drug which is under the terms of national sunstance of drug Law 2313. FL6M38 + la muestra 2014/1(SM1) IS POSITIVE TO 1-(3-clorofenil)-piperazine, more traces of Morphine. FO8JOE + Retention time and MS spectra in GC analysis (FID and MS) compared with 3 isomers (o-, m-, p-)- CPP. Cloudy CHCl3 solution and FTIR/ATR indicates a mixture with some carbohydrate (e.g. glucose - confirmation not performed). mCPP as hydrochloride. G222HF +

GCGWXG + Chlorophenylpiperazine, known as CPP, is a class C controlled drug subject to the provisions of the Misuse of Drugs Act 1971 (Amendment) Order 2009 as it is structurally derived from 1- benzylpiperazine by substitution at the second nitrogen atom of the piperazine ring with a benzyl substituent. Morphine is a Class A controlled drug subject to the provisions of the Misuse of Drugs Act 1971. GEZZ2P +

26 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 1-(3-Chlorophenyl) piperazine GK8FTC + contain also traces of morphine and codeine H4TJQT +

H74EH5 + m-CPP 46,2 % and glucose HCW3AW + No color change with Marquis and Cobalt thiocyanate. Positive with Simon (Purple to Blue). Silver Nitrate Test--> Chloride Positive.TLC(TA,TE),GCMS -->1-(3-Chlorophenyl)piperazine confirmed. GC--> 1-(3-Chlorophenyl)piperazine base 40.68% HCZG6T + The sample was found to contain 1-(3-chlorophenyl)piperazine. In addition, trace amounts of morphine was also detected. HYEPEU + The powder is a psychotropic substance - 1-(3-Chlorophenyl)piperazine (m-CPP) powder. The powder contains 45.9 % pure m-CPP (base form). HYRH0O + mCPP, Morphine, Codeine I3W3SW + TRACES OF MORPHINE AND CODEINE WERE ALSO IDENTIFIED. I9MZ11 + SM-1 contained 1-(3-chlorophenyl)piperazine. IJ37J2 + In the test sample 2014/1/SM-1 was detected 1-(3-Chlorophenyl)piperazine IM8WG1 +

IMEQDK ANP Marquis reagent was negative at the begining, but a few seconds later, it turns into purple. The retention time was different from the heroin´s one, so we have our chromatogram with a single peak, but we can not identify any drug with our current method. IOP7DS + The sample contains 1-(3-Chlorophenyl)piperazine (not quantified). IRIBPI + We also found glucose and traces of morphine and codein IT3XHS + Red Precipitate with Dragendorff's Reagent indicates the possible presence of piperizine .Retention Time(RT 12.8) and Base peaks(154)of SM1 and library search in GCMS shows SM1 being 1-3 Chloro-Phenyl piperizine. We couldn't performed the percentage (Quantification)of SM1 because piperizine Reference Standard was not including in Ref Std box which you sent. J1X7S4 + SM1 contains also Glucose and trace amounts of morphine and codeine. JA3JJQ + 1-(3-Chlorophenyl)piperazine JIRDRI + 1-(3-Chlorophenyl) piperazine positive K2D2PO + we have found 1-(3-chlorophenyl)piperazine, but it`s not drug in Albania. In this sm-1 we have found also trace of codeine and morphine.

27 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 1-(3-Chlorophenyl) piperazine KEANRN + In the tested sample was detected and confirmed the presence of 1 - (3 Chlorophenyl) piperazine plus codeine and morphine

KGJIJS + SIGN IN DETECTED 2014/1/SM-1 labeled 1 - (3-Chlorophenyl) piperazine (mCPP). KN4PSK + 1-(3-Chlorophenyl)piperazine KPAKKD + The sample contains piperazine KX18KO + Off-white powder containing chlorophenyl piperazine which is a class C controlled drug under the provisions of the Misuse of Drugs Act 1971 (as amended). (Note: morphine would not be reported as detected at a very low level). KYGWUS + Vial containing 0.224 grams of off-white powder that was found to contain Chlorophenylpiperazine (CPP) . Chlorophenylpiperazine is controlled by the Misuse of Drugs Act 1971 (as amended) as a Class C drug, by virtue of the fact that it is structurally derived from Phenylpiperazine by substitution in the aromatic ring with a halide substituent LG45WT + The sample was soluble in water, ethanol and methanol. The sample had positive reaction for alkaloid with tanred reagent . The sample had positive reaction for chlorides with silver nitrate reagent . LLLSLL + mCPP HCl - not under control in Polish Law additional substance - glucose LYWXR6 + We have also found 1-(3-Chlorophenyl) piperazine (mCPP) which is a piperazine-like molecule. However, mCPP is not under illicit drugs legislation control in Spain. M1Q1F5 + The sample contain illegal drug meta-Chlorophenyl)piperazine (m-CPP) MJHGVG + hydrochloride form +GLUCOSE MRWDWG + white powder containing 1-(3-Chlorophenyl)piperazine, potential hazard substance, not considered under control in Italy. NBI4J4 +

NHY1ZE + SM1 contain opiates and psychoactive drugs. NNBNTN + 1-(3-chlorophenyl)piperazine confirmed in one unit tested of one unit recieved. Not a controlled substance in the USA. NSJNGB + 1-(3-Chlorophenyl)piperazine NU06C7 +

NVENEN + The Sample 2014/1/SM1 was found to contain 1-(3-Chlorophenyl)Piperazine. O2WSYF + The sample is a preparation that contains meta-chlorophenylpiperazine and traces of morphine and codeine.

28 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 1-(3-Chlorophenyl) piperazine OGLNKI + 1-(3-Chlorophenyl)piperazine OLLRLR + the white powder contains 1-(3-Chlorophenyl)piperazine . The amount of m-CPP was not determined because this laboratory hasn't got the correspondant certified reference material. ORHNDM + M-CPP , substance non classée stupéfiant OW2RIV + Sample containing mCPP PF5IJN + marquis, scott, chen cao. simon´s, FT-IR, HPLC PIRHNH +

PPHBGP + The results of the tests of the SM1 () received confirmed that the mentioned sample contains 1,3 CLOROPHENYLPIPERAZINE but we are not able to give a cuantification result because we can not do it with our gas chromatography-gas spectometer and we have not got a gas chromatography FID which is the suitable analytical technique.

PSQS7F - The simple No 2014/1/SM-1 was found MORFINE and PIPERAZINE 1(4-CLOROPHENYL) Q11YO1 + white powder containing 1-(3-Chlorophenyl)piperazine Q8ECTW + the powder is a mixture of 1-(3-Chlorophenyl)piperazine also known as mCPP and glucose. The concentration of mCPP in the sample is 29.9% by weight QIEBZB + The substance contains 39.40% of 1-(3-Chlorophenyl)piperazine QOOCT8 + Sample 2014/1/SM-1 was found to contain 1-(3-Chlorophenyl)piperazine.

QTTSCI + Examination of the powder SM-1 revealed the presence of controlled drug 1-(3-Chlophenyl) piperazine. RJXPPP +

RV9IZA +

RXKBFM +

S4B5OL + The test sample 2014/1/SM-1 was analysed by colour test and Thin layer Chromatography (TLC) techniques and found to contain 1-(3-Chlorophenyl)piperazine and Lactose. SAZ3ZW + De acuerdo a los análisis realizados se concluye que se trata de 1-(3-clorofenil)piperazina SF9898 + 1-(3-Chlorophenyl)piperazine was identified by TLC and GC/MS SGDY90 +

29 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 1-(3-Chlorophenyl) piperazine SUOIOI + PDGHWKHFKHPLFDODQGLQVWUXPHQWDODQDO\VLVLWUHVXOWHGWKDWWKHVDPSOHFRQWDLQV1 - (3- Chlorophenyl) piperazine TIILNU +

TLVU3E + The sample SM1 contained 38.2 % m-CPP calculated as a base. In the sample was identified glucose, morphine and codeine. U54UUY - Field test employing the Marquis Test was positive as the spot turned purple. TLC analysis using two(2) solvents systems and HPLC confirmed the sample as HEROIN with purity 54.60%. UIIF4G +

ULQHBK + 2014/1/SM-1 contains 1-(3-chlorophenyl)piperazine. ULXUTD + glucose V3BKMA +

V43UFL + mCPP, glucose, traces of morphine and codeine VGVOLX + MR and CT reagents: positive. GC/MS: Retention time, mass-charge (M/Z) similar characteristics with the substances used as standar or pattern. VJMKCE + A white powder containing MORPHINE, CODEINE and CHLOROPHENYLPIPERAZINE. VLJXIU + Was found DEXTROSA VLLLV0 ANP sin identificar VMHH2Y +

VXXFXK + morphine contamination by GC-MS VZSIJV + 1-(3-chlorophenyl)piperazine is controlled (KB 22/01/1998 changed by KB 22/10/2006). Also a small amount of morphine (controlled KB 31/12/1930 changed by KB 8/10/1963) and codeine were found in the sample. W33NYG + To reach such a conclusion were performed the following tests: Preliminary tests: SCOOT REAGENT; MARQUIS REAGENT and SOLUBILITY Confirmation tests: Thin Layer Chromatography - TLC; Gas Chromatography Coupled to the Flame- Ionizacion Detector - GC/FID

XFPUFJ ANP

XGELS2 + mCPP is not considerated as a drug (in France) XH2D7F +

30 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 1-(3-Chlorophenyl) piperazine XL5KA0 + Presence of 1-(3-chlorophenyl) piperazine hydrochloride and glucose was detected in the sample. The seizure also contained trace amount of codeine and morphine. XMAYN4 + *Results of screening tests were positive for opiates and piperazines. *Retention time and fragmentation pattern obtained with sample are equivalent to those obtained with 1-(3- chlorophenylpiperazine, morphine and codeine. XVDW7X + The sample SM-1 presents fragmentation pattern similar to the chemical substance 1-(3- Chlorophenyl)piperazine, also known as mCPP, which is included in List F2 (List of psychotropic substances banned in Brazil) of Annex I of SVS / MS 344, May 12, 1998. We can't confirm results due lack of mCPP standard. YCYBYW -

YVAVK8 + morphine YWZYAR +

YYDEDD +

Z154TB + The sample contain trace morphine Z8YS9F + - ZM99S9 ANP

ZZKXPP + CONFIRMED BY GC MS

31 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Identification methods for Test Sample 1

Legend: S ... used for Screening I ... used for Identification SI ... used for both

Analytical Technique Codes Code 140 141 142 150 160 161 170 171 180 190 200 211 230 231 210 0J0PYS S I I 0LN2QE I SI I 0N05YR S I I 0RE0L0 S S I I 1SAEBM S I I SI SI 20LMZF S S SI I 28YACH S I I 2H9171 SI 33HOOD S I 3BY3P6 S S S I I 3MGTTL I S 3RV3F7 S I I I 3UMO3Y SI I 3V0OFD I SI 4FA8F0 I I SI I 555YH5 S S S I I I SI I Tollens reagent 5V22WM S S I I 5WSWTT S S I I I 5ZW2N9 I SI 6306WG SI SI I I 666F66 SI SI SI I I 7FH7HV S I 7K1RKK S S I I GC/MS dERIVITISATION 7WPIJX S I I 888Z8S S S I 8GORYY I I 8SVPRT I SI 8YSG8M SI 8ZZZO7 S S S I A3AH32 S S S I I AEE5WA SI I AGNIZI SI I I SI AIPPIG S I SI SI I AJ22ZI S I

32 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 140 141 142 150 160 161 170 171 180 190 200 211 230 231 210 AKJ5JY S S I I ANHVML S S I I BLZZMB S I SI SI BPLP0L S I I C9TTRY S S S I CWGDML S S I I S CWLQJ1 S S I CZV766 S S S SI D5BVEI SI D8DHQW SI S I I I DFCXDG I SI I LC/RI DLDLOB SI I GC-IRD DNKLDD I SI DQEDDN SI I DQMISD SI I DYEYYG S I EBQAXY SI EDRLTN I SI ELN44T I SI EMZZIW I SI ET1YHT I SI S UPLC_PDA FFFAFF SI S SI I S Simon's reagent FIKSPK S I I FL6M38 S S S I SI FO8JOE I I I SI G222HF S S I SI GCGWXG S S I I GEZZ2P S I GK8FTC I SI FPIA H4TJQT S S S I I I I H74EH5 S I I I XRD HCW3AW S S S I I HCZG6T SI HYEPEU S S I I HYRH0O I SI I3W3SW I SI I9MZ11 S S I I I IJ37J2 I IM8WG1 S S SI SI

33 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 140 141 142 150 160 161 170 171 180 190 200 211 230 231 210 IMEQDK S S I IOP7DS S S S I I IRIBPI SI I IT3XHS S S I I I Dragendorff test J1X7S4 I S I I JA3JJQ S I I JIRDRI I SI K2D2PO S S SI S duenois levin KEANRN S SI SI KGJIJS S S S I KN4PSK I SI KPAKKD SI KX18KO S S S I I KYGWUS S S I LG45WT S S S I LLLSLL I SI ATR LYWXR6 I SI M1Q1F5 SI ASAP-TOF MJHGVG SI MRWDW I SI G NBI4J4 SI S I I NHY1ZE S SI I SI NNBNTN SI I I I CE NSJNGB I SI NU06C7 SI S S I I SI NVENEN S S S I I O2WSYF I S I OGLNKI SI OLLRLR I SI ORHNDM I SI I OW2RIV SI I PF5IJN S S S I I I PIRHNH S I I PPHBGP SI SI SI I PSQS7F SI I Q11YO1 SI Q8ECTW I I I SI I I xrd QIEBZB S S I S Simon QOOCT8 S I

34 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 140 141 142 150 160 161 170 171 180 190 200 211 230 231 210 QTTSCI S SI RJXPPP SI I RV9IZA S SI RXKBFM S S I I S tanred S4B5OL S S SI I A SAZ3ZW S S I SI Ion Mobility Spectrometry SF9898 S S S I I SGDY90 I I SI SUOIOI S I TIILNU S I I TLVU3E I I U54UUY S S S I I S Test strips UIIF4G S I I ULQHBK S S S I I ULXUTD S I V3BKMA S I I V43UFL SI VGVOLX S S I I VJMKCE S S S I I VLJXIU S S I I VLLLV0 S S I VMHH2Y I SI VXXFXK S I SI SI VZSIJV I S W33NYG S S S I I XFPUFJ I XGELS2 I SI SI XH2D7F I I XL5KA0 S S S I I I I XMAYN4 S S S I I XVDW7X S S S I YCYBYW SI YVAVK8 S I SI SI YWZYAR SI SI YYDEDD SI I Z154TB S I SI SI Z8YS9F SI ZM99S9 S S S I I ZZKXPP SI I

35 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary for test sample 1 The response summary of all 151 participating laboratories for the identification of SM-1, frequency of use of screening and identification techniques and false positives and negatives: Identification of test sample 1: Response Summary Participants: 151

1-(3-Chlorophenyl)piperazine: 141

False positives for Test Sample 1

Code Name Technique 7FH7HV Metamfetamine 150 PSQS7F 1-(4-Chlorophenyl)piperazine 140/180 U54UUY Heroin 150/161 W33NYG Heroin 150/171

False negatives for SM-1 (techinque(s) used or ANP)

Code:7FH7HV (150), PSQS7F (140/180), U54UUY (150/161), YCYBYW (180), XFPUFJ (ANP)

A3AH32 (ANP), CZV766 (ANP), IMEQDK (ANP), VLLLV0 (ANP) ZM99S9 (ANP)

Frequency of use of screening and identification techniques:

Response Summary Participants: 151130 Section 140 141 142 150 160 161 170 171 180 190 200 211 230 231 210 Screening 52 63 50 14 0 2 0 3 57 16 3 0 0 0 9 34.4% 41.7% 33.1% 9.3% 0.0% 1.3% 0.0% 2.0% 37.7% 10.6% 2.0% 0.0% 0.0% 0.0% 6.0% Identification 11 3 2 40 6 13 2 26 135 56 3 2 2 1 13 7.3% 2.0% 1.3% 26.5% 4.0% 8.6% 1.3% 17.2% 89.4% 37.1% 2.0% 1.3% 1.3% 0.7% 8.6% # labs using 55 63 50 47 6 14 2 27 135 59 4 2 2 1 18 this technique 36.4% 41.7% 33.1% 31.1% 4.0% 9.3% 1.3% 17.9% 89.4% 39.1% 2.6% 1.3% 1.3% 0.7% 11.9%

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Z-Scores for Test Sample 1

1-(3-Chlorophenyl)piperazine Deviation Code Concentration from robust z-score (mass%) average 0J0PYS 25.2 -8.3 -0.9 0LN2QE 40.5 7.0 0.8 1SAEBM 37.7 4.2 0.5 20LMZF 39.0 5.5 0.6 28YACH 20.5 -13.0 -1.5 2H9171 29.6 -3.9 -0.4 3UMO3Y 37.8 4.3 0.5 555YH5 5.9 -27.6 -3.1 666F66 60.0 26.5 3.0 7WPIJX 18.0 -15.5 -1.8 8SVPRT 40.6 7.1 0.8 AGNIZI 9.0 -24.5 -2.8 BPLP0L 40.4 6.9 0.8 D5BVEI 38.1 4.6 0.5 DFCXDG 45.0 11.5 1.3 DLDLOB 36.4 2.9 0.3 DNKLDD 40.0 6.5 0.7 DQEDDN 23.9 -9.6 -1.1 DQMISD 43.1 9.6 1.1 EMZZIW 20.0 -13.5 -1.5 ET1YHT 47.7 14.2 1.6 FIKSPK 26.0 -7.5 -0.9 FO8JOE 39.0 5.5 0.6 GEZZ2P 34.0 0.5 0.1 H74EH5 46.2 12.7 1.4 HCW3AW 40.7 7.2 0.8 HYRH0O 24.0 -9.5 -1.1 IJ37J2 24.0 -9.5 -1.1 IM8WG1 31.9 -1.6 -0.2 IRIBPI 34.1 0.6 0.1 J1X7S4 34.2 0.7 0.1 KN4PSK 31.6 -1.9 -0.2 NNBNTN 38.6 5.1 0.6 NSJNGB 32.2 -1.3 -0.2 O2WSYF 17.4 -16.1 -1.8 OGLNKI 31.9 -1.6 -0.2 PF5IJN 23.4 -10.1 -1.2 Q8ECTW 29.9 -3.6 -0.4 QIEBZB 39.4 5.9 0.7 QOOCT8 35.0 1.5 0.2 RJXPPP 44.6 11.1 1.3 SF9898 25.6 -7.9 -0.9 SGDY90 30.0 -3.5 -0.4 TLVU3E 38.2 4.7 0.5 VZSIJV 38.1 4.6 0.5 XH2D7F 18.9 -14.6 -1.7 XL5KA0 35.0 1.5 0.2 Z8YS9F 36.2 2.7 0.3

37 Z-Score Report per Sample per Substance

Round: 2014/1 Substance: SM-1/1-(3-Chlorophenyl)piperazine Robust average = 33.5 UNODC value = 40.1

4.0 3.0 3.0

2.0 1.6 1.4 1.3 1.2 1.1 0.8 0.8 0.8 0.8

1.0 0.7 0.7 0.6 0.6 0.6 0.5 0.5 0.5 0.5 0.5 0.3 0.3 0.2 0.2 0.1 0.1 0.1 0.0 0.2 0.2 0.2 0.2 ‐ ‐ ‐ ‐ 0.4 0.4 0.4 ‐ ‐ ‐1.0 ‐ 0.9 0.9 ‐ 0.9 ‐ ‐ 1.1 1.1 1.1 ‐ ‐ 1.1 ‐ ‐ 1.5 1.5 ‐ ‐

‐2.0 1.7 ‐ 1.8 1.8 ‐ ‐

‐3.0 2.8 ‐ 3.1 ‐

‐4.0 IRIBPI IJ37J2 VZSIJV PF5IJN FIKSPK 0J0PYS AGNIZI J1X7S4 Z8YS9F BPLP0L SF9898 RJXPPP QIEBZB D5BVEI 7WPIJX 666F66 XL5KA0 GEZZ2P 8SVPRT ET1YHT FO8JOE TLVU3E 555YH5 OGLNKI 2H9171 KN4PSK 20LMZF SGDY90 XH2D7F 28YACH 0LN2QE NSJNGB H74EH5 DLDLOB DFCXDG EMZZIW 1SAEBM DNKLDD HYRH0O O2WSYF DQMISD QOOCT8 Q8ECTW NNBNTN DQEDDN IM8WG1 3UMO3Y HCW3AW

z-scores can be interpreted by participants in line with ISO 13528:2005, section 7.4.2 and ISO/IEC guide43- 1:1997(E) as follows: |z| < 2 = satisfactory 2 ≤ |z| ≤ 3 = questionable |z| > 3 = unsatisfactory

38 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Sample 2 Analysis

Identified substances for Test Sample 2

Code Identified Substances 0J0PYS metamfetamine 0LN2QE Metamfetamine 0N05YR methamphetamine 0RE0L0 metamfetamine 1SAEBM methamphetamine 20LMZF Methamphetamine hydrochloride 28YACH Metamfetamine 33HOOD Methamphetamine 3BY3P6 Metamfetamine 3MGTTL methamphetamine 3RV3F7 metamfetamine 3UMO3Y methamphetamine 3V0OFD methamphetamine 4FA8F0 Metamfetamine 555YH5 Metamfetamine 5V22WM Methylamphetamine 5WSWTT amphetamine 5ZW2N9 metamfetamine 6306WG metamphetamine 666F66 methamphetamine 7FH7HV Méthamphétamine 7K1RKK Methamphetamine 7WPIJX methamphetamine 888Z8S Metamphetamine 8GORYY Metamfetamine 8SVPRT metamfetamine 8YSG8M metamphetamine 8ZZZO7 methamphetamine A3AH32 Metanfetamina AEE5WA Methamphetamine AGNIZI metamphetamine AIPPIG Methamphetamine AJ22ZI metamfetamine AKJ5JY Methamphetamine ANHVML Methylamphetamine BLZZMB methamphetamine BPLP0L methamphetamine C9TTRY metamphetamine CWGDML Methamphetamine CWLQJ1 Metamfetamine

39 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances CZV766 Methamphetamine D5BVEI Methamphetamine D8DHQW Metamfetamine DFCXDG Metamfetamine DLDLOB methamphetamine DNKLDD Methamphetamine DQMISD metamfetamine DYEYYG Metamfetamine EBQAXY Metamfetamine EDRLTN Methylamphetamine ELN44T Methamphetamine EMZZIW Methamphetamine ET1YHT Metamfetamine FFFAFF methamphetamine FIKSPK Metamfetamine FL6M38 Metamfetamine FO8JOE metamfetamine GCGWXG N-Methylamphetamine GEZZ2P Metamfetamine GK8FTC methamphetamine H74EH5 Metanphetamine hcl HCW3AW Methamphetamine HCl HCZG6T Methamphetamine HYEPEU Methamphetamine HYRH0O Metamphetamine I3W3SW METHAMFETAMINE I9MZ11 Metamfetamine IJ37J2 Metamfetamine IM8WG1 Metamfetamine IMEQDK Metamfetamine IOP7DS Metamfetamine IRIBPI Metamfetamine IT3XHS Methamphetamine J1X7S4 Methamphetamine HCl JA3JJQ Metamfetamine JIRDRI Metamfetamine K2D2PO Methamphetamine KEANRN Metamfetamine KGJIJS Metamfetamine KPAKKD Metamfetamine KX18KO Methylamphetamine hydrochloride KYGWUS Methylamphetamine LG45WT Metamfetamine LLLSLL metamphetamine HCl

40 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances LYWXR6 Metamfetamine M1Q1F5 Metamphetamine MJHGVG METHAMPHETAMINE MRWDWG metamfetamine NBI4J4 Metamfenamine NHY1ZE Methamphetamine NNBNTN d-methamphetamine hydrochloride NSJNGB Metamfetamine NU06C7 Metamfetamine 72,5% NVENEN Amfetamine O2WSYF methamphetamine OGLNKI Metamfetamine OLLRLR methamphetamine ORHNDM metamphétamine OW2RIV Methamfatamine PF5IJN METANFETAMINA PIRHNH metamfetamine PPHBGP METAMPHETAMINE PSQS7F METHANPHETAMINE Q11YO1 metamfetamine Q8ECTW methamphetamine QIEBZB Metamfetamine QOOCT8 Metamfetamine QTTSCI Methamphetamine RJXPPP Metamphetamine RV9IZA , Methamphetamine RXKBFM metanfetamina S4B5OL Metamfetamine SAZ3ZW Metanfetamina SF9898 Metamfetamine SUOIOI Methamphetamine TIILNU Methamphetamine TLVU3E Methamphetamine U54UUY METHAMPHETAMINE UIIF4G Metanfetamina ULQHBK Methamphetamine ULXUTD metamfetamine V3BKMA Metamfetamine V43UFL metamfetamine, HCl VGVOLX Metamfetamine VJMKCE Methylamphetamine Hydrochloride VLJXIU Metamfetamine VLLLV0 metanfetamina VMHH2Y Methamfetamine

41 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances VXXFXK metamfetamine VZSIJV metamfetamine W33NYG Methanphetamine XFPUFJ methamphetanime XGELS2 Metamfetamine XH2D7F metamphetamine XL5KA0 Metamfetamine XMAYN4 metamfetamine XVDW7X methamphetamine YCYBYW Metamphetamine YVAVK8 methamphetamine YWZYAR methampetamine YYDEDD Methamfetamine Z154TB methamphetamine Z8YS9F Metamfetamine ZM99S9 Methamphetamine ZZKXPP METHANPHETAMINE

42 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Statement of findings for Test Sample 2

Code Metamfetamine 0J0PYS + Sample two contains metamfetamine,HCL (73.3% as base) 0LN2QE + Metamfetamine 0N05YR +

0RE0L0 + The sample contains metamfetamine which is scheduled as illicit drug in France. 1SAEBM + Sample contains 72.6± 3.2 % (w/w) methamphetamine base in HCL salt form. 20LMZF + One glass bottle containing 0.22 grammes of a powder containing 0.20 grammes of methamphetamine hydrochloride (a salt of methamphetamine). 28YACH + Metamfetamine existed in salt form. 2H9171 +

33HOOD + Based on the above analysis, the sample was found to contain methamphetamine. 3BY3P6 + White powder was found to contain Metamfetamine. 3MGTTL +

3RV3F7 + in the sample ismetamfetamine who is on the list of drugs in Montenegro 3UMO3Y + white powder, also contain dimethylsulfone 3V0OFD + white powder containing 74.7% metamphetamine 4FA8F0 + Metamfetamine 555YH5 +

5V22WM + The powder was analysed and found to contain Methylamphetamine. 5WSWTT - after chemical analysis was performed, the sample was found to contain 84.9% amphetamine. 5ZW2N9 + metamfetamine was detected by GC/MS screening and it was confirmed and quantified by GC-FID using calibration curve 6306WG +

666F66 + methamphetamine 7FH7HV + L'échantillon 2014/1/SM-2 contient de la méthamphétamine

43 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Metamfetamine 7K1RKK + A sample of the powder was analysed and found to contain methamphetamine, which is a class A controlled substance under the Misuse of Drugs Act 1971. 7WPIJX + +creatinine 888Z8S + On analysis, I found the substance to contain 70.5% Methamphetamine 8GORYY + The sample contains metamfetamine which is listed as a controlled drug according to french order, appendix III of February 22nd 1990. 8SVPRT + The results of TLC of test sample and reference substance was same as metamfetamine. the peak of IR of test sample was shown same as metamfetamine 8YSG8M + found methamphetamine with 64.0% w/w 8ZZZO7 + On analysis, I found the sustances to contain 70.33% (by weight) of methamphetamine A3AH32 + Metanfetamina AEE5WA +

AGNIZI +

AIPPIG + White powder containing methamphetamine. AJ22ZI + The sample was found to contain metamfetamine AKJ5JY + Sample 2014/1/SM-2, a white, odourless powder, gave a positive result for Methamphetamine, a controlled substance under national legislation on drugs. ANHVML + White powder containing an average of 73% methylamphetamine. Methylamphetamine is a Class A controlled drug under the provisions of the Misuse of Drugs Act 1971 (as amended). BLZZMB + dimethylsulfone BPLP0L + This sample is methamphetamine. C9TTRY +

CWGDML +

CWLQJ1 + The chemical tests and the coincidence in the time of retention and mass fragmentogram with the material reference used in the same conditions that the analyzed sample, they indicates in this one the metanfetamine's presence. CZV766 + The white powder contains Methamphetamine. D5BVEI + Powder containing methamphetamine.

44 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Metamfetamine D8DHQW + Metamfetamine, a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. DFCXDG + The sample contains metamfetamine 75.62 %, m/m. DLDLOB + narcotics: methamphetamine concentration: approx 79 % as free base DNKLDD +

DQEDDN +

DQMISD + powder with 74,7 % of metamfetamine as a active substance and DMS as a adulterant DYEYYG + Metamfetamine EBQAXY + The sample 2014/1/SM-2 contains 70% of metamfetamine. Metamfetamine is a controlled substance in France EDRLTN + The exhibit item was found to contain Methylamphetamine ELN44T + On analysis, I found the sample to contain methamphetamine EMZZIW +

ET1YHT + 85.7 % Metamfetamine FFFAFF + White powder that contains substance under control - methamphetamine. FIKSPK + It has been detecded that tehe subject of study including White colour dust substance was Metamfetamine. This is a drug which is under the terms of national sunstance of drug Law 2313. FL6M38 + metamfetamine FO8JOE + Retention time and MS spectra in GC analysis (FID and MS) compared with ICE reference material. Metamfetamine as hydrochloride. G222HF +

GCGWXG + N-Methylamphetamine is a Class A controlled drug subject to the provisions of the Misuse of Drugs Act 1971. GEZZ2P +

GK8FTC +

H4TJQT +

H74EH5 + Base Metanphetamine 77,5%

45 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Metamfetamine HCW3AW + Positive with Marquis (orange turn to brown). Positive with Simon (Blue). Silver Nitrate Test--> Chloride Positive.TLC(TA,TE),GCMS -->Methamphetamine confirmed, and trace of Dimethyl sulfone found. GC--> Methamphetamine base 71.38% HCZG6T + The sample was found to contain 72.8% of methamphetamine (as base). HYEPEU + The powder is a psychotropic substance - methamphetamine powder. The powder contains 76.6 % pure methamphetamine (base form). HYRH0O + Metamphetamine I3W3SW + METHAMFETAMINE IS PRESENT IN HYDROCHLORIDE FORM. I9MZ11 + SM-2 contained Metamfetamine IJ37J2 + In the test sample 2014/1/SM-2 was detected Metamfetamine IM8WG1 +

IMEQDK +

IOP7DS + The sample contains metamfetamine (72.4%). IRIBPI +

IT3XHS + Orange changes to brown color in Marquis Reagent indicates the possible presence of methamphetamine.By TLC,Rf and color of std Methamphetamine are equal to those of SM2.Retention Time (RT12.833) and Base peaks( 138.05 ) of SM2 are mostly identical to std methamphetamine and library search in GCMS shows SM2 being Methamphetamine. J1X7S4 + SM2 contains also Dimethylsulfone. JA3JJQ + Metamfetamine JIRDRI + metemfetamine positive K2D2PO +

KEANRN + In the tested sample was detected and confirmed the presence of metamfetamine KGJIJS + SIGN IN DETECTED Metamfetamine 2014/1/SM-2 labeled. KN4PSK + Metamfetamine KPAKKD + The sample contains metamfetamine KX18KO + White powder containing Methylamphetamine which is a class A controlled drug with a purity of 72% (as base) under the provisions of the Misuse of Drugs Act 1971 (as amended).

46 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Metamfetamine KYGWUS + O.229 grams of off white powder found to contain methylamphetamine at a concentration of 74%. Methylamphetamine is controlled by the Misuse of Drugs Act 1971 (as amended) as a Class A drug LG45WT + The sample was soluble in water and ethanol. The sample had positive reaction for amphetamine with marquis reagent . LLLSLL +

LYWXR6 + We have also found dimethylsulphone, which is a synthesis product and also a common adulterant agent for Metamfetamine. M1Q1F5 + The sample contain controlled drug metamphetamine MJHGVG + hydrochloride form MRWDWG + white powder containing 73.2%mM7 of metamfetamine NBI4J4 +

NHY1ZE + SM2 was contain methamphetamine NNBNTN + d-methamphetamine hydrochloride and dimethyl sulfone confirmed in one unit tested of one unit recieved. NSJNGB + Metamfetamine NU06C7 +

NVENEN + The Sample 2014/1/SM2 was found to contain Amfetamine. O2WSYF + The sample is identified as methamphetamine OGLNKI + Metamfetamine OLLRLR + the white powder contains metamphetamine (74.4%w/w), which is controlled bt national law ORHNDM + métamphétamione,substance classée stupéfiant OW2RIV + Sample containing Methamfetamine PF5IJN + MARQUIS, SCOTT, SIMON´S, UV, HPLC, GC-MS, FT-IR, HPLC PIRHNH +

47 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Metamfetamine PPHBGP + The results of the tests of the SM2 () received confirmed that the mentioned sample contains METAMPHETAMINE but we are not able to give a cuantification result because we can not do it with our gas chromatography-gas spectometer and we have not got a gas chromatography FID which is the suitable analytical technique. The sample 2 also contains caffein as not controlled drug. PSQS7F + The simple No 2014/1/SM-2 was found METHANPHETAMINE Q11YO1 + white powder containing metamfetamine Q8ECTW + The powder contains methamphetamine with a concentration in the sample of 73.6% by weight as free base QIEBZB + The substance contains 74.96% of Metamfetamine QOOCT8 + Sample 2014/1/SM-2 was found to contain Metamfetamine. QTTSCI + Examination of the powder SM-2 revealed the presence of controlled drug Methamphetamine RJXPPP -

RV9IZA +

RXKBFM +

S4B5OL + The test sample 2014/1/SM-2 was analysed by colour test and Thin layer Chromatography (TLC) techniques and found to contain Metamfetamine. SAZ3ZW + De acuerdo a los análisis realizados se concluye que se trata Metanfetamina SF9898 + Metamfetamine was identified by TLC and GC/MS SGDY90 +

SUOIOI + ,PDGHWKHFKHPLFDODQGLQVWUXPHQWDODQDO\VLVLWUHVXOWHGWKDWWKHVDPSOHFRQWDLQV methamphetamine TIILNU +

TLVU3E + The sample SM2 contained 73.8 % methamphetamine calculated as a base. In the sample was identified dimethylsulphone (MSM). U54UUY - Field Test employing the Marquis Test was positive because the spot was brown. TLC analysis employing two(2) solvent systems and HPLC confirmed the sample as Methamphetamine. UIIF4G +

ULQHBK + 2014/1/SM-2 contains Methamphetamine.

48 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Metamfetamine ULXUTD +

V3BKMA +

V43UFL +

VGVOLX + MR and CT reagents: positive. GC/MS: Retention time, mass-charge (M/Z) similar characteristics with the substances used as standar or pattern. FTIR: Absorption bands conicident with the substances used as pattern VJMKCE + A white powder containing an average of 91% of METHYLAMPHETAMINE HYDROCHLORIDE VLJXIU +

VLLLV0 +

VMHH2Y +

VXXFXK + dimetil-sulfone VZSIJV + metamfetamine is controlled (KB 22/01/1998) W33NYG + In this sample were performed the same tests but with preliminary testing (MARQUIS reagent) coloration is not very clear for that class of drugs (amphetamines and their derivatives), or thin-layer Cromatofrafia-TLC and even gas chromatography coupled to the flame-Ionization Detector GC/FID but according to the obtained results it was verified that we are in the presence of methamphetamine. XFPUFJ +

XGELS2 +

XH2D7F + Illegal substances on the basis of the italian law DPR 309/90 XL5KA0 + Presence of metamfetamine hydrochloride was detected in the sample. XMAYN4 + *Results of screening tests were positive for metamfetamine. *Retention time and fragmentation pattern obtained with sample are equivalent to those obtained with metamfetamine. XVDW7X + The sample SM-2 contains methamphetamine, which is included in List F2 (List of psychotropic substances banned in Brazil) of Annex I of SVS / MS 344, May 12, 1998. YCYBYW +

YVAVK8 + dimethylsulfone YWZYAR + dimethylsulfone YYDEDD +

49 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Metamfetamine Z154TB +

Z8YS9F +

ZM99S9 + The sample obtains with the positive result with Marquis reagent. TLC : The Rf sample obtain with the same Rf Methamphetamine standard. GC: The Rt sample obtain with the same Rt Methamphetamine standard. ZZKXPP + CONFIRMED BY GC MS

50 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Identification methods for Test Sample 2

Legend: S ... used for Screening I ... used for Identification SI ... used for both

51 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

52 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

53 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

54 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary for test sample 2 The response summary of all 151 participating laboratories for the identification of SM-2, frequency of use of screening and identification techniques and false positives and negatives: Identification of test sample 2:

Response Summary Participants: 151

Metamfetamine: 148

False positives for Test Sample 2

Code Name Technique 5WSWTT A mfetamine 180/200 W33NYG MDEA 1 5 0/1 71 NVENEN Amfetamine 180

False negatives for SM-2 (techinque(s) used or ANP)

Code: U54UUY (150/161), RJXPPP (180/230) 5WSWTT (180)

Frequency of use of screening and identification techniques:

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Z-Scores for Test Sample 2

Metamfetamine Metamfetamine Deviation Deviation Code Concentration Code Concentration from robust z-score from robust z-score (mass%) (mass%) average average 0J0PYS 73.3 -0.5 -0.1 I3W3SW 72.8 -1.0 -0.3 0LN2QE 73.4 -0.4 -0.1 I9MZ11 70.4 -3.4 -0.9 0RE0L0 76.0 2.2 0.6 IJ37J2 73.0 -0.8 -0.2 1SAEBM 72.6 -1.2 -0.3 IM8WG1 75.2 1.4 0.4 20LMZF 72.6 -1.2 -0.3 IMEQDK 88.3 14.5 4.1 28YACH 72.5 -1.3 -0.4 IOP7DS 72.4 -1.4 -0.4 2H9171 71.3 -2.5 -0.7 IRIBPI 77.3 3.5 1.0 3UMO3Y 72.5 -1.3 -0.4 IT3XHS 94.7 20.9 5.8 3V0OFD 74.7 0.9 0.3 J1X7S4 74.0 0.2 0.1 555YH5 78.6 4.8 1.4 K2D2PO 77.6 3.8 1.1 5ZW2N9 15.1 -58.7 -16.4 KN4PSK 76.2 2.4 0.7 6306WG 68.1 -5.7 -1.6 KX18KO 72.0 -1.8 -0.5 666F66 79.0 5.2 1.5 KYGWUS 74.0 0.2 0.1 7WPIJX 79.0 5.2 1.5 LLLSLL 70.0 -3.8 -1.1 888Z8S 70.5 -3.3 -0.9 LYWXR6 72.0 -1.8 -0.5 8GORYY 74.6 0.8 0.2 MRWDWG 73.2 -0.6 -0.2 8YSG8M 64.0 -9.8 -2.7 NHY1ZE 11.0 -62.8 -17.5 8ZZZO7 70.3 -3.5 -1.0 NNBNTN 72.6 -1.2 -0.3 AEE5WA 80.0 6.2 1.7 NSJNGB 75.2 1.4 0.4 AGNIZI 72.0 -1.8 -0.5 NU06C7 72.5 -1.3 -0.4 ANHVML 73.0 -0.8 -0.2 OGLNKI 74.7 0.9 0.3 BPLP0L 74.4 0.6 0.2 OLLRLR 74.4 0.6 0.2 D5BVEI 72.2 -1.6 -0.4 PF5IJN 78.6 4.8 1.3 DFCXDG 75.6 1.8 0.5 Q8ECTW 73.6 -0.2 0.0 DLDLOB 78.9 5.1 1.4 QIEBZB 75.0 1.2 0.3 DNKLDD 73.5 -0.3 -0.1 QOOCT8 66.0 -7.8 -2.2 DQEDDN 71.2 -2.6 -0.7 RJXPPP 77.5 3.7 1.0 DQMISD 74.7 0.9 0.3 SF9898 21.6 -52.2 -14.5 DYEYYG 70.7 -3.1 -0.9 SGDY90 70.0 -3.8 -1.1 EBQAXY 70.0 -3.8 -1.1 TLVU3E 73.8 0.0 0.0 EDRLTN 72.9 -0.9 -0.2 ULXUTD 72.8 -1.0 -0.3 EMZZIW 85.0 11.2 3.1 V3BKMA 72.6 -1.2 -0.3 ET1YHT 85.7 11.9 3.3 V43UFL 76.0 2.2 0.6 FIKSPK 69.0 -4.8 -1.3 VJMKCE 73.0 -0.8 -0.2 FO8JOE 76.7 2.9 0.8 VZSIJV 76.9 3.1 0.9 GEZZ2P 73.0 -0.8 -0.2 XH2D7F 86.7 12.9 3.6 H74EH5 77.5 3.7 1.0 XL5KA0 74.6 0.8 0.2 HCW3AW 71.4 -2.4 -0.7 XVDW7X 79.6 5.8 1.6 HCZG6T 72.8 -1.0 -0.3 YCYBYW 83.5 9.7 2.7 HYEPEU 76.0 2.2 0.6 YYDEDD 70.1 -3.8 -1.0 HYRH0O 81.9 8.1 2.3 Z8YS9F 67.1 -6.7 -1.9 ZM99S9 39.9 -33.9 -9.4

56 Z-Score Report per Sample per Substance

Round: 2014/1 Substance: SM-2/Metamfetamine Robust average = 73.8 UNODC value = 73.6

4 3.6 3.3 3.1

3 2.7 3 2.

2 1.7 1.6 1.5 1.5 1.4 1.4 1.3 1.1 1.0 1.0 1.0 0.9 1 0.8 0.7 0.6 0.6 0.6 0.5 0.4 0.4 0.3 0.3 0.3 0.3 0.2 0.2 0.2 0.2 0.1 0.1 14.5 9.4 16.4 0.0 ‐ ‐ ‐ 17.5 0 ‐ 4.1 5.8 0.0 0.1 0.1 0.1 ‐ 0.2 ‐ ‐ 0.2 0.2 0.2 0.2 ‐ 0.2 0.3 0.3 0.3 ‐ ‐ ‐ ‐ ‐ 0.3 0.3 0.3 0.3 ‐ ‐ ‐ 0.3 0.3 0.3 0.4 ‐ ‐ ‐ ‐ ‐ ‐ ‐ 0.4 ‐ 0.5 0.5 0.5 ‐ ‐ ‐ ‐ 0.7

‐1 0.7 0.7 ‐ ‐ ‐ 0.9 0.9 ‐ 0.9 1.0 ‐ ‐ ‐ 1.0 1.0 1.0 1.0 ‐ ‐ ‐ ‐ 1.3 ‐ 1.6

‐2 ‐ 1.9 ‐ 2.2 ‐

‐3 2.7 ‐

‐4 IRIBPI IJ37J2 LLLSLL VZSIJV PF5IJN FIKSPK 0J0PYS J1X7S4 AGNIZI IT3XHS Z8YS9F RJXPPP BPLP0L SF9898 888Z8S 0RE0L0 D5BVEI QIEBZB 7WPIJX 666F66 IOP7DS OLLRLR XL5KA0 ET1YHT 8ZZZO7 GEZZ2P I9MZ11 FO8JOE V43UFL TLVU3E 555YH5 OGLNKI 2H9171 KN4PSK DYEYYG EDRLTN NHY1ZE SGDY90 20LMZF XH2D7F KX18KO 28YACH H74EH5 HCZG6T 0LN2QE NSJNGB HYEPEU DLDLOB EBQAXY VJMKCE ZM99S9 YYDEDD 8GORYY 3V0OFD K2D2PO ULXUTD NU06C7 LYWXR6 DFCXDG IMEQDK YCYBYW EMZZIW DNKLDD 1SAEBM 8YSG8M HYRH0O DQMISD I3W3SW 5ZW2N9 QOOCT8 AEE5WA 6306WG V3BKMA Q8ECTW XVDW7X NNBNTN KYGWUS DQEDDN IM8WG1 3UMO3Y ANHVML HCW3AW MRWDWG

57 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Sample 3 Analysis

Identified substances for Test Sample 3

Code Identified Substances 0J0PYS ketamine 0LN2QE Ketamine 0N05YR ketamine 0RE0L0 ketamine, lactose 1SAEBM ketamine 20LMZF Ketamine 28YACH Ketamine 33HOOD Ketamine 3BY3P6 Ketamine 3MGTTL ketamine 3RV3F7 ketamine 3UMO3Y ketamine 3V0OFD ketamine 4FA8F0 Ketamine 555YH5 Ketamine 5V22WM Ketamine 5WSWTT - 5ZW2N9 ketamine 6306WG ketamine 666F66 ketamine 7FH7HV Kétamine 7K1RKK Ketamine 7WPIJX ketamine 888Z8S Ketamine 8GORYY Ketamine 8SVPRT Ketamine 8YSG8M ketamine 8ZZZO7 ketamine A3AH32 Ketamina AIPPIG Ketamine AJ22ZI ketamine AKJ5JY Ketamine ANHVML Ketamine BLZZMB ketamine BPLP0L ketamine C9TTRY ketamine CWLQJ1 Ketamine CZV766 Ketamine D5BVEI Ketamine D8DHQW Ketamine

58 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances DFCXDG Ketamine DLDLOB Ketamine DNKLDD Ketamine DQMISD ketamine DYEYYG Ketamine EBQAXY Kétamine EDRLTN Ketamine ELN44T Ketamine EMZZIW ketamine ET1YHT Ketamine FFFAFF ketamine FIKSPK Ketamine FL6M38 Ketamine FO8JOE ketamine GCGWXG Ketamine GEZZ2P Ketamine GK8FTC ketamine H4TJQT chlormezanone H74EH5 Ketamine hcl HCW3AW Ketamine HCl HCZG6T Ketamine HYEPEU Ketamine HYRH0O Ketamine I3W3SW KETAMINE I9MZ11 Ketamine IJ37J2 Ketamine IM8WG1 Ketamine IMEQDK Ketamine IOP7DS Ketamine IRIBPI ketamine IT3XHS ketamine J1X7S4 Ketamine HCl JA3JJQ Ketamine JIRDRI Ketamine K2D2PO Ketamine KEANRN Ketamine KGJIJS Ketamine KN4PSK Ketamine KPAKKD Ketamine KX18KO Ketamine KYGWUS Ketamine LG45WT Ketamine LLLSLL ketamine LYWXR6 Ketamine

59 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances M1Q1F5 Ketamine MJHGVG KETAMINE MRWDWG ketamine NBI4J4 ketamine and lactose NHY1ZE Ketamine NNBNTN ketamine NSJNGB Ketamine NU06C7 Ketamine NVENEN Ketamine O2WSYF ketamine OGLNKI Ketamine OLLRLR ketamine ORHNDM kétamine chlorhydrate OW2RIV Ketamine PIRHNH ketamine PPHBGP KETAMINE PSQS7F KETAMINE Q11YO1 ketamine Q8ECTW ketamine QIEBZB Ketamine QOOCT8 Ketamine QTTSCI Ketamine RJXPPP Ketamine RV9IZA Ketamine RXKBFM ketamina S4B5OL Ketamine and Lactose SAZ3ZW Ketamina SF9898 Ketamine SUOIOI Ketamine TIILNU Ketamine TLVU3E Ketamine U54UUY N/A UIIF4G Ketamina ULQHBK Ketamine ULXUTD ketamine V3BKMA Ketamine V43UFL Ketamine VGVOLX Ketamine and Lactose VJMKCE Ketamine VLJXIU Ketamine VLLLV0 ketamina VMHH2Y Ketamine VXXFXK ketamine VZSIJV ketamine

60 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances W33NYG Ketamine XFPUFJ ketamine XGELS2 Ketamine XH2D7F ketamine XL5KA0 Ketamine XMAYN4 ketamine XVDW7X Ketamine YCYBYW Ketamine YVAVK8 ketamine YWZYAR ketamine YYDEDD Ketamine Z154TB ketamine Z8YS9F Ketamine ZM99S9 Ketamine ZZKXPP KETAMINE

61 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Statement of findings for Test Sample 3

Code Ketamine Lactose 0J0PYS + + Sample three contains ketamine,HCL (16.6% as base) cut with lactose 0LN2QE + + Contained Ketamine and lactose 0N05YR + ANP resolution 1478 de 2006. Incluided Ministerio de Salud y Protección Social/ Colombia 0RE0L0 + + The ketamine is scheduled as illicit drug in France. The lactose is not scheduled as illicit drug in France. It's a cutting agent. 1SAEBM + + Sample contains 16.31± 0.92 % (w/w) ketamine base.The sample also contains lactose. 20LMZF + + One glass bottle containing 0.22 grammes of a powder containing 0.03 grammes of ketamine. 28YACH + ANP Ketamine existed in salt form. We were found Lactose in the sample. 2H9171 + +

33HOOD + ANP Based on the above analysis, the sample was found to contain ketamine 3BY3P6 + +

3MGTTL + ANP

3RV3F7 + + in the sample are ketamine and lactose who is not on the list in Montenegro 3UMO3Y + + white powder, diluted by lactose 3V0OFD + + white powder containing 15.1% ketamine. Contains also lactose. 4FA8F0 + + Ketamine, Lactose 555YH5 + -

5V22WM + + The powder was analysed and found to contain Ketamine. 5WSWTT ANP + after chemical analysis was performed, the sample was found to contain: 1. lactose. 2. no controlled drugs. 5ZW2N9 + ANP ketamine was detected by GC/MS screening and it was confirmed and quantified by GC-FID using calibration curve 6306WG + -

666F66 + - ketamine 7FH7HV + - l'analyse de l'échantillon 2014/1/SM-3 révèle la présence de la kétamine

62 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Ketamine Lactose 7K1RKK + ANP A sample of the powder was analysed and found to contain Ketamine at a concentration of 14% , which is a class B controlled substance under the Misuse of Drugs Act 1971 7WPIJX + + +lactose 888Z8S + ANP On analysis, I found the substance to contain 22.5% Ketamine 8GORYY + + The sample contains ketamine which is listed as a controlled drug according to french order, appendix IV of February 22nd 1990. 8SVPRT + ANP The peak of IR of test sample was same as ketamine 8YSG8M + ANP found ketamine with 21.3% w/w 8ZZZO7 + - On analysis, I found the sustances to contain 17.99% (by weight) of ketamine A3AH32 + ANP ketamina AEE5WA + + Ketamine and Lactose AGNIZI + + mixture of ketamine and lactose AIPPIG + ANP White powder containing Ketamine. AJ22ZI + ANP The sample was found to contain ketamine AKJ5JY + ANP Sample 2014/1/SM-3, a white, odourless powder, gave a positive result for Ketamine, a controlled substance under national legislation on drugs. ANHVML + + White powder containing ketamine. Ketamine seized prior to 10th June 2014 is a Class C controlled drug under the provisions of the Misuse of Drugs Act 1971 (as amended). Ketamine seized on or after 10th June 2014 is a Class B controlled drug under the provisions of the Misuse of Drugs Act 1971 (as amended). BLZZMB + + lactose BPLP0L + + This sample is ketamine C9TTRY - -

CWGDML + + Ketamine was detected on Sample SM-3, this drug is not controlled by national legislation in Costa Rica. Ketamine it is not included on United Nations lists. CWLQJ1 + - The coincidence in the time of retention and mass fragmentogram with the material reference used in the same conditions that the analyzed sample, they indicates in this one the ketamine's presence. CZV766 + ANP The white powder contains Ketamine. D5BVEI + ANP Powder containing ketamine.

63 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Ketamine Lactose D8DHQW + + Ketamine, a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. DFCXDG + + The sample contains ketamine 17.48 %, m/m. DLDLOB + ANP narcotics: ketamine concentration: approx 16 % as free base DNKLDD + ANP

DQEDDN + +

DQMISD + + powder with 17,0 % of ketamine as a active substance and lactose as a adulterant DYEYYG + + Ketamine and lactose EBQAXY + - The sample 2014/1/SM-3 contains ketamine. Ketamine is a controlled substance in France EDRLTN + + The exhibit item was found to contain Ketamine ELN44T + ANP On analysis, I found the sample to contain ketamine EMZZIW + -

ET1YHT + ANP 17.8 % Ketamine FFFAFF + ANP White powder that contains substance ketamine. FIKSPK + ANP It has been detecded that tehe subject of study including White colour dust substance was Ketamine. This is a drug which is under the terms of national sunstance of drug Law 2313. FL6M38 + - polvo cristalino blanco FO8JOE + + Ketamine retention time and MS spectra in GC analysis (FID and MS) compared with ICE reference material. Cloudy CHCl3 solution and FTIR/ATR indicates a mixture with lactose (confirmation performed by FTIR). Ketamine as hydrochloride. G222HF ANP ANP

GCGWXG + + Ketamine is a Class C controlled drug subject to the provisions of the Misuse of Drugs Act 1971. GEZZ2P + -

GK8FTC + ANP

H4TJQT + +

H74EH5 + + Base Ketamine 16,0% and Lactose

64 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Ketamine Lactose HCW3AW + ANP Negative with Marquis, Cobalt thiocyanate and Simon (No color change). Silver Nitrate Test--> Chloride Positive. TLC(TA,TE), GCMS --> Ketamine confirmed. GC--> Ketamine base 15.58% HCZG6T + + The sample was found to contain 16.0% of ketamine (as base). HYEPEU + ANP The powder is a psychotropic substance - ketamine powder. Quantity of pure substance not detected. HYRH0O + - Ketamine I3W3SW + + KETAMINE IS PRESENT IN HYDROCHLORIDE FORM. LACTOSE WAS ALSO IDENTIFIED. I9MZ11 + + SM-3 contained Ketamine IJ37J2 + - In the test sample 2014/1/SM-3 was detected Ketamine IM8WG1 + ANP

IMEQDK + ANP We have identified the drug, but we are unable to quantify it because we do not have Ketamine certified reference. IOP7DS + ANP The sample contains ketamine (15.5%). IRIBPI + + We also found lactose IT3XHS + - Viloet color in cobalt Thiocyanate test indicates possible presence of Ketamine.Rf and color of std Ketamine equal to those of SM3.Retention Time(RT 13.129) and base peaks 180 of SM3 are mostly identical to those of std Ketamine and library search in GCMS shows SM3 being Ketamine. J1X7S4 + + SM3 contains also Lactose. JA3JJQ + + Ketamine and lactose JIRDRI + ANP Ketamine positive K2D2PO + ANP We have used only GC/MS as screening and identification. KEANRN + ANP In the tested sample was detected and confirmed the presence of Ketamine KGJIJS + - SIGN IN DETECTED 2014/1/SM-2 labeled Ketamine. KN4PSK + - Ketamine KPAKKD + ANP The sample contains Ketamine KX18KO + + White powder containing ketamine which is a class B controlled drug under the provisions of the Misuse of Drugs Act 1971 (as amended). The results also indicated the presence of lactose which is not subject to control under the provisions of the Misuse of Drugs Act 1971 (as amended).

65 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Ketamine Lactose KYGWUS + ANP 0.236 grams of off-white powder found to contain Ketamine. At the time of seizure Ketamine was controlled by the Misuse of Drugs Act 1971 (as amended) as a Class C drug. Since 10th June 2014, Ketamine has been controlled by the Misuse of Drugs Act 1971 as amended), as a Class B drug. LG45WT + ANP The sample was soluble in water, ethanol, methanol and chlorofom. The sample had positive reaction for alkaloid with tanred reagent . The sample had positive reaction for chlorides with silver nitrate reagent . LLLSLL + + additional substance - lactose LYWXR6 + ANP Ketamine is under illicit drugs legislation control in Spain since 2010. M1Q1F5 + ANP The sample contain controled drug ketamine MJHGVG + + hydrochloride form + lactose MRWDWG + ANP white powder containing 17.1%mM7 of ketamine NBI4J4 + +

NHY1ZE + - SM3 was contain dissociative anesthetic (Ketamine) NNBNTN + + Ketamine and lactose confirmed in one unit tested of one unit recieved. NSJNGB + - Ketamine NU06C7 + -

NVENEN + ANP The Sample 2014/1/SM3 was found to contain Ketamine. O2WSYF + + The sample is a preparation that contains ketamine and lactose. OGLNKI + - Ketamine OLLRLR + ANP the white powder contains ketamine (17.8%w/w), which is controlled bt national law ORHNDM + + kétamine, substance classée stupéfiant OW2RIV + ANP Sample containing Ketamine PF5IJN + + MARQUIS, SCOTT, SIMON´S, UV, HPLC, GC-MS, FT-IR PIRHNH + +

66 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Ketamine Lactose PPHBGP + - The results of the tests of the SM3 () received confirmed that the mentioned sample contains KETAMINE but we are not able to give a cuantification result because we can not do it with our gas chromatography-gas spectometer and we have not got a gas chromatography FID which is the suitable analytical technique.

PSQS7F + - The simple No 2014/1/SM-2 was found KETAMINE Q11YO1 + ANP white powder containing ketamine Q8ECTW + + The powder is a mixture of ketamine and lactose. The concentration of ketamine in the sample is 16.9% by weight QIEBZB + ANP The substance contains 16.27% of Ketamine QOOCT8 + ANP Sample 2014/1/SM-2 was found to contain Ketamine. QTTSCI + ANP Examination of the powder SM-3 revealed the presence of controlled drug Ketamine RJXPPP + ANP

RV9IZA + ANP

RXKBFM + +

S4B5OL + + The test sample 2014/1/SM-3 was analysed by colour test and Thin layer Chromatography (TLC) techniques and found to contain Ketamine and Lactose. SAZ3ZW + - De acuerdo a los análisis realizados se concluye que se trata Ketamina SF9898 + + Ketamine was identified by TLC and GC/MS SGDY90 + -

SUOIOI + ANP ,PDGHWKHFKHPLFDODQGLQVWUXPHQWDODQDO\VLVLWUHVXOWHGWKDWWKHVDPSOHFRQWDLQVNHWDPLQH TIILNU + + Also contain Lactose TLVU3E + + The sample SM3 contained 16.8 % ketamine calculated as a base. In the sample was identified lactose. U54UUY - + The sample tested positive for Lactose using TLC with two (2) solvent systems. The sample could have been an adulterant used in seized materials (SM). UIIF4G + +

ULQHBK + - 2014/1/SM-3 contains Ketamine.

67 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Ketamine Lactose ULXUTD + - lactose V3BKMA + ANP

V43UFL + + lactose VGVOLX + + CT reagent: positive. GC/MS: Retention time, mass-charge (M/Z) similar characteristics with the substances used as standar or pattern. FTIR: Absorption bands conicident with the substances used as pattern VJMKCE + + A white powder containing KETAMINE VLJXIU + + Was found too LACTOSE VLLLV0 + ANP

VMHH2Y + +

VXXFXK + + lactose VZSIJV + ANP ketamine is controlled (KB 22/01/1998) W33NYG + ANP Analyzing the results obtained by the three tests cited above we have come to the conclusion that we are in the presence of a drug bids the KETAMINE. XFPUFJ + ANP

XGELS2 + +

XH2D7F + + Illegal substances on the basis of the italian law DPR 309/90 XL5KA0 + + Presence of ketamine hydrochloride and lactose was detected in the sample. XMAYN4 + + *Retention time and fragmentation patterns obtained with sample are equivalent to those obtained with ketamine. *Spectroscopic parameters obtained with sample are equivalent to those obtained with lactose. XVDW7X + ANP The sample SM-3 contains ketamine, which is included in List C1 (List of other substances under special control) of Annex I of SVS / MS 344, May 12, 1998. YCYBYW + -

YVAVK8 + + lactose YWZYAR + + lactose YYDEDD + -

Z154TB + + The sample contain lactose

68 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Ketamine Lactose Z8YS9F + ANP

ZM99S9 + ANP The sample obtains with the positive result with Marquis reagent. TLC : The Rf sample obtain with the same Rf Ketamine standard. GC: The Rt sample obtain with the same Rt Ketamine standard. ZZKXPP + ANP CONFIRMED BY GC MS

69 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Identification methods for Test Sample 3

Legend: S ... used for Screening I ... used for Identification SI ... used for both

70 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

71 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

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73 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary for test sample 3 The response summary of all 151 participating laboratories for the identification of SM-3, frequency of use of screening and identification techniques and false positives and negatives: Identification of test sample 3:

Response Summary

Participants: 151

Ketamine: 147

False positives for Test Sample 3

Code Name Technique PF5IJN Cocaine 180/190 H4TJQT Chlormezanone 1 5 0/1 60/161/180

False negatives for SM-3 (techinque(s) used or ANP)

Code: U54UUY (150/161), 5WSWTT (ANP), G222HF (ANP)

Frequency of use of screening and identification techniques:

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Z-Scores for Test Sample 3

Ketamine Ketamine Deviation Deviation Code Concentration Code Concentration from robust z-score from robust z-score (mass%) (mass%) average average 0J0PYS 16.6 0.1 0.0 HYRH0O 20.2 3.7 2.1 0LN2QE 15.6 -0.9 -0.5 I9MZ11 20.3 3.8 2.1 1SAEBM 16.3 -0.2 -0.1 IJ37J2 16.0 -0.5 -0.3 20LMZF 14.7 -1.8 -1.0 IM8WG1 14.7 -1.8 -1.0 28YACH 17.0 0.5 0.3 IOP7DS 15.5 -1.0 -0.6 2H9171 16.3 -0.2 -0.1 IRIBPI 14.4 -2.1 -1.2 3MGTTL 20.9 4.4 2.5 IT3XHS 9.2 -7.3 -4.2 3UMO3Y 16.3 -0.2 -0.1 J1X7S4 16.7 0.2 0.1 3V0OFD 15.1 -1.4 -0.8 KN4PSK 16.5 0.0 0.0 555YH5 6.9 -9.6 -5.5 LYWXR6 14.7 -1.8 -1.0 5ZW2N9 19.1 2.6 1.5 MRWDWG 17.1 0.6 0.3 6306WG 14.4 -2.1 -1.2 NHY1ZE 9.0 -7.5 -4.3 7K1RKK 14.0 -2.5 -1.4 NNBNTN 15.9 -0.6 -0.4 7WPIJX 21.0 4.5 2.5 NSJNGB 16.8 0.3 0.2 888Z8S 22.5 6.0 3.4 OGLNKI 15.8 -0.7 -0.4 8GORYY 18.0 1.5 0.8 OLLRLR 17.8 1.3 0.7 8SVPRT 15.2 -1.3 -0.8 PF5IJN 10.7 -5.8 -3.3 8YSG8M 21.3 4.8 2.7 Q8ECTW 16.9 0.4 0.2 8ZZZO7 18.0 1.5 0.8 QIEBZB 16.3 -0.2 -0.1 AGNIZI 17.0 0.5 0.3 QOOCT8 16.0 -0.5 -0.3 BPLP0L 15.4 -1.1 -0.6 RJXPPP 17.0 0.5 0.3 DFCXDG 17.5 1.0 0.5 SF9898 12.9 -3.6 -2.1 DLDLOB 15.8 -0.7 -0.4 SGDY90 15.0 -1.5 -0.9 DNKLDD 15.9 -0.6 -0.4 TLVU3E 16.2 -0.3 -0.2 DQEDDN 9.4 -7.1 -4.1 ULXUTD 16.5 0.0 0.0 DQMISD 17.0 0.5 0.3 V3BKMA 17.0 0.5 0.3 EDRLTN 14.6 -1.9 -1.1 VZSIJV 16.6 0.1 0.0 EMZZIW 20.0 3.5 2.0 XH2D7F 21.0 4.5 2.5 ET1YHT 17.8 1.3 0.7 XL5KA0 16.9 0.4 0.2 FIKSPK 24.0 7.5 4.2 XVDW7X 18.8 2.3 1.3 FO8JOE 16.7 0.2 0.1 YWZYAR 27.0 10.5 5.9 GEZZ2P 31.4 14.9 8.4 YYDEDD 17.1 0.6 0.3 H74EH5 16.0 -0.5 -0.3 Z8YS9F 16.3 -0.2 -0.1 HCW3AW 15.6 -0.9 -0.5 ZM99S9 19.7 3.2 1.8 HCZG6T 16.0 -0.5 -0.3

75 Z-Score Report per Sample per Substance

Round: 2014/1 Substance: SM-3/Ketamine

.Robust average = 16.5 UNODC value = 16.1

4.0 3.4

3.0 2.7 2.5 2.5 2.5 2.1 2.1 2.0

2.0 1.8 1.5 1.3 0.8 0.8

1.0 0.7 0.7 0.5 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.2 0.2 0.2 0.1 0.1 0.0 0.0 4.2 5.5 4.3 ‐ 4.1 ‐ ‐ 0.0 ‐ 5.9 8..4 4.2 0.0 0.0 0.1 0.1 0.1 0.1 0.1 ‐ 0.2 ‐ ‐ ‐ ‐ ‐ 0.3 0.3 0.3 0.3 0.4 0.4 ‐ ‐ ‐ ‐ 0.4 0.4 ‐ ‐ ‐ ‐ 0.5 0.5 0.6 ‐ ‐

‐1.0 0.6 ‐ ‐ 0.8 0.8 ‐ 0.9 ‐ ‐ 1.0 1.0 1.0 1.1 ‐ ‐ ‐ ‐ 1.2 1.2 ‐ ‐ 1.4 ‐2.0 ‐ 2.1 ‐

‐3.0 3.3 ‐ ‐4.0 IRIBPI IJ37J2 VZSIJV PF5IJN FIKSPK 0J0PYS J1X7S4 AGNIZI IT3XHS Z8YS9F BPLP0L SF9898 RJXPPP 888Z8S QIEBZB 7WPIJX IOP7DS OLLRLR XL5KA0 8SVPRT ET1YHT 8ZZZO7 GEZZ2P FO8JOE I9MZ11 7K1RKK TLVU3E OGLNKI 555YH5 2H9171 KN4PSK EDRLTN NHY1ZE 20LMZF SGDY90 0LN2QE 28YACH XH2D7F HCZG6T H74EH5 NSJNGB DLDLOB 3V0OFD 8GORYY YYDEDD ZM99S9 ULXUTD LYWXR6 DFCXDG 3MGTTL DNKLDD 1SAEBM EMZZIW HYRH0O 8YSG8M YWZYAR DQMISD QOOCT8 5ZW2N9 6306WG V3BKMA Q8ECTW NNBNTN XVDW7X IM8WG1 DQEDDN 3UMO3Y HCW3AW MRWDWG

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Sample 4 Analysis

Identified substances for Test Sample 4

Code Identified Substances 0J0PYS cocaine 0LN2QE Cocaine 0N05YR Cocaine 0RE0L0 cocaine 1SAEBM cocaine 20LMZF Cocaine 28YACH Cocaine 33HOOD Cocaine 3BY3P6 Cocaine 3MGTTL cocaine 3RV3F7 cocaine 3UMO3Y cocaine 3V0OFD cocaine 4FA8F0 Cocaine 555YH5 Cocaine 5V22WM Cocaine Hydrochloride 5WSWTT cocaine. 5ZW2N9 cocaine 6306WG cocaine 666F66 cocaine 7FH7HV Cocaïne et MDMA 7K1RKK Cocaine 7WPIJX cocaine 888Z8S Cocaine 8GORYY Cocaine 8SVPRT Cocaine 8YSG8M cocaine 8ZZZO7 cocaine A3AH32 Cocaina AEE5WA Cocaine AGNIZI cocaine AIPPIG Cocaine AJ22ZI cocaine AKJ5JY Cocaine ANHVML Cocaine BLZZMB cocaine BPLP0L cocaine C9TTRY cocaine CWGDML Cocaine hydrochloride CWLQJ1 Cocaine

77 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances CZV766 Cocaine D5BVEI Cocaine D8DHQW Cocaine DFCXDG Cocaine DLDLOB Cocaine DNKLDD Cocaine DQMISD cocaine DYEYYG Cocaine EBQAXY Cocaïne EDRLTN Cocaine ELN44T Cocaine EMZZIW cocaine ET1YHT Cocaine FFFAFF cocaine FIKSPK Cocaine FL6M38 Cocaine FO8JOE cocaine GCGWXG Cocaine hydrochloride GEZZ2P Cocaine GK8FTC cocaine H74EH5 Cocaine hcl HCW3AW Cocaine HCl HCZG6T Cocaine HYEPEU Cocaine HYRH0O Cocaine I3W3SW COCAINE I9MZ11 Cocaine IJ37J2 Cocaine IM8WG1 Cocaine IMEQDK Cocaine IOP7DS Cocaine IRIBPI cocaine IT3XHS cocaine J1X7S4 Cocaine HCl JA3JJQ Cocaine JIRDRI Cocaine K2D2PO cocaine KEANRN Cocaine KGJIJS COCAINE KN4PSK Cocaine KPAKKD Cocaine KX18KO Cocaine Hydrochloride KYGWUS Cocaine LG45WT Cocaine

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Code Identified Substances LLLSLL cocaine HCl LYWXR6 Cocaine M1Q1F5 Cocaine MJHGVG COCAIN MRWDWG cocaine NBI4J4 cocaine NHY1ZE Cocaine NNBNTN cocaine hydrochloride NSJNGB Cocaine NU06C7 Cocaine 76,8% NVENEN Cocaine O2WSYF cocaine OGLNKI Cocaine OLLRLR cocaine ORHNDM cocaine chlorhydrate OW2RIV Cocaine PF5IJN COCAÍNA PIRHNH cocaine PPHBGP COCAÍNE PSQS7F COCAINE Q11YO1 cocaine Q8ECTW cocaine QIEBZB Cocaine QOOCT8 Cocaine QTTSCI Cocaine RJXPPP Cocaine RV9IZA Cocaine RXKBFM cocaina S4B5OL Cocaine SAZ3ZW Cocaína clorhidrato SF9898 Cocaine SUOIOI Cocaine TIILNU Cocaine TLVU3E Cocaine U54UUY COCAINE UIIF4G Cocaina ULQHBK Cocaine ULXUTD cocaine V3BKMA Cocaine V43UFL cocaine, HCl VGVOLX Cocaine VJMKCE Cocaine Hydrochloride VLJXIU COCAINE VLLLV0 cocaina

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Code Identified Substances VMHH2Y Cocaine VXXFXK cocaine VZSIJV cocaine W33NYG Cocaine XFPUFJ cocaine XGELS2 Cocaïne XH2D7F cocaine XL5KA0 Cocaine XMAYN4 cocaine XVDW7X Cocaine YCYBYW Cocaine YVAVK8 cocaine YWZYAR cocaine YYDEDD Cocaine Z154TB cocaine Z8YS9F Cocaine ZM99S9 Cocaine ZZKXPP COCAINE

80 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Statement of findings for Test Sample 4

Code Cocaine 0J0PYS + Sample four contains cocaine,HCL (83.5% as base) 0LN2QE + Contained cocaine and cinnamoylcocaine, methylecgonine, methylecgonidine 0N05YR + Different procedures were performed to the sample. Starting with colorimetric reactions, after confirmation instrumental analysis using GC-MS and GC-FID. Finally simple was quantified using GC-FID 0RE0L0 + The sample contains cocaine which is scheduled as illicit drug in France. 1SAEBM + Sample contains 78.9± 3.2 % (w/w) cocaine base in HCL salt form. 20LMZF + One glass bottle containing 0.22 grammes of a solid containing 0.17 grammes of cocaine. 28YACH + Cocaine existed in salt form. Were found Ergonine-methyl-ester and Benzoylergonine in the sample. 2H9171 +

33HOOD + Based on the above analysis, the sample was found to contain cocaine. 3BY3P6 + White substance contains Cocaine 3MGTTL +

3RV3F7 + in the sample is cocaine who is on the list of drugs in Montenegro 3UMO3Y + white powder, also contain typical "natural" impurities, ethyl benzoate, ecgonidine methylester ecgonine methylester, norcocaine and cinnamoylcocaine (cis and trans isomers) 3V0OFD + white powder containing 72.0% cocaine 4FA8F0 + Cocaine, caffeine 555YH5 +

5V22WM + The powder was analysed and found to contain Cociane Hydrochloride. 5WSWTT + after chemical analysis was performed, the sample was found to contain89.5 cocaine. 5ZW2N9 + cocaine was detected by GC/MS screening and it was confirmed and quantified by GC-FID using calibration curve 6306WG +

666F66 + cocaine

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Code Cocaine 7FH7HV + Après analyse, l'échantillon 2014/1/SM-4 contient de la cocaïne et du MDMA 7K1RKK + A sample of the powder was analysed and found to contain Cocaine at a concentration of 79%, which is a class A controlled substance under the Misuse of Drugs Act 1971 7WPIJX +

888Z8S + On analysis, I found the substance to contain Cocaine. 8GORYY + The sample contains cocaine which is listed as a controlled drug according to french order, appendix I of February 22nd 1990. 8SVPRT + The result of TLC and IR of test sample was same as cocaine 8YSG8M + found cocaine with 78.3%w/w 8ZZZO7 + On analysis, I found the sustances to contain 75.23% (by weight) of cocaine A3AH32 + Cocaina AEE5WA +

AGNIZI + mixture of cocaine and lactose AIPPIG + Off-white powder containing cocaine. AJ22ZI + The sample was found to contain cocaine AKJ5JY + Sample 2014/1/SM-4, a white powder with acrid odour, gave a positive result for Cocaine, a controlled substance under national legislation on drugs. ANHVML + Off-white powder containing an average of 81% cocaine. Cocaine is a Class A controlled drug under the provisions of the Misuse of Drugs Act 1971 (as amended). BLZZMB +

BPLP0L + This sample is cocaine. C9TTRY +

CWGDML +

CWLQJ1 + The chemical tests and the coincidence in the time of retention and mass fragmentogram with the material reference used in the same conditions that the analyzed sample, they indicates in this one the cocaine's presence. CZV766 + The white powder contains Cocaine. D5BVEI + Powder containing cocaine

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Code Cocaine D8DHQW + Cocaine, a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. DFCXDG + The sample contains cocaine 66.34 %, m/m. DLDLOB + narcotics: cocaine concentration: approx 73 % as free base DNKLDD +

DQEDDN +

DQMISD + powder with 80,8 % of cocaine DYEYYG + Cocaine EBQAXY + The sample 2014/1/SM-4 contains 78% of cocaïne base. Cocaïne is a controlled substance in France EDRLTN + The exhibit item was found to contain Cocaine ELN44T + On analysis, I found the sample to contain cocaine EMZZIW +

ET1YHT + 84.4 % Cocaine FFFAFF + White powder that contains substance under control - cocaine. FIKSPK + It has been detecded that tehe subject of study including White colour dust substance was Cocaine. This is a drug which is under the terms of national sunstance of drug Law 2313. FL6M38 + polvo blanco is cocaine FO8JOE + Retention time and MS spectra in GC analysis (FID and MS) compared with ICE reference material. Cocaine as hydrochloride. G222HF +

GCGWXG + Cocaine is a Class A controlled drug subject to the provisions of the Misuse of Drugs Act 1971. GEZZ2P +

GK8FTC +

H4TJQT + benzoic acid - ecgonine methylester-benzoylecgonine H74EH5 + Base Cocaine 77,0%

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Code Cocaine HCW3AW + Negative with Marquis and Simon. Positive with Cobalt thiocyanate. Silver Nitrate Test--> Chloride Positive. TLC(TA,TE), GCMS --> Cocaine confirmed. GC--> Cocaine base 74.83% HCZG6T + The sample was found to contain 77.4% of cocaine (as base). HYEPEU + The powder is a narcotic substance - cocaine powder. The powder contains 80.0 % pure cocaine (base form). HYRH0O + Cocaine, Methylecgonine I3W3SW + COCAINE IS PRESENT IN HYDROCHLORIDE FORM. OTHER COCA PRODUCTS WERE IDENTIFIED. I9MZ11 + SM-4 contained Cocaine IJ37J2 + In the test sample 2014/1/SM-4 was detected Cocaine IM8WG1 +

IMEQDK +

IOP7DS + The sample contains cocaine (74.3%). IRIBPI + We also found traces of methylecgonine, cinnamoyl cocaine, benzoylecgonine and norcocaine IT3XHS + Blue color in cobalt thiocyanate test indicates possible presence of cocaine.Rf anf colour in TLC of std Cocaine equal to those of SM4.Retention Time(RT16.4) and base Peaks of SM4( )82are mostly identical to std Cocaine and library search in GCMS also indicates SM4 being Cocaine. J1X7S4 +

JA3JJQ + Cocaine JIRDRI + Cocaine positive K2D2PO +

KEANRN + In the tested sample was detected and confirmed the presence of Cocaine KGJIJS + SIGN IN COCAINE labeled 2014/1/SM-2 DETECTED. KN4PSK + contained cocaine and trace of methylecgonine, methylecgonidine, cinnamoilcocaine

KPAKKD + The sample contains Cocaine KX18KO + White powder containing Cocaine which is a class A controlled drug with a purity of 79% (as base) under the provisions of the Misuse of Drugs Act 1971 (as amended).

84 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Cocaine KYGWUS + 0.232 grams of off-white powder found to contain Cocaine at a concentration of 77%. Cocaine is controlled by the Misuse of Drugs Act 1971 (as amended) as a Class A drug. LG45WT + The sample has 94.9% cocaine chloride, or 84.8% cociane base LLLSLL +

LYWXR6 +

M1Q1F5 + The sample contain controlled drug cocaine MJHGVG + hydrochloride form MRWDWG + white powder containing 74.7%m/m of cocaine NBI4J4 +

NHY1ZE + SM4 was contain CNS stimulant (Cocaine). NNBNTN + Cocaine hydrochloride confirmed in one unit tested of one unit received. NSJNGB + Cocaine NU06C7 +

NVENEN + The Sample 2014/1/SM3 was found to contain Cocaine. O2WSYF + The sample is identified as cocaine. OGLNKI + contained cocaine and trace of methylecgonine, methylecgonidine, cinnamoilcocaine OLLRLR + the white powder contains cocaine (72.9%w/w), which is controlled bt national law ORHNDM + cocaine ,substance classée stupéfiant OW2RIV + Sample containing cocaine PF5IJN ANP MARQUIS, SCOTT, SIMON´S, SE ANALIZO Y CUANTIFICO POR UV HPLC, GC-MS, FT-IR, HPLC PIRHNH +

PPHBGP + The results of the tests of the SM4 () received confirmed that the mentioned sample contains COCAÍNE with 48.7 percentage by weight (48.7%) PSQS7F + The simple No 2014/1/SM-2 was found COCAINE

85 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Cocaine Q11YO1 + white powder containing 75%w/w of cocaine Q8ECTW + the powder is cocaine.HCl with a concentration of cocaine as base in the sample of 77.3% QIEBZB + The substance contains 79.39% of Cocaine QOOCT8 + Sample 2014/1/SM-2 was found to contain Cocaine. QTTSCI + Examination of the powder SM-4 revealed the presence of controlled drug cocaine RJXPPP +

RV9IZA +

RXKBFM +

S4B5OL + The test sample 2014/1/SM-4 was analysed by colour test and Thin layer Chromatography (TLC) techniques and found to contain Cocaine. SAZ3ZW + De acuerdo a los análisis realizados se concluye que se trata cocaína clorhidrato SF9898 + Cocaine was identified by TLC and GC/MS SGDY90 +

SUOIOI + PDGHWKHFKHPLFDODQGLQVWUXPHQWDODQDO\VLVLWUHVXOWHGWKDWWKHVDPSOHFRQWDLQV&RFDLQH TIILNU + The sample contains 78.9 % ± 5.7 % of Cocaine TLVU3E + The sample SM4 contained 77.8 % cocaine calculated as a base. U54UUY + Field test employing the Cobalt Thiocynate Test was positive result because the spot turned blue. TLC analysis using two(2) solvents systems and HPLC confirmed the sample as COCAINE with purity 80.23%. UIIF4G +

ULQHBK + 2014/1/SM-4 contains Cocaine. ULXUTD +

V3BKMA +

V43UFL +

VGVOLX + CT reagent: positive. GC/MS: Retention time, mass-charge (M/Z) similar characteristics with the substances used as standar or pattern. FTIR: Absorption bands conicident with the substances used as pattern

86 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Cocaine VJMKCE + A white powder containing an average of 87% of COCAINE HYDROCHLORIDE. VLJXIU +

VLLLV0 +

VMHH2Y +

VXXFXK +

VZSIJV + cocaine is controlled (KB 31/12/1930 changed by KB 8/10/1963) W33NYG + In this sample the three tests conducted have shown that we are in the presence of COCAINE. XFPUFJ +

XGELS2 +

XH2D7F + Illegal substances on the basis of the italian law DPR 309/90 XL5KA0 + Presence of cocaine hydrochloride was detected in the sample.The seizure also contained trace amount of cinnamoylcocaine, benzoic acid, benzoylecgonine,ecgonine methyl estar. XMAYN4 + *Results of screening tests were positive for cocaine. *Retention time and fragmentation pattern obtained with sample are equivalent to cocaine. XVDW7X + The sample SM-4 contains cocaine, which is included in List F1 (List of narcotic substances banned in Brazil) of Annex I of SVS / MS 344, May 12, 1998. YCYBYW +

YVAVK8 +

YWZYAR +

YYDEDD + Sample also contains benzoyl ecgonine, cis-cinnamoylcocaine, trans-cinnamoylcocaine Z154TB +

Z8YS9F +

ZM99S9 + The sample obtains with the positive result with Cobalt thiocyanate reagent. TLC : The Rf sample obtain with the same Rf Cocaine standard. GC: The Rt sample obtain with the same Rt Cocaine standard. ZZKXPP + CONFIRMED BY GC/MS

87 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Identification methods for Test Sample 4

Legend: S ... used for Screening I ... used for Identification SI ... used for both

88 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

89 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

90 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

91 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary for test sample 4 The response summary of all 151 participating laboratories for the identification of SM-4, frequency of use of screening and identification techniques and false positives and negatives: Identification of test sample 4:

Response Summary Participants: 151

Cocaine: 150

False positives for Test Sample 4

Code Name Technique 7FH7HV MDMA 150

False negatives for SM-4 (controlled substances) (techinque(s) used or ANP)

Code: PF5IJN (ANP)

Frequency of use of screening and identification techniques:

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Z-Scores for Test Sample 4

Cocaine Cocaine Deviation Code Concentration Deviation from Code Concentration z-score from robust z-score (mass%) robust average (mass%) average 0J0PYS 83.5 5.5 1.3 HYEPEU 80.0 2.0 0.5 0LN2QE 78.1 0.1 0.0 HYRH0O 93.5 15.5 3.6 0N05YR 88.0 10.0 2.4 I3W3SW 80.6 2.6 0.6 0RE0L0 71.0 -7.0 -1.6 IJ37J2 81.0 3.0 0.7 1SAEBM 78.9 0.9 0.2 IM8WG1 80.7 2.7 0.6 20LMZF 76.4 -1.6 -0.4 IMEQDK 81.7 3.7 0.9 28YACH 85.5 7.5 1.8 IOP7DS 74.3 -3.7 -0.9 2H9171 73.6 -4.4 -1.0 IRIBPI 78.0 0.0 0.0 3MGTTL 78.2 0.2 0.0 IT3XHS 92.7 14.7 3.5 3UMO3Y 77.3 -0.7 -0.2 J1X7S4 81.9 3.9 0.9 3V0OFD 72.0 -6.0 -1.4 JA3JJQ 74.9 -3.1 -0.7 555YH5 61.8 -16.2 -3.8 K2D2PO 81.8 3.8 0.9 5WSWTT 89.5 11.5 2.7 KN4PSK 76.7 -1.3 -0.3 5ZW2N9 68.0 -10.0 -2.3 KX18KO 79.0 1.0 0.2 6306WG 79.8 1.8 0.4 KYGWUS 77.0 -1.0 -0.2 666F66 72.0 -6.0 -1.4 LG45WT 84.8 6.8 1.6 7K1RKK 79.0 1.0 0.2 LLLSLL 80.0 2.0 0.5 7WPIJX 78.0 0.0 0.0 LYWXR6 79.2 1.2 0.3 8GORYY 77.6 -0.4 -0.1 MJHGVG 79.4 1.4 0.3 8SVPRT 66.6 -11.4 -2.7 MRWDWG 74.7 -3.3 -0.8 8YSG8M 78.3 0.3 0.1 NHY1ZE 10.4 -67.6 -15.9 8ZZZO7 75.2 -2.8 -0.7 NNBNTN 79.2 1.2 0.3 AEE5WA 72.0 -6.0 -1.4 NSJNGB 78.9 0.9 0.2 AGNIZI 68.7 -9.3 -2.2 NU06C7 76.8 -1.2 -0.3 AIPPIG 72.0 -6.0 -1.4 OGLNKI 77.3 -0.7 -0.2 ANHVML 81.0 3.0 0.7 OLLRLR 72.9 -5.1 -1.2 BPLP0L 83.7 5.7 1.3 ORHNDM 78.0 0.0 0.0 C9TTRY 82.0 4.0 0.9 PF5IJN 88.5 10.5 2.5 CWGDML 80.0 2.0 0.5 PPHBGP 48.7 -29.3 -6.9 D5BVEI 76.6 -1.4 -0.3 Q11YO1 75.5 -2.5 -0.6 DFCXDG 66.3 -11.7 -2.7 Q8ECTW 77.3 -0.7 -0.2 DLDLOB 72.7 -5.3 -1.2 QIEBZB 79.4 1.4 0.3 DNKLDD 77.0 -1.0 -0.2 QOOCT8 77.0 -1.0 -0.2 DQEDDN 76.8 -1.2 -0.3 QTTSCI 73.0 -5.0 -1.2 DQMISD 80.8 2.8 0.7 RJXPPP 88.0 10.0 2.4 DYEYYG 78.3 0.3 0.1 RXKBFM 76.7 -1.3 -0.3 EBQAXY 78.0 0.0 0.0 SF9898 78.4 0.4 0.1 ELN44T 75.9 -2.1 -0.5 SGDY90 70.0 -8.0 -1.9 EMZZIW 35.0 -43.0 -10.1 TIILNU 78.9 0.9 0.2 ET1YHT 84.4 6.4 1.5 TLVU3E 77.8 -0.2 0.0 FIKSPK 73.0 -5.0 -1.2 U54UUY 80.2 2.2 0.5 FL6M38 78.0 0.0 0.0 ULXUTD 76.8 -1.2 -0.3 FO8JOE 79.1 1.1 0.3 V3BKMA 76.0 -2.0 -0.5 GCGWXG 84.0 6.0 1.4 V43UFL 80.0 2.0 0.5 GEZZ2P 100.0 22.0 5.2 VJMKCE 78.0 0.0 0.0 H74EH5 77.0 -1.0 -0.2 VLJXIU 77.0 -1.0 -0.2 HCW3AW 74.8 -3.2 -0.7 VLLLV0 84.9 6.9 1.6 HCZG6T 77.4 -0.6 -0.1 VMHH2Y 72.0 -6.0 -1.4

93 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Cocaine Deviation Code Concentration from robust z-score (mass%) average VZSIJV 81.1 3.1 0.7 XGELS2 80.3 2.3 0.5 XH2D7F 80.5 2.5 0.6 XL5KA0 81.6 3.6 0.8 XVDW7X 60.0 -18.0 -4.2 YCYBYW 90.5 12.5 2.9 YWZYAR 80.0 2.0 0.5 YYDEDD 80.3 2.3 0.5 Z8YS9F 79.5 1.5 0.4 ZM99S9 93.1 15.1 3.6 ZZKXPP 70.0 -8.0 -1.9

94 Z-Score Report per Sample per Substance

Round: 2014/1 Substance: SM-4/Cocaine Robust average = 78.0 UNODC value = 75.8

4.0 3.6 3.6 3.5

3.0 2.9 2.7 2.5 2.4 2.4

2.0 1.8 1.6 1.6 1.5 1.4 1.3 1.3 0.9 0.9 0.9 0.9 1.0 0.8 0.7 0.7 0.7 0.7 0.6 0.6 0.6 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 3 0.4 0.4 0.3 0. 0.3 0.3 0.3 0.2 0.2 0.2 0.2 0.2 0.1 0.1 0.1 15.9 0.0 6.9 0.0 ‐ 0.0 0.0 0.0 0.0 ‐ 4.2 10.1 ‐ 0.0 ‐ 5.2 0.0 0.0 0.0 0.1 0.1 ‐ 0.2 0.2 0.2 ‐ ‐ ‐ ‐ 0.2 0.2 0.2 0.2 0.2 0.3 0.3 0.3 ‐ ‐ ‐ ‐ ‐ 0.3 0.3 0.3 ‐ ‐ ‐ ‐ ‐ 0.4 ‐ ‐ 0.5 0.5 ‐ ‐ 0.6 ‐ 0.7 ‐

‐1.0 0.7 0.7 0.8 ‐ ‐ ‐ 0.9 ‐ 1.0 ‐ 1.2 1.2 1.2 ‐ ‐ 1.2 ‐ ‐ 1.4 1.4 1.4 1.4 1.4 ‐ ‐ ‐ ‐ ‐ 1.6

‐2.0 ‐ 1.9 1.9 ‐ ‐ 2.2 ‐ 2.3 ‐

‐3.0 2.7 ‐ 2.7 ‐

‐4.0 3.8 ‐ 99S9 IRIBPI IJ37J2 LLLSLL VZSIJV TIILNU JA3JJQ PF5IJN VLJXIU FIKSPK AIPPIG J1X7S4 0J0PYS AGNIZI IT3XHS Z8YS9F QTTSCI VLLLV0 BPLP0L RJXPPP QIEBZB SF9898 666F66 0RE0L0 D5BVEI 7WPIJX ZZKXPP OLLRLR IOP7DS XGELS2 XL5KA0 C9TTRY ELN44T ET1YHT 8SVPRT 8ZZZO7 GEZZ2P 7K1RKK FO8JOE V43UFL TLVU3E 555YH5 OGLNKI 2H9171 KN4PSK DYEYYG 0N05YR SGDY90 20LMZF 0LN2QE NSJNGB KX18KO XH2D7F 28YACH NHY1ZE HYEPEU FL6M38 H74EH5 HCZG6T EBQAXY VJMKCE DLDLOB YYDEDD ZM 3V0OFD 8GORYY Q11YO1 K2D2PO ULXUTD NU06C7 LYWXR6 PPHBGP 3MGTTL DFCXDG IMEQDK 1SAEBM U54UUY LG45WT YCYBYW EMZZIW RXKBFM DNKLDD 8YSG8M YWZYAR HYRH0O DQMISD I3W3SW 5ZW2N9 AEE5WA QOOCT8 6306WG V3BKMA Q8ECTW NNBNTN XVDW7X MJHGVG IM8WG1 KYGWUS VMHH2Y DQEDDN 3UMO3Y ANHVML 5WSWTT GCGWXG CWGDML ORHNDM HCW3AW MRWDWG

95 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

The Laboratory and Scientific Section UNODC, International Centre Wagramer Strasse 5, P.O. Box 500 A-1400, Vienna, AUSTRIA Email: [email protected]