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INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary Report

SEIZED MATERIALS 2013/1 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Table of contents Introduction Page 3 Comments from the International Panel of Forensic Experts Page 3 Codes and Abbreviations Page 5 Sample 1 Analysis Page 6 Identified substances Page 6 Statement of findings Page 10 Identification methods Page 19 Summary Page 23 Z-Scores Page 24 Sample 2 Analysis Page 27 Identified substances Page 27 Statement of findings Page 30 Identification methods Page 38 Summary Page 42 Z-Scores Page 43 Sample 3 Analysis Page 45 Identified substances Page 45 Statement of findings Page 48 Identification methods Page 56 Summary Page 60 Z-Scores Page 61 Sample 4 Analysis Page 63 Identified substances Page 63 Statement of findings Page 66 Identification methods Page 74 Summary Page 78 Z-Scores Page 79 Test Samples Information

Samples Comments on samples Sample 1 SM-1 was prepared from a seizure containing 47.9% base. The seizure also contained 6- monoacetylmorphine, acetylcodeine, , , dextrometorphan and . Trace amounts of and could also be detected Sample 2 SM-2 was prepared from a seizure containing 68.7% Morphine base. The seizure also contained codeine and trace amounts of 6-monoacetylmorphine and heroin.

Sample 3 SM-3 was prepared from a seizure containing 3.7% . The seizure also contained lactose and glucose

Sample 4 SM-4 was prepared from a seizure containing 10.3% Amfetamine base. The seizure also contained sucrose and trace amounts of and diphenylisopropylamine

Samples Substances from the ICE Menu Concentrations Comments on substances Sample 1 Heroin 47.9 % Caffeine N/A Sample 2 Morphine 68.7 % Sample 3 Lactose N/A Nimetazepam 3.7 % Sample 4 Amfetamine 10.3 %

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.

2013/1-SM (2) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

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 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.

Comments from the International Panel of Forensic Experts

Participation of Laboratories

Samples within both the Seized materials (SM) and Biological Specimens (BS) test groups were sent to 165 laboratories in 57 countries. Within the SM test group, samples were sent to 139 laboratories and 132 laboratories (95%) submitted the results of their analysis in time for inclusion in the summary report, with 128 (97%) using the ICE portal for return of results. The almost universal usage of the ICE portal is a high endorsement of its utility. Some laboratories had difficulty in obtaining import authorization particularly for the new psychoactive substances included in the ICE menu and this resulted in an extension of the deadline for submission of results. It is hoped that these delays will be decreased in the future as both participants and competent authorities become more familiar with the international import/export requirements for these emerging substances.

Qualitative Analysis

The results for the qualitative identification of the controlled substances were good for all test samples in the SM group. In particular, with correct identification of the heroin in SM-1 and the morphine in SM-2 by 100% and 95% of participants respectively. SM-3 containing nimetazepam and SM-4 containing were identified by 91% and 94% of participants respectively. Some 89.4% of participants overall used GC- MS for the qualitative analysis indicating access to this technique which is one of the most commonly used tandem techniques for the confirmation of controlled substances. It is encouraging to note that only six false positive results for controlled substances within the ICE menu were reported for the four test samples in the SM group, while there were a total of 24 false negative results. The seizure used for SM-1 contained at least nine components and 35 laboratories identified the trace amounts of morphine present. Participants who identified the morphine may have in error received a false positive result upon submission of results via the portal. As the amount of morphine present was low, those laboratories who did not identify it need not consider the result a false negative. For SM-4, five laboratories using GC/MS also identified trace amounts of methamphetamine present and similarly, this result need not be considered a false positive. The detection limits of the different analytical techniques shall be taken into consideration when ascribing false positive results in future ICE rounds.

Quantitative Analysis

A modified Z-score was used for the statistical examination of the quantitative results, as it is a robust method based on absolute deviations from the median of all participant values and is relatively insensitive to outliers. The proportion of participants who carried out quantitative analysis, 90 (68%) for SM-1, 54 (41%) for SM-2, 41 (31%) for SM-3 and 76 (58%) for SM-4 continues to be encouraging. The percentages of laboratories performing quantitative analysis for heroin has remained stable at 68% for ICE 2012/1, 70% for ICE 2012/2 and 68% for this current round. The percentages of laboratories performing quantitative analysis for morphine is also stable at 46% for ICE 2011/1 and 41% for the current round. Similarly, the percentages of laboratories performing quantitative analysis for amphetamine are comparable with 59% for

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both ICE 2011/2 and 2012/1, and 58% for the current round. Nimetazepam is a new substance on the ICE menu for this current round and it is encouraging to see 31% of laboratory already performing quantitative analysis for this drug. It is understood that quantitative analysis of controlled substances is often governed by local legislation and the prosecution requirements. Analysis of the Z-scores showed that 77 out of 90 (86%) of participants provided acceptable quantitative results with Z-scores within 3.5 for heroin in SM-1, 52 out of 54 (96%) for morphine in SM-2, 32 of 41 (78%) laboratories for nimetazepam in SM-3 and 68 of 76 (87%) for the amphetamine in SM-4. Participants with Z- scores outside acceptable limits should review their quantification procedures. 69% of participants in this round quantified at least one test sample and 30% quantified all four test samples. Z-score values obtained from quantitative analysis assist participating laboratories in evaluating their performance and Z-scores should be monitored over time as part of each laboratory’s quality assurance programme.

(4) 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 (sulphuric acid, ) 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

2013/1-SM (5) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Sample 1 Analysis

Identified substances for Test Sample 1 Code Identified Substances 00H0DT heroin 0DAKSM Heroin 0SRDXD heroin 0T0BVS HEROINA 1HR18P Heroin, 6-Monoacetylmorphine, acetylcodeine 1R7FTA Heroin and Monoacetylmorphines 1SWNJJ heroin, caffeine 22JWSL Heroine 2ACHVO 2FELET Heroin 2IOV6B héroine 2QK02D Heroína Clorhidrato 2SMWYX Herion,caffeine,6-monoacetylmorphine 3E3XE3 Heroin, 6-MAM, Acetylcodeine, Dextromethorphane, caffeine 400BTP Heroin 424NFI Heroin 4ED4U4 Diamorphine 4FLYLL HEROINE 4P9OST Heroin 4ZRH5B Heroine 5AL4YL Heroine and codeine 5ZSPFZ Heroin 6CS6GB Heroina 77H7IH Heroin 78CN24 morphine, héroïne, lidocaïne 7BREL7 Heroin, Monoacetylmorphine, Morphine 7H5WS7 heroine 88O8O8 heroin.morphine. 8KXYZQ Heroin 8LLTJE caffeine, dextromethorphane, morphine, 6-acetylcodeine, 6-monoacetylmorphine, diacethylmorphine 8QXEZ5 heroine 99WMWJ heroin,mprphine,codiene,papaverine 9EU3UC heroin 9WEC99 HEROIN; MORPHINE AJWS6O Diamorphine AMA50Q Heroin. Traces of , codeine and morphine APYADP we found heroin B824TN Heroin and morphine BBEBBB Heroin HCl BPBBMB Heroin

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Code Identified Substances BZBJBP Heroin C2WUON Heroin,Morphine,Caffeine, C5ZRZ2 HEROIN CIIE5Y YES, MORPHINE Y CODEINE, ACETAMINOPHEN.) CLW6JW Heroin CQC6CC HEROIN CSDDCC HEROIN CHLORHYDRATE DDXKOD HEROIN. CAFFEINE DVAVS7 heroin, caffeine EIJIBE HEROIN EK1BZR Heroin EYBQOO Heroin, morphine EYEEEV Heroin, codeine, papaverine, morphine, caffeine, 6-acetylmorphine, 6-acetylcodeine, dextromethorphan F66RUS Heroin FF11HE heroin G9XDGK Heroine GUEUUR Diamorphine HPPPFP Héroin, probably morphine, 6MAM, acétylcodeine HRHXY5 Heroin HSJGXV Heroin IBADDP Diamorphine, Caffeine, Dextromethorphan indicated IQXIII heroin IYZYBB opiates (heroin) J9KZ5A Morphine, codeine, heroin JBRMJJ Heroin JCJPKW Diamorphine JGOKP5 Heroin JNYC8O Heroin, Morphine, Caffeine JQIGMD HEROIN JTSJJD Heroin, Caffeine JUNUUU heroin, caffeine, acetylcodeine, 6-MAM K7QIQW Heroin, Codeine, 6-monoacetylmorphine, Acetylcodeine, Dextromethorphan KBTTYE heroin KFTKVQ heroin, morphine KW3BDH heroin (DAM) and monoacetylmorphine (MAM) L1N1AS Heroin, Morphine LACFSF Heroina, Cafeina LLDWGL heroin LTLGBL Heroin LTXFMY Heroin; caffeine; M5FWNJ heroin MDPWHT heroin MKND72 Heroin, Morphine, 6-monoacetylmorphine,Acetylcodeine

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Code Identified Substances MMHHSD Heroin MRHASS Heroin N0NNLS heroin N1M8LG Heroin N666MQ Heroin and Caffeine. NA2AKJ Diamorphine HCL NO9OBB Heroine HCl NPDHYI heroin O0LRTK heroin (DAM) and monoacetylmorphine (MAM) OPBW2C Heroin OVCNJF Heroin PCIBIV dextromethorphan PDGMFW Heroin, Morphine, O6-MAM, Codeine PPHC9X heroin PQLTDR heroin PSOAIJ Heroin PUS7H2 6-Monoacetilmorfina, Acetilcodeina, Morfina y Heroina QJIQTJ Heroin R8O18R Heroine RIJOTJ heroin RPGPEM heroin hydrochloride RXGBPA heroine S2O5GO Heroína S6OORI heroine SADCGQ Heroin, Morphine SOQRQ9 HEROIN SSOSVY Heroin SSSCSJ heroin, morphine T0QNTU Heroin TBBUSK heroin, morphine TDDURM DIACETIYL MORPHFINE (HEROIN) (MORPHINE) TXQHJG heroin, caffeine, 6 Mono acetilmorphine and acetilcodeine. UHMVSZ HEROINA, MORFINA, CODEINA, MONOACETILMORFINA Y CAFEINA UT6VEX 6-Monoacetylmorphine and Diacetylmorphine UTL3JI Heroin VFLGQF Heroin, VLZ8LL heroine, morphine VMSX5E HEROIN HCL W4SM4Y Heroin WKJAI3 heroine WPYVIW Base Heroin XKGJ2G Diamorphine XPE2VZ Heroin YCSW1Z heroin

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Code Identified Substances YETFFI Heroin hydrochloride YULAAJ heroin, caffeine YYMCDP heroin Z4FNNZ Heroin

2013/1-SM (9) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Statement of findings for Test Sample 1

Code Caffeine Heroin 00H0DT - + Heroin is controlled by law (KB 31/12/1930 changed by KB 8/10/1963). 0DAKSM - + The sample contains the controlled drug heroin 47.36 %, m/m. 0SRDXD + + The powder is a mixture of heroin and caffeine. The concentration of heroin in the sample is 47.3% by weight 0T0BVS ANP + La sustancia analizada se trata de heroína 1HR18P + + Caffeine 1R7FTA + + Based on the above analysis, the sample was found to contain Heroin and Monoacetylmorphines 1SWNJJ + +

22JWSL + + The sample SM-1 contains a mixture of caffeine, heroine, 6-acetylcodeine and dextromethorphan.

2ACHVO + + heroin morphine cafeine acetyl codeine 2FELET - + SM-1 was found to be contain Heroin. Monoacetyl Morphine and acetyl codeine also was detected in this sample 2IOV6B + + 6 monoacetylmorphine , acetylcodéine, levometorphane, papvérine, noscapine 2QK02D + + Se detectan cafeína, 6-Monoacetilmorfina, Acetilcodeína y Codeína. 2SMWYX + + SM1 was prepared from a seizure containing 39.8% w/w herion base. The seizure also contained caffeine and 6-monoacetylmorphine. 3E3XE3 + +

400BTP + + In the dust sample analyzed was detected the presence of Heroin, Acetylcodeine,6 monoacetylmorphine and caffeine.

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Code Caffeine Heroin 424NFI + + Sample 2013/1/SM-1 consists of light yellow powder. Heroin, a prohibited sudstance included in the National Law for , is found to be present in this sample. The seizure also contains morphine, codeine, , acetylcodeine and 6-mono-acetyl-morphine. 4ED4U4 + + 0.228 grams of a powder containing 54% Diamorphine. Diamorphine is a Class A controlled drug subject to the provisions of the Misuse of Act 1971. 4FLYLL + +

4P9OST + + Sample 2013/1/SM-1 was found to contain controlled substance HEROIN, a Schedule I drug under the Single Convention on Drugs. 4ZRH5B + + the sizure also contained heroine, acetylcodeine, 6-monoacetylmorphine, dextrometorphan, cofeine and trace amounds of codeine and morphine 5AL4YL + +

5ZSPFZ + + we found aswell in this sample caffeine and 6-acetyl morphine and acetyl codeine 6CS6GB + + Cafeina, Acetil Codeina, 6-Monoacetil Morfina 77H7IH + + We found Heroin in SM-1 as controlled drug 78CN24 - + l'analyse de l'échantillon 2013/1/SM-1 révèle la présence de la morphine, de l'héroïne et de la lidocaïne 7BREL7 + + On analysis, i found the substances to contain 47.59% of heroin, 1.31% of morphine and 16.09% of monoacetylmorphine 7H5WS7 ANP + The seizure contained heroine 88O8O8 ANP +

8KXYZQ + + Sample contain heroin. The sample contain also caffeine, acetyl-codeine, and 6-monoacetyl- morphine 8LLTJE + + heroin was as hydrochloride form 8QXEZ5 + + heroine, caffeine, dextromethorphane,6-monoacetylmorphine,morphine,codeine

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Code Caffeine Heroin 99WMWJ + + the sample conatins 41.2 % Heroin and 2.8 % Morphine 9EU3UC + +

9WEC99 + + / AJWS6O ANP + One glass bottle labelled '2013/1/SM-1 containing 0.225g of beige coloured powder. This powder contained on average of 45% diamorphine which is commonly referred to as 'heroin'. Diamorphine is a class A controlled drug under the misuse of Drugs Act (1971)(as ammended). AMA50Q + + Cream-coloured powder containing heroin. Also dected traces of dextromethorphan, codeine and morphine, as well as acetylcodeine, monoacetylmorphine and caffeine. APYADP + + the sample also contains caffeine and 6MAM and acetylcodeine as metabolites B824TN + + Heroin and morphine and caffeine BBEBBB + + SM 1 contain also Coffeine and Dextromethorphan BPBBMB + + SM-1 was identified as illicit Heroin BZBJBP + + Heroin. The seizure also contained 6-monoacetylmorphine, acetylcodein, dextromethorphan and trace amounds of morphine, codeine and morphine-3-acetate C2WUON + + - C5ZRZ2 + + CAFFEINE, ACETYLCODEINE, MONOACETILMORPHINE CIIE5Y + + IN THE SAMPLE RECEIVED IN BOTTLE AMBER LID GREEN LETTERING 2013/1/SM-1 WAS FOUND HEROIN, MORPHINE, CAFFEINE, CODEINE, PAPAVERINE AND NOSCAPINE. CLW6JW + + Diluted with caffeine CQC6CC + + HEROIN 48.2% AS BASE. CAFFEINE WAS IDENTIFIED AS ADULTERANT CSDDCC + + caffein, glucose

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Code Caffeine Heroin DDXKOD + + The sample 2013/1/SM-1 was found to contain and Caffeine. DVAVS7 + + The sample contains heroin which is scheduled as illicit drug in XXXX. Caffeine is also present as cutting agent. EIJIBE + + HEROIN CHLORIDRATE (45.4% as base) - CAFFEINE EK1BZR + + The powder was analysed and found to contain heroin (diamorphine). EYBQOO + + SM-1 contains heroin, 46% and trace quantity of morphine EYEEEV + + *Results of screening tests were positive for opiates. *Retention time and fragmentation pattern obtained with the sample are equivalent to those obtained with heroin, codeine, papaverine, morphine, caffeine, 6-acetylmorphine, 6-acetylcodeine and dextromethorphan. F66RUS + + Sample contain drug- Heroin FF11HE + + mixture of heroin and coffeine FNZI88 + +

G9XDGK + + The sample SM1 contained 44.1 % heroine calculated as a base. In this sample was identified caffenie, dextromethorphan, codeine, acethylcodeine, 6- monoacetylmorphine, diacetylmorphine (heroine), papaverine, noscapine GUEUUR + + One glass vial with lid attached containing 218mg of pale brown powder containing an average of 46% diamorphine (heroin) together with the adulterant caffeine. HPPPFP + + Morphine, 6MAM, acetylcodeine are not quantified routinely in our laboratory HRHXY5 + + The saple contains heroin (47.2%), caffeine, acetylcodeine and 6-monoacetylmorphine.

HSJGXV + + Heroin (47.65% base), caffein, monoacetylmorphine and acetylcodeine. IBADDP + + On analysis, the powder was found to contain diamorphine.

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Code Caffeine Heroin IQXIII + + found heroin with 46.3% w/w , 6-monoacetylmorphine, 6-acetylcodeine, caffeine, and oleamide IYZYBB + + we have not received standards J9KZ5A + + Souble in Methanol, The Sample contains 47.5% Heroine, 1.7% Morphine as a base. In the sample was identified caffeine as adulterant . JBRMJJ + +

JCJPKW + + Brown powder found to contain diamorphine at a concentration of 41 per cent JGOKP5 + + Related compound: Morphine; Adulterant: Caffeine JNYC8O + + 50.71% +/- 5.58% Heroin detected in sample SM-1. Morphine detected in sample SM-1 but quantitation not performed. JQIGMD + + THE SAMPLE ALSO CONTAINS CAFEIN AND d,l- JTSJJD + + At first Screening Test was performed and confirmed by TLC method in two different system. JUNUUU + + color test : Marquis = purple violet , Mecke = deep green , Frohde = purple becoming green/purple TLC : TA = heroin or 6-MAM , system diehtylether :acetone: diethylamine (85:8:7) = heroin, acetylcodeine, 6-MAM, caffeine

GC : Heroin base = 46.13%, caffeine 9.81% GC/MS : Heroin, acetylcodeine, 6-MAM ,caffeine K7QIQW + + Heroin was found and the purity was 53.41%. Other drugs found were Codeine, 6- monoacetylmorphine, Acetylcodeine, Dextromethorphan. KBTTYE ANP + After analysis, the sample was found to contain heroin. KFTKVQ + + On analysis, I found the substance to contain morphine and 46.99% Heroin. KW3BDH + + powder containing 43.1% of heroin and 13.9% of 6-monoacetylmorphine. The sample contains also caffeine, methorphan and acetylcodeine not quantified L1N1AS + + heroin and Morphine were identified by TLC and GC/MS. Caffeine and lactose were also identified by TLC and GC/MS

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Code Caffeine Heroin LACFSF + + Las pruebas químicas y la coincidencia en los tiempos de retención y fragmentos de masas del material de referencia usado en las mismas condiciones que la muestra analizada, indican la presencia de heroina y cafeina. LLDWGL + + Sample contains 49.4 ± 2.9 % heroin-base. Sample also contains caffeine, acetylcodeine, 6- monoacetylmorphine, papaverin and dextrometorphan. LTLGBL + +

LTXFMY + + Marquis reagent, Scott reagent have been applied, the TLC and GC/FID M5FWNJ + + caffeine, acetylcodeine, 6-monoacetylmorphine, papaverine, dextrometorphan MDPWHT + + The sample is heroin. MKND72 + +

MMHHSD + + Beige, fine powder with acrid smell, tested positive for Heroin, a substance listed in Table A of the Law on Addictive Substances. MRHASS + + The sample contains heroin, 6-monoacetylmorphine, acetylcodeine and caffeine. N0NNLS + +

N1M8LG + + We also found 6-acethyl-codeine, 6-acethyl-morphine, caffein, papaverine and noscapine and traces of dextrometrorphane, codeine and morphine and also traces of glucose and lactose. N666MQ + + Applied chemical tests and instrumental chemical analysis, that sample 2013/1/SM1 contains Heroin and Caffeine. NA2AKJ ANP + One brown glass bottle containing 222mg of a yellow powder. this yellow powdercontained an average of 58% of diamorphine hydrochloride (also known as heroin). NO9OBB + + The power contained Heroine chlorhydrate with caféine. NPDHYI + + Presence of heroin hydrochloride, acetylcodeine, monoacetylmorphine, papaverine, noscapine, methorphan, glucose and caffeine was detected in the sample. O0LRTK + + white powder containing heroin (52.1%) and monoacetylmorphine (6.6%). It contains also acetylcodeine and caffeine

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Code Caffeine Heroin OPBW2C - +

OVCNJF + + Beige powder containing Heroin with a 37.99% as a base. PCIBIV + +

PDGMFW + + Caffeine, Metorphan, Noscapine, Papaverine, Acetyl Codeine PPHC9X + + powder contains heroin with caffeine PQLTDR + + acetil-kodein, 6-MAM, koffein, dextromorphan PSOAIJ ANP + Positive to heroin , contains morphine, 6- Monoacetylmorphine, Acetylcodein PUS7H2 + + Cafeina y Dextromethorphan QJIQTJ +

R8O18R + + Powder contains Heroine wich is a controlled substance RIJOTJ + + yellow powder containing heroin (42.1%), 6-monoacetylmorphine, acetylcodeine, and caffeine. RPGPEM + + sample contains also caffeine, O6-monoacetylmorphine and acetylcodeine RXGBPA + + cafeine, dextromethorphane, morphine, acetylcodeine,6MAM,noscapine S2O5GO ANP + Pruebas colorimétricas, Marquis, Lieberman, FT-IR, UV-visible y TLC S6OORI + + acetyl-codein, 6-monoacetyl-morphine, dextromorphan, SADCGQ + +

SOQRQ9 + + POWDER CONTAINING HEROIN. ADDITIONALLY IDENTIFIED CAFFEINE, ACETYLCODEINE, 6-MONOACETYLMORPHINE, METHORPHAW, STEREOCHEMICAL COMPOSITION NOT DETERMINED.

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Code Caffeine Heroin SSOSVY + + The sample contains heroin which is listed as a controlled drug according to XXX order, appendix I of February 22nd 1990. SSSCSJ - +

T0QNTU + + In the test sample 2013/1/SM-1 were detected heroin, acetylcodeine, 6-monoacetylmorphine, noscapine, dextromethorphan and caffeine TBBUSK + + browny powder, other - papaverine, morphine, noscapine, and 6-MAM, dextromethorphan, caffeine as diluent ingredient TDDURM + + The sample correspond: Diacetyl (morphine) mixed with morphine, cafeine and dextrormetofano. TXQHJG + +

UHMVSZ + +

UT6VEX - + Test sample 2013/1/SM-1 was found to contain the following controlled drugs 6- Monoacetylmorphine and Diacetylmorphine UTL3JI - + The results of the tests of the SM 1 (20) received confirmed that the mentioned sample contains heroín with 56.3 percentage by weight (56.3%) VFLGQF + + The sample was founf to contain Heroin, 6-MAM, acetylcodeine, Dextrometorphan and caffeine VLZ8LL + + The sample SM-1 found to contain 47,5 % heroine, 2,2 % morphine. The seizure also contains caffeine, dextromethorphan, codeine, acetylcodeine, 6-monoacetylmorphine, papaverine, noscapine. VMSX5E + + caffeine 10.84, acetylcodeine, 06 Monoacetylmorphine, noscapine, papaverine, glucose W4SM4Y + + One glass bottle containing 0.22 grammes of a mixture containing 0.11 grammes of heroin hydrochloride (being a salt of heroin). WKJAI3 + + CR, TLC, FTIR, GC, GC/MS WPYVIW + + Base Heroin 47,2 +/-2,14% (w/w); Acetylcodeine, 6-Monoacetylmorphine, Morphine,Dextrometorphane, Caffeine XKGJ2G + + The sample was found to contain 46.5% of diamorphine (as base).

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Code Caffeine Heroin XPE2VZ + + In the 0,225 g unknown powder it is found 39% Heroin. YCSW1Z + + This sample also contains 6-monoacetyl-morphine, acetyl-codeine, dextrometorphan and caffeine. YETFFI + + This sample contains heroin HCl (44.9 % as base) cut with caffein (10.7%), dextromethorphan (<2%). We also identify O.6 MAM (15.4% as base) and acetylcodein (2.2% as base) YULAAJ + +

YYMCDP ANP + Marquis reagent is positive (violet) to morphine derivates and Scott reagent is positive too. In the chromatogram the retention time is like heroin. So, the substance is heroin. Z4FNNZ + + Test Sample 2013/1/SM-1 contains Heroin, Acetylcodeine, 6-Acetylmorphine, 3-Acetylmorphine and Caffeine

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Identification methods for Test Sample 1

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

Analytical Technique Codes Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 00H0DT I S 0DAKSM I SI 0SRDXD I I I SI I I XRD 0T0BVS SI I 1HR18P I SI 1R7FTA S I 1SWNJJ I SI SI 22JWSL S S I I 2ACHVO SI I 2FELET S S I I 2IOV6B SI I I I 2QK02D SI S I I SI I 2SMWYX SI 3E3XE3 SI 400BTP S S I I 424NFI S S I I I I 4ED4U4 S S I 4FLYLL I SI 4P9OST S I 4ZRH5B SI 5AL4YL S I 5ZSPFZ S I 6CS6GB S I 77H7IH S I I 78CN24 S I 7BREL7 S S S I 7H5WS7 I SI 88O8O8 SI S S I 8KXYZQ SI ASAP-TOF 8LLTJE S I 8QXEZ5 SI I I I I 99WMWJ SI 9EU3UC S I I 9WEC99 I SI SI

2013/1-SM (19) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 AJWS6O S S I AMA50Q S SI I SI APYADP S S I B824TN I I SI I BBEBBB I S I I I BPBBMB S SI I I BZBJBP SI I C2WUON SI C5ZRZ2 S I I CIIE5Y S S S I CLW6JW S S S I I CQC6CC I SI I CSDDCC SI DDXKOD S S S I I DVAVS7 I SI EIJIBE S S S I EK1BZR S S I I EYBQOO SI S S S I I I EYEEEV S S I I F66RUS I SI I I LCMS FF11HE S I I I I FNZI88 SI G9XDGK I I GUEUUR S S I I HPPPFP S I I SI I HRHXY5 S S I I HSJGXV S I IBADDP I IQXIII SI IYZYBB I I S IMMUNOCHEMICAL J9KZ5A I I SI JBRMJJ SI JCJPKW S S I JGOKP5 I SI JNYC8O S S I I JQIGMD S S I I JTSJJD S S I S 210(Fast Blue B salt Test) JUNUUU S I I I K7QIQW S S S I

2013/1-SM (20) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 KBTTYE S I KFTKVQ S S S I KW3BDH SI L1N1AS S S S I I LACFSF S S I LLDWGL SI SI LTLGBL S S S I I LTXFMY S SI S I M5FWNJ S SI I MDPWHT S I I MKND72 S S SI SI MMHHSD S S S I I MRHASS SI N0NNLS S I I N1M8LG SI I N666MQ S S I NA2AKJ I I NO9OBB I SI I NPDHYI S S S S I I I O0LRTK I I SI OPBW2C I SI OVCNJF S S S I I PCIBIV I S S SI I SI I PDGMFW I I SI PPHC9X SI I PQLTDR S SI I I PSOAIJ S I I PUS7H2 S I QJIQTJ I R8O18R SI I I RIJOTJ SI RPGPEM S I I I RXGBPA SI I S2O5GO I S I I SI I I I liberman S6OORI I SI I SADCGQ I SI SOQRQ9 SI SSOSVY I I SSSCSJ I SI

2013/1-SM (21) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 T0QNTU I TBBUSK SI I TDDURM I SI TXQHJG S I I UHMVSZ S S I I UT6VEX SI UTL3JI S I VFLGQF I S Immunochromatography VLZ8LL S S S S I I VMSX5E SI W4SM4Y S S I SI I WKJAI3 SI S SI I I WPYVIW S S S I I I I XRD XKGJ2G SI I UPHLC/ELSD XPE2VZ S I I YCSW1Z I SI I YETFFI S S I I YULAAJ S S I YYMCDP S I Z4FNNZ S I I I RAMAN

2013/1-SM (22) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary for test sample 1 The response summary of all 126 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: 132

Caffeine: 114 Heroin: 132

False positives for Test Sample 1 (controlled substances)

Code Name Technique LTXFMY Mephedrone 141, 150 424NFI Methadone 150, 170

Frequency of use of screening and identification techniques:

Response Summary Participants: 132

SectionSection 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 Screening 42 50 35 18 0 2 0 2 45 7 0 0 0 1 4 31.8% 37.9% 26.5% 13.6% 0.0% 1.5% 0.0% 1.5% 34.1% 5.3% 0.0% 0.0% 0.0% 0.8% 3.0% Identification 10 5 2 32 9 15 1 21 118 45 2 2 2 3 7 7.6% 3.8% 1.5% 24.2% 6.8% 11.4% 0.8% 15.9% 89.4% 34.1% 1.5% 1.5% 1.5% 2.3% 5.3% # labs using 47 52 37 41 9 16 1 22 118 46 2 2 2 3 10 this 35.6% 39.4% 28.0% 31.1% 6.8% 12.1% 0.8% 16.7% 89.4% 34.8% 1.5% 1.5% 1.5% 2.3% 7.6% technique

2013/1-SM (23) Copyright (c) 2013 UNODC

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Z-Scores for Test Sample 1

Heroin Heroin CODE MAD: 1.7 CODE MAD: 1.7 Conc. * AbsDev ZScore Conc. * AbsDev ZScore IQXIII 46.3 0.9 0.4 00H0DT 47.2 0.0 0.0 IYZYBB 61.3 14.1 5.5 0DAKSM 47.4 0.2 0.1 J9KZ5A 47.5 0.3 0.1 0SRDXD 47.3 0.1 0.0 JBRMJJ 56.3 9.1 3.6 1HR18P 49.6 2.4 0.9 JCJPKW 41.0 6.2 2.4 1SWNJJ 47.0 0.2 0.1 JGOKP5 45.7 1.5 0.6 22JWSL 46.0 1.2 0.5 JNYC8O 50.7 3.5 1.4 2FELET 77.9 30.7 12.0 JQIGMD 46.7 0.5 0.2 2IOV6B 47.4 0.2 0.1 JUNUUU 46.1 1.1 0.4 2SMWYX 39.8 7.4 2.9 K7QIQW 53.4 6.2 2.4 3E3XE3 44.3 2.9 1.1 KBTTYE 48.2 1.0 0.4 4ED4U4 54.0 6.8 2.7 KFTKVQ 47.0 0.2 0.1 4FLYLL 63.0 15.8 6.2 KW3BDH 43.1 4.1 1.6 4P9OST 50.0 2.8 1.1 L1N1AS 48.1 0.9 0.4 4ZRH5B 49.3 2.1 0.8 LLDWGL 49.4 2.2 0.9 5ZSPFZ 45.6 1.6 0.6 MDPWHT 48.2 1.0 0.4 7BREL7 47.6 0.4 0.2 MKND72 52.5 5.3 2.1 88O8O8 47.2 0.0 0.0 MMHHSD 45.2 2.0 0.8 8LLTJE 65.2 18.0 7.0 MRHASS 33.3 13.9 5.4 8QXEZ5 43.0 4.2 1.6 N1M8LG 64.9 17.7 6.9 99WMWJ 41.2 6.0 2.3 NA2AKJ 51.0 3.8 1.5 9EU3UC 47.9 0.7 0.3 NO9OBB 46.7 0.5 0.2 9WEC99 46.5 0.7 0.3 NPDHYI 45.0 2.2 0.9 AJWS6O 45.0 2.2 0.9 O0LRTK 52.1 4.9 1.9 BBEBBB 45.5 1.7 0.7 OPBW2C 45.2 2.0 0.8 BPBBMB 36.0 11.2 4.4 OVCNJF 38.0 9.2 3.6 BZBJBP 52.5 5.3 2.1 PDGMFW 47.8 0.6 0.2 C2WUON 50.1 2.9 1.1 PPHC9X 48.2 1.0 0.4 C5ZRZ2 49.9 2.7 1.1 RIJOTJ 42.1 5.1 2.0 CQC6CC 48.2 0.9 0.4 RPGPEM 48.0 0.8 0.3 CSDDCC 47.0 0.2 0.1 RXGBPA 52.7 5.5 2.1 DVAVS7 46.0 1.2 0.5 SADCGQ 52.6 5.4 2.1 EIJIBE 45.4 1.8 0.7 SOQRQ9 47.4 0.2 0.1 EYBQOO 46.0 1.2 0.5 SSOSVY 45.5 1.7 0.7 FF11HE 22.0 25.2 9.8 SSSCSJ 59.0 11.8 4.6 FNZI88 48.9 1.7 0.7 T0QNTU 48.0 0.8 0.3 G9XDGK 44.1 3.1 1.2 TBBUSK 49.0 1.8 0.7 GUEUUR 46.0 1.2 0.5 UHMVSZ 33.5 13.7 5.3 HPPPFP 46.0 1.2 0.5 UTL3JI 56.3 9.1 3.6 HRHXY5 47.2 0.0 0.0 VLZ8LL 47.5 0.3 0.1 HSJGXV 47.7 0.4 0.2 VMSX5E 47.1 0.1 0.1 IBADDP 49.0 1.8 0.7 W4SM4Y 46.2 1.0 0.4

2013/1-SM (24) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Heroin CODE MAD: 1.7 Conc. * AbsDev ZScore WKJAI3 46.0 1.2 0.5 WPYVIW 47.2 0.0 0.0 XKGJ2G 46.5 0.7 0.3 XPE2VZ 39.0 8.2 3.2 YETFFI 44.9 2.3 0.9 YULAAJ 47.6 0.4 0.2 YYMCDP 40.6 6.6 2.6

*) Concentration: w/w %

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

2013/1-SM (25) Copyright (c) 2013 UNODC Z-Score Report per Sample per Substance

Round: 2013/1 Substance: SM-1/Heroin Lab Median = 47.2 MAD = 1.7 UNODC value = 47.9

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

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

Sample 2 Analysis

Identified substances for Test Sample 2 Code Identified Substances 00H0DT morphine 0DAKSM Morphine 0SRDXD morphine, codeine 0T0BVS MORFINA 1HR18P Morphine, Codeine 1R7FTA Morphine and Codeine 1SWNJJ morphine 22JWSL Morphine 2ACHVO opiates 2FELET Morphine 2IOV6B morphine 2QK02D Morfina 2SMWYX Morphine,codeine. 3E3XE3 Morphine, Codeine 400BTP Morphine 424NFI Morphine 4ED4U4 Morphine & Codeine 4FLYLL MORPHINE 4P9OST Morphine 4ZRH5B morphine 5AL4YL Morphine 5ZSPFZ morphine, codeine 6CS6GB Morfina 77H7IH Morphine 78CN24 Morphine 7BREL7 Morphine 7H5WS7 morphine 88O8O8 morphine 8KXYZQ Morphine 8LLTJE codeine, morphine 8QXEZ5 morphine 99WMWJ Codeine and Morphine 9EU3UC Morphine 9WEC99 MORPHINE; CODEIN AJWS6O Codeine and morphine AMA50Q Morphine, as well as codeine APYADP we found morphine B824TN Morphine BBEBBB Morphine HCL BZBJBP codeine and morphine

2013/1-SM (27) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances C2WUON Morphine C5ZRZ2 MORPHINE CIIE5Y YES, MORPHINE Y CODEINE. CLW6JW Morphine CQC6CC MORPHINE CSDDCC MORPHIN CHLORHYDRATE, CODEIN DDXKOD MORPHINE DVAVS7 morphine EIJIBE MORPHINE EK1BZR Morphine and codeine EYBQOO Morphine EYEEEV morphine, codeine F66RUS Morphine FF11HE morfphine G9XDGK Morphine, codeine GUEUUR Codeine and morphine HPPPFP Morphine and codeine HRHXY5 Morphine HSJGXV Morfine IBADDP Codeine, Morphine IQXIII morphine IYZYBB opiates (morphine) J9KZ5A Morphine, codeine JBRMJJ Heronin and morphine JCJPKW Codeine and morphine JGOKP5 Morphine JNYC8O Morphine, Codeine JQIGMD MORPHINE AND CODEINE JTSJJD Morphine, Codeine JUNUUU Morphine, codeine phosphate K7QIQW Morphine KBTTYE Morphine KFTKVQ morphine L1N1AS Morphine LACFSF Morfina LLDWGL morphine LTLGBL Morphine LTXFMY Morphine, m-CPP HCl M5FWNJ codeine, morfin MDPWHT morphine, codeine MKND72 Morphine, Codeine MMHHSD Morphine and Codeine MRHASS Morphine N0NNLS morphine, codeine

2013/1-SM (28) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances N1M8LG Morphine N666MQ Morphine and Codeine. NA2AKJ Morphine hydrochloride and codeine NO9OBB Morphine, codeine NPDHYI morphine O0LRTK morphine OPBW2C Morphine OVCNJF Morphine PDGMFW Morphine, Codeine PPHC9X morphine, codeine PQLTDR morfin, kodein PSOAIJ Morphine PUS7H2 Codeina y Morfina R8O18R Morphine RIJOTJ morphine RPGPEM morphine hydrochloride RXGBPA morphine S2O5GO Morfina S6OORI morphine, codein SADCGQ Morphine SOQRQ9 MORPHINE AND CODEINE SSOSVY Morphine SSSCSJ morphine T0QNTU Morphine TBBUSK morphine TDDURM MORPHINE and CODEINE TXQHJG morphine and codeine UHMVSZ MORFINA Y CODEINA UT6VEX Morphine UTL3JI morphine VFLGQF codeine VLZ8LL morphine VMSX5E MORPHINE HCL W4SM4Y Morphine WKJAI3 morphine, codeine WPYVIW Morphine hidrochlorhide XKGJ2G Morphine and Codeine XPE2VZ Morphine & Codeine YCSW1Z morphine, codeine YETFFI Morphine hydrochloride YULAAJ codeine, morphine YYMCDP morphine Z4FNNZ Morphine and Codeine

2013/1-SM (29) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Statement of findings for Test Sample 2

Code Morphine 00H0DT + Morphine is controlled by law (KB 31/12/1930 changed by KB 8/10/1963). 0DAKSM + The sample contains the controlled drug morphine 70.67 %, m/m and codeine 12.94 %, m/m. 0SRDXD + the powder is a mixture of morphine and codeine. The concentration of morphine in the sample is 90.3% by weight, codeine is 9% by weight. 0T0BVS + La sustancia analizada se trata de morfina 1HR18P +

1R7FTA + Based on the above analysis, the sample was found to contain Morphine and Codeine 1SWNJJ +

22JWSL + The sample SM-2 contains a mixture of morphine and codeine. 2ACHVO + codeine morphine 2FELET + SM-1 was found to be contain Morphine. Codeine also was detected in this sample. 2IOV6B + codéine, 6 monoacetylmorphine 2QK02D + Ademas Codeína. 2SMWYX + SM2 was prepared from a seizure containing 60.6% w/w morphine base. The seizure also contained codeine. 3E3XE3 +

400BTP + In the powder sample analyzed was detected the presence of morphine and codeine. 424NFI + Sample 2013/1/SM-2 consists of white powder. Morphine, a prohibited sudstance included in the National Law for Narcotics, is found to be present in this sample. The seizure also contains codeine.

2013/1-SM (30) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Morphine 4ED4U4 + 0.225 grams of a powder containing Morphine. Morphine is a Class A controlled drug subject to the provisions of the . 4FLYLL +

4P9OST + Sample 2013/1/SM-2 was found to contain controlled substance MORPHINE, a Schedule I drug under the Single Convention on Narcotic Drugs. 4ZRH5B + morphine and codeine 5AL4YL +

5ZSPFZ +

6CS6GB + Monomorfinan-6-ol 77H7IH + We found Morphine in SM-2 as controlled drug 78CN24 + L'analyse de l'échantilon 2013/1/SM-2 révèle la présence de la morphine 7BREL7 + On analysis, i found the substances to contain 63.14% of morphine. 7H5WS7 + The seizure contained morphine 88O8O8 +

8KXYZQ + sample contain Morphine. 8LLTJE + morphine was as hydrochloride form 8QXEZ5 + morphine, codeine 99WMWJ + The sample contains 8.3 % Morphine. 9EU3UC +

2013/1-SM (31) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Morphine 9WEC99 + / AJWS6O + One glass bottle labelled '2013/1/SM-2' containing 0.221g of off-white powder. This powder contained codeine and morphine. Please see part 5 (4) for further comments. AMA50Q + White powder containing morphine and codeine. APYADP + the sample also contains codeine and acetylcodeine as metabolite B824TN + Morphine BBEBBB + SM 2 contain also Codeine BPBBMB - Analysis of the Powder did not reveal the presence of any controlled drugs BZBJBP + codeine and morphine C2WUON + - C5ZRZ2 + CODEINE CIIE5Y + IN THE SAMPLE RECEIVED IN BOTTLE AMBER LID GREEN LETTERING 2013/1/SM-2 WAS FOUND MORPHINE Y CODEINE. CLW6JW + With codeine also CQC6CC + MORPHINE AND CODEINE WERE IDENTIFIED CSDDCC +

DDXKOD + The sample 2013/1/SM-2 was found to contain Morphine. DVAVS7 + The sample contains morphine which is scheduled as illicit drug in France. EIJIBE + MORPHINE CHLORYDRATE (67.4% as base) - CODEINE CHLORYDRATE (11.6 as base)

2013/1-SM (32) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Morphine EK1BZR + The powder was analysed and found to contain morphine and codeine. EYBQOO + SM-2 contains morphine, 59% EYEEEV + *Results of screening tests were positive for opiates. *Retention time and fragmentation pattern obtained with the sample are equivalent to those obtained with morphine and codeine. F66RUS + Sample contain drug- Morphine FF11HE + mixture of morphine and codeine FNZI88 +

G9XDGK + The sample SM2 contained morphine and codeine. Quantification of morphine we do not performed. GUEUUR + One glass vial with lid attached containing 217mg of off-white powder containing codeine and morphine. HPPPFP + Morphine and codeine are not quantified routinely in our laboratory HRHXY5 + The sample contains morphine and codeine. HSJGXV + Morfine (not quantified) and codeine IBADDP + On analysis, the powder was found to contain morphine.

IQXIII + found morphine with 59.0% w/w, 6-acetylcodeine, and oleamide (calibration curve performed with UNODC standard) IYZYBB + we have not received standards J9KZ5A + Souble in Methanol, The Sample contains 64.9% Morphine, 11.8% Codeine as a base. JBRMJJ +

2013/1-SM (33) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Morphine JCJPKW + Off-white powder found to contain codeine and morphine. I am satisfied that morphine is present at a concentration greater than 0.2%. JGOKP5 + Also found Codeine JNYC8O + Morphine and Codeine detected in sample SM-2 but quantitation not performed. JQIGMD + MORPHINE 79.6% CODEINE 13.3% JTSJJD + At first Screening Test was performed and confirmed by TLC method in two different solvent system. JUNUUU + color test : Marquis = purple violet , Mecke = deep green , Frohde = purple becoming green/purple TLC : TA = Morphine or codeine, system diehtylether :acetone: diethylamine (85:8:7) = Morphine and codeine

GC : Morphine base = 78.66%, codeine base 13.33% GC/MS : Heroin, acetylcodeine, 6-MAM ,caffeine K7QIQW + Morphine was found and the purity was 72.03%. Other drug found was codeine. KBTTYE + After analysis, the sample was found to contain morphine. KFTKVQ + The sample was found to contain morphine. KW3BDH -

L1N1AS + Morphine was identified by TLC and GC/MS LACFSF + Las pruebas químicas y la coincidencia en los tiempos de retención y fragmentos de masas del material de referencia usado en las mismas condiciones que la muestra analizada, indican la presencia de morfina. LLDWGL + Sample contains 72,8 ± 3.2 % morphine-base. Sample also contains codeine. LTLGBL +

LTXFMY + Marquis reagent and Scott reagent have been applied, the TLC and GC/FID

2013/1-SM (34) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Morphine M5FWNJ +

MDPWHT + The sample is a mixture of morphine and codeine. MKND72 +

MMHHSD + White, odourless powder, tested positive for Morphine and Codeine, substances listed in Table B and C respectively of the Law on Addictive Substances. MRHASS + The sample contains morphine and codeine. N0NNLS +

N1M8LG + We also found codeine and traces of heroin. N666MQ + Applied chemical tests and instrumental chemical analysis, that sample 2013/1/SM2 contains Morphine and Codeine. NA2AKJ + One brown glass bottle containing 224mg of an off-white powder. This off-white powder contained morphine hydrochloride and codeine. NO9OBB + The power contained morphine and codéine. NPDHYI + Presence of morphine and codeine was detected in the sample. O0LRTK + white powder containing morphine (69.4%). In addition is present codeine OPBW2C +

OVCNJF + The analyze sample was identify as Morphine, however the quantification was not possible due to the degradation of the standard sample. PCIBIV +

PDGMFW +

PPHC9X + powder contains morphine and codeine

2013/1-SM (35) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Morphine PQLTDR +

PSOAIJ + Positive to morphine, contains codeine sulfate. PUS7H2 +

QJIQTJ ANP

R8O18R + Powder contains morphine wich is a controlled substance RIJOTJ + white powder containing morphine (58.9%) and codeine RPGPEM +

RXGBPA + codeine S2O5GO + Pruebas colorimétricas, Marquis, Lieberman, FT-IR, UV-visible , TLC y microcristales S6OORI +

SADCGQ +

SOQRQ9 + POWDER CONTAINING MORPHINE AND CODEINE SSOSVY + The sample contains morphine which is listed as controlled drug according to french order, appendix I of February 22nd 1990. SSSCSJ +

T0QNTU + In the test sample 2013/1/SM-2 were detected codeine and morphine TBBUSK + white powder, mixture of the morphine and codeine TDDURM + The sample correspond: MORPHINE mixed with CODEINE

2013/1-SM (36) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Morphine TXQHJG +

UHMVSZ +

UT6VEX + Test sample 2013/1/SM-2 was found to contain the following controlled drug Morphine UTL3JI + The results of the tests of the SM 2 (29) received confirmed that the mentioned sample contains morphine but we are not able to give a cuantification result because we have not got the pattern of the mentioned controlled drug. The SM 2 also contains codein as not controlled drug VFLGQF - the sample was found to contain codeine VLZ8LL + The sample SM-2 found to contain 73,0 % morphine. The seizure also contains codeine. VMSX5E + codéine W4SM4Y + One glass bottle containing 0.22 grammes of a powder containing 0.15 grammes of morphine. WKJAI3 + CR, TLC, FTIR, GC, GC/MS WPYVIW + Morphine hidrochloride, Codeine XKGJ2G + The sample was found to contain 68.4% of morphine (as base) and 12.5% of codeine (as base). XPE2VZ + In the 0,230 g unknown powder it is found 50% Morphine and 10% Codeine. YCSW1Z +

YETFFI + This sample contains morphine HCl (67.3% as base) and codein (13.8% as base) YULAAJ +

YYMCDP + marquis reagent is positive (violet) ant Scott reagent is positive too. In the chromatogram the retention time is like morphine. So, the substance is morphine. Z4FNNZ + Test Sample 2013/1/SM-2 contains Morphine and Codeine

2013/1-SM (37) Copyright (c) 2013 UNODC 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

Analytical Technique Codes Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 00H0DT I S 0DAKSM I SI 0SRDXD I I I SI I I XRD 0T0BVS SI I 1HR18P I SI 1R7FTA S I 1SWNJJ I SI SI 22JWSL S S I I 2ACHVO SI I 2FELET S S I I 2IOV6B SI I I I 2QK02D SI S I I SI I 2SMWYX SI 3E3XE3 SI 400BTP S S I I 424NFI S S I I I I 4ED4U4 S S I 4FLYLL I SI 4P9OST S I 4ZRH5B SI 5AL4YL S I 5ZSPFZ S I 6CS6GB S I 77H7IH S I I 78CN24 S I 7BREL7 S S S I 7H5WS7 I SI 88O8O8 SI S S I 8KXYZQ SI ASAP-TOF 8LLTJE S I 8QXEZ5 SI I I I I 99WMWJ SI 9EU3UC S I I 9WEC99 I SI SI

2013/1-SM (38) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 AJWS6O S S I AMA50Q S SI I SI APYADP S S I B824TN I I SI I BBEBBB I S I I I BPBBMB S SI I I BZBJBP SI I C2WUON SI C5ZRZ2 S I I CIIE5Y S S S I CLW6JW S S S I I CQC6CC I SI I CSDDCC SI DDXKOD S S S I I DVAVS7 I SI EIJIBE S S S I EK1BZR S S I I EYBQOO SI S S S I I I EYEEEV S S I I F66RUS I SI I I LCMS FF11HE S I I I I FNZI88 SI G9XDGK I I GUEUUR S S I I HPPPFP S I I SI I HRHXY5 S S I I HSJGXV S I IBADDP I IQXIII SI IYZYBB I I S IMMUNOCHEMICAL J9KZ5A I I SI JBRMJJ SI JCJPKW S S I JGOKP5 I SI JNYC8O S S I I JQIGMD S S I I JTSJJD S S I S 210(Fast Blue B salt Test) JUNUUU S I I I K7QIQW S S S I

2013/1-SM (39) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 KBTTYE S I KFTKVQ S S S I KW3BDH SI L1N1AS S S S I I LACFSF S S I LLDWGL SI SI LTLGBL S S S I I LTXFMY S SI S I M5FWNJ S SI I MDPWHT S I I MKND72 S S SI SI MMHHSD S S S I I MRHASS SI N0NNLS S I I N1M8LG SI I N666MQ S S I NA2AKJ I I NO9OBB I SI I NPDHYI S S S S I I I O0LRTK I I SI OPBW2C I SI OVCNJF S S S I I PCIBIV I S S SI I SI I PDGMFW I I SI PPHC9X SI I PQLTDR S SI I I PSOAIJ S I I PUS7H2 S I QJIQTJ I R8O18R SI I I RIJOTJ SI RPGPEM S I I I RXGBPA SI I S2O5GO I S I I SI I I I liberman S6OORI I SI I SADCGQ I SI SOQRQ9 SI SSOSVY I I SSSCSJ I SI

2013/1-SM (40) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 T0QNTU I TBBUSK SI I TDDURM I SI TXQHJG S I I UHMVSZ S S I I UT6VEX SI UTL3JI S I VFLGQF I S Immunochromatography VLZ8LL S S S S I I VMSX5E SI W4SM4Y S S I SI I WKJAI3 SI S SI I I WPYVIW S S S I I I I XRD XKGJ2G SI I UPHLC/ELSD XPE2VZ S I I YCSW1Z I SI I YETFFI S S I I YULAAJ S S I YYMCDP S I Z4FNNZ S I I I RAMAN

2013/1-SM (41) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary for test sample 2 The response summary of all 126 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: 132

Morphine: 126

False positives for Test Sample 2 (controlled substances)

Code Name Technique LTXFMY 1-(3-Chlorophenyl) 141, 150 JBRMJJ Heroin 180

False negatives for SM-2 (techinque(s) used or ANP) . Code - BPBBMB (180), VFLGQF (180), QJIQTJ (ANP),KW3BDH (ANP)

Frequency of use of screening and identification techniques:

Response Summary Participants: 132

Section 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 Screening 42 50 35 18 0 2 0 2 45 7 0 0 0 1 4 31.8% 37.9% 26.5% 13.6% 0.0% 1.5% 0.0% 1.5% 34.1% 5.3% 0.0% 0.0% 0.0% 0.8% 3.0% Identification 10 5 2 32 9 15 1 21 118 45 2 2 2 3 7 7.6% 3.8% 1.5% 24.2% 6.8% 11.4% 0.8% 15.9% 89.4% 34.1% 1.5% 1.5% 1.5% 2.3% 5.3% # labs using 47 52 37 41 9 16 1 22 118 46 2 2 2 3 10 this 35.6% 39.4% 28.0% 31.1% 6.8% 12.1% 0.8% 16.7% 89.4% 34.8% 1.5% 1.5% 1.5% 2.3% 7.6% technique

2013/1-SM (42) Copyright (c) 2013 UNODC

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

Z-Scores for Test Sample 2

Morphine CODE MAD: 5.4 Morphine Conc. * AbsDev ZScore CODE MAD: 5.4 00H0DT 87.1 18.6 2.3 Conc. * AbsDev ZScore 83.8 15.3 1.9 0DAKSM 70.7 2.2 0.3 RPGPEM 81.0 12.5 1.6 0SRDXD 90.3 21.8 2.7 RXGBPA 73.8 5.3 0.7 1HR18P 77.8 9.3 1.2 SADCGQ 68.0 0.5 0.1 1SWNJJ 76.1 7.6 1.0 SOQRQ9 64.0 4.5 0.6 2FELET 65.8 2.7 0.3 SSSCSJ 87.5 19.0 2.4 2IOV6B 78.8 10.4 1.3 UHMVSZ 73.0 4.5 0.6 2SMWYX 60.6 7.9 1.0 VLZ8LL 81.0 12.5 1.6 3E3XE3 81.0 12.5 1.6 VMSX5E 66.9 1.6 0.2 4P9OST 65.0 3.5 0.4 W4SM4Y 79.0 10.5 1.3 4ZRH5B 77.8 9.3 1.2 WKJAI3 68.4 0.1 0.0 7BREL7 63.1 5.3 0.7 XKGJ2G 50.0 18.5 2.3 8LLTJE 81.5 13.0 1.6 XPE2VZ 67.3 1.2 0.1 8QXEZ5 35.0 33.5 4.2 YETFFI 8.3 60.2 7.5 99WMWJ *) Concentration: w/w % 9EU3UC 51.8 16.7 2.1 BBEBBB 58.0 10.5 1.3 BZBJBP 75.5 7.0 0.9 C2WUON 71.6 3.1 0.4 CSDDCC 63.0 5.5 0.7 EIJIBE 67.4 1.1 0.1 EYBQOO 59.0 9.5 1.2 FF11HE 68.9 0.5 0.1 FNZI88 71.4 3.0 0.4 IQXIII 59.0 9.5 1.2 IYZYBB 80.3 11.8 1.5 J9KZ5A 64.9 3.6 0.4 JGOKP5 61.2 7.3 0.9 JQIGMD 79.6 11.1 1.4 JUNUUU 78.7 10.2 1.3 K7QIQW 72.0 3.6 0.4 L1N1AS 67.4 1.0 0.1 LLDWGL 72.8 4.3 0.5 MKND72 74.5 6.0 0.8 MRHASS 69.7 1.3 0.2 N1M8LG 76.9 8.4 1.1 NPDHYI 67.3 1.2 0.1 O0LRTK 69.4 0.9 0.1 OPBW2C 71.8 3.3 0.4 PDGMFW 67.2 1.3 0.2 RIJOTJ 58.9 9.6 1.2

2013/1-SM (43) Copyright (c) 2013 UNODC Z-Score Report per Sample per Substance

Round: 2013/1 Substance: SM-2/Morphine Median = 68.5 MAD = 5.4 UNODC value = 68.8

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

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

Sample 3 Analysis

Identified substances for Test Sample 3 Code Identified Substances 00H0DT nimetazepam 0DAKSM Nimetazepam 0SRDXD nimetazepam 0T0BVS NIMETAZEPAM 1HR18P Nimetazepam 1R7FTA Nimetazepam 1SWNJJ nimetazepam, lactose 22JWSL Nimetazepam 2ACHVO 2FELET Nimetazepam 2IOV6B nimétazepam 2QK02D Nimetazepam 2SMWYX Nimetazepam 3E3XE3 Nimetazepam 400BTP Nimetazepam 4ED4U4 Nimetazepam 4P9OST NIMETAZEPAM 4ZRH5B nimetozepam 5AL4YL Nimetazepam 5ZSPFZ nimetazepam 6CS6GB Nimetazepam 77H7IH Nimetazepam 78CN24 Lidocaïne 7BREL7 Nimetazepam 8KXYZQ Nimetazepam 8QXEZ5 nimetazepam 99WMWJ Nimetazepam 9EU3UC Nimetazepam 9WEC99 NIMETAZEPAM AJWS6O Nimetazepam AMA50Q Nimetazepam APYADP we found nimetazepam B824TN Nimetazepam BBEBBB Nimetazepam BPBBMB Nimetazepam BZBJBP Nimetazepam C2WUON Nimetazepam C5ZRZ2 NIMETAZEPAM CIIE5Y YES, NIMETAZEPAM CLW6JW Nimetazepam

2013/1-SM (45) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances CQC6CC NIMETAZEPAM DDXKOD Nimetazepam DVAVS7 nimetazepam, lactose EIJIBE MIMETAZEPAM EK1BZR Nimetazepam EYBQOO Nimetazepam EYEEEV Nimetazepam, lactose F66RUS Nimetazepm G9XDGK Nimetazepam GUEUUR Nimetazepam HPPPFP Nimetazepam HRHXY5 Nimetazepam HSJGXV Nimetazepam IBADDP Nimetazepam IQXIII nimetazepam IYZYBB benzodiazepines (nimetazepam) J9KZ5A Nimetazepam JBRMJJ controlled substance JCJPKW Nimetazepam JGOKP5 Nimetazepam JNYC8O Nimetazepam JQIGMD NIMETAZEPAM JTSJJD Nimetazepam JUNUUU Nimetazepam K7QIQW Nimetazepam KBTTYE Nimetazepam KFTKVQ Nimetazepam KW3BDH nimetazepam L1N1AS Nimetazepam LACFSF Nimetazepam LLDWGL Nimetazepam LTLGBL Nimetazepam LTXFMY Nimetazepam M5FWNJ nimetazepam MDPWHT nimetazepam MKND72 Nimetazepam MMHHSD Nimetazepame MRHASS Nimetazepam N0NNLS nimetazepam N1M8LG Nimetazepam N666MQ Nimetazepam. NA2AKJ Nimetazepam NO9OBB NIMETAZEPAM NPDHYI nimetazepam

2013/1-SM (46) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances O0LRTK nimetazepam OPBW2C Nimetazepam and Lactose OVCNJF Nimetazepam PDGMFW Nimetazepam PPHC9X nimetazepam PSOAIJ Nimetazepam PUS7H2 Nimetazepam R8O18R Nimetazepam RIJOTJ nimetazepam RPGPEM nimetazepam RXGBPA nimetazepam SADCGQ Nimetazepam SOQRQ9 NIMETAZEPAM SSOSVY Nimetazepam SSSCSJ nimetazepam TDDURM Nimetazepam TXQHJG nimetazepam UTL3JI NONE VFLGQF methamphetamine VLZ8LL nimetazepam VMSX5E NIMETAZEPAM W4SM4Y Nimetazepam WKJAI3 nimetazepam WPYVIW Nimetazepam XKGJ2G Nimetazepam XPE2VZ Nimetazepam YCSW1Z nimetazepam YETFFI Nimetazepam YULAAJ nimetazepam Z4FNNZ Nimetazepam

2013/1-SM (47) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Statement of findings for Test Sample 3

Code Lactose Nimetazepam 00H0DT ANP + Nimetazepam is controlled by law (KB 22/01/1998). 0DAKSM + + The sample contains the controlled drug nimetazepam 3.75 %, m/m and lactose. 0SRDXD + + The powder is a mixture of nimetazepam and lactose. The concentration of nimetazepam in the sample is 10% by weight. 0T0BVS ANP + La sustancia analizada se trata de una benzodiacepina, probablemente nimetazepam 1HR18P ANP +

1R7FTA ANP + Based on the above analysis, the sample was found to contain Nimetazepam 1SWNJJ + +

22JWSL + + The sample SM-3 contains a mixture of lactose and nimetazepam 2ACHVO ANP + nimetazepam 2FELET - + SM-1 was found to be contain Nimetazepam. 2IOV6B + + lactose 2QK02D + + Se detecto lactosa. 2SMWYX - + SM3 was prepared from a seizure containing 3.78% w/w nimetazepam. 3E3XE3 ANP +

400BTP + + In the powder sample analyzed was detected the presence of Nimetazepam and Lactose. 424NFI + ANP Sample 2013/1/SM-3 consists of light pink powder. No prohibited sudstances are detected in this sample.

2013/1-SM (48) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Lactose Nimetazepam 4ED4U4 ANP + 0.220 grams of a powder containing Nimetazepam. Nimetazepam is a Class C controlled drug subject to the provisions of the Misuse of Drugs Act 1971. 4FLYLL + -

4P9OST ANP + Sample 2013/1/SM-3 was found to contain controlled substance NIMETAZEPAM, a Schedule IV drug under the international Convention on Psychotropic Substances. 4ZRH5B - + nimetozepam 5AL4YL ANP + lactose and Nimetazepam 5ZSPFZ ANP +

6CS6GB ANP + Fenil Alanina 77H7IH ANP + We found Nimetazepam in SM-3 as controlled drug 78CN24 - - Après analyse, l'échantillon 2013/1/SM-3 contient la Lidocaïne 7BREL7 + + On analysis, i found the substances to contain 3.58% of nimetazepam. 7H5WS7 ANP ANP

88O8O8 ANP ANP

8KXYZQ ANP + Sample contain Nimetazepam. 8LLTJE ANP +

8QXEZ5 - + nimetazepam 99WMWJ ANP + the sample contains Nimetazepam 9EU3UC + +

2013/1-SM (49) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Lactose Nimetazepam 9WEC99 + + / AJWS6O ANP + One glass bottle labelled '2013/1/SM-3' containing 0.231g of pink powder. This powder contained Nimetazepam. Nimetazepam is a class C controlled drug under the misuse of Drugs Act (1971)(as ammended). AMA50Q ANP + Pink powder containing nimetazepam. APYADP ANP + the sample was confirmed by gc ms B824TN + + Nimetazepam and lactose BBEBBB + + SM 3 contain also Lactose BPBBMB ANP + Analysis of the powder revealed the presence of Nimetazepam BZBJBP + + Nimetazepam, lactose C2WUON ANP + - C5ZRZ2 + + LACTOSE, GLUCOSE CIIE5Y - + IN THE SAMPLE RECEIVED IN BOTTLE AMBER LID GREEN LETTERING 2013/1/SM-3 WAS FOUND NIMETAZEPAM. CLW6JW + + Diluted with lactose CQC6CC + + NIMETAZEPAM IN LACTOSE POWDER CSDDCC + + NIMETAZEPAM, LACTOSE, GLUCOSE DDXKOD ANP + The Sample 2013/1/SM-3 was found to contain Nimetazepam. DVAVS7 + + The sample contains nimetazepam which is scheduled as psychotrope in France. Lactose is also present as cutting agent. EIJIBE ANP + NIMETAZEPAM CHLORYDRATE

2013/1-SM (50) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Lactose Nimetazepam EK1BZR + + The powder was analysed and found to contain nimetazepam. EYBQOO - + SM-3 contains nimetazepam, 7,2% EYEEEV + + *Retention time and fragmentation pattern obtained with the sample are equivalent to those obtained nimetazepam. *The spectroscopic parameters obtained with the sample are equivalent to those obtained lactose. F66RUS + + Sample contain drug- Nimetazepam FF11HE + + mixture of lactose and nimetazepam FNZI88 - +

G9XDGK + + The sample SM3 contained nimetazepam and lactose. Pharmaceuticals with psychoactive compunds, we do not quantify. GUEUUR + + One glass vial with lid attached containing 210mg of pink powder cotaining nimetazepam HPPPFP + + Probably nimetazepam (We don't have the standard product in the laboratory). This product is not found en France. Lactose and probably glucose traces HRHXY5 ANP + The sample contains nimetazepam. HSJGXV - + Nimetazepam IBADDP ANP + On analysis, the powder was found to contain nimetazepam.

IQXIII ANP + sample was found to contain nimetazepam but quantification was not performed IYZYBB + + we have not received standards J9KZ5A + + The sample contains 3.8% Nimetazepam and Lactose. JBRMJJ - + Nimetazepam is a benzodiacepine drugs

2013/1-SM (51) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Lactose Nimetazepam JCJPKW ANP + Pink powder found to contain nimetazepam JGOKP5 ANP +

JNYC8O + + 3.33% +/- 0.30% Nimetazepam detected in sample SM-3. JQIGMD - +

JTSJJD - + At first Screening Test was performed and confirmed by TLC method in two different solvent system. JUNUUU ANP + TLC : TA and TE = nimetazepam GC : Nimetazepam 3.59% GC/MS : Nimetazepam K7QIQW - + Nimetazepam was found and the purity was 2.75%. KBTTYE ANP + After analysis, the sample was found to contain nimetazepam. KFTKVQ - + On analysis, I found the substance to contain 3.07 % nimetazepam. KW3BDH ANP + powder containing nimetazepam L1N1AS + + Nimetazepam was identified by TLC and GC/MS LACFSF ANP + El análisis cromatográfico realizado a la muestra produjo coincidencias significativas con la librería de compuestos del software, lo que indica la presencia de Nimetazepam en la muestra analizada. LLDWGL + + Sample contains nimetazepam and lactose. According to the Hungarian low we not quantify nimetazepam routinely. LTLGBL + +

LTXFMY ANP + Marquis reagent and Scott reagent have been applied, the TLC and GC/FID M5FWNJ ANP +

2013/1-SM (52) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Lactose Nimetazepam MDPWHT + + The sample contains nimetazepam. MKND72 ANP +

MMHHSD ANP + Pink, odourless powder, tested positive for Nimetazepam, a substance listed in Table D of the Law on Addictive Substances. MRHASS + + The sample contains nimetazepam and lactose. N0NNLS - +

N1M8LG + + We also found lactose N666MQ ANP + Applied chemical tests and instrumental chemical analysis, that sample 2013/1/SM3 contains Nimetazepam. NA2AKJ ANP + One brown glass bottle containing 231mg of a pink powder. this pink powder contained nimetazepam. NO9OBB + + The power contained Nimetazepam with lactose. Nimetazepam is a psychotropic substance NPDHYI + + Presence of nimetazepam and lactose was detected in the sample. O0LRTK + + Pink powder containing nimetazepam. The amount of nimetazepam was not quantified. The sample contains also lactose and glucose (not quantified) OPBW2C + +

OVCNJF + + Pink powder containing Nimetazepam with a 24.8% of base. Nimetazepam is clasify as a psychotropic by the Ministry of Health of Guatemala, it is not clasify as a seized material. PCIBIV - +

PDGMFW + + Sugar PPHC9X + + powder contains nimetazepam PQLTDR + + nimetazepam, laktóz

2013/1-SM (53) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Lactose Nimetazepam PSOAIJ + + Positive to Nimetazepam and lactose PUS7H2 ANP +

QJIQTJ ANP ANP

R8O18R ANP + Powder contains Nimetazepam wich is a controlled substance RIJOTJ ANP + Pink powder containing nimetazepam. The amount of nimetazepam was not determined because there is not the righr standard reference material in the laboratory. RPGPEM + + sample contains also lactose RXGBPA + + suggar, fatty acids S2O5GO + ANP Pruebas colorimétricas, Marquis, Scott, Lieberman, Chen Cao,FT-IR. S6OORI - + nimatazepam SADCGQ - +

SOQRQ9 ANP + POWDER CONTAINING NOMETAZEPAM SSOSVY + + The sample contains nimetazepam which is listed as a controlled psychotropic substance according to french order, 1st part of appendix of February 22nd 1990. SSSCSJ ANP +

T0QNTU - + In the test sample 2013/1/SM-3 was detected nimetazepam TBBUSK + + white powder, mixture of the nimetazepam and lactose TDDURM - + The sample correspond: Nimetazepam mixed with lactoce TXQHJG + +

2013/1-SM (54) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Lactose Nimetazepam UHMVSZ - -

UT6VEX ANP - Test sample 2013/1/SM-3 was found to contain No controlled drugs . UTL3JI - - we have not found any controlled drug in the SM 3 (36) VFLGQF ANP ANP the sample was found to contain methamphetamine VLZ8LL + + The sample SM-3 found to contain 3,6 % nimetazepam. The seizure also contains lactose. VMSX5E + + lactose, glucose W4SM4Y + + One glass bottle containing 0.23 grammes of a powder containing 7 milligrammes of nimetazepam. WKJAI3 + + TLC, FTIR, GC, GC/MS WPYVIW + + Nimetazepam, Lactose XKGJ2G + + The sample was found to contain nimetazepam. XPE2VZ - + In the 0,230 g unknown powder it is found 10% Nimetazepam. YCSW1Z + + This sample also contains lactose. YETFFI + + This sample contains Nimetazepam (not quantified) with lactose. YULAAJ ANP +

YYMCDP ANP ANP marquis reagent is negative ant Scott reagent is positive. In the chromatogram the retention time does not like the retention time patterns we have. So, we can not know the drug. Z4FNNZ + + Test Sample 2013/1/SM-3 contains Nimetazepam and Lactose

2013/1-SM (55) Copyright (c) 2013 UNODC 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

Analytical Technique Codes Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 00H0DT I S 0DAKSM I SI 0SRDXD I I I SI I I XRD 0T0BVS SI I 1HR18P I SI 1R7FTA S I 1SWNJJ I SI SI 22JWSL S S I I 2ACHVO SI I 2FELET S S I I 2IOV6B SI I I I 2QK02D SI S I I SI I 2SMWYX SI 3E3XE3 SI 400BTP S S I I 424NFI S S I I I I 4ED4U4 S S I 4FLYLL I SI 4P9OST S I 4ZRH5B SI 5AL4YL S I 5ZSPFZ S I 6CS6GB S I 77H7IH S I I 78CN24 S I 7BREL7 S S S I 7H5WS7 I SI 88O8O8 SI S S I 8KXYZQ SI ASAP-TOF 8LLTJE S I 8QXEZ5 SI I I I I 99WMWJ SI 9EU3UC S I I 9WEC99 I SI SI

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Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 AJWS6O S S I AMA50Q S SI I SI APYADP S S I B824TN I I SI I BBEBBB I S I I I BPBBMB S SI I I BZBJBP SI I C2WUON SI C5ZRZ2 S I I CIIE5Y S S S I CLW6JW S S S I I CQC6CC I SI I CSDDCC SI DDXKOD S S S I I DVAVS7 I SI EIJIBE S S S I EK1BZR S S I I EYBQOO SI S S S I I I EYEEEV S S I I F66RUS I SI I I LCMS FF11HE S I I I I FNZI88 SI G9XDGK I I GUEUUR S S I I HPPPFP S I I SI I HRHXY5 S S I I HSJGXV S I IBADDP I IQXIII SI IYZYBB I I S IMMUNOCHEMICAL J9KZ5A I I SI JBRMJJ SI JCJPKW S S I JGOKP5 I SI JNYC8O S S I I JQIGMD S S I I JTSJJD S S I S 210(Fast Blue B salt Test) JUNUUU S I I I K7QIQW S S S I

2013/1-SM (57) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 KBTTYE S I KFTKVQ S S S I KW3BDH SI L1N1AS S S S I I LACFSF S S I LLDWGL SI SI LTLGBL S S S I I LTXFMY S SI S I M5FWNJ S SI I MDPWHT S I I MKND72 S S SI SI MMHHSD S S S I I MRHASS SI N0NNLS S I I N1M8LG SI I N666MQ S S I NA2AKJ I I NO9OBB I SI I NPDHYI S S S S I I I O0LRTK I I SI OPBW2C I SI OVCNJF S S S I I PCIBIV I S S SI I SI I PDGMFW I I SI PPHC9X SI I PQLTDR S SI I I PSOAIJ S I I PUS7H2 S I QJIQTJ I R8O18R SI I I RIJOTJ SI RPGPEM S I I I RXGBPA SI I S2O5GO I S I I SI I I I liberman S6OORI I SI I SADCGQ I SI SOQRQ9 SI SSOSVY I I SSSCSJ I SI

2013/1-SM (58) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 T0QNTU I TBBUSK SI I TDDURM I SI TXQHJG S I I UHMVSZ S S I I UT6VEX SI UTL3JI S I VFLGQF I S Immunochromatography VLZ8LL S S S S I I VMSX5E SI W4SM4Y S S I SI I WKJAI3 SI S SI I I WPYVIW S S S I I I I XRD XKGJ2G SI I UPHLC/ELSD XPE2VZ S I I YCSW1Z I SI I YETFFI S S I I YULAAJ S S I YYMCDP S I Z4FNNZ S I I I RAMAN

2013/1-SM (59) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary for test sample 3 The response summary of all 126 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: 132

Lactose: 60 Nimetazepam: 120

False positives for Test Sample 3 (controlled substances)

Code Name Technique VFLGQF Metamfetamine 180

False negatives for SM-3 (techinque(s) used or ANP) . Code - 4FLYLL (180), 78CN24 (150), UHNVSZ (171/180 ), UT6VEX ( 180) UTL3JI (180), 424NFI (ANP), 7H5W57 (ANP), 88O8O8 (ANP), QJIQTJ (ANP), S2O5GO (ANP), YYMCDP (ANP), VFLGQF (ANP)

Frequency of use of screening and identification techniques: Response Summary Participants: Response 126 Summary Participants: 132 Section 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 Screening 42 50 35 18 0 2 0 2 45 7 0 0 0 1 4 31.8% 37.9% 26.5% 13.6% 0.0% 1.5% 0.0% 1.5% 34.1% 5.3% 0.0% 0.0% 0.0% 0.8% 3.0% Identification 10 5 2 32 9 15 1 21 118 45 2 2 2 3 7 7.6% 3.8% 1.5% 24.2% 6.8% 11.4% 0.8% 15.9% 89.4% 34.1% 1.5% 1.5% 1.5% 2.3% 5.3% # labs using 47 52 37 41 9 16 1 22 118 46 2 2 2 3 10 this 35.6% 39.4% 28.0% 31.1% 6.8% 12.1% 0.8% 16.7% 89.4% 34.8% 1.5% 1.5% 1.5% 2.3% 7.6% technique

2013/1-SM (60) Copyright (c) 2013 UNODC

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

Z-Scores for Test Sample 3

Nimetazepam CODE MAD: 0.3 Conc. * AbsDev ZScore 0DAKSM 3.8 0.0 0.1 0SRDXD 10.0 6.3 15.2 1HR18P 4.1 0.4 1.0 1SWNJJ 3.6 0.1 0.2 2FELET 0.1 3.7 8.8 2SMWYX 3.8 0.1 0.2 4ZRH5B 3.5 0.2 0.5 7BREL7 3.6 0.1 0.3 8LLTJE 2.8 0.9 2.2 8QXEZ5 7.0 3.3 8.0 9EU3UC 8.2 4.5 10.8 BBEBBB 3.5 0.2 0.5 BZBJBP 3.1 0.6 1.4 C2WUON 3.8 0.1 0.3 EYBQOO 7.2 3.5 8.4 FNZI88 3.0 0.7 1.6 IYZYBB 13.6 9.9 23.9 J9KZ5A 3.8 0.1 0.2 JGOKP5 3.8 0.1 0.2 JNYC8O 3.3 0.4 0.9 JUNUUU 3.6 0.1 0.3 K7QIQW 2.7 1.0 2.3 KBTTYE 3.5 0.2 0.5 KFTKVQ 3.1 0.6 1.5 L1N1AS 3.2 0.5 1.1 MKND72 2.9 0.8 1.9 MRHASS 3.8 0.1 0.2 N1M8LG 2.9 0.9 2.0 NPDHYI 3.8 0.1 0.2 OPBW2C 3.2 0.5 1.3 OVCNJF 24.8 21.1 50.9 PDGMFW 2.7 1.0 2.4 RPGPEM 3.7 0.0 0.0 RXGBPA 15.5 11.8 28.4 SADCGQ 3.7 0.1 0.1 SOQRQ9 3.8 0.1 0.2 SSSCSJ 4.0 0.3 0.7 VLZ8LL 3.6 0.1 0.2 W4SM4Y 3.4 0.3 0.7 WKJAI3 3.8 0.1 0.2 XPE2VZ 10.0 6.3 15.2

2013/1-SM (61) Copyright (c) 2013 UNODC Z-Score Report per Sample per Substance

Round: 2013/1 Substance: SM-3/Nimetazepam Median = 3.7 MAD = 0.3 UNODC value = 3.7

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

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

Sample 4 Analysis

Identified substances for Test Sample 4 Code Identified Substances 00H0DT amphetamine 0DAKSM Amfetamine 0SRDXD amphetamine 0T0BVS ANFETAMINA 1HR18P Amphetamine 1SWNJJ amfetamine 22JWSL Amfetamine 2ACHVO 2FELET Amfetamine 2IOV6B metamphétamine 2QK02D Anfetamina 2SMWYX Amfetamine 3E3XE3 Amphetamine 400BTP Amphetamine 424NFI Amfetamine 4ED4U4 Amfetamine 4FLYLL AMFETAMINE 4P9OST Amphetamine 4ZRH5B amfetamine 5AL4YL amfetamine sulphate 5ZSPFZ anfetamine 6CS6GB Anfetamina 77H7IH Amphetamine 78CN24 Amphétamine 7BREL7 Amphetamine 88O8O8 amfetamine 8KXYZQ Amphetamine 8LLTJE amphetamine 8QXEZ5 amfetamine 99WMWJ Amfetamine 9EU3UC Amphetamine 9WEC99 AMFETAMINE AJWS6O Amphetamine AMA50Q Amphetamine APYADP we found amphetamine B824TN Amfetamine BBEBBB Amphetamine Sulphate BPBBMB Amphetamine BZBJBP Amphetamine C2WUON Amfetamine

2013/1-SM (63) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances C5ZRZ2 AMPHETAMINE CIIE5Y NO CLW6JW Amphetamine CQC6CC AMPHETAMINE CSDDCC AMFETAMIN SULFATE DDXKOD Amphetamine DVAVS7 amphetamine EIJIBE AMPHETAMINE EK1BZR Amphetamine EYBQOO Amfetamine, metamfetamine EYEEEV amfetamine F66RUS Amphetamine FF11HE amphetamine G9XDGK Amfetamine GUEUUR Amphetamine HPPPFP amphetamine HRHXY5 Amfetamine HSJGXV Amphetamine IBADDP Amphetamine IQXIII amphetamine IYZYBB amphetamines (amphetamine) J9KZ5A Amphetamine JBRMJJ Amphetamine JCJPKW Amphetamine JGOKP5 Amphetamine JQIGMD AMFETAMINE JTSJJD Amfetamine JUNUUU Amphetamine KBTTYE Amphetamine KFTKVQ Amphetamine L1N1AS Amphetamine LACFSF Anfetamina LLDWGL Amfetamine LTLGBL Amfetamine LTXFMY Amphetamine M5FWNJ amfetamine MDPWHT amfetamine, metamfetamine MKND72 Amfetamine MMHHSD Amphetamine MRHASS Amfetamine N0NNLS amfetamine N1M8LG Amphetamine N666MQ Amfetamine. NA2AKJ amphetamine sulphate

2013/1-SM (64) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Identified Substances NO9OBB Amphetamine NPDHYI amfetamine O0LRTK amfetamine OPBW2C Amphetamine and sucrose OVCNJF Amfetamine PCIBIV Isosorbide PDGMFW Amphetamine PPHC9X amfetamine PQLTDR amfetamin PSOAIJ Anfetamine PUS7H2 Anfetamina QJIQTJ amfetamine R8O18R Amphetamine RIJOTJ amphetamine RPGPEM amphetamine sulphate RXGBPA amfetamine S2O5GO anfetamina S6OORI amphetamine SADCGQ Amfetamine SOQRQ9 AMPHETAMINE SSOSVY Amphetamine SSSCSJ amfetamine T0QNTU Amfetamine TBBUSK amphetamine TXQHJG amphetamine UHMVSZ ANFETAMINA UT6VEX Amfetamine UTL3JI anphetamine VFLGQF amphetamine VLZ8LL amphetamine VMSX5E AMFETAMINE SO4 W4SM4Y Amphetamine WKJAI3 amphetamine WPYVIW Amphetamine sulphate XKGJ2G Amphetamine and Methamphetamine XPE2VZ Amphetamine YCSW1Z amfetamine YETFFI Amfetamine sulphate YULAAJ afetamine YYMCDP amfetamine Z4FNNZ Amphetamine

2013/1-SM (65) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Statement of findings for Test Sample 4

Code Amfetamine 00H0DT + Amphetamine is controlled by law (KB 22/01/1998). 0DAKSM + The sample contains the controlled drug amfetamine 9.55 %, m/m. 0SRDXD + The powder is a mixture of sucrose and amphetamine. The concentration of amphetamine in the sample is 4.9% by weight. 0T0BVS + La sustancia analizada se trata de anfetamina 1HR18P +

1R7FTA - Based on the above analysis, dangerous drugs were not detected in the sample 1SWNJJ +

22JWSL + The sample SM-4 contains amfetamine. 2ACHVO + amphetamine also trace of methamphetamine 2FELET + SM-1 was found to be contain Amfetamine 2IOV6B - sucrose 2QK02D + se identificó como D-Anfetamina 2SMWYX + SM4 was prepared from a seizure containing 8.34% w/w amfetamine base. 3E3XE3 +

400BTP + In the sample analyzed was detected the presence of amphetamine, piperidine 2-(phenyl methyl) and sucrose. 424NFI + Sample 2013/1/SM-4 consists of white powder. Amfetamine, a prohibited sudstance included in the National Law for Narcotics, is found to be present in this sample.

2013/1-SM (66) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Amfetamine 4ED4U4 + 0.229 grams of a powder containing 10% Amfetamine. Amfetamine is a Class B drug subject to the provisions of the Misuse of Drugs Act 1971. 4FLYLL +

4P9OST + Sample 2013/1/SM-4 was found to contain controlled substance AMPHETAMINE, a Schedule II drug under the Convention on Psychotropic Substances. 4ZRH5B + amfetamine 5AL4YL +

5ZSPFZ + we found in that sample many different sugars. 6CS6GB + Hexosa, 1,6 Anhidro-alfa-D-Galactosa 77H7IH + We found Amphetamine in SM-4 as controlled drug 78CN24 + Après analyse, l'échantillon 2013/1/SM-4 contient l'amphétamine 7BREL7 + On analysis, i found the substances to contain 10.83% of amphetamine. 7H5WS7 ANP

88O8O8 +

8KXYZQ + Sample contain Amphetamine. 8LLTJE + amphetamine was as sulfate form 8QXEZ5 + amfetamine,sorbitol, trimethyltriborate 99WMWJ + The sample contains 8.3 % amfetamine 9EU3UC +

2013/1-SM (67) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Amfetamine 9WEC99 + / AJWS6O + One glass bottle labelled '2013/1/SM-4' containing 0.221g of off-white powder. This powder contained on average of 10% amphetamine. Amphetamine is a class B controlled drug under the misuse of Drugs Act (1971)(as ammended). AMA50Q + White powder containing amphpetamine. APYADP + the sample was confirmed by gc ms B824TN + Amfetamine BBEBBB + SM 4 contain also Sucrose BPBBMB + Analysis of the powder revealed the presence of Amphetamine BZBJBP + Amphetamine, sucrose C2WUON + - C5ZRZ2 + SORBITOL CIIE5Y - IN THE SAMPLE RECEIVED IN COLOR AMBER GLASS BOTTLE WITH PLASTIC CAP STAMPED GREEN MISSING AS DRUGS 2013/1/SM-4. CLW6JW + Diluted with sucrose CQC6CC + AMPHETAMINE 10.3% AS BASE. CSDDCC + saccharose, sorbitol or DDXKOD + The sample 2013/1/SM-4 was found to contain Amphetamine. DVAVS7 + The sample contains amphetamine which is scheduled as illicit drug in France. EIJIBE + AMPHETAMINE SULFATE (15.5 as base)

2013/1-SM (68) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Amfetamine EK1BZR + The powder was analysed and found to contain amphetamine. EYBQOO + SM-4 contains amfetamine, 4,1% and trace quantity of metamfetamine EYEEEV + *Retention time and fragmentation pattern obtained with the sample are equivalent to those obtained with amfetamine. F66RUS + Sample contain drug- Amphetamine FF11HE + amphetamine with traces of metamphetamine and sucrose FNZI88 +

G9XDGK + The sample SM4 contained 9,9 % amfetamine calculated as a base. In this sample was identified saccharose GUEUUR + One glass vial with lid attached containing 225mg of off-white powder containing an average of 10% amphetamine. HPPPFP + + saccharose HRHXY5 + The sample contains amfetamine and caffeine. HSJGXV + Amphetamine (9.68% base) and glucitol IBADDP + On analysis, the powder was found to contain amphetamine.

IQXIII + found amphetamine with 9.5% w/w, mannitol, N-methyliminopropylbenzene, oleamide, 5- (hydroxymethyl)-2-furfural IYZYBB + we have not received standards J9KZ5A + The sample contains 13.1% Amphetamine as a base. In the sample was identified glucose and Sucrose as adulterant. JBRMJJ +

2013/1-SM (69) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Amfetamine JCJPKW + Off -white powder found to contain amphetamine at a concentration of 9 per cent. JGOKP5 +

JNYC8O - No dangerous drug detected in sample SM-4. JQIGMD +

JTSJJD + At first Screening Test was performed and confirmed by TLC method in two different solvent system. JUNUUU + Color test : Marquis = orange becoming brown, Simon = pnk to cherry-red TLC : TA and TE = Amphetamine GC : Amphetamine base 10.89% K7QIQW - No drug was found in SM-4. KBTTYE + After analysis, the sample was found to contain amphetamine. KFTKVQ + The sample was found to contain amphetamine. KW3BDH -

L1N1AS + Amfetamine was identified by TLC and GC/MS LACFSF + Las pruebas químicas y la coincidencia en los tiempos de retención y fragmentos de masas del material de referencia usado en las mismas condiciones que la muestra analizada, indican la presencia de anfetamina. LLDWGL + Sample contains 9.82 ± 0.54 % amfetamine-base. Sample also contains sucrose and DPIA in trace level. LTLGBL +

LTXFMY + Marquis reagent and Scott reagent have been applied, the TLC and GC/FID M5FWNJ +

2013/1-SM (70) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Amfetamine MDPWHT + The sample is amfetamine with metamfetamine traces. MKND72 +

MMHHSD + White, odourless powder, tested positive for Amphetamine, a substance listed in Table C of the Law on Addictive Substances. MRHASS + The sample contains amfetamine. N0NNLS +

N1M8LG + We also found sucrose. N666MQ + Applied chemical tests and instrumental chemical analysis, that sample 2013/1/SM4 contains Amfetamine. NA2AKJ + One brown glass bottle containing 233mg of an off-white powder. This off-white powder contained an average of 13% of amphetamine sulphate. (Note 9% base). NO9OBB + The power contained amphetamine sulfate with saccharose. NPDHYI + Presence of amfetamin sulphate was detected in the sample. O0LRTK + White powder containing amfetamine (9.3%). It contains also sucrose and sorbitol (not quantified) OPBW2C +

OVCNJF + White powder containing amfetamine with a 9.59% as base. PCIBIV +

PDGMFW + Sugar PPHC9X + powder contains amfetamine with saccharose and manitol PQLTDR + szacharóz

2013/1-SM (71) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Amfetamine PSOAIJ + Contains sucrose and sorbitol PUS7H2 + D-Manitol, Beta-D-Glucopyranose,1,6 Anhydro y 1,6-Anhydro-Įd-galactofuranose QJIQTJ +

R8O18R + Powder contains Amphetamine wich is a controlled substance RIJOTJ + white powder containing amphetamine (6.9%). RPGPEM + sample contains also sorbitol RXGBPA + suggar, fatty acids , S2O5GO + Pruebas colorimétricas, Marquis, FT-IR, HPLC-DAD Y TLC S6OORI + saccharose SADCGQ +

SOQRQ9 + POWDER CONTAINING AMPHETAMINE SSOSVY + The sample contains amphetamine which is listed as a controlled drug according to french order, appendix III of February 22nd 1990. SSSCSJ +

T0QNTU + In the test sample 2013/1/SM-2 was detected amfetamine TBBUSK + white powder, mixture of the amphetamine and sucrose TDDURM - the sample not correspond is abuse drugs TXQHJG +

2013/1-SM (72) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code Amfetamine UHMVSZ +

UT6VEX + Test sample 2013/1/SM-4 was found to contain the following controlled drug Amphetamine. UTL3JI + The results of the tests of the SM 4 (134) received confirmed that the mentioned sample contains anphetamine but we are not able to give a cuantification result because we have not got the pattern of the mentioned controlled drug VFLGQF + the sample was found to contain amphetamine VLZ8LL + The sample SM-4 found to contain 10,5 % amphetamine. The seizure also contains metamfetamine (trace quantity), sucrose and unidentified substance. VMSX5E + MANNITOL, SACCHAROSE W4SM4Y + One glass bottle containing 0.20 grammes of a powder containing 0.01 grammes of amphetamine. WKJAI3 + CR, TLC, FTIR, GC, GC/MS WPYVIW + Base Amphetamine 10,72%, Sorbitol and Sucrose XKGJ2G + The sample was found to contain amphetamine and trace amounts of methamphetamine. XPE2VZ + In the 0,230 g unknown powder it is found 20% Amphetamine. YCSW1Z + This sample also contains saccharose. YETFFI + This sample contains amfetamine sulphate (11.7% as base) with mannitol and sucrose YULAAJ +

YYMCDP + marquis reagent is positive (orange) to amfetamine ant Scott reagent is negative. In the chromatogram the retention time is like amfetamine. So, the substance is amfetamine. Z4FNNZ + Test Sample 2013/1/SM-4 contains Amphetamine

2013/1-SM (73) Copyright (c) 2013 UNODC 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

Analytical Technique Codes Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 00H0DT I S 0DAKSM I SI 0SRDXD I I I SI I I XRD 0T0BVS SI I 1HR18P I SI 1R7FTA S I 1SWNJJ I SI SI 22JWSL S S I I 2ACHVO SI I 2FELET S S I I 2IOV6B SI I I I 2QK02D SI S I I SI I 2SMWYX SI 3E3XE3 SI 400BTP S S I I 424NFI S S I I I I 4ED4U4 S S I 4FLYLL I SI 4P9OST S I 4ZRH5B SI 5AL4YL S I 5ZSPFZ S I 6CS6GB S I 77H7IH S I I 78CN24 S I 7BREL7 S S S I 7H5WS7 I SI 88O8O8 SI S S I 8KXYZQ SI ASAP-TOF 8LLTJE S I 8QXEZ5 SI I I I I 99WMWJ SI 9EU3UC S I I 9WEC99 I SI SI

2013/1-SM (74) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 AJWS6O S S I AMA50Q S SI I SI APYADP S S I B824TN I I SI I BBEBBB I S I I I BPBBMB S SI I I BZBJBP SI I C2WUON SI C5ZRZ2 S I I CIIE5Y S S S I CLW6JW S S S I I CQC6CC I SI I CSDDCC SI DDXKOD S S S I I DVAVS7 I SI EIJIBE S S S I EK1BZR S S I I EYBQOO SI S S S I I I EYEEEV S S I I F66RUS I SI I I LCMS FF11HE S I I I I FNZI88 SI G9XDGK I I GUEUUR S S I I HPPPFP S I I SI I HRHXY5 S S I I HSJGXV S I IBADDP I IQXIII SI IYZYBB I I S IMMUNOCHEMICAL J9KZ5A I I SI JBRMJJ SI JCJPKW S S I JGOKP5 I SI JNYC8O S S I I JQIGMD S S I I JTSJJD S S I S 210(Fast Blue B salt Test) JUNUUU S I I I K7QIQW S S S I

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Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 KBTTYE S I KFTKVQ S S S I KW3BDH SI L1N1AS S S S I I LACFSF S S I LLDWGL SI SI LTLGBL S S S I I LTXFMY S SI S I M5FWNJ S SI I MDPWHT S I I MKND72 S S SI SI MMHHSD S S S I I MRHASS SI N0NNLS S I I N1M8LG SI I N666MQ S S I NA2AKJ I I NO9OBB I SI I NPDHYI S S S S I I I O0LRTK I I SI OPBW2C I SI OVCNJF S S S I I PCIBIV I S S SI I SI I PDGMFW I I SI PPHC9X SI I PQLTDR S SI I I PSOAIJ S I I PUS7H2 S I QJIQTJ I R8O18R SI I I RIJOTJ SI RPGPEM S I I I RXGBPA SI I S2O5GO I S I I SI I I I liberman S6OORI I SI I SADCGQ I SI SOQRQ9 SI SSOSVY I I SSSCSJ I SI

2013/1-SM (76) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 T0QNTU I TBBUSK SI I TDDURM I SI TXQHJG S I I UHMVSZ S S I I UT6VEX SI UTL3JI S I VFLGQF I S Immunochromatography VLZ8LL S S S S I I VMSX5E SI W4SM4Y S S I SI I WKJAI3 SI S SI I I WPYVIW S S S I I I I XRD XKGJ2G SI I UPHLC/ELSD XPE2VZ S I I YCSW1Z I SI I YETFFI S S I I YULAAJ S S I YYMCDP S I Z4FNNZ S I I I RAMAN

2013/1-SM (77) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary for test sample 4 The response summary of all 126 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:

H Response Summary Participants: 132

Amfetamine: 124

False positives for Test Sample 4 (controlled substances)

Code Name Technique S2O5GO 142/190

False negatives for SM-4 (techinque(s) used or ANP) . Code - CIIE5Y (180), IR7FTA (180), 2IOV6B (180 ), 7H5WS7 (ANP) JNYC8O, (180), K7QIQW (180), KW3BDH (180), TDDURM (140/180)

Frequency of use of screening and identification techniques: Response Summary Response Summary Participants: 126 Participants: 132 Section 141 Section 140 141 142 150 160 161 170 171 180 190 200 220 230 231 210 Screening 42 50 35 18 0 2 0 2 45 7 0 0 0 1 4 31.8% 37.9% 26.5% 13.6% 0.0% 1.5% 0.0% 1.5% 34.1% 5.3% 0.0% 0.0% 0.0% 0.8% 3.0% Identification 10 5 2 32 9 15 1 21 118 45 2 2 2 3 7 7.6% 3.8% 1.5% 24.2% 6.8% 11.4% 0.8% 15.9% 89.4% 34.1% 1.5% 1.5% 1.5% 2.3% 5.3% # labs using 47 52 37 41 9 16 1 22 118 46 2 2 2 3 10 this 35.6% 39.4% 28.0% 31.1% 6.8% 12.1% 0.8% 16.7% 89.4% 34.8% 1.5% 1.5% 1.5% 2.3% 7.6% technique

2013/1-SM (78) Copyright (c) 2013 UNODC

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

Z-Scores for Test Sample 4

Amfetamine Amfetamine MAD: 0.9 CODE MAD: 0.9 CODE Conc. * AbsDev ZScore Conc. * AbsDev ZScore 00H0DT 9.2 0.7 0.5 JQIGMD 8.9 1.0 0.8 0DAKSM 9.6 0.4 0.3 JUNUUU 10.9 1.0 0.7 0SRDXD 4.9 5.0 3.8 L1N1AS 11.3 1.4 1.1 1HR18P 10.7 0.8 0.6 LLDWGL 9.8 0.1 0.1 1SWNJJ 9.6 0.3 0.2 MDPWHT 10.4 0.5 0.4 2FELET 10.4 0.5 0.4 MKND72 8.2 1.7 1.3 2SMWYX 8.3 1.6 1.2 MMHHSD 9.1 0.8 0.6 3E3XE3 11.2 1.3 1.0 MRHASS 5.5 4.4 3.3 4ED4U4 10.0 0.1 0.1 N1M8LG 6.9 3.0 2.3 4P9OST 11.0 1.1 0.8 NA2AKJ 9.0 0.9 0.7 4ZRH5B 10.0 0.1 0.1 NPDHYI 9.2 0.7 0.5 5ZSPFZ 9.0 0.9 0.7 O0LRTK 9.3 0.6 0.5 7BREL7 10.8 0.9 0.7 OPBW2C 10.0 0.1 0.1 8LLTJE 12.6 2.7 2.0 OVCNJF 9.6 0.3 0.2 8QXEZ5 10.0 0.1 0.1 PDGMFW 10.6 0.7 0.5 99WMWJ 8.3 1.6 1.2 PPHC9X 11.0 1.1 0.8 9EU3UC 6.6 3.3 2.5 RIJOTJ 6.9 3.0 2.3 9WEC99 8.9 1.0 0.8 RPGPEM 9.8 0.1 0.1 AJWS6O 10.0 0.1 0.1 RXGBPA 0.8 9.1 6.8 BBEBBB 10.4 0.5 0.4 SADCGQ 8.7 1.2 0.9 BZBJBP 7.9 2.0 1.5 SOQRQ9 9.8 0.1 0.1 C2WUON 10.7 0.8 0.6 SSOSVY 10.4 0.5 0.4 C5ZRZ2 10.2 0.3 0.2 SSSCSJ 12.0 2.1 1.6 CQC6CC 10.3 0.4 0.3 T0QNTU 8.0 1.9 1.4 CSDDCC 11.0 1.1 0.8 TBBUSK 10.0 0.1 0.1 DVAVS7 9.0 0.9 0.7 UHMVSZ 25.2 15.3 11.5 EIJIBE 15.5 5.6 4.2 VFLGQF 5.1 4.9 3.6 EYBQOO 4.1 5.8 4.4 VLZ8LL 10.5 0.6 0.5 FF11HE 11.2 1.3 1.0 W4SM4Y 9.9 0.1 0.0 FNZI88 9.8 0.1 0.1 WKJAI3 7.0 2.9 2.2 G9XDGK 9.9 0.0 0.0 WPYVIW 10.7 0.8 0.6 GUEUUR 11.0 1.1 0.8 XPE2VZ 20.0 10.1 7.6 HPPPFP 9.0 0.9 0.7 YETFFI 11.7 1.8 1.4 HRHXY5 9.7 0.2 0.2 YULAAJ 12.0 2.1 1.6 HSJGXV 9.7 0.2 0.2 YYMCDP 9.0 0.9 0.7 IBADDP 9.9 0.0 0.0 *) Concentration: w/w % IQXIII 9.5 0.4 0.3 IYZYBB 15.6 5.7 4.3 J9KZ5A 13.1 3.2 2.4 JCJPKW 9.0 0.9 0.7 JGOKP5 10.4 0.5 0.4

2013/1-SM (79) Copyright (c) 2013 UNODC Z-Score Report per Sample per Substance

Round: 2013/1 Substance: SM-4/Amfetamine Median = 9.9 MAD = 0.9 UNODC value = 10.3

Z-Score has been calculated as modified Z-Score as it is a robust method and therefore relatively insensitive to outliers. Modified Z-Score = 0.6745 * AbsDev/MAD AbsDev = Absolute value of the difference between a laboratory value and the median of all the laboratory values for the given drug; MAD = median absolute deviation about the median. Modified Z-scores with an absolute value of greater than 3.5 should be considered as potential outliers. Reference: Iglewicz, B. and Hoaglin, D. C.: 1993 How to Detect and Handle Outliers, American Society for Quality Control, Milwaukee, WI

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

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2013/1-SM (81) Copyright (c) 2013 UNODC