INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report

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INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary Report

SEIZED MATERIALS 2016/1

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

Table of contents Sample 1 Analysis Page 6 Identified substances Page 6 Statement of findings Page 11 Identification methods Page 20 False positives Page 26 Z-Scores Page 27 Sample 2 Analysis Page 31 Identified substances Page 31 Statement of findings Page 36 Identification methods Page 46 False positives Page 52 Z-Scores Page 53 Sample 3 Analysis Page 56 Identified substances Page 56 Statement of findings Page 61 Identification methods Page 70 False positives Page 76 Z-Scores Page 77 Sample 4 Analysis Page 80 Identified substances Page 80 Statement of findings Page 82 Identification methods Page 88 False positives Page 94 Z-Scores Page 95 Test Samples Information

Samples Comments on samples Sample 1 SM-1 was prepared from a seizure containing 50.5 % (w/w) Cocaine base. The test sample also contained caffeine and levamisole. Benzoylecgonine and cinnamoyl cocaine were also detected as minor components. Sample 2 SM-2 was prepared from a seizure containing 13.8 % (w/w) MDMA. The test sample also contained lactose.

Sample 3 SM-3 was prepared from a seizure containing 5.5 % (w/w) Amfetamine base. The test sample also contained caffeine and creatine.

Sample 4 SM-4 wss a blank test sample prepared from plant material and contained no substances from the ICE menu

Samples Substances Concentrations Comments on substances Sample 1 Caffeine - Quantification not required Cocaine 50.5 % Sample 2 3,4-Methylenedioxymetamfetamine (MDMA) 13.8 % Lactose - Quantification not required Sample 3 Amfetamine 5.5 % Caffeine - Quantification not required Sample 4 [blank sample]

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. 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

In the 2016/1 round of the ICE programme, results were submitted within both the Seized Materials (SM) and Biological Specimens (BS) test groups by 220 laboratories in 68 countries. Within the SM test group, there were 183 participating laboratories from 65 countries and within the BS test group, results were submitted by 92 laboratories from 46 countries.

Qualitative Analysis

The analytical technique most commonly used for screening of test samples in the SM test group was the marquis reagent (40% of participants), while GC-MS (91% of participants) was the most commonly used technique for identification/confirmation of the components in the test samples followed by FTIR (43% of participants). The results for the qualitative identification of the controlled substances in the SM test group, the number of false positive/negative results and the analyses not performed are shown in the table 1.

Table 1. Performance of participants in the 2015/2 round of ICE.

SM-1 SM-2 SM-3 Test sample SM-4 (blank) (Cocaine) (MDMA) (Amfetamine)

Correct identification by 100% 98% 93% N/A participants Number of false positives 3 4 7 14 Number of false negatives 0 2 9 - Number of Analyses not performed 0 2 2 -

While the overall number of false positive/negative results reported by ICE participants is encouragingly low, 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. There were only a total of four analyses not performed. ICE participants should note that test samples can contain any of the substances in the ICE menu and screening and identification carried out should take this into account.

Quantitative Analysis

The number of participants who carried out quantitative analysis, 126 (69%) for SM-1, 107 (58%) for SM-2 and 94 (51%) for SM-3 continues to be encouraging, particularly the high percentage of participants who quantified the cocaine in SM-1. It is also encouraging that 130 (71%) of participants in the SM test group

3 performed quantitation and of these, 110 (84%) quantified more than one substance and 87 (67%) quantified all three test samples containing controlled substances. 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, 53% used GC-FID, 29% used HPLC and 18% used mass spectrometry. z-scores obtained by participants in quantification are shown in table 2 below.

Table 2. Quantitative performance of participants in the 2016/1 round of ICE.

Test sample z-score SM-1 SM-2 SM-3 SM-4 (Cocaine) (MDMA) (Amfetamine) (Blank) |z| < 2, satisfactory 83% 87% 81%

2 ≤ |z| ≤ 3, questionable 6% 8% 9%

|z| > 3, unsatisfactory 11% 5% 10%

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. Participants with z-scores outside acceptable limits should review their quantification procedures.

In the 2015/2 round of ICE, 16 laboratories obtained questionable z-scores with 2 ≤ |z| < 3. 13 of these laboratories participated and performed quantification in the 2016/1 round with 11, (84%) improving their performance and obtaining acceptable z-scores with |z| < 2 for at least one substance. Four of these laboratories also obtained questionable z-scores and five laboratories also obtained unsatisfactory z-scores in 2016/1.

25 laboratories obtained unsatisfactory z-scores in ICE 2015/2 with |z| ≥ 3. Of these laboratories, 15 participated in ICE 2016/1 and performed quantification, with 14 (93%) improving their performance in at least one substance. Seven (47%) of these laboratories also obtained an unsatisfactory z-score in the 2016/1 round of the ICE programme

Laboratories that need to perform quantitation routinely are encouraged to participate regularly in external proficiency testing or collaborative exercises such as the ICE programme. This will enable laboratories to assess the quality of their quantitative methods through the z-score values obtained. In addition to the use of z-scores as a measure of performance in quantitation, participants are encouraged to compare their results with the assigned values provided in individual quantification reports, to assess the accuracy of their quantitative performance. Laboratories reporting false positive or false negative results should investigate the root causes and corrective actions taken promptly in order to continuously improve performance. Participation in the ICE programme also helps in monitoring the effect of corrective actions. 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.

New Psychoactive Substances (NPS) reported by laboratories participating in the 2016/1 round of the ICE programme

During the 2016/1 round of ICE, participating laboratories provided information on NPS that had been identified in their laboratories. In total there were 214 reports of 136 substances. The most commonly reported substances were synthetic cathinones (33%) followed by synthetic cannabinoids (30%) as shown in figure 1.

4 Synthetic cannabinoids 5% 1% 1% 3% Synthetic cathinones 32% 15% Phenethylamines

Others

Piperazines 10% Ketamine and phencyclidine type substances Aminoindanes

33% Tryptamines

Figure 1. NPS reported by ICE laboratories during the 2016/1 round of ICE

In terms of the mechanism of action of the NPS reported by ICE participants, the predominant substances reported were stimulants (52%), while 30% were synthetic cannabinoid receptor agonists (SCRA’s) and 6% were dissociative substances as shown in figure 2.

3% 6% 4%

Stimulants 52% SCRAs Hallucinogens Sedatives/Hypnotics Dissociatives Opioids

30%

Figure 2. Mode of action of NPS most commonly reported by ICE participants in the 2016/1 round of ICE

NPS most commonly reported by laboratories participating in ICE 2016/1

The substance most often reported by ICE participants was the stimulant ethylone followed by the dissociative ketamine and the synthetic cannabinoid receptor agonists 5F-AKB48 and 5F-MDMB-PINACA. For further details on these substances and others reported to the UNODC Early Warning Advisory, ICE participants can log on to the UNODC ICE portal and select the icon for the Early Warning Advisory on New Psychoactive substances as shown below.

6 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

Sample 1 Analysis

Identified substances for Test Sample 1 Code Identified Substances 00T0J0 cocaine 1GZVLB cocaina 2IQBJI cocaine 2MO2K2 cocaine 2Q2RKB Cocaine 331I33 Cocaine 3HKZSM Cocaine 3J30PJ Cocaina (pseudococaina) 3QY6YS cocaine 3UCRFA cocaine 43D6WO Cocaine, purity 52.7% 4EUEWU COCAINE 4LYNGL cocaine, caffeine 4PGIDD cocaine HCl 4Z40VI cocaine 55STC5 Cocaine 5NU8Q8 Cocaine 5XSWBZ cocaine 66BMCC cocaine 6AKET8 Cocaine 6DWSSS cocaine hydrochloride 6ILHTL Cocaine 6QO4X5 cocaine hydrochloride 6UM71W cocaine 77DRQT cocaine 7BTAAO Cocaine 7VKRTZ Cocaine 8F8I8T cocaine 8IHHJF COCAINA 8IXV43 Cocaine 8LZBLR Cocaine 8NM0BB Cocaine and Caffeine 8PHIP8 Cocaine Hydrochloride 8YMBJO Cocaine 91AIRR Cocaine 9EWNN5 Cocaine A1O2PU cocaine AA3A9G Cocaine AAL7YF cocaine AD2NVY COCAINE

Code Identified Substances AJO81E Cocaine and caffeine ASUW2S Cocaine AZCZ5Z cocaine B54OW4 cocaine BABKJE Cocaine BAYYXO cocaine BEUIGW Cocaina BPJ4JR Cocaine hydrochloride BT6Y0Y Cocaine C7G4DH cocaine, CE7TB2 Cocaine CIFQC8 Cocaine CSJXFO Cocaine DALAM7 COCAINE DWWWGY COCAINA DY0EG9 cocaine E8S7ZT Cocaine EAE6LE Cocaine EDUYDD Cocaine EJBJCJ cocaine ELQNHU Cocaine ENI7TJ Cocaine EXIP84 cocaine hydrochloride EYAWUL Cocaine EYAZVH Cocaine F1M4VD Cocaine F9I31B cocaine hcl FJ44OK Cocaine G1C7O1 Cocaine GCHGCL Cocaine GDGBEX Cocaine GLYEEK cocaine H7SE4O cocaine HCVNSQ cocaine HNG20U Cocaine 50.5% +/- 3.7% HW0WRM Cocaine IBPJLJ Cocaine hydrochloride, (caffeine and levamisole also present) ICQNLB Cocaine IIX7UR Cocaine, caffeine and Levamisole ISA8Y8 Cocaine IUW8JU Cocaine IXUGYG Cocaine J28855 COCAINE J5YB55 Cocaine

Code Identified Substances JJLJOU Cocaine, Caffeine, Levamisole KBC4MU COCAINE KHHK0G Cocaine KJU4OU cocaine,caffeine KLL25F Cocaine KNZKKP cocaine KTJBZA cocaine, methylecgonine, cis-trans cynnamoyl cocaine KWPD3V cocaine KYO332 Cocaine L9LTEO Cocaine LEPP7L cocaine and caffeine LFCJGM Cocaine LGECDN Cocaine LLLLTB cocaine LNR2DR Cocaine chlorydrate M5LL0L cocaine M9MFMP Cocaine, caffeine MBOMMM cocaine HCl MCOLDO cocaine MOOSOO cocaine MQXQRQ Cocaine MVVNXZ Cocaine NNNNDW Cocaine O1DHE1 Cocaine mixed with caffeine and levamisole O28H4R Cocaine OF6Y6D cocaine OFP7ET Cocaine OOOIMO Cocaine OOXOOI COCAINE OSTFUT cocaine OWRO6K Cocaine OYX2R3 COCAINE OZLPCC Cocaine P3Y0QX cocaine P5A5W5 Cocaine P7ZPBP Yes Cocaine and Ketamine PPPKPP Cocaine QOMLQQ cocaine QS88SU Cocaine QUZQUQ Cocaine QWO4OF COCAINE R25T2B cocaine R2XKWH Cocaine R3QRYO Cocaine and Caffeine

Code Identified Substances RC98IL COCAINE HCL RV3YT3 Cocaine S9YJGM COCAINE SDFWC8 Cocaine HCl SEF3EE Cocaine SK102M cocaine SLDIJQ cocaine SSOFTB cocaine T7YTFO cocaine TBK0V2 MEFEDRONA, COCAINA TDVDNQ Cocaine TEZEE4 COCAINE, CAFFEINE, LEVAMISOL TIKKKK Cocaine TRQBQ8 COCAINE HCL TSGAGB COCAINE, CAFFEINE TWTWPH Cocaine TWYAAL cocaine U90SWA cocaine chlorhydrate UFVIOP Cocaine UQMBX2 COCAINE, CAFFEINE UYPU5U Cocaine Hydrochloride VFD46A cocaine VKNECE Cocaine 52.28 VNZ61V COCAINE VQT273 Cocaine VXFBR6 Cocaine VXXXL4 cocaine VYZC85 cocaine WDNNGN cocaine/MDMA WDQWLH Cocaine X2JISE Cocaine X456G5 COCAINE, CAFFEINE X70OZ9 cocaine XFVW1V Cocaine XNQ60K cocaine XQJTD9 Cocaine XRKU5U Cocaine Y38I3T cocaine YAH8BE cocaine YAIIVO Cocaine Hydrochloride YEKYTF cocaine YXZMMX Cocaine YY5Y1A Cocaine YY7MQP cocaine, caffeine y levamisole

Code Identified Substances YYZUYY Cocaine Z5LF55 cocaine Z887DL Cocaine ZF1EFF Cocaine ZFFEHN COCAINE 52.9%, CAFFEINE ZH0THY Cocaine ZOIJZ3 COCAINE ZRG6U6 cocaine ZSX0SS Cocaine ZXIIII Cocaine

Statement of findings for Test Sample 1

Code Caffeine Cocaine 00T0J0 + + Sample was found to contain cocaine-HCl, anhydrecgonine methylester, pseudo ecgonine methyl ester, caffein and levamisole 1GZVLB + +

2IQBJI + + found cocaine with 48.2%w/w 2MO2K2 + + ./. 2Q2RKB + + Cocaine and Caffeine confirmed 331I33 + + Caffeine, levamisole, trans-cinnamoyl cocaine, methylecgonine 3HKZSM + + Mixture of cocaine, caffeine and Levamisole. 3J30PJ - + contiene adulterantes como la Cafeina y Levamisol 3QY6YS ANP +

3UCRFA + + the sample contains a mixture cocaine and caffeine 43D6WO + + Cocaine is a Class A drug subject to the provisions of the Misuse of Drugs Act 1971 4EUEWU - + The sample 2016/1/SM-1 was found to contain the illicit drug COCAINE. 4LYNGL + + The sample contains also levamisole. The cocaine is scheduled as illicit drug in XXXX. The caffeine and the levamisole are cutting agents. 4PGIDD + + The sample contains cocaine, caféine and lévamisole. Cocaine is sheduled as illicit drug. 4Z40VI + + cocaine, levamisole, caffeine, ecgonine methyl ester, ecgonidine methyl ester, cis/trans-cinnamoyl cocaine, tropacocaine-GCMS-compare mass spectra with library, retention time of reference sample and FTIR-cocaine 55STC5 + +

5NU8Q8 + + The powder was analysed and found to contain cocaine hydrochloride and caffeine. 5XSWBZ + + cocaine and caffeine, levamisole 66BMCC - + found cocaine with 59.79% w/w in SM-1 6AKET8 + + SM-1 found to contain Cocaine 6DWSSS + + white powder containing cocaine, caffeine and levamisol as diluents and ecgonidine methyl ester and ecgonine methyl ester as cocaine impurities

Code Caffeine Cocaine 6ILHTL + + The sample contained 49.56% w/w cocaine (base) Substances detected include caffeine and tetramisole 6QO4X5 + + cocaine base 50,5 % 6UM71W + + Cocaine is controlled by KB 31/12/1930 77DRQT + + COCAINE Hydrochloride 49.4% AS BASE - CAFFEINE - LEVAMISOLE 7BTAAO ANP + There was evidence of cocaine 7VKRTZ + + This sample is cocaine. 8F8I8T + + Caffeine, levamisole, ecgonidine. 8IHHJF + +

8IXV43 + + A sample of the powder was found to contain cocaine at a purity of 52%. This sample was also found to contain caffeine and tetramisole. 8LZBLR - + SM-1 to contain Cocaine 8NM0BB + + The Test sample 2016/1/SM-1 was analyzed by Colour test and Thin Layer Chromatography technique and found to contain Cocaine and Caffeine. 8PHIP8 + + A sealed glass vial containing a white powder. This powder contained an average of 57% Cocaine Hydrochloride. 8YMBJO + + The sample consist controlled drugs - cocaine 91AIRR + +

9EWNN5 + + the item 1 is a powder with cocaine hydrocloride, caffeine and levamisole. The percent of free base psycoactive substance cocaine is 55.7% . A1O2PU ANP + white powder and typical smell AA3A9G + + White powder containing Cocaine. Also detected Levamisole and Caffeine AAL7YF + + Colorimetrics reactions showed positive results for substances like alcaloids that was confirmed by GC-MS. COcaine, caffeine and levamisole was detected an identified. AD2NVY + + LEVAMISOL, CAFFEINE AJO81E + +

ASUW2S + + The sample contains 51.5% ± 1.5% Also contain caffeine and levamisole AZCZ5Z + + cocaine and caffeine

Code Caffeine Cocaine B54OW4 + + white powder containing cocaine (51.4%w/w), caffeine and levamisole BABKJE + + The powder, which weighed 0.21 grams, was analysed and found to contain Cocaine. A sample of the powder was further analysed and found to contain 51% (weight for weight) Cocaine. Cocaine is a class A controlled drug within the provisions of the Misuse of Drugs Act 1971.

BAYYXO + + Sample contains cocaine hydrochloride, tetramisole and caffeine. BEUIGW + + La muestra contiene Cocaína. BPJ4JR + + It has been detected the presence of cocaine hydrochloride in the sample BT6Y0Y + + Sample 2016/1/SM-1 consists of white powder. Cocaine, a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. C7G4DH + + Levamisole, Caffeine CE7TB2 + + The sample contains cocaine. The content of cocaine (as cocainehydrochloride) is determined to 58 %. Cocaine is a controlled substance in X. CIFQC8 + + Sample 2016/1/SM-1, a white odourless powder, gave a positive result for cocaine, a controlled substance under national legislation on drugs. CSJXFO + + Examination revealed the presence of cocaine. DALAM7 + + The sample 1 contains cocaïne chlorhydrate at 53% per weight (47% base), which is a controlled substance in XXXX. DWWWGY + + COCAINA BASE, CAFEINA, LEVAMIZOL DY0EG9 + + the results of the screening test "TLC (Tech:150)" and identification , confirmation analytic techniques HPLC (160) and GC/MS (180). E8S7ZT ANP + 2016/1/SM-1 contient en plus de la cocaine des composés insolubles dans le methanol. Il y a un composé non identifié qui est commun à 2016/1/SM-1 et 2016/1/SM-3 qui apparâit par la technique 150 (Chromatographie sur couche mince). EAE6LE + + The sample contains Cocaine and Caffeine. The content of Conaine as base is 49.3% EDUYDD + + The sample contains cocaine which is listed as a controlled drug according to XXX order, appendix I of February 22nd 1990. EJBJCJ + + In the test sample 2016/1/SM-1 were detected cocaine, caffeine and levamisole ELQNHU + + Based on the above analysis, the sample was found to contain cocaine, levamisole and caffeine. ENI7TJ + + From screening test using (CT), (FTIR) and ion scan and from confirmatory test using (GC-MS), the sample was found to contain the controlled drug Cocaine.

Code Caffeine Cocaine EXIP84 + + Sample also contain caffeine and levamisole. The presence of drug confirmed by GC-MS and FTIR spectroscopy analysis.The hydrochloride form of cocaine was confirmed by the anion analysis and FTIR spectroscopy. EYAWUL + + SM1 contains Cocaine, Caffeine and Levamisol.Methyecgonine an cinnamoylcocaine werw detected as minor components. EYAZVH + + The sample contains a controlled substance as cocaine and other substances besides cutting caffeine and levamisol. F1M4VD + + Cocaine was identified by TLC and GC-MS. F9I31B + + cocaine, anhidromethylecgonine, cis&trans cinnamoilecgonine, caffeine,levamisole. BASE COCAINE 50,14+/-1,3 % (w/w) FJ44OK + +

G1C7O1 + + Caffeine and Levamisol GCHGCL + + Sample contains 52.6 ± 2.2 % Cocaine base. Caffeine and levamisole were also detected GDGBEX + + Sample SM-1 was found to contain cocaine. GLYEEK + + The sample 2016/1/SM-1 contains cocaine (53,4 %), caffeine and levamisole H7SE4O + + Adulterantes: cafeína y levamisol HCVNSQ + + cocaine,caffeine,levomisole HNG20U + + Was found Caffeine, levanisole and trace of Benzoilecgonine HW0WRM + +

IBPJLJ + + The powder contained cocaine Hydrochloride, together with the adulterants caffeine and levamisole ICQNLB + + Powder from test sample 2016/1/SM-1 contain cocaine with caffeine and tetramisol IIX7UR + + Cobalt thiocyanate (CT) positive. GC/MS Retention time and mass charge ratio (M/Z), similar characteristics whit the subtances used as standar or pattern. ISA8Y8 + + Sample 2016/1/SM-1 found to contain cocaine and caffeine IUW8JU + + De los análisis realizados, se concluye que la sustancia se trata de cocaína IXUGYG + + - J28855 + + COCAINE, CAFEINE AND LEVAMISOLE J5YB55 + + Cocaine HCl. Caffeine and levamilole-tetramisole were also identified.

Code Caffeine Cocaine JJLJOU + + in the sample labeled as 2016/1 / SM-1 they were found cocaine, caffeine and levamisole. KBC4MU + + White powder that contains controlled substance COCAINE and adulterant CAFFEINE. KHHK0G + + The sample was found to contain 52.1% of cocaine (as base). The sample was also found to contain caffeine and levamisole/tetramisole (isomeric form not determined). KJU4OU + + Blue colour appear with Cobalt Thiocyanate test and blue colour appear in the lower layer by Modified Cobalt Thiocyanate test which indicates possible presence of Cocaine.Amalic Acid test indicates possable presence of Caffeine.Analysis of GCMS shows the similarity as Cocaine and Caffeine.During quantitative analysis,absebce of reference standard is the challenge for us. KLL25F + + From GCMS analysis, cocaine and caffeine were detected KNZKKP + +

KTJBZA + + The test sample also contained levamisole and caffeine KWPD3V + + cocaine was detected by GC/MS screening nad it was quantified by GC/FID KYO332 + + It is an usually detected drug in our laboratory. L9LTEO + + Test Sample 2016/1/SM-1 contains Cocaine, a dangerous drug. It also contains caffeine, levamisole, benzoylecgonine, cinnamoyl cocaine and methyl ecgonine. LEPP7L + +

LFCJGM + + ɫontained cocaine, caffeine, levamisole, cinnamoilcocaine, cis-cinnamoilcocaine and trace of methylecgonidine, methylecgonine

LGECDN + + The sample contains cocaine (54,8%), caffeine and levamisole. LLLLTB + + The test sample number SM-1 containing a psycho narcotic drug cocaine. LNR2DR + + levamisole, caffeine M5LL0L ANP +

M9MFMP + + screening by colorimetric test confirmation by GC-MS and FTIR quantification by GC-MS

Other substances in the sample: levamisole MBOMMM + + caffeine, levamisole MCOLDO ANP +

MOOSOO + + Test sample 2016/1/SM-1 contains cocaine base 51.0 %, m/m, caffeine and cocaine related compounds.

Code Caffeine Cocaine MQXQRQ + + In Sample 1 was identified cocaine and caffeine, levamisole. MVVNXZ ANP + The white powder contains Cocaine. NNNNDW + + It contain 48.6 % of Cocaine and also contains Caffein, Levamisole/Tetramisole and traces of Benzoylecgonine O1DHE1 + + the sample was confirmed by GC MS and quantified by GC FID O28H4R - + GC-MS OF6Y6D + +

OFP7ET + + Caffeine Levamisole OOOIMO + + Cocaine, conc. 50% as free base, other substances found are caffeine and tetramisol OOXOOI + + COCAINE OSTFUT + + caffeine OWRO6K + + Cocaine and Caffeine were identified. OYX2R3 + + COCAINA CLORHIDRATO + CAFEINA+ LEVAMISOL OZLPCC ANP +

P3Y0QX + + white powder containing 58.1%w/w of cocaine P5A5W5 + + Presence of cocaine, concentration of 49.68%, with the presence of the following adulterants: caffeine, levamisole. We detected even the presece of Methyl-egonina, Methyl-egonidina, Cynnamoilcocaina. P7ZPBP - + A preliminary test SCOTT and MARQUIS to know what kind of drugs were present in the samples that have been sent and two confirmation tests TLC and GC-FID. In the case of the sample referenced with the code 2016/1/SM-1 was able to verify the presence of Cocaíne Scott test and other tests it was also verified the presence of Cocaíne and Ketamine PPPKPP + + Powder was analysed and found to contain cocaine, levamisole and caffeine. QOMLQQ +

QS88SU + + The sample contained 52.3% cocaine. Additionally caffeine and levamisol was detected int the sample. QUZQUQ + + Mass spectrometry profile correlation between sample and reference material certified QWO4OF + +

Code Caffeine Cocaine R25T2B + + We diluited 1 mg of the sample in 10 mL of methanol and analized by CG-MS. R2XKWH - +

R3QRYO + + Nil RC98IL + + SM1 was prepared from a seizure containing 54% w/w cocaïne base. Thesample also contained caffeine and levamisole RV3YT3 + + Powder containing cocaine, additionally identified caffeine and levomisole S9YJGM + + The results of the test of SM1 (142) received confirmed that the mentioned simple contains cocaine with 49.5 percentage by weight (49.5%). The sample 1 also contains caffeine as not controlled drugs. SDFWC8 + + additional substance: caffeine, levamisol SEF3EE + + The sample contained cocaine HCl. In addition to that, caffeine,Levamisole, norcocaine, cinnamoylcocaine and trans-cinnamoylcocaine were identified. Analysis revealed percentage of cocaine base is 41.82%. SK102M + +

SLDIJQ + + the sample is mixture of cocaine, caffeine,cis-cynamoylcocaine and imidazol SSOFTB + + Presence of cocaine: retention time and MS spectra in GC analysis (FID and MS), DRX and FTIR analysis. Cocaine as hydrochloride. Presence of caffeine and levamisole: retention time and MS spectra in GC analysis (FID and MS) and XRD analysis. Caffeine as base. T7YTFO + +

TBK0V2 ANP + SUSTANCIAS DISUELTAS EN METANOL E IDENTIFICADAS MEDIANTE CG/FID TDVDNQ + + x grams of powder containing 51% cocaine . Caffeine and levamisole were also present TEZEE4 + + We determined a mixture of Cocaine, Caffeine and Levamisol. The Cocaine concentration is 54.6 %w/w this is an average of two measures. THQ2CH + +

TIKKKK + + SM-1 contains cocaine TRQBQ8 + + CAFEIN LEVAMISOLE COCAIN IMPURITIES TSGAGB + + The 2016/1/SM-1 Sample was found to contain Cocaine and Caffeine. TWTWPH + +

Code Caffeine Cocaine TWYAAL + + The sample contains cocaine, caffeine, levamisole U90SWA + + quantification HPLC : 49 % UFVIOP + + The sample contains Cocaine and Caffeine. UQMBX2 + + WHITE POWDER SAMPLE ANALYZED CONTAINS COCAINE AND CAFFEINE UYPU5U + + 220 milligrams of a white powder containing cocaine hydrochloride and caffeine. This white powder contained an average of 50% of cocaine (purity has been calculated in the base form). VFD46A + + the SM-1 sample contains 64.6% of cocaine cut by the caffeine and lactose VKNECE + + After analyzing the sample with CR, MSD confirmation and subsequent cuantification with FID, we can confirm that sample contents cocaine, levamisole and caffeine. VNZ61V - + THE SAMPLE CORRESPOND COCAINE MIIXED WITH CAFFEINE AND LEVAMISOL VQT273 + + Caffeine, levamisole VXFBR6 + + cocaine - 51.93%, ecgonidine methyl ester, cis-cinnamoylcocaine, caffeine, levamisole VXXXL4 + + the white powder contains cocaine (43,97%) wich is controlled by national law. In addition caffeine and levamisole were found in the sample. VYZC85 + + cocaine is on the list of drugs WDNNGN + + after chemical analysis was performed the sample was found to contain 1/ cocaine 57.4 % 2/ MDMA 0.05 % 3/ caffiene WDQWLH + + Powder containing cocaine X2JISE + + Tetramisol and caffeine were also detected X456G5 + +

X70OZ9 + +

XFVW1V + + In this Sample Contain three substance Cocaine ,Caffeine and Sugar XNQ60K + +

XQJTD9 + + Cocaine existed in salt form. We found caffeine in the sample XRKU5U + + On analysis, I found the sample "SM-1" containing Cocaine and Caffeine.

Code Caffeine Cocaine Y38I3T ANP + En la muestra SM-1, se encontra la presencia de cocaina, tambien se realizola preuba para cloruras YAH8BE + + caffeine, levamisole YAIIVO + + Cocaine hydrochloride, caffeine, and phenyltetrahydroimidazothiazole confirmed in 1 unit tested of 1 unit received. YEKYTF + + powder contains cocaine with caffeine and levamisole YXZMMX + + Cocaine is a controlled drug. Indications of caffeine and levamisole. YY5Y1A + + Results of screening tests were positive for cocaine. Retention time and fragmentation pattern obtained with sample are equivalent to those obtained with cocaine. Cocaine was detected at 52.6% by weight. YY7MQP + +

YYZUYY + + The sample contains 52,07 % cocaine ( as free base) Z5LF55 + + the powder is a mixture of cocaine hidrochloride and caffeine. The concentration of cocaine (base) in the sample is 52.1% by weight. Z887DL + + The test sample 2016/1/SM-1 was found to contain the controlled drug cocaine. The test sample was also found to contain caffeine. ZF1EFF + + Presence of cocaine hydrochloride was detected in the sample. The sample also contained caffeine, levamisole and multitude of trace level alkaloid impurities: (cis/trans)cinnamoylcocaine, benzoylecgonine, methylecgonine, ethylecgonine. ZFFEHN + +

ZH0THY + + Cocaine, caffeine, levamisole, methilesterecgonine, cinnamoilcocaine, 48% +/- 4 ZOIJZ3 + +

ZRG6U6 + + Analysis of a representative sample of the powder revealed the presence of cocaine with a purity of approximately 59% (calculated as base). ZSX0SS + + One glass bottle containing 0.22 grammes of a solid containing 0.11 grammes of cocaine. ZXIIII + + Cocaine, caffeine and levamisol

Identification methods for Test Sample 1

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

Analytical Technique Codes Code 140 141 142 150 160 161 171 180 190 200 211 220 230 231 210 00T0J0 S I I I I 1GZVLB SI SI SI I 2IQBJI SI 2MO2K2 I SI SI 2Q2RKB S S S I I 331I33 SI 3HKZSM I I S Raman 3J30PJ S SI I I I 3QY6YS I SI 3UCRFA S S S I I 43D6WO S S I 4EUEWU S I 4LYNGL S I I 4PGIDD I SI 4Z40VI S S SI I 55STC5 SI 5NU8Q8 S I I 5XSWBZ I SI 66BMCC I S I 6AKET8 S S I 6DWSSS SI I 6ILHTL S S S I I 6QO4X5 S I I 6UM71W I SI 77DRQT S S S I I 7BTAAO SI I 7VKRTZ S I I 8F8I8T S S I S 8IHHJF S S I I 8IXV43 SI SI I I I I 8LZBLR S S S SI I 8NM0BB S S SI S Fast Blue B Salt test 8PHIP8 S S I I 8YMBJO I SI

Code 140 141 142 150 160 161 171 180 190 200 211 220 230 231 210 91AIRR I SI 9EWNN5 I A1O2PU SI AA3A9G S SI SI SI AAL7YF S S S I I AD2NVY I SI AJO81E SI I HPLC-RID ASUW2S S I I AZCZ5Z SI I B54OW4 I SI BABKJE S I BAYYXO S S S SI I I S microscopic and macroscopic examination BEUIGW S S S I I BPJ4JR I S I BT6Y0Y S S I I C7G4DH S SI SI I CE7TB2 I I CIFQC8 S S S I CSJXFO SI DALAM7 SI DWWWG S S S I I Y DY0EG9 S I I S E8S7ZT S S I EAE6LE S S S SI I EDUYDD I I EJBJCJ I ELQNHU S I I ENI7TJ S S I I S Negm's test EXIP84 S I I EYAWUL S I EYAZVH S I SI F1M4VD S S S I I F9I31B S S S I I I RDX FJ44OK SI G1C7O1 S I I I GCHGCL S I SI I GDGBEX S I I GLYEEK S S S I S tanred

Code 140 141 142 150 160 161 171 180 190 200 211 220 230 231 210 H7SE4O I I SI HCVNSQ SI SI SI SI I SI I HNG20U S S I I HW0WR S S S I M IBPJLJ S S S I I ICQNLB S S I I IIX7UR S S S I ISA8Y8 S I IUW8JU S SI SI macroscopic analysis IXUGYG SI J28855 S I I J5YB55 I SI I JJLJOU I I SI KBC4MU S S SI I I S Simon KHHK0G SI I LC/ELSD KJU4OU S I KLL25F S I KNZKKP SI KTJBZA I I KWPD3V SI KYO332 S I I I Fehling Reagent L9LTEO S S S I I I Duquenois-Levine reagent LEPP7L S S S I I LFCJGM SI LGECDN S S S I I LLLLTB I SI S I SI LNR2DR SI SI M5LL0L I M9MFMP S S I I MBOMM SI M MCOLDO I I S not stated MOOSOO I SI MQXQRQ I I MVVNXZ S S S I I NNNNDW SI I O1DHE1 I I SI O28H4R SI OF6Y6D I SI

Code 140 141 142 150 160 161 171 180 190 200 211 220 230 231 210 OFP7ET S S S I I OOOIMO SI OOXOOI S S S I I OSTFUT S SI SI I OWRO6K S I I OYX2R3 S S I I S RAMAN OZLPCC SI I S SI Rapid Test P3Y0QX I SI P5A5W5 I I P7ZPBP S S S I I PPPKPP S S S I I QOMLQQ S S S I QS88SU I I SI I QUZQUQ I I QWO4OF SI S S I R25T2B SI R2XKWH I S R3QRYO S I RC98IL I I RV3YT3 SI S9YJGM S S S I I SDFWC8 SI I SEF3EE S S I I I S fast blue B salt test SK102M S S I S microscopy SLDIJQ SI I I I I SSOFTB I I SI I XRD T7YTFO S I I TBK0V2 I I S TDVDNQ S S I I TEZEE4 SI S S SI I I I THQ2CH S S S SI I I I I TIKKKK S S S I I S TRQBQ8 SI TSGAGB I SI TWTWPH I S TWYAAL S S I I SI U90SWA SI I UFVIOP SI I UQMBX2 S S S I I

Code 140 141 142 150 160 161 171 180 190 200 211 220 230 231 210 UYPU5U S S I I I Ehrlich VFD46A S I I I I HPLC/RID VKNECE SI I VNZ61V I SI VQT273 S I VXFBR6 I SI VXXXL4 I SI VYZC85 I I S I WDNNGN SI WDQWLH S S S I X2JISE I X456G5 SI X70OZ9 I XFVW1V S I I XNQ60K SI I XQJTD9 S I I XRKU5U S I I Y38I3T SI SI SI YAH8BE I SI SI YAIIVO SI I I YEKYTF SI I YXZMMX I I YY5Y1A S S S I YY7MQP S S S I I YYZUYY SI Z5LF55 I I I SI I xrd Z887DL S S S I I ZF1EFF S I I I I ZFFEHN S S S SI I SI ZH0THY S S S I ZOIJZ3 S S SI ZRG6U6 S S S I I ZSX0SS S S SI ZXIIII S I

Summary for test sample 1 The response summary of all 183 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: 183

Caffeine: 164 Cocaine: 183

False positives for Test Sample 1

Code Name Technique P7ZPBP Ketamin e 150/171 TBK0V2 Mephedrone 171 WDNNGN MDMA 180

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

There were no false negative results or ANP for the cocaine in SM-1

Frequency of use of screening and identification techniques: Response Summary Response Summary Participants: Response 130 Summary Participants:Participants: 176183177

Section 140 141142142 150150 160160 161 161 171 180 190190200 200 211 220 230220 230 231 231 210 Screening 66 73 60 22 0 1 4 61 17 2 0 1 0 0 11 36.3% 40.1% 33.0% 12.1% 0.0% 0.5% 2.2% 33.5% 9.3% 1.1% 0.0% 0.5% 0.0% 0.0% 6.0% Identification 14 6 4 36 8 15 29 165 72 4 3 0 5 1 12 7.7% 3.3% 2.2% 19.8% 4.4% 8.2% 15.9% 90.7% 39.6% 2.2% 1.6% 0.0% 2.7% 0.5% 6.6% # labs using 71 75 61 45 8 15 30 165 79 6 3 1 5 1 21 this 39.0% 41.2% 33.5% 24.7% 4.4% 8.2% 16.5% 90.7% 43.4% 3.3% 1.6% 0.5% 2.7% 0.5% 11.5% technique 27 2016/1-SM Copyright (c) 2016 UNODC

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

Cocaine Cocaine Deviation Code Concentration Deviation from Code Concentration z-score from robust z-score (mass%) robust average (mass%) average 3UCRFA 26.0 -25.7 -10.1 J5YB55 51.4 -0.3 -0.1 SLDIJQ 33.2 -18.5 -7.2 LEPP7L 51.4 -0.3 -0.1 4EUEWU 40.0 -11.7 -4.6 ASUW2S 51.5 -0.2 -0.1 O1DHE1 40.0 -11.7 -4.6 5XSWBZ 51.6 -0.1 -0.1 SEF3EE 41.8 -9.9 -3.9 AJO81E 51.6 -0.1 -0.1 WDQWLH 42.1 -9.6 -3.8 AD2NVY 51.6 -0.1 -0.1 KNZKKP 43.0 -8.7 -3.4 BEUIGW 51.6 -0.1 -0.1 VXXXL4 43.9 -7.8 -3.1 KYO332 51.6 -0.1 -0.1 ZOIJZ3 44.5 -7.2 -2.8 TIKKKK 51.6 -0.1 -0.1 OYX2R3 46.3 -5.4 -2.1 ZSX0SS 51.7 0.0 0.0 DALAM7 47.0 -4.7 -1.9 QUZQUQ 51.7 0.0 0.0 91AIRR 47.1 -4.6 -1.8 UFVIOP 51.8 0.1 0.0 AAL7YF 47.5 -4.2 -1.7 J28855 51.9 0.2 0.1 ZH0THY 48.0 -3.7 -1.5 VXFBR6 51.9 0.2 0.1 8YMBJO 48.1 -3.6 -1.4 VYZC85 51.9 0.2 0.1 2IQBJI 48.2 -3.5 -1.4 OOXOOI 52.0 0.3 0.1 ZXIIII 48.5 -3.3 -1.3 4LYNGL 52.0 0.3 0.1 NNNNDW 48.6 -3.1 -1.2 EDUYDD 52.0 0.3 0.1 VQT273 48.8 -2.9 -1.2 IBPJLJ 52.0 0.3 0.1 U90SWA 49.0 -2.7 -1.1 MBOMMM 52.0 0.3 0.1 EAE6LE 49.3 -2.4 -1.0 QOMLQQ 52.0 0.3 0.1 77DRQT 49.4 -2.3 -0.9 YYZUYY 52.1 0.4 0.1 S9YJGM 49.5 -2.2 -0.9 KHHK0G 52.1 0.4 0.1 6ILHTL 49.6 -2.1 -0.9 LNR2DR 52.1 0.4 0.1 TRQBQ8 49.6 -2.1 -0.8 Z5LF55 52.1 0.4 0.1 P5A5W5 49.7 -2.0 -0.8 CE7TB2 52.2 0.5 0.2 OOOIMO 49.7 -2.0 -0.8 HW0WRM 52.2 0.5 0.2 XQJTD9 49.7 -2.0 -0.8 X70OZ9 52.2 0.5 0.2 SSOFTB 49.9 -1.8 -0.7 VKNECE 52.3 0.6 0.2 KTJBZA 50.0 -1.7 -0.7 QS88SU 52.3 0.6 0.2 UYPU5U 50.0 -1.7 -0.7 TWTWPH 52.3 0.6 0.2 EXIP84 50.1 -1.6 -0.7 8IXV43 52.3 0.6 0.2 LFCJGM 50.1 -1.6 -0.6 7VKRTZ 52.4 0.7 0.3 RV3YT3 50.1 -1.6 -0.6 1GZVLB 52.5 0.8 0.3 F9I31B 50.1 -1.6 -0.6 DWWWGY 52.5 0.8 0.3 HNG20U 50.5 -1.2 -0.5 GCHGCL 52.6 0.9 0.3 A1O2PU 50.5 -1.2 -0.5 YY5Y1A 52.6 0.9 0.3 YEKYTF 50.5 -1.2 -0.5 43D6WO 52.7 1.0 0.4 SK102M 50.8 -0.9 -0.4 3HKZSM 52.8 1.1 0.4 FJ44OK 50.9 -0.8 -0.3 MQXQRQ 52.8 1.1 0.4 6QO4X5 50.9 -0.8 -0.3 HCVNSQ 52.9 1.2 0.5 8PHIP8 51.0 -0.7 -0.3 ZFFEHN 52.9 1.2 0.5 BABKJE 51.0 -0.7 -0.3 YXZMMX 53.1 1.4 0.5 TDVDNQ 51.0 -0.7 -0.3 GLYEEK 53.4 1.7 0.6 YAIIVO 51.0 -0.7 -0.3 BAYYXO 53.5 1.8 0.7 MOOSOO 51.1 -0.6 -0.2 00T0J0 53.5 1.8 0.7 QWO4OF 51.2 -0.5 -0.2 OFP7ET 53.5 1.8 0.7 2MO2K2 51.2 -0.5 -0.2 H7SE4O 53.5 1.8 0.7 BPJ4JR 51.3 -0.4 -0.2 EJBJCJ 53.7 2.0 0.8 ZF1EFF 51.3 -0.4 -0.2 R25T2B 54.0 2.3 0.9 B54OW4 51.4 -0.3 -0.1 RC98IL 54.0 2.3 0.9 28 2016/1-SM Copyright (c) 2016 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Cocaine Deviation Code Concentration from robust z-score (mass%) average 4PGIDD 54.1 2.4 0.9 6UM71W 54.3 2.6 1.0 EYAZVH 54.3 2.6 1.0 SDFWC8 54.4 2.7 1.0 OF6Y6D 54.4 2.7 1.0 TEZEE4 54.6 2.9 1.1 IXUGYG 54.8 3.1 1.2 KWPD3V 54.8 3.1 1.2 LGECDN 54.8 3.1 1.2 F1M4VD 54.9 3.2 1.2 6DWSSS 55.0 3.3 1.3 G1C7O1 55.0 3.3 1.3 9EWNN5 55.7 4.0 1.5 X2JISE 57.2 5.5 2.1 WDNNGN 57.4 5.7 2.2 P3Y0QX 58.1 6.4 2.5 ZRG6U6 59.0 7.3 2.8 66BMCC 59.8 8.1 3.2 5NU8Q8 61.0 9.3 3.6 VFD46A 64.6 12.9 5.0 M9MFMP 67.5 15.8 6.2 3QY6YS 74.0 22.3 8.7 KJU4OU 83.0 31.3 12.2 MCOLDO 85.6 33.9 13.2

Robust average = 51.7% UNODC value = 50.5%

4.0 3.6 3.2

3.0 2.8 2.5 2.2 2.1

2.0 1.5 1.3 1.3 1.2 1.2 1.2 1.2 1.1 1.0 1.0 1.0 1.0 0.9 0.9

1.0 0.9 0.8 0.7 0.7 0.7 0.7 0.6 0.5 0.5 0.5 0.4 0.4 0.4 3.8 0.3 0.3 ‐ 0.3 0.3 7.2 4.6 0.3 ‐ ‐ 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.1 0.1 0.1 0.1 .4.6 0.1 0.1 0.1 0.1 0.1 0.1 3.9 0.1 0.1 ‐ 0.1 10.1 ‐ ‐ 0.0 0.0 0.0 5.0 1 8.7 13.2 0.0 0. 0.1 0.1 0.1 0.1 0.1 ‐ ‐ ‐ ‐ 0.1 ‐ ‐ 0.1 ‐ 0.1 0.1 ‐ ‐ ‐ 0.2 0.2 6.2 12.2 ‐ ‐ 0.2 0.2 ‐ 0.2 ‐ ‐ 0.3 0.3 0.3 0.3 0.3 ‐ ‐ ‐ ‐ 0.3 ‐ ‐ 0.4 ‐ 0.5 0.5 0.5 ‐ ‐ ‐ 0.6 0.6 0.6 0.7 ‐ ‐ ‐ 0.7 0.7 ‐ ‐ ‐ 0.7 ‐ 0.8 0.8 ‐1.0 0.8 ‐ ‐ 0.8 ‐ 0.9 0.9 ‐ ‐ ‐ 0.9 ‐ 1.0 ‐ 1.1 ‐ 1.2 ‐ 1.2 ‐ 1.3 ‐ 1.4 1.4 ‐ ‐ 1.5 ‐ 1.7 ‐

‐2.0 1.8 ‐ 1.9 ‐ 2.1 ‐

‐3.0 2.8 ‐ 3.1 ‐ 3.4 ‐

‐4.0 VH ZXIIII IBPJLJ EJBJCJ X2JISE 2IQBJI ZOIJZ3 6ILHTL SLDIJQ RC98IL BPJ4JR YAIIVO EXIP84 F9I31B TIKKKK 00T0J0 ZF1EFF J28855 8IXV43 J5YB55 LEPP7L ZSX0SS Z5LF55 SEF3EE TEZEE4 91AIRR KTJBZA YEKYTF 8PHIP8 FJ44OK EAE6LE BABKJE AAL7YF VXXXL4 YY5Y1A GLYEEK YYZUYY SSOFTB AJO81E CE7TB2 VYZC85 7VKRTZ R25T2B RV3YT3 UFVIOP 4LYNGL 3QY6YS 1GZVLB OFP7ET 4PGIDD XQJTD9 ZFFEHN VXFBR6 IXUGYG X70OZ9 KNZKKP ZH0THY KYO332 P3Y0QX VFD46A OYX2R3 LFCJGM EYAZ 3UCRFA OF6Y6D H7SE4O VQT273 S9YJGM VKNECE QS88SU KJU4OU BAYYXO LNR2DR ZRG6U6 LGECDN G1C7O1 77DRQT 8YMBJO SK102M 6QO4X5 GCHGCL 6DWSSS O1DHE1 5XSWBZ AD2NVY TRQBQ8 UYPU5U A1O2PU 3HKZSM KHHK0G OOXOOI SDFWC8 BEUIGW EDUYDD 66BMCC 5NU8Q8 F1M4VD P5A5W5 HCVNSQ DALAM7 ASUW2S U90SWA HNG20U 2MO2K2 TDVDNQ KWPD3V B54OW4 4EUEWU 9EWNN5 43D6WO YXZMMX MCOLDO OOOIMO QUZQUQ QWO4OF TWTWPH 6UM71W MQXQRQ QOMLQQ MOOSOO WDNNGN M9MFMP NNNNDW WDQWLH HW0WRM DWWWGY MBOMMM 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 Round: 2016/1 |z| > 3 = unsatisfactory

Substance: SM-1; Cocaine 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. 30

Z-Score Report per Sample per Substance

Round: 2016/1

Dispersion of z-scores using different analytical techniques for the quantification of cocaine in 2016/1 SM-1 10

0 z-score

-2

-4

-6

-8 HPLC GC-FID GC-MS/LC-MS -10

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

Sample 2 Analysis

Identified substances for Test Sample 2 Code Identified Substances 00T0J0 Ecstasy(MDMA) 1GZVLB MDMA 2IQBJI MDMA 2MO2K2 MDMA 2Q2RKB MDMA 331I33 3,4-Methylenedioxymetamfetamine (MDMA) 3HKZSM MDMA 3J30PJ MDMA 3QY6YS MDMA 3UCRFA MDMA 43D6WO MDMA 4EUEWU MDMA 4LYNGL 3,4-Methylenedioxymetamfetamine (MDMA), lactose 4PGIDD MDMA HCl 4Z40VI MDMA 55STC5 MDMA 5NU8Q8 MDMA 5XSWBZ MDMA 66BMCC MDMA 6AKET8 MDMA 6DWSSS MDMA hydrochloride 6ILHTL 3,4-Methylenedioxymethamphetamine (MDMA) 6QO4X5 MDMA hydrochloride 6UM71W MDMA 77DRQT 3,4-Methylenedioxymetamfetamine (MDMA) 7BTAAO Metamphatamine and Amphetamine 7VKRTZ MDMA 8F8I8T N-methyl-3,4-methylendioxyamphetamine 8IHHJF MDMA 8IXV43 MDMA 8LZBLR MDMA 8NM0BB MDMA and Lactose 8PHIP8 3,4-methylenedioxymethylamphetamine Hydrochloride (MDMA) 8YMBJO 3,4-Methylenedioxymetamfetamine (MDMA) 91AIRR MDMA 9EWNN5 MDMA A1O2PU MDMA AA3A9G MDMA AAL7YF 3,4 Metylenedioxymethamfetamina (MDMA) AD2NVY MDMA (3,4-METHYLENEDIOXYMETAMFETAMINE)

Code Identified Substances AJO81E MDMA ASUW2S 3,4-Methylenedioxymetamfetamine (MDMA) AZCZ5Z MDMA B54OW4 mdma BABKJE Methylenedioxymethylamphetamine (MDMA) BAYYXO MDMA BEUIGW MDMA BPJ4JR 3,4-Methylenedioxymetamfetamine hydrochoride BT6Y0Y 3,4-Methylenedioxy-metamfetamine (MDMA) C7G4DH MDMA CE7TB2 MDMA (3,4-methylenedioxymethamphetamine) CIFQC8 3,4-Methylenedioxymetamfetamine (MDMA) CSJXFO MDMA DALAM7 MDMA DWWWGY MDMA DY0EG9 MDMA EAE6LE MDMA EDUYDD MDMA EJBJCJ MDMA ELQNHU 3,4-Methylenedioxymethamfetamine (MDMA) ENI7TJ 3,4-Methylendioxy-metamfetamine (MDMA) EXIP84 MDMA EYAWUL MDMA EYAZVH 3,4-Methylenedioxymetamfetamine (MDMA) F1M4VD MDMA F9I31B MDMA hcl FJ44OK MDMA G1C7O1 MDMA GCHGCL MDMA GDGBEX MDMA GLYEEK MDMA H7SE4O MDMA HCVNSQ MDMA HNG20U MDMA HW0WRM MDMA IBPJLJ MDMA (Lactose also present) ICQNLB 3,4 - methylenedioxymethamphetamine IIX7UR 3,4-Metilenedioximetamfemine ISA8Y8 3,4-Methylenedioxymetamfetamine (MDMA) IUW8JU Methyl-3,4-methylenedioxyamphetamine IXUGYG MDMA J28855 MDMA J5YB55 MDMA JJLJOU 3,4-Methylenedioxymetamfetamine (MDMA)

Code Identified Substances KBC4MU MDMA KHHK0G MDMA KJU4OU MDMA,lactose KLL25F MDMA (N-Methyl-3,4-Methylenedioxyamphetamine KNZKKP MDMA KTJBZA MDMA KWPD3V MDMA KYO332 MDMA L9LTEO 3,4-Methylenedioxymetamfetamine (MDMA) LEPP7L 3,4 Methylenedioxymetamfetamine (MDMA) and Lactose LFCJGM MDMA LGECDN MDMA LLLLTB MDMA LNR2DR MDMA M5LL0L MDMA M9MFMP 3,4 methylendioxymethylamphetamine MBOMMM MDMA HCl MOOSOO MDMA MQXQRQ MDMA MVVNXZ MDMA NNNNDW MDMA O1DHE1 MDMA O28H4R MDMA OF6Y6D MDMA OFP7ET MDMA OOOIMO MDMA (3,4-metylendioximethamfetamine) OOXOOI MDMA OSTFUT MDMA OWRO6K MDMA OYX2R3 N-metil-3-4-metillendioxianfetamina (MDMA) OZLPCC MDMA,Synthetic cathinones P3Y0QX MDMA P5A5W5 MDMA P7ZPBP Yes MDMA PPPKPP MDMA QOMLQQ MDMA QS88SU MDMA QUZQUQ MDMA QWO4OF MDMA R25T2B MDEA R2XKWH MDMA R3QRYO MDMA RC98IL MDMA HCL RV3YT3 MDMA

Code Identified Substances S9YJGM MDMA SDFWC8 MDMA HCl SEF3EE 3,4-methylenedioxy-metamfetamine (MDMA) SK102M MDMA SLDIJQ MDMA SSOFTB 3,4-Methylenedioxymetamfetamine (MDMA) T7YTFO 3,4-methylenedioxy-metamfetamine (MDMA) TBK0V2 MDMA TDVDNQ MDMA TEZEE4 MDMA, LACTOSE TIKKKK MDMA TRQBQ8 MDMA HCL TSGAGB 3, 4 - METHYLENEDIOXY-METAMFETAMINE(MDMA) TWTWPH MDMA TWYAAL MDMA U90SWA MDMA UFVIOP MDMA UQMBX2 MDMA UYPU5U MDMA HCL VFD46A MDMA VKNECE MDMA 14.08 VNZ61V 3,4-Methylenedioxymetamfetamine VQT273 MDMA VXFBR6 3,4-Methylenedioxymetamfetamine (MDMA) VXXXL4 3,4-MDMA VYZC85 MDMA WDNNGN MDMA WDQWLH MDMA X2JISE MDMA X456G5 MDMA, LACTOSE X70OZ9 MDMA XFVW1V MDMA XNQ60K MDMA XQJTD9 MDMA XRKU5U MDMA Y38I3T MDMA YAH8BE MDMA YAIIVO 3,4-Methylenedioxymethamphetamine Hydrochloride YEKYTF MDMA YXZMMX MDMA YY5Y1A MDMA YY7MQP MDMA, lactose YYZUYY MDMA Z5LF55 MDMA

Code Identified Substances Z887DL MDMA ZF1EFF MDMA ZFFEHN MDMA 13.9% ZH0THY MDMA ZOIJZ3 MDMA ZRG6U6 MDMA ZSX0SS MDMA ZXIIII MDMA

Statement of findings for Test Sample 2

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

00T0J0 + + Sample contained MDMA cut with Lactose 1GZVLB + ANP

2IQBJI + ANP found MDMA with 14.3%w/w 2MO2K2 + + ./. 2Q2RKB + - MDMA Confirmed 331I33 + ANP

3HKZSM + + Mixture of MDMA in lactose. Content of lactose is approx.70 % w/w. 3J30PJ + ANP

3QY6YS + ANP

3UCRFA + + the sample contains a mixture of MDMA and lactose 43D6WO + ANP MDMA is the common name for methylenedioxymethyl amphetamine. It is a Class A controlled drug subject to the provisions of the Misuse of Drugs Act 1971 as it is structurally derived from an N- alkyl-alpha methylphenethylamine by substitution in the ring with an alkylenedioxy substituent. 4EUEWU + - The sample 2016/1/SM-2 was found to contain the illicit drug MDMA. 4LYNGL + + The 3,4-Methylenedioxymetamfetamine (MDMA) is scheduled as illicit drug in XXXX. The lactose is a cutting agent. 4PGIDD + + The sample contains MDMA and lactose. MDMA is sheduled as illicit drug. 4Z40VI + + MDMA, lactose-GCMS-compare mass spectra with library, retention time of sreference sample and MDMA, FTIR-lactose 55STC5 + ANP

5NU8Q8 + + The powder was analysed and found to contain methylenedioxymethylamphetamine (MDMA) and lactose. 5XSWBZ + + MDMA and lactose 66BMCC + - found MDMA with 18.23% w/w in SM-2 6AKET8 + ANP SM-1 found to contain MDMA

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

6DWSSS + + white powder containing MDMA and lactose as diluent 6ILHTL + + The sample contained 13.71% w/w MDMA (base). Substance detected include lactose. 6QO4X5 + + MDMA base 13,5 % 6UM71W + + MDMA is controlled by KB 22/01/1998 77DRQT + + 3,4-Methylenedioxymetamfetamine (MDMA) Hydrochloride 14.7% as base - LACTOSE 7BTAAO ANP ANP There was evidence of Metamphetamine and Amphetamine in sample 2 7VKRTZ + + This sample contains MDMA 8F8I8T + + Lactose 8IHHJF + ANP

8IXV43 + - A sample of this powder was analysed and found to contain MDMA at a concentration of 16%. 8LZBLR + + SM-2 to contain MDMA 8NM0BB + + The Test sample 2016/1/SM-2 was analyzed by Colour test and Thin Layer Chromatography technique and found to contain MDMA and Lactose. 8PHIP8 + + A sealed glass vial containing a white powder. This powder contained an average of 16% 3,4- methylenedioxymethylamphetamine Hydrochloride (MDMA) 8YMBJO + ANP The sample consist controlled drugs - 3,4-Methylenedioxymetamfetamine (MDMA) 91AIRR + ANP

9EWNN5 + - The item is a powder containing MDMA hydrocloride , the percent of free base of MDMA is 16.3% A1O2PU + ANP white powder without any smell AA3A9G + ANP White powder containing MDMA. AAL7YF + + Marquis Reagent: black; Simon´s: blue GC/MS: RT 10,91 min / Mass Spectrum principal peaks at m/Z 58, 135, 77, 51, 55 AD2NVY + ANP

AJO81E + +

ASUW2S + + Also contain lactose

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

AZCZ5Z + ANP MDMA B54OW4 + ANP white powder containing MDMA (14,4%w/w) BABKJE + ANP The powder, which weighed 0.22 grams, was analysed and found to contain Methylenedioxymethylamphetamine (MDMA). Methylenedioxymethylamphetamine (MDMA) is a compound structurally derived from an N-alkyl- alpha-methylphenethylamine by substitution in the ring with an alkylenedioxy substituent, and as such is a class A controlled drug within the provisions of the Misuse of Drugs Act 1971.

BAYYXO + + Sample contains MDMA hydrochloride and lactose. BEUIGW + + La muestra contiene MDMA. BPJ4JR + + It has been detected the presence of 3,4-Methylenedioxymetamfetamine hydrochoride in the sample BT6Y0Y + + Sample 2016/1/SM-2 consists of white powder. 3,4-Methylenedioxy-metamfetamine (MDMA), a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. C7G4DH + + lactose CE7TB2 + + The sample contains MDMA (3,4-methylenedioxymethamphetamine). The content of MDMA(as hydrochloride) is determined to 16 %. MDMA is a controlled substance in X. CIFQC8 + ANP Sample 2016/1/SM-2, an off-white odourless powder, gave a positive result for 3,4- methylenedioxymetamfetamine (MDMA), a controlled substance under national legislation on drugs. CSJXFO + ANP Examination revealed the presence of N methyl-3,4 methylenedioxyamphetamine (MDMA) DALAM7 + + The sample 2 contains MDMA chlorhydrate at 14% per weight (12% base), which is a controlled substance in XXXXX. DWWWGY + + MDMA, LACTOSA DY0EG9 + - the results of the screening test "TLC (Tech:150)" and identification , confirmation analytic techniques HPLC (160) and GC/MS (180). E8S7ZT ANP ANP nous avions en screening des substances sous contrôle (Méthamphétamine, opium, safrole ou isosafrole) mais l'identification et la confirmation n'ayant pas pu être faute de standards, nous ne pouvons pas les mentionner. A la limite des techniques utilisées et le manque de standards nous n'avons pas pu identifier de substances sous contrôle. EAE6LE + ANP The sample contains MDMA. The content of MDMA as base is 15.6%. EDUYDD + + The sample contains MDMA which is listed as a controlled drug according to XXXX order, appendix III of February 22nd 1990.

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

EJBJCJ + ANP In the test sample 2016/1/SM-2 was detected MDMA ELQNHU + + Based on the above analysis, the sample was found to contain 3,4-Methylenedioxymetamfetamine (MDMA) and lactose. ENI7TJ + ANP From screening test using (MR), (FTIR) and ion scan and from confirmatory test using (GC-MS), the sample was found to contain controlled drug MDMA. EXIP84 + + Sample also contain lactose. The presence of drug confirmed by GC-MS and FTIR spectroscopy analysis.The hydrochloride form of MDMA was confirmed by the anion analysis and FTIR spectroscopy. EYAWUL + + SM2 contains MDMA and Lactose. EYAZVH + ANP The sample contains a controlled substance as MDMA and caffeine cutting. F1M4VD + + MDMA was identified by GC-MS. F9I31B + + MDMA and Lactose. BASE MDMA 13,33 +/- 1,49% (w/w) FJ44OK + -

G1C7O1 + + Lactose GCHGCL + + Sample contains 12.43 ± 0.68 % MDMA base. Lactose was also detected. GDGBEX + ANP Sample SM-2 was found to contain MDMA. GLYEEK + ANP The sample 2016/1/SM-2 contains MDMA and lactose H7SE4O + -

HCVNSQ + + MDMA, lactose HNG20U + + Was found lactose HW0WRM + ANP

IBPJLJ + + The powder contained 3,4-Methylenedioxymethamphetamine (MDMA), together with the adulterant lactose ICQNLB + ANP Powder from test sample 2016/1/SM-2 contain 3,4- methylenedioxymethamphetamine (MDMA) IIX7UR + ANP Marquis reagent (MR) positive. GC/MS Retention time and mass charge ratio (M/Z), similar characteristics whit the subtances used as standar or pattern. ISA8Y8 + ANP Sample 2016/1/SM-2 found to contain 3,4 Methylenedioxymetamfetamine (MDMA) 40 2016/1-SM Copyright (c) 2016 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

IUW8JU + ANP De los análisis realizados, se concluye que la sustancia se trata de Metil-3,4- metilendioxianfetamina (MDMA) IXUGYG + ANP - J28855 + + MDMA AND LACTOSE J5YB55 + + MDMA and lactose as a diluent JJLJOU + ANP in the sample labeled as 2016/1 / SM-2 3,4-Methylenedioxymetamfetamine (MDMA) was found. KBC4MU + ANP White powder that contains controlled substance MDMA. KHHK0G + + The sample was found to contain 13.5% of MDMA (as base). The sample was also found to contain lactose. KJU4OU + + Black colour appear with Marquis Test.Blue colour with Simon test indicates the possable presence of MDMA.Analysis of GCMS shows the similarity as MDMA and lactose. KLL25F + ANP - From colorimetric reaction it gave black color with Marquis Reagent and blue color with Simon Reagent - From GCMS analysis, MDMA was detected KNZKKP + +

KTJBZA + + The test sample also contained lactose KWPD3V + ANP MDMA was detected by GC/MS screening and it was quantified by GC/FID KYO332 + + It is an usually detected drug in our laboratory. L9LTEO + + Test sample 2016/1/SM-2 contains MDMA, a dangerous drug. It also contains Lactose. LEPP7L + +

LFCJGM + -

LGECDN + - The sample contains MDMA (13,6%). LLLLTB + - The test sample SM-2 contains stimulating narcotic drugs MDMA. LNR2DR + + Lactose M5LL0L + ANP

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

M9MFMP + ANP screening by colorimetric test confirmation by GC-MS quantification by GC-MS

MBOMMM + + lactose MCOLDO ANP ANP

MOOSOO + + Test sample 2016/1/SM-2 contains MDMA 14.8 %, m/m and lactose. MQXQRQ + + In Sample 2 was identified MDMA and lactose. MVVNXZ + ANP The white powder contains MDMA (3,4-Methylene-dioxyamphetamine. NNNNDW + ANP It contains 13.43% of MDMA O1DHE1 + ANP Confirmed by gc ms O28H4R + - GC-MS OF6Y6D + +

OFP7ET + + lactose OOOIMO + ANP MDMA, conc. 14% as free base OOXOOI + + MDMA OSTFUT + + lactose OWRO6K + - MDMA was analysed. OYX2R3 + + CONTIENE ADEMÁS LACTOSA MONOHIDRATADA, FUE IDENTIFICADA POR FTIR, Y CON EL RAMAN TRUNARC SE IDENTIFICO MDMA, CONFIRMADO CON GC/MS, NO SE CUANTIFICÓ POR NO CONTAR CON ESTANDAR CERTIFICADO. OZLPCC + ANP Synthetic cathinones have not been determine for the lak of reagents P3Y0QX + ANP white powder containing 14,0%w/w of MDMA P5A5W5 + - Presence of MDMA, concentration of 13.50%, without adulterants. P7ZPBP + ANP A preliminary test SCOTT and MARQUIS to know what kind of drugs were present in the samples that have been sent and two confirmation tests TLC and GC-FID. In the case of the sample referenced with the code 2016/1/SM-2 was able to verify the presence of MDMA Marquis test.

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

PPPKPP + ANP Powder was analysed and found to contain 3,4-methylenedioxymethamphetamine. QOMLQQ + ANP

QS88SU + + The sample contianed 14.1 % MDMA and lactose. QUZQUQ + + Mass spectrometry profile correlation between sample and reference material certified QWO4OF + -

R25T2B - - We diluited 1 mg of the sample in 10 mL of methanol and analized by CG-MS. R2XKWH + -

R3QRYO + ANP Nil RC98IL + + SM2 was prepared from a seizure containing 15% w/w MDMA base. The sample also contained lactose RV3YT3 + ANP Powder containing MDMA S9YJGM + - The results of the test of SM2 (46) received confirmed that the mentioned simple contains MDMA but we are not able to give a cuantification result. SDFWC8 + + additional substance: lactose SEF3EE + + MDMA and lactose were identified in the sample.Analysis revealed that percentage of MDMA is 4.40%. SK102M + ANP

SLDIJQ + + the sample is mixutre od MDMA and lactose SSOFTB + + Presence of MDMA: retention time and MS spectra in GC analysis (FID and MS). MDMA as hydrochloride. Presence of lactose: FTIR and XRD analysis. T7YTFO + +

TBK0V2 + ANP SUSTANCIA DISUELTA EN METANOL E IDENTIFICADA MEDIANTE CG/FID Y UV TDVDNQ + ANP x grams of powder containing 13% MDMA (methylenedioxymethylamphetamine) TEZEE4 + + We determined a mixture of MDMA and Lactose. THQ2CH + -

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

TIKKKK + ANP SM-2 contains MDMA TRQBQ8 + + LACTOSE TSGAGB + ANP The 2016/1/SM1-2 was found to contain 3,4-Methylenedioxymetamfetamine (MDMA). TWTWPH + ANP

TWYAAL + + The sample contains MDMA and lactose U90SWA + + Quantification HPLC : 14.4 % UFVIOP + + The sample contains MDMA and lactose. UQMBX2 + + WHITE POWDER SAMPLE ANALYZED CONTAINS MDMA UYPU5U + + 229 milligrams of a white powder containing 3,4-methylenedioxymethylamphetamine hydrochloride and lactose. This white powder contained an average of 13% of 3,4- methylenedioxymethylamphetamine (purity has been calculated in the base form). VFD46A + - the SM-2 sample contains 15.41% of MDMA VKNECE + - After analyzing the sample with CR, MSD confirmation and FID quantification we can confirm that sample contains MDMA. VNZ61V + ANP THE SAMPLE CORRESPOND IS 3,4-Methylenedioxymetamfetamine (MDMA) VQT273 + + lactose VXFBR6 + ANP 3,4-Methylenedioxymetamfetamine (MDMA) - 12.45% VXXXL4 + ANP the white powder contains MDMA (19.5%) which is controlled by national law. VYZC85 + + MDMA is on the list of drugs WDNNGN + + after chemical analysis was performed the sample was found to contain 1/ MDMA 0.22 % 2/Lactose WDQWLH + ANP Powder containing MDMA X2JISE + ANP

X456G5 + +

X70OZ9 + ANP

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

XFVW1V + + In this Sample Contain tow substance MDMA and Lactose XNQ60K + ANP

XQJTD9 + + Cocaine existed in baseform. We found lactose in the sample XRKU5U + + On analysis, I found the sample "SM-2" containing MDMA and Lactose. Y38I3T + ANP En la muestra SM-2, se encontro la presencia de MDMA YAH8BE + + lactose YAIIVO + + 3,4-Methylenedioxymethamphetamine hydrochloride and lactose were confirmed in 1 unit tested of 1 unit received. YEKYTF + + powder contains MDMA and lactose YXZMMX + ANP MDMA is a controlled drug.

YY5Y1A + ANP Results of screening tests were positive for secondary amfetamines. Retention time and fragmentation pattern obtained with sample are equivalent to those obtained with MDMA. YY7MQP + +

YYZUYY + - The sample contains 14,25 % 3,4-Methylendioxymethamphetamine (as free base) Z5LF55 + + the powder is a mixture of MDMA hydrochloride and lactose hydrate. The concentration of MDMA (base) in the sample is 13.1% by weight. Z887DL + - The test sample 2016/1/SM-2 was found to contain the controlled drug 3,4-Methylenedioxy- metamfetamine (MDMA). ZF1EFF + + Presence of 3,4-Methylenedioxymetamfetamine hydrochloride and lactose was detected in the sample. ZFFEHN + -

ZH0THY + -

ZOIJZ3 + ANP

ZRG6U6 + ANP Analysis of a representative sample of the powder revealed the presence of methylenedioxymethylamphetamine (MDMA) with a purity of approximately 13% (calculated as base). ZSX0SS + ANP One glass bottle containing 0.23 grammes of a powder containing 0.03 grammes of 3,4- methylenedioxy-methamphetamine.

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

ZXIIII + + MDMA and Lactose

Identification methods for Test Sample 2

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

Summary for test sample 2 The response summary of all 183 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: 183

3,4-Methylenedioxymetamfetamine 179 (MDMA):

False positives for Test Sample 2

Code Name Technique XQJTD9 cocaine 171/180 76BTAAO metamfetamine, amfetamine 140/200 R25T2B MDEA 180

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

Code: R25T2B (180), 7BTAAO (140/200) (MCOLDO (ANP), E8S7ZT (ANP)

Frequency of use of screening and identification techniques: Response Summary ResponseResponse Summary Summary Participants: 130 Participants:Participants: 18 1773 Response Summary 142 150 160 161 190 200 220 SectionParticipants: 176140 141 142 150 160160 161 171 180 190 200 211 220 230 231 210 ScreeningSection 66 73142 60 150 22 160 0 161 1 171 4 180 61 190 17 200 2 211 0 230 1 231 0 0 11 36.3% 40.1% 33.0% 12.1% 0.0% 0.5% 2.2% 33.5% 9.3% 1.1% 0.0% 0.5% 0.0% 0.0% 6.0% Identification 14 6 4 36 8 15 29 165 72 4 3 0 5 1 12 7.7% 3.3% 2.2% 19.8% 4.4% 8.2% 15.9% 90.7% 39.6% 2.2% 1.6% 0.0% 2.7% 0.5% 6.6% # labs using 71 75 61 45 8 15 30 165 79 6 3 1 5 1 21 this 39.0% 41.2% 33.5% 24.7% 4.4% 8.2% 16.5% 90.7% 43.4% 3.3% 1.6% 0.5% 2.7% 0.5% 11.5% technique 52 2016/1-SM Copyright (c) 2016 UNODC

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

MDMA MDMA Deviation Deviation Code Concentration Code Concentration from from robust z-score z-score (mass%) (mass%) robust average average WDNNGN 0.2 -13.6 -11.1 SSOFTB 13.6 -0.2 -0.2 SEF3EE 4.4 -9.4 -7.7 ZF1EFF 13.7 -0.1 -0.1 A1O2PU 8.7 -5.1 -4.2 7VKRTZ 13.7 -0.1 -0.1 KNZKKP 10.2 -3.6 -3.0 6ILHTL 13.7 -0.1 -0.1 KJU4OU 10.2 -3.6 -2.9 UFVIOP 13.7 -0.1 -0.1 TWTWPH 10.6 -3.2 -2.6 MQXQRQ 13.8 0.0 0.0 WDQWLH 11.4 -2.4 -2.0 H7SE4O 13.8 0.0 0.0 G1C7O1 11.5 -2.3 -1.9 EDUYDD 13.8 0.0 0.0 EXIP84 11.9 -1.9 -1.6 ZFFEHN 13.9 0.1 0.1 LNR2DR 12.0 -1.8 -1.5 RV3YT3 13.9 0.1 0.1 DALAM7 12.0 -1.8 -1.5 P3Y0QX 14.0 0.2 0.1 BPJ4JR 12.3 -1.5 -1.2 HCVNSQ 14.0 0.2 0.1 X70OZ9 12.4 -1.4 -1.2 8PHIP8 14.0 0.2 0.1 GCHGCL 12.4 -1.4 -1.2 SLDIJQ 14.0 0.2 0.2 VXFBR6 12.5 -1.4 -1.1 VYZC85 14.1 0.3 0.2 AD2NVY 12.5 -1.3 -1.1 VKNECE 14.1 0.3 0.2 YEKYTF 12.7 -1.1 -0.9 6DWSSS 14.1 0.3 0.2 OOXOOI 12.7 -1.1 -0.9 QS88SU 14.1 0.3 0.2 HW0WRM 12.8 -1.0 -0.8 KTJBZA 14.2 0.4 0.3 SDFWC8 12.8 -1.0 -0.8 BEUIGW 14.2 0.4 0.3 VQT273 12.9 -0.9 -0.8 OFP7ET 14.2 0.4 0.3 R2XKWH 12.9 -0.9 -0.7 YYZUYY 14.3 0.4 0.4 F1M4VD 12.9 -0.9 -0.7 2IQBJI 14.3 0.5 0.4 4EUEWU 13.0 -0.8 -0.7 4PGIDD 14.3 0.5 0.4 YAIIVO 13.0 -0.8 -0.7 ZOIJZ3 14.3 0.5 0.4 ZRG6U6 13.0 -0.8 -0.7 6UM71W 14.3 0.5 0.4 IBPJLJ 13.0 -0.8 -0.7 ZSX0SS 14.3 0.5 0.4 UYPU5U 13.0 -0.8 -0.7 B54OW4 14.4 0.6 0.5 TDVDNQ 13.0 -0.8 -0.7 U90SWA 14.4 0.6 0.5 Z5LF55 13.1 -0.7 -0.6 MBOMMM 14.4 0.6 0.5 EJBJCJ 13.2 -0.6 -0.5 KYO332 14.4 0.6 0.5 QUZQUQ 13.2 -0.6 -0.5 AJO81E 14.4 0.6 0.5 TIKKKK 13.3 -0.5 -0.4 3QY6YS 14.5 0.7 0.6 X2JISE 13.3 -0.5 -0.4 77DRQT 14.7 0.9 0.7 F9I31B 13.3 -0.5 -0.4 J5YB55 14.7 0.9 0.7 FJ44OK 13.4 -0.4 -0.3 331I33 14.8 1.0 0.8 CE7TB2 13.4 -0.4 -0.3 8YMBJO 14.8 1.0 0.8 XQJTD9 13.4 -0.4 -0.3 MOOSOO 14.8 1.0 0.8 5XSWBZ 13.4 -0.4 -0.3 ZXIIII 14.9 1.1 0.9 2MO2K2 13.4 -0.4 -0.3 4LYNGL 15.0 1.2 1.0 NNNNDW 13.4 -0.4 -0.3 RC98IL 15.0 1.2 1.0 P5A5W5 13.5 -0.3 -0.3 91AIRR 15.0 1.2 1.0 3HKZSM 13.5 -0.3 -0.3 LFCJGM 15.2 1.4 1.1 KHHK0G 13.5 -0.3 -0.3 OF6Y6D 15.2 1.4 1.1 6QO4X5 13.5 -0.3 -0.2 ISA8Y8 15.2 1.4 1.1 SK102M 13.6 -0.2 -0.2 VFD46A 15.4 1.6 1.3 LGECDN 13.6 -0.2 -0.2 KWPD3V 15.5 1.7 1.4 OOOIMO 13.6 -0.2 -0.2 EAE6LE 15.6 1.8 1.5

MDMA Deviation Code Concentration from z-score (mass%) robust average 8IXV43 15.6 1.8 1.5 EYAZVH 16.0 2.2 1.8 IXUGYG 16.0 2.2 1.8 QOMLQQ 16.2 2.4 1.9 QWO4OF 16.2 2.4 2.0 9EWNN5 16.3 2.5 2.0 BAYYXO 16.5 2.7 2.2 00T0J0 17.3 3.5 2.8 66BMCC 18.2 4.4 3.6 VXXXL4 19.5 5.7 4.7 DWWWGY 32.0 18.2 14.9

Round: 2016/1 Robust average = 13.8% UNODC value = 13.8% Substance: SM-2; MDMA

4.0 3.6

3.0 2.8 2.2 2.0 2.0 2.0 1.9 1.8 1.8 1.5 1.5 1.4 1.3 1.1 1.1 1.1 1.0 1.0 1.0

1.0 0.9 0.8 0.8 0.8 0.7 0.7 0.6 0.5 0.5 0.5 0.5 0.5 0.4 0.4 0.4 0.4 0.4 0.4 0.3 0.3 0.3 0.2 0.2 0.2 0.2 0.2 0.1 0.1 0.1 11.1 0.1 0.1 ‐ 4.2 7.7 ‐ ‐ 0.0 0 0.0 0.0 0. 14.9 0.1 4.7 0.1 0.1 0.1 ‐ ‐ ‐ ‐ 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 ‐ ‐ ‐ ‐ ‐ ‐ 0.4 0.4 0.4 ‐ ‐ ‐ 0.5 0.5 ‐ ‐ 0.6 ‐ 0.7 0.7 0.7 0.7 0.7 0.7 ‐ ‐ ‐ ‐ ‐ ‐ 0.7 0.7 ‐ ‐ ‐1.0 0.8 ‐ 0.8 0.8 ‐ ‐ 0.9 0.9 ‐ ‐ 1.1 ‐ 1.1 1.2 ‐ 1.2 ‐ ‐ 1.2 ‐ 1.5 1.5 ‐ ‐ 1.6 ‐ ‐2.0 1.9 ‐ 2.0 ‐ 2.6 ‐3.0 ‐ 2.9 3.0 ‐ ‐

‐4.0 ZXIIII IBPJLJ EJBJCJ X2JISE 2IQBJI ZOIJZ3 6ILHTL AYYXO SLDIJQ BPJ4JR RC98IL EXIP84 F9I31B 331I33 ISA8Y8 YAIIVO TIKKKK 00T0J0 ZF1EFF Z5LF55 J5YB55 ZSX0SS 8IXV43 SEF3EE 8PHIP8 KTJBZA YEKYTF 91AIRR FJ44OK EAE6LE VXXXL4 CE7TB2 SSOFTB AJO81E VYZC85 YYZUYY 7VKRTZ UFVIOP RV3YT3 XQJTD9 4LYNGL 3QY6YS OFP7ET VXFBR6 ZFFEHN 4PGIDD X70OZ9 IXUGYG KNZKKP KYO332 LFCJGM P3Y0QX EYAZVH VQT273 H7SE4O OF6Y6D VFD46A VKNECE QS88SU LNR2DR B KJU4OU ZRG6U6 G1C7O1 SK102M LGECDN 77DRQT GCHGCL 8YMBJO 6QO4X5 AD2NVY 5XSWBZ 6DWSSS A1O2PU OOXOOI 3HKZSM KHHK0G UYPU5U BEUIGW 66BMCC SDFWC8 EDUYDD P5A5W5 HCVNSQ F1M4VD DALAM7 2MO2K2 U90SWA R2XKWH TDVDNQ B54OW4 KWPD3V 4EUEWU 9EWNN5 OOOIMO QUZQUQ QWO4OF TWTWPH 6UM71W MQXQRQ MOOSOO QOMLQQ WDNNGN NNNNDW WDQWLH HW0WRM DWWWGY MBOMMM

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

Z-Score Report per Sample per Substance

Round: 2016/1

Dispersion of z-scores using different analytical techniques for the quantification of MDMA in 2016/1 SM-2 10

0 z-score

-2

-4

-6

-8 HPLC GC-FID GC-MS/LC-MS

-10

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

Sample 3 Analysis

Identified substances for Test Sample 3 Code Identified Substances 00T0J0 Amphetamine 1GZVLB anfetamina 2MO2K2 AMFETAMINE 2Q2RKB Amfetamine 331I33 Amfetamine 3HKZSM Amfetamine 3J30PJ Cafeina 3QY6YS amfetamine 3UCRFA Amfetamine 43D6WO Amphetamine, purity 5.4% 4EUEWU AMPHETAMINE 4LYNGL amfetamine, caffeine 4PGIDD amphétamine 4Z40VI Amfetamine 55STC5 Amphetamine 5NU8Q8 Amfetamine 5XSWBZ amphetamine 66BMCC AMFETAMINE 6AKET8 Amphetamine 6DWSSS amphetamine sulphate 6ILHTL Amphetamine 6QO4X5 amphethamine sulphate 6UM71W amphetamine 77DRQT Amfetamine 7BTAAO Metamphetamine and Amphetamine 7VKRTZ Amphetamine 8F8I8T Amphetamine 8IHHJF ANFETAMINA 8IXV43 Amphetamine 8LZBLR Amfetamine 8NM0BB Amfetamine and Caffeine 8PHIP8 Amphetamine 8YMBJO Amphetamine 91AIRR Amphetamine 9EWNN5 Amphetamine A1O2PU --- AA3A9G Amphetamine AAL7YF Amfetamine AD2NVY AMFETAMINE AJO81E amphetamine

Code Identified Substances ASUW2S Amfetamine AZCZ5Z Amphetamine B54OW4 --- BABKJE Amphetamine BAYYXO amphetamine BEUIGW Anfetamina BPJ4JR amfetamine BT6Y0Y Amfetamine C7G4DH amphetamine CE7TB2 Amphetamine CIFQC8 Amfetamine CSJXFO Amphetamine DALAM7 AMFETAMINE DWWWGY ANFETAMINA DY0EG9 AMPHETAMINE EAE6LE Amphetamine EDUYDD Amfetamine EJBJCJ Amfetamine ELQNHU Amphetamine ENI7TJ Amphetamine EYAWUL Amfetamine EYAZVH Amfetamine F1M4VD Amphetamine F9I31B Amphetamine sulphate G1C7O1 Amfetamine GCHGCL Amfetamine GDGBEX Amfetamine GLYEEK amphetamine H7SE4O Anfetamina HCVNSQ amphetamine HNG20U Amphetamine HW0WRM Amphetamine IBPJLJ amphetamine (caffine and creatine monohydrate also present) ICQNLB Amphetamine IIX7UR Caffeine ISA8Y8 Amfetamine IUW8JU Cafeine IXUGYG Amfetamine J28855 AMFETAMINE J5YB55 amfetamine JJLJOU amphetamine, caffeine KBC4MU AMPHETAMINE KHHK0G Amphetamine KJU4OU Amphetamine,Caffeine

Code Identified Substances KLL25F Amphetamine KNZKKP AMFETAMINE KTJBZA amphetamine KWPD3V amfetamine KYO332 Amphetamine L9LTEO Amfetamine LEPP7L Caffeine LFCJGM Amfetamine LGECDN Amfetamine LLLLTB amfetamine LNR2DR Amphétamine M5LL0L ANPHETAMINE M9MFMP Amphetamine, caffeine MBOMMM Amfetamine Sulfate MCOLDO Amfetamine MOOSOO amphetamine MQXQRQ Amphetamine MVVNXZ Amphetamine NNNNDW Amphetamine O1DHE1 Amphetamine mixed with caffeine O28H4R Amp OF6Y6D amfetamine OFP7ET Amfetamine OOOIMO Amphetamine OOXOOI AMFETAMINE, CAFFEINE OSTFUT amphetamine OWRO6K Amphetamine OYX2R3 ANFETAMINA OZLPCC Amfetamine, Synthetic cathinones P3Y0QX amfetamine P5A5W5 Amfetamine P7ZPBP Yes Amfetamine and Caffeine PPPKPP Amphetamine QOMLQQ Anfetamine QS88SU Amphetamine QUZQUQ Amfetamine QWO4OF AMFETAMINE R25T2B CAFFEINE R2XKWH Amphetamine R3QRYO Amphetamine and Caffeine RC98IL sulphate amfetamine RV3YT3 Amphetamine S9YJGM AMPHETAMINE SDFWC8 Amphetamine sulfate

Code Identified Substances SEF3EE - SK102M amphetamine SLDIJQ amfetamine SSOFTB Amfetamine T7YTFO amfetamine TBK0V2 MDMA, ANFETAMINA, METANFETAMINA, MDA, GHB, FENOBARBITAL TDVDNQ Amphetamine TEZEE4 AMPHETAMINE, CAFFEINE TIKKKK Amfetamine TRQBQ8 AMPHETAMIN SO4 TSGAGB AMFETAMINE, CAFFEINE TWTWPH Amphetamine TWYAAL amfetamine U90SWA AMFETAMINE UFVIOP Amfetamine UQMBX2 AMPHETAMINE, CAFFEINE UYPU5U Amphetamine VFD46A Amphetamine VKNECE amphetamine 5.28 VNZ61V Amfetamine VQT273 dextroamphetamine VXFBR6 Amfetamine VXXXL4 amphetamine VYZC85 Amphetamine WDNNGN Amphetamine WDQWLH Amphetamine X2JISE Amfetamina X456G5 AMFETAMINE, CAFFEINE X70OZ9 AMPHETAMINE XFVW1V Amphetamine XNQ60K amphetamine XQJTD9 Amfetamine XRKU5U Amphetamine YAH8BE amphetamine YAIIVO Amphetamine YEKYTF amfetamine YXZMMX Amphetamine YY5Y1A Amfetamine YY7MQP anfetamine, caffeine YYZUYY Amphetamine Z5LF55 amphetamine Z887DL Amfetamine ZF1EFF Amphetamine ZFFEHN AMFETAMINE 5.2%, CAFFEINE

Code Identified Substances ZH0THY Amphetamine ZOIJZ3 ANPHETAMINE ZRG6U6 Amphetamine ZSX0SS Amphetamine ZXIIII Amphetamine

Statement of findings for Test Sample 3

Code Amfetamine Caffeine 00T0J0 + + Sample contained amphetamine cut with caffeine 1GZVLB + +

2IQBJI - +

2MO2K2 + + ./. 2Q2RKB + + Amfetamine and Caffeine confirmed 331I33 - + Caffeine 3HKZSM + + Mixture of amfetamine (low content) in caffeine and creatine. Content of caffeine approx. 30 % w/w. 3J30PJ ANP + es considerado un estimulante de uso legal en XXX 3QY6YS + ANP

3UCRFA + + the sample contains a mixture Amfetamine and caffeine 43D6WO + + Amphetamine is a Class B controlled drug subject to the provisions of the Misuse of Drugs Act 1971. 4EUEWU + - The sample 2016/1/SM-3 was found to contain the illicit drug AMPHETAMINE. 4LYNGL + + The sample contains also creatine which is not scheduled as illicit drug in XXXX. The amfetamine is scheduled as illicit drug in XXXX. The caffeine is a cutting agent. 4PGIDD + + The sample contains amphétamine, caféine and créatine. Amphétamine is sheduled as illicit drug. 4Z40VI + + Amfetamine, caffeine, creatine-compare mass spectra with library, retention time of sreference sample, Amfetamine, FTIR creatine 55STC5 + +

5NU8Q8 + + The powder was analysed and found to contain amphetamine and caffeine. 5XSWBZ + + amphetamine and caffeine 66BMCC + - found amfetamine with 1.23% in SM-3 6AKET8 + + SM-1 found to contain Amphetamine 6DWSSS + + white powder containing also caffeine and creatine as diluents

Code Amfetamine Caffeine 6ILHTL + + Quantitative analysis of amphetamine is not routinely carried out by our laboratory. Substances detected include caffeine and creatine. 6QO4X5 + + amphetamine base 5,1 % 6UM71W + + Amphetamine is controlled by KB 22/01/1998 77DRQT + + Amfetamine SULFATE 5.5% AS BASE - CAFFEINE - MALTOSE 7BTAAO + ANP There was evidence of Metamphetamine and Amphetamine 7VKRTZ + + This sample is amphetamine 8F8I8T + + caffeine. 8IHHJF + +

8IXV43 + + A sample of this powder was analysed and found to contain amphetamine at a concentration of 5%. This sample was also found to contain caffeine and creatine. 8LZBLR + - SM-3 to contain Amfetamine 8NM0BB + + The Test sample 2016/1/SM-3 was analyzed by Colour test and Thin Layer Chromatography technique and found to contain Amfetamine and Caffeine. 8PHIP8 + + A sealed glass vial containing a white powder. This powder contained an average of 5% Amphetamine. 8YMBJO + + The sample consist controlled drugs - amphetamine 91AIRR + +

9EWNN5 + + The item is a powder containing Amphetamine and creatine and caffeine. The percent of free base is 7.5% A1O2PU ANP ANP wite powder with unknown smell AA3A9G + + White powder containing Amphetamine. Also detected Caffeine AAL7YF + + Colorimetrics reactions showed positive result for substances like amphetamines. That was confirmed by GC/MS. Caffeine and Amphetamine was detected and identified AD2NVY + + CAFFEINE AJO81E + +

ASUW2S + + Also contain caffeine AZCZ5Z + + amphetamine and caffeine

Code Amfetamine Caffeine B54OW4 - + white powder containing caffeine BABKJE + + The powder, which weighed 0.22 grams, was analysed and found to contain Amphetamine. Amphetamine is a class B controlled drug within the provisions of the Misuse of Drugs Act 1971.

BAYYXO + + Sample contains amphetamine sulphate, caffeine and creatine BEUIGW + - La muestra contiene Anfetamina. BPJ4JR + + It has been detected the presence of amfetamine in the sample BT6Y0Y + + Sample 2016/1/SM-3 consists of white powder. Amfetamine, a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. C7G4DH + + caffeine, creatine monohydrate CE7TB2 + + The sample contains amphetamine. The content of amphetamine (as amphetaminesulphate) is determined to 7 %. Amphetamine is a controlled substance in X. CIFQC8 + + Sample 2016/1/SM-3, a white powder with acrid odour, gave a positive result for amfetamine, a controlled substance under national legislation on drugs. CSJXFO + + Examination revealed the presence of Amphetamine DALAM7 + + The sample 3 contains AMFETAMINE, which is a controlled substance in XXXX. DWWWGY + + ANFETAMINA, CAFEINA, OTRA SUBSTANCIA NO IDENTIFICADA DY0EG9 + + the results of the screening test "TLC (Tech:150)" and identification , confirmation analytic techniques HPLC (160) and GC/MS (180). E8S7ZT ANP ANP nous avions en screening des substances sous contrôle (amphétamine, toluène) mais l'identification et la confirmation n'ayant pas pu être faites faute de standards, nous ne pouvons pas le mentionner. Il y a un composé non identifié qui est commun à 2016/1/SM-3 et 2016/1/SM-1 qui apparâit par la technique 150 (Chromatographie sur couche mince). A la limite des techniques utilisées et le manque de standards nous n'avons pas pu identifier d'autres substances sous contrôle. EAE6LE + + The sample contains Amphetamine and Caffeine. The content of Amphetamine as base is 15.6%. EDUYDD + + The sample contains amfetamine which is listed as a controlled drug according to XXXX order, appendix III of February 22nd 1990. EJBJCJ + + In the test sample 2016/1/SM-3 were detected amfetamine and caffeine ELQNHU + + Based on the above analysis, the sample was found to contain amphetamine and caffeine. ENI7TJ + + From screening test using (MR), (FTIR) and ion scan and from confirmatory test using (GC-MS), the sample was found to contain controlled drug Amphetamine.

Code Amfetamine Caffeine EXIP84 - + Sample contain caffeine. EYAWUL + + SM3 contains Amfetamine Sulphat, Caffeine and Creatinine. EYAZVH + + The sample contains a controlled substance as Amfetamine and caffeine cutting. F1M4VD + + Amphetamine was identified by TLC and GC-MS. F9I31B + + Amphetamine, caffeine, Creatine. BASE AMPHETAMINE 5,9% FJ44OK + +

G1C7O1 + + Caffeine GCHGCL + + Sample contains 5.39 ± 0.42 % Amfetamine base. Caffeine and creatine were also detected. GDGBEX + + Sample SM-3 was found to contain amfetamine. GLYEEK + + The sample 2016/1/SM-3 contains amphetamine and caffeine. H7SE4O + + Adulterantes: cafeína HCVNSQ + + amphetamine,caffeine,creatinin HNG20U + + Was found Caffeine HW0WRM + +

IBPJLJ + + The powder contained amphetamine, together with the adulterants caffeine and creatine monohydrate ICQNLB + + Powder from test sample 2016/1/SM-3 contain Amphetamine with Caffeine IIX7UR - + Marquis reagent (MR) positive. GC/MS Retention time and mass charge ratio (M/Z), similar characteristics whit the subtances used as standar or pattern. ISA8Y8 + + Sample 2016/1/SM-3 found to contain amfetamine and caffeine IUW8JU - + De los análisis realizados, se concluye que la sustancia se trata de cafeina IXUGYG + + - J28855 + + AMFETAMINE AND CAFEINE J5YB55 + + Amfetamine. Caffeine and creatine were also identified JJLJOU + + in the sample labeled as 2016/1 / SM-3 they were found amphetamine and caffeine.

Code Amfetamine Caffeine KBC4MU + + White powder that contains controlled substance AMPHETAMINE and adulterant CAFFEINE. KHHK0G + + The sample was found to contain amphetamine, caffeine and fructose. KJU4OU + + Amalic Acid test indicates the possable presence of Caffeine.Analysis by GCMS shows the similarity as Caffeine. KLL25F + + From colorimetric reaction, it gave orange color with Marquis Reagent and GCMS results gave amphetamine and caffeine KNZKKP + +

KTJBZA + + The test sample also contained caffeine KWPD3V + + Amfetamine was detected by GC/MS screening and it was quantified by LC/MS/MS KYO332 + + It is an usually detected drug in our laboratory. L9LTEO + + Test sample 2016/1/SM-3 contains Amfetamine, a dangerous drug. It also contains caffeine. LEPP7L - +

LFCJGM + + contained amfetamine and cofeine LGECDN + + The sample contains amfetamine (6.0%) and caffeine. LLLLTB + + The test sample SM-3 contains stimulating narcotic drugs amfetamine. LNR2DR + + caffeine, lactose M5LL0L + ANP

M9MFMP + + screening by colorimetric test confirmation by GC-MS and FTIR MBOMMM + + Caffeine, Creatine MCOLDO + ANP

MOOSOO + + Test sample 2016/1/SM-3 contains amphetamine 5.1 %, m/m and caffeine. MQXQRQ + + In Sample 3 was identified amphetamine and caffeine, creatine. MVVNXZ + ANP The off-white powder contains amphetamine. NNNNDW + + It contains 5.00 % of Amphetamine and also contains Caffein O1DHE1 + + the sample was confirmed by GC MS

Code Amfetamine Caffeine O28H4R + + GC-MS OF6Y6D + +

OFP7ET + + Caffeine OOOIMO + + Amphetamine, conc. 5% as free base, other substance found is caffeine OOXOOI + + CAFFEINE AS CUT AND FOUND CREATININE AS TRACE LEVEL OSTFUT + + creatine, caffeine OWRO6K + + Amphetamine and Caffeine were identified. OYX2R3 + + SE ENCONTRÓ ADEMÁS CAFEINA OZLPCC + ANP

P3Y0QX + + white powder containing 1.0%w/w of amfetamine P5A5W5 + + Presence of Amfetamine, concentration of 2.56%, with the presence of the following adulterants:caffeine and creatine. P7ZPBP + + A preliminary test SCOTT and MARQUIS to know what kind of drugs were present in the samples that have been sent and two confirmation tests TLC and GC-FID. In the case of the sample referenced with the 2016/code 1/SM-3 was able to verify the presence of Amfetamina Marquis test and other tests it was also verified the presence of Amfetamine and Cafeine. PPPKPP + + Powder was analysed and found to contain amphetamine and caffeine. QOMLQQ +

QS88SU + + The sample contained 5.8 % amphetamine. Additionally caffeine and creatine was detected in the sample. QUZQUQ + + Mass spectrometry profile correlation between sample and reference material certified QWO4OF + +

R25T2B - + We diluited 1 mg of the sample in 10 mL of methanol and analized by CG-MS. R2XKWH + -

R3QRYO + + Nil RC98IL + + SM3 was prepared from a seizure containing 7% w/w amfetamine base. The sample also contained caffeine and creatinine RV3YT3 + + Powder containing amphetamine and caffeine

Code Amfetamine Caffeine S9YJGM + + The results of the test of SM3 (228) received confirmed that the mentioned simple contains AMPHETAMINE but we are not able to give a cuantification result. The sample 3 also contains caffeine as not controlled drugs. SDFWC8 + + additional substance: caffeine, creatine SEF3EE - + Caffeine was identified as the main component. In addition, propanoic acid, 3,3-thiobis-didodecyl ester was also identified in the sample. SK102M + +

SLDIJQ + + the sample is miture of amfetamine, caffeine and creatine SSOFTB + + Presence of amfetamine: retention time and MS spectra in GC analysis (FID and MS) and DRX analysis. Amfetamine as hydrochloride. Presence of caffeine: GC-MS and XRD analysis. Presence of creatine: FTIR and XRD analysis. T7YTFO + +

TBK0V2 + ANP SUSTANCIAS DISUELTAS EN METANOL E IDENTIFICADAS MEDIANTE CG/FID Y UV TDVDNQ + + x grams of powder containing 5% amphetamine. Caffeine was also detected. TEZEE4 + + We determined a mixture of Amphetamine and Caffeine. THQ2CH + +

TIKKKK + + SM-3 contains amfetamine TRQBQ8 + + CAFEIN TSGAGB + + The 2016/1/SM-3 sample was found to contain Amfetamine and Caffeine. TWTWPH + +

TWYAAL + + The sample contains amfetamine and caffeine U90SWA + + Not quantified UFVIOP + + The sample contains Amfetamine and Caffeine. UQMBX2 + + WHITE POWDER SAMPLE ANALYZED CONTAINS AMPHETAMINE AND CAFFEINE UYPU5U + + 225 milligrams of an off-white powder containing amphetamine, caffeine and creatine monohydrate. This off-white powder contained an average of 5% of amphetamine (purity has been calculated in the base form). VFD46A + + the SM-3 sample contains 9.46% of Amphetamine cut by caffeine

Code Amfetamine Caffeine VKNECE + + After analyzing the sample with CR, MSD confirmation and FID quantification we can confirm that sample contains amphetamine and caffeine. VNZ61V + - THYE SAMPLE CORRESPOND IS Amfetamine VQT273 + + caffeine VXFBR6 + + Amfetamine - 5.15%, caffeine VXXXL4 + + the light brown powder could contain amphetamine which is controlled by national law, but it's content is under the limit of quantification of our laboratory. VYZC85 + + Amphetamine is on the list of drug WDNNGN + + after chemical analysis was performed the sample was found to contain 1/ Amphetamine 5 %. 2/ Caffeine. WDQWLH + + Powder containing amphetamine X2JISE + -

X456G5 + +

X70OZ9 + +

XFVW1V + + In this Sample Contain tow Substance Amphetamine and Caffeine XNQ60K + +

XQJTD9 + + Amfetamine existed in salt form. We found caffeine in the sample XRKU5U + + On analysis, I found the sample "SM-3" containing Amphetamine and Caffeine. Y38I3T + ANP En la muestra SM-3, se encontro la presencia de Anfetamina YAH8BE + + caffeine, creatine YAIIVO + + Amphetamine (salt form and isomer not determined), caffeine, and creatine were confirmed in 1 unit tested of 1 unit received. YEKYTF + + powder contains amfetamine with caffeine and creatin YXZMMX + + Amphetamine is a controlled drug. Indications of caffeine. YY5Y1A + + Results of screening tests were positive for amfetamine. Retention time and fragmentation pattern obtained with sample are equivalent to those obtained with anfetamine. YY7MQP + +

Code Amfetamine Caffeine YYZUYY + + The sample contains 5.68 % amphetamine (as free base) Z5LF55 + + the powder is a mixture of amphetamine sulfate, caffeine and creatine hydrate. The concentration of amphetamine (as base) in the sample is 5.2% by weight. Z887DL + + The test sample 2016/1/SM-3 was found to contain the controlled drug amfetamine. The sample was also found to contain caffeine. ZF1EFF + + Presence of amphetamine hydrochloride, caffeine, creatine was detected in the sample. ZFFEHN + +

ZH0THY + + Amphetamine + caffeine ZOIJZ3 + +

ZRG6U6 + + Analysis of a representative sample of the powder revealed the presence of amphetamine with a purity of 6% (calculated as base). ZSX0SS + + One glass bottle containing 0.21 grammes of a powder containing 0.01 grammes of amphetamine. ZXIIII + + Amphetamine and caffeine.

Identification methods for Test Sample 3

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

Summary for test sample 3 The response summary of all 183 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: 183

Amfetamine: 171 Caffeine: 165

False positives for Test Sample 3

Code Name Technique 331I33 MDMA 180 TBK0V2 Metamfetamine, MDMA 171 TBKOVZ M DA, GHB, Phenobarbital 171 7BTAAO Metamfetamine 140/200

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

2IQBJI (180), EXIP84 (180/190), B54OW4 (171/180), 331I33 (180), IIX7UR (180), SEF3E (180),

LEPP7L (180/190), IUW8JU (180), R25T2B (180), 3J3OPJ (ANP), A1O2PU (ANP), E8S7ZT (ANP)

Frequency of use of screening and identification techniques: Response Summary ResponseResponse Summary Summary Participants: Response 130 Summary Participants:Participants:Participants: 183 17633 77

Section 140 141142142142 150150 150 160160 160 161 161 161171 171180 180190 190190200 200 200 211 211220 230220 230 231 231 210 Screening 66 73 60 22 0 1 4 61 17 2 0 1 0 0 11 36.3% 40.1% 33.0% 12.1% 0.0% 0.5% 2.2% 33.5% 9.3% 1.1% 0.0% 0.5% 0.0% 0.0% 6.0% Identification 14 6 4 36 8 15 29 165 72 4 3 0 5 1 12 7.7% 3.3% 2.2% 19.8% 4.4% 8.2% 15.9% 90.7% 39.6% 2.2% 1.6% 0.0% 2.7% 0.5% 6.6% # labs using 71 75 61 45 8 15 30 165 79 6 3 1 5 1 21 this 39.0% 41.2% 33.5% 24.7% 4.4% 8.2% 16.5% 90.7% 43.4% 3.3% 1.6% 0.5% 2.7% 0.5% 11.5% technique

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

Amfetamine Amfetamine Deviation Code Concentration Deviation from Code Concentration z-score from robust z-score (mass%) robust average (mass%) average P3Y0QX 1.0 -4.5 -6.9 J5YB55 5.4 -0.1 -0.1 66BMCC 1.2 -4.3 -6.6 5XSWBZ 5.4 -0.1 -0.1 P5A5W5 2.6 -2.9 -4.5 SK102M 5.5 0.0 0.0 X70OZ9 3.8 -1.8 -2.7 77DRQT 5.5 0.0 0.0 3HKZSM 3.9 -1.6 -2.4 ZOIJZ3 5.5 0.0 0.0 ZXIIII 4.1 -1.4 -2.1 KWPD3V 5.5 0.0 0.0 R2XKWH 4.1 -1.4 -2.1 4Z40VI 5.5 0.0 0.0 AJO81E 4.4 -1.2 -1.8 ZSX0SS 5.5 0.0 0.0 X2JISE 4.4 -1.1 -1.7 91AIRR 5.6 0.1 0.1 331I33 4.5 -1.0 -1.5 EDUYDD 5.6 0.1 0.2 8YMBJO 4.5 -1.0 -1.5 6UM71W 5.6 0.1 0.2 YXZMMX 4.7 -0.8 -1.2 YYZUYY 5.7 0.2 0.3 VQT273 4.7 -0.8 -1.2 WDQWLH 5.7 0.2 0.3 LFCJGM 4.8 -0.7 -1.1 SSOFTB 5.7 0.2 0.3 XQJTD9 4.9 -0.6 -0.9 KYO332 5.8 0.3 0.4 WDNNGN 5.0 -0.5 -0.8 RV3YT3 5.8 0.3 0.5 NNNNDW 5.0 -0.5 -0.8 QS88SU 5.8 0.3 0.5 UYPU5U 5.0 -0.5 -0.8 F9I31B 5.9 0.4 0.6 8PHIP8 5.0 -0.5 -0.8 HCVNSQ 5.9 0.4 0.6 TDVDNQ 5.0 -0.5 -0.8 AD2NVY 5.9 0.4 0.6 MOOSOO 5.1 -0.4 -0.6 QOMLQQ 5.9 0.4 0.6 HW0WRM 5.1 -0.4 -0.6 TWTWPH 6.0 0.5 0.7 6DWSSS 5.1 -0.4 -0.6 LGECDN 6.0 0.5 0.8 6QO4X5 5.1 -0.4 -0.6 ZRG6U6 6.0 0.5 0.8 MBOMMM 5.1 -0.4 -0.6 4LYNGL 6.0 0.5 0.8 VXFBR6 5.2 -0.4 -0.5 IBPJLJ 6.0 0.5 0.8 Z5LF55 5.2 -0.3 -0.5 SLDIJQ 6.1 0.6 0.9 TIKKKK 5.2 -0.3 -0.5 UFVIOP 6.1 0.6 0.9 ZFFEHN 5.2 -0.3 -0.5 KTJBZA 6.2 0.7 1.1 8IXV43 5.2 -0.3 -0.4 H7SE4O 6.2 0.7 1.1 VYZC85 5.3 -0.3 -0.4 IXUGYG 6.3 0.8 1.1 SDFWC8 5.3 -0.2 -0.4 7VKRTZ 6.4 0.9 1.4 VKNECE 5.3 -0.2 -0.3 00T0J0 6.5 1.0 1.5 YAIIVO 5.3 -0.2 -0.3 4EUEWU 6.5 1.0 1.5 MQXQRQ 5.3 -0.2 -0.3 G1C7O1 6.7 1.2 1.8 CE7TB2 5.3 -0.2 -0.3 KNZKKP 6.9 1.4 2.1 YEKYTF 5.3 -0.2 -0.3 DWWWGY 7.0 1.5 2.3 3QY6YS 5.3 -0.2 -0.3 RC98IL 7.0 1.5 2.3 EJBJCJ 5.4 -0.1 -0.2 EYAZVH 7.2 1.7 2.6 1GZVLB 5.4 -0.1 -0.2 9EWNN5 7.5 2.0 3.1 OOXOOI 5.4 -0.1 -0.2 KJU4OU 8.0 2.5 3.8 ZF1EFF 5.4 -0.1 -0.2 QWO4OF 8.6 3.1 4.8 43D6WO 5.4 -0.1 -0.2 VFD46A 9.5 4.0 6.0 OOOIMO 5.4 -0.1 -0.2 F1M4VD 9.6 4.1 6.3 BPJ4JR 5.4 -0.1 -0.2 OFP7ET 11.1 5.6 8.5 GCHGCL 5.4 -0.1 -0.2 QUZQUQ 22.4 16.9 25.8 EAE6LE 5.4 -0.1 -0.2 MCOLDO 35.6 30.1 45.9

Robust average = 5.5% UNODC value = 5.5%

4.0 3.1 3.0 2.6 2.3 2.3 2.1

2.0 1.8 1.5 1.5 1.4 1.1 1.1 1.1 9 0.9 1.0 0. 0.8 0.8 0.8 0.8 0.7 0.6 0.6 0.6 0.6 0.5 0.5 0.4 0.3 0.3 0.3 0.2 0.2 0.1 6.6 6.9 4.5 0.0 0.0 0.0 0.0 0.0 ‐ ‐ 0.0 ‐ 0.0 45.9 3.8 25.8 4.8 6.3 0.1 6.0 8.5 0.1 ‐ 0.2 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 ‐ 0.4 ‐ ‐ 0.4 0.5 0.5 0.5 ‐ ‐ ‐ ‐ 0.5 ‐ 0.6 0.6 0.6 0.6 0.6 ‐ ‐ ‐ ‐ ‐ 0.8 0.8 0.8 0.8 0.8

‐1.0 ‐ ‐ ‐ ‐ ‐ 0.9 ‐ 1.1 ‐ 1.2 ‐ 1.2 ‐ 1.5 1.5 ‐ ‐ 1.7 ‐ 1.8

‐2.0 ‐ 2.1 2.1 ‐ ‐ 2.4 ‐ 2.7 ‐3.0 ‐

‐4.0 ZXIIII IBPJLJ EJBJCJ X2JISE ZOIJZ3 SLDIJQ BPJ4JR RC98IL 331I33 F9I31B 4Z40VI YAIIVO TIKKKK ZF1EFF 00T0J0 J5YB55 ZSX0SS Z5LF55 8IXV43 8PHIP8 91AIRR YEKYTF KTJBZA EAE6LE AJO81E YYZUYY VYZC85 CE7TB2 SSOFTB 7VKRTZ UFVIOP RV3YT3 XQJTD9 OFP7ET 3QY6YS 4LYNGL 1GZVLB VXFBR6 ZFFEHN IXUGYG X70OZ9 KNZKKP KYO332 P3Y0QX LFCJGM EYAZVH VQT273 VFD46A VKNECE H7SE4O QS88SU KJU4OU ZRG6U6 77DRQT LGECDN SK102M G1C7O1 8YMBJO GCHGCL 6QO4X5 6DWSSS 5XSWBZ AD2NVY OOXOOI 3HKZSM UYPU5U EDUYDD SDFWC8 66BMCC P5A5W5 HCVNSQ F1M4VD R2XKWH TDVDNQ KWPD3V 4EUEWU 43D6WO 9EWNN5 YXZMMX OOOIMO MCOLDO QUZQUQ QWO4OF 6UM71W TWTWPH MQXQRQ MOOSOO QOMLQQ WDNNGN NNNNDW WDQWLH HW0WRM DWWWGY MBOMMM

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 Round: 2016/1 |z| > 3 = unsatisfactory Substance: SM-3; Amfetamine 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. 78

Z-Score Report per Sample per Substance

Round: 2016/1

Dispersion of z-scores using different analytical techniques for the quantification of Amfetamine in 2016/1 SM-3 10

0 z-score

-2

-4

-6

-8 HPLC GC-FID GC-MS/LC-MS

-10

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

Sample 4 Analysis

Identified substances for Test Sample 4 Code Identified Substances 3J30PJ Canabinol 4PGIDD none 5XSWBZ the drug is not revealed 6ILHTL No drugs was found 8NM0BB No Drugs found A1O2PU --- AA3A9G ----- B54OW4 --- BABKJE None BAYYXO no drugs CIFQC8 - EAE6LE No controlled drugs detected in the sample. ELQNHU None ENI7TJ Cocaine (coca leaves) EYAWUL - EYAZVH W 18 G1C7O1 No drugs H7SE4O Negative HCVNSQ - IIX7UR none ISA8Y8 none IXUGYG - JJLJOU none KBC4MU NONE KHHK0G none KJU4OU lactose KLL25F Not detected KWPD3V --- KYO332 Negative LFCJGM Drugs not found LGECDN None O28H4R CBD,CBN OF6Y6D --- OOOIMO - OWRO6K none OYX2R3 NO SUSTANCIAS CONTROLADAS OZLPCC Synthetic cathinones P5A5W5 No drugs P7ZPBP No drug found QWO4OF LSD

Code Identified Substances R3QRYO Nil RV3YT3 - S9YJGM NONE SDFWC8 none SEF3EE Heroin SSOFTB No drug TBK0V2 MDMA, HEROINA, 1-BENZILPIPERAZINA, NORBUPRENORFINA TEZEE4 delta-9-THC, CANNABINOL TSGAGB NIL TWYAAL - VNZ61V THE SAMPLE CONTAINS NO DRUG ABUSE VXXXL4 --- XFVW1V No Controll Drugs YAH8BE blank YY7MQP blank Z5LF55 ---

Statement of findings for Test Sample 4

Code [blank sample] 00T0J0 Blank sample containing Starch and Henna(caracteristic smell) 1GZVLB 2IQBJI 2MO2K2 ./. 2Q2RKB It does not contain any controlled substance included in ICE/2016/1/SM Menu. 331I33 3HKZSM Plant material (cellulose, hemicellulose). Also contains sucrose (approx. 10 % w/w). 3J30PJ 3QY6YS 3UCRFA 43D6WO No controlled drugs were detected. 4EUEWU The sample 2016/1/SM-4 was NOT found to contain illicit drugs. 4LYNGL 4PGIDD 4Z40VI This sample is plant material- no controlled substance 55STC5 5NU8Q8 The vegetable matter was analysed for common controlled drugs with a negative result. 5XSWBZ the drug is not revealed 66BMCC 6AKET8 6DWSSS green color powder no drugs detected 6ILHTL No controlled drugs were detected. 6QO4X5 6UM71W No controlled drugs detected. 77DRQT 7BTAAO 7VKRTZ This sample does not contain drugs. 8F8I8T 8IHHJF 8IXV43 A sample of the powder was analysed and found to contain no controlled substances. 8LZBLR No drugs found in SM-4 8NM0BB The Test sample 2016/1/SM-4 was analyzed by Colour test and Thin Layer Chromatography technique and found not to contain drugs. 8PHIP8 A sealed glass vial containing a green powder. No controlled drugs were detected in this powder 8YMBJO 91AIRR 9EWNN5 the item, accordingly to our laboratory procedures doesn't contain any psycoactive substance. A1O2PU green vegetable powder and tea smell AA3A9G Green powder. No scheduled substances detected.

Code [blank sample] AAL7YF AD2NVY AJO81E ASUW2S AZCZ5Z B54OW4 green powder not containing any of the substances listed in part. 2 or 1 BABKJE The powder, which weighed 0.22 grams, was analysed for the presence of drugs controlled within the provisions of the Misuse of Drugs Act 1971, with a negative result. BAYYXO Sample does not containe any drug. BEUIGW Sustancia No controlada. BPJ4JR BT6Y0Y Sample 2016/1/SM-4 consists of green powder. No prohibited substances are detected in this sample. C7G4DH CE7TB2 The sample is not identified. With the methods used, no controlled substance are detected in the sample. CIFQC8 Sample 2016/1/SM-4, a green powder with fruity odour, was not found to contain any controlled substance under national legislation on drugs. CSJXFO No Controlled Substances was detected. DALAM7 The sample 4 doesn't contain a controlled substance. DWWWGY CLOROFILA DY0EG9 E8S7ZT Nous avions en screening obtenu une substance sous control (le pipéronal ou l'acide phénylacétique) mais l'identification et la confirmation n'ayant pas pu été faites faute de standards et de méthod, nous ne pouvons pas la mentionner. A la limite des techniques utilisées et le manque de standards nous n'avons pas pu identifier de substances sous contrôle. EAE6LE EDUYDD The analysis did not reveal any controlled drug according to XXXX order, decree of February 22nd 1990. EJBJCJ ELQNHU Based on the above analysis, the sample was found not to contain any controlled drugs. ENI7TJ From screening test using (FTIR) and from confirmatory test using (GC-MS), the sample was found to contain controlled drug Cocaine. EXIP84 EYAWUL Sucrose was identified. EYAZVH The sample contains W-18, an analgesic drug. F1M4VD F9I31B FJ44OK G1C7O1 GCHGCL Sample contains no controlled drugs. GDGBEX GLYEEK The sample 2016/1/SM-4 doesn't contains drugs

Code [blank sample] H7SE4O Cromatografía de gases FID: negative HCVNSQ - HNG20U Was found sucrose HW0WRM IBPJLJ This powder was analysed for the presence of controlled drugs with negative results ICQNLB Powder from test sample 2016/1/SM-4 does not contain any controled drugs IIX7UR Marquis reagent (MR),Cobalt Thiocyanate and colorimetric reactions, Negative. GC/MS Retention time and mass charge ratio (M/Z), not concide whit the reference material used as pattern. ISA8Y8 No drugs detected on sample 2016/1/SM-4 IUW8JU De los análisis realizados, se concluye que la sustancia no contiene alguna droga sujeta a fiscalización ni otros componentes de interés toxicológico. IXUGYG - J28855 CRUSHING PLANT MATERIAL ,DOES NOT CONTAIN CONTROLLED SUBSTANCES J5YB55 JJLJOU In the sample labeled as 2016/1/SM-4 not controlled substances were detected. KBC4MU Pulverized plant material that contains sugar without any of controlled substance. KHHK0G The sample was analysed and found to contain no common controlled drug. KJU4OU No reactions with Marquis Test,Simon Test,Chen-Kao Test and Fast Blue B Salt Test.Analysis by GCMS shows the similarity as lactose. KLL25F Negative common drugs/unknown KNZKKP KTJBZA The test sample contained glucose and sucrose KWPD3V only caffeine found KYO332 L9LTEO Test sample 2016/1/SM-4 does not contain substances listed in the ICE menu. LEPP7L LFCJGM LGECDN No controlled drugs detected. LLLLTB LNR2DR M5LL0L M9MFMP colorimetric test: negative for drugs confirmation by GM-MS: negative for drugs MBOMMM vegetal, saccharose MCOLDO Unofrtunately, we dont have the proer derivitization reagent fot the analysis of THC and its derivatives MOOSOO Test sample 2016/1/SM-4 do not contain drugs. MQXQRQ Plant material MVVNXZ Negative for controlled drugs. NNNNDW The sample is free from any ICE programme drugs O1DHE1 the sample was confirmed by GC MS and no illict compounds were found

Code [blank sample] O28H4R GC-MS OF6Y6D OFP7ET OOOIMO No substance controlled in legislation is found, vitamine E was found OOXOOI SAMPLE OF PLANT ORIGIN OSTFUT OWRO6K none was found in the sample. OYX2R3 La muestra recibida es material vegetal pulverizada en la que no se detectan sustancias controlas. OZLPCC P3Y0QX green powder not containing any controlled drug. P5A5W5 We detected Vitamine E and compounds related to vegetable substances (palmitic acid, linolenic acid and Glycerol palmitate). P7ZPBP A preliminary test SCOTT and MARQUIS to know what kind of drugs were present in the samples that have been sent and two confirmation tests TLC and GC-FID. In the case of the sample referenced with the code 2016/1/SM-4 was able to verify no presence of drug Marquis test and other tests it was also verified no presence of drugs. PPPKPP Powder was analysed and found to contain a mixture of different synthetic cannabinoids. QOMLQQ QS88SU The sample did not containe any controlled drugs. QUZQUQ QWO4OF R25T2B R2XKWH No controlled substance detected R3QRYO Nil RC98IL SM4 is a blank sample RV3YT3 Green powder containing no illicit drugs S9YJGM We have not found any controlled drug in the simple 4 (223) SDFWC8 SEF3EE Heroin was identified in the sample. Also 6-monoacetyl morphine, caffeine, dronabinol and vitamin E were identified. Analysis revealed that percentage of heroin is 2.25% SK102M SLDIJQ the sampled is fine grinded plant material SSOFTB No drugs detected by FTIR, XRD, GC-MS. T7YTFO TBK0V2 SUSTANCIAS DISUELTAS EN METANOL E IDENTIFICADAS MEDIANTE CG/FID Y UV TDVDNQ x grams of powder. No controlled drugs were detected. TEZEE4 We determined a mixture of delta-9-THC and Cannabinol. THQ2CH TIKKKK SM-4 contains no drugs, it is a blank sample TRQBQ8 INOSITOL SACCHAROSE TSGAGB The 2016/1/SM-4 sample was found to contain no Narcotic drug.

Code [blank sample] TWTWPH TWYAAL U90SWA UFVIOP UQMBX2 GREEN POWDER SAMPLE ANALYZED DOESN'T CONTAIN CONTROLLED SUBSTANCES UYPU5U 225 milligrams of a green powder was examined and no evidence was found for the presence of substances controlled under the provisions of the Misuse of Drugs Act 1971 (as amended) or common cutting agents and adulterants. VFD46A the SM-4 contains no drug target VKNECE VNZ61V THE SAMPLE IS A MIXED OF SUCROSA VQT273 sugars VXFBR6 VXXXL4 the green powder doesn't contain drugs controlled by law. VYZC85 there is no drug in this sample WDNNGN after chemical analysis was performed the sample was not found to contain controlled drugs. it was found to contain Caffeine.

WDQWLH No controlled substances found X2JISE X456G5 X70OZ9 XFVW1V We found in this Sample Sugar XNQ60K XQJTD9 XRKU5U Y38I3T La mestra M4, dio positivo (+) para hojas de coca en polvo YAH8BE blank YAIIVO No controlled substances found in 1 unit tested of 1 unit received. YEKYTF YXZMMX No controlled drug was detected. YY5Y1A Any controlled substance was detected. YY7MQP YYZUYY No illegal substances were identified Z5LF55 the sample doesn't contain controlled substances. Z887DL The test sample 2016/1/SM-4 do not found to contain the substances listed in the ICE menu of 2016/1. ZF1EFF Presence of substances from the ICE menu was not detected in the sample. Blank test sample is plant powder. ZFFEHN ZH0THY ZOIJZ3

Code [blank sample] ZRG6U6 A representative sample of the powder was analysed for the presence of a range of commonly encountered controlled drugs; none were detected. ZSX0SS One glass bottle containing 0.22 grammes of a powder which did not contain any substances controlled under the Dangerous Drugs Ordinance (CAP. 134). ZXIIII Inositol and sucrose

Identification methods for Test Sample 4

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

Summary for test sample 4 The response summary of all 183 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: 183

Blank 174

False positives for Test Sample 4

Code Name Technique 3J3OPJ Cannabinol 150/200 ENI7TJ Cocaine 180/190 EYAZVH W-18 N/A O28H4R Cannabinol, Cannabidiol 180 QWO4OF Lysergide 140 SEF3EE Heroin 150/180 TBKOVZ MDMA, Heroin, BZP, Norbuprenorphin171 TEZEE4 ∆-9-THC, Cannabinol 171/180 PPPKPP Synthetic cannabinoid 150/180

Frequency of use of screening and identification techniques:

Response Summary Participants: 18 3

Section 140 141 142 150 160 161161 170171 171180 180190 190200 200211 211220 230230 231231 210 Screening 66 73 60 22 0 1 4 61 17 2 0 1 0 0 11 36.3% 40.1% 33.0% 12.1% 0.0% 0.5% 2.2% 33.5% 9.3% 1.1% 0.0% 0.5% 0.0% 0.0% 6.0% Identification 14 6 4 36 8 15 29 165 72 4 3 0 5 1 12 7.7% 3.3% 2.2% 19.8% 4.4% 8.2% 15.9% 90.7% 39.6% 2.2% 1.6% 0.0% 2.7% 0.5% 6.6% # labs using 71 75 61 45 8 15 30 165 79 6 3 1 5 1 21 this 39.0% 41.2% 33.5% 24.7% 4.4% 8.2% 16.5% 90.7% 43.4% 3.3% 1.6% 0.5% 2.7% 0.5% 11.5% technique 93

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

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