(ICE) Summary Report

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INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary Report

SEIZED MATERIALS 2016/2 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Table of contents Introduction Page 3 Comments from the International Panel of Forensic Experts Page 3 NPS reported by ICE participants Page 5 Codes and Abbreviations Page 7 Sample 1 Analysis Page 8 Identified substances Page 8 Statement of findings Page 13 Identification methods Page 22 Summary Page 27 Z-Scores Page 28 Sample 2 Analysis Page 32 Identified substances Page 32 Statement of findings Page 36 Identification methods Page 45 Summary Page 50 Z-Scores Page 51 Sample 3 Analysis Page 54 Identified substances Page 54 Statement of findings Page 59 Identification methods Page 68 Summary Page 73 Z-Scores Page 74 Sample 4 Analysis Page 77 Identified substances Page 77 Statement of findings Page 82 Identification methods Page 91 Summary Page 96 Z-Scores Page 97 Test Samples Information Samples Comments on samples Sample 1 SM-1 was prepared from a seizure containing 77.0 % (w/w) Cocaine base. The test sample also contained benzoylecgonine with methylecgonine and cinnamoyl cocaine isomers as minor components.

Sample 2 SM-2 was prepared from a seizure containing 14.5 % (w/w) JWH-073. The test sample also contained lactose.

Sample 3 SM-3 contained 11.4% % (w/w) Ketamine base. The test sample also contained lactose.

Sample 4 SM-4 was prepared from a seizure containing 28.4 % (w/w) Heroin base. The test sample also contained lactose, acetylcodeine, 6-monoacetylmorphine with morphine, noscapine and papaverine as minor components

Samples Substances Concentrations Comments on substances Sample 1 Cocaine 77.0 % Sample 2 JWH-073 14.5 % Lactose - % Quantification not required Sample 3 Ketamine 11.4 % Lactose - % Quantification not required Sample 4 Heroin 28.4 % Lactose - % Quantification not required Morphine minor component - % Quantification not required

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. The ICE programme is a UNODC mandated activity and is implemented through regular budget funds and through the UNODC Global Scientific and Forensic Programme – Support Project (GLOU54), which operationalizes the forensic aspects of the UNODC Thematic Programme on Research, Trend Analysis and Forensics"

Comments from the International Panel of Forensic Experts

Participation of Laboratories

In the 2016/2 round of the ICE programme, results were submitted within both the Seized Materials (SM) and Biological Specimens (BS) test groups by 225 laboratories in 73 countries. Within the SM test group, there were 181 participating laboratories from 67 countries and within the BS test group, results were submitted by 89 laboratories from 44 countries.

Qualitative Analysis

The analytical technique most commonly used for screening of test samples in the SM test group was the marquis reagent (41% of participants), while GC-MS (93% of participants) was the most commonly used technique for identification/confirmation of the components in the test samples followed by FTIR (44% 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 2016/2 round of ICE.

SM-1 SM-2 SM-3 SM-4 Test sample (Cocaine) (JWH-073) (Ketamine) (Heroin)

Correct identification by 100% 90% 99% 99% participants Number of false positives 0 3 2 1 Number of false negatives 0 11 1 1 Number of Analyses not performed 0 8 0 0

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 eight analyses not performed, however 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, 125 (69%) for SM-1, 40 (22%) for SM-2, 94 (43%) for SM-3 and 122 (67%) for SM-4 continues to be encouraging, particularly the high percentage of participants who quantified the cocaine and heroin in SM-1 and SM-4 respectively. It is also encouraging that 129 (71%) of participants in the SM test group performed quantitation and of these, 120 (93%) quantified more than one substance and 40 (31%) quantified all four test samples. It is understood that quantitative analysis of controlled substances is often governed by local legislation and the requirements of prosecution. With regard to the analytical techniques used by participants performing quantitation, 59% used GC-FID, 26% used mass spectrometry and 25% used HPLC. z-scores obtained by participants in quantification are shown in table 2 below.

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

Test sample z-score SM-1 SM-2 SM-3 SM-4 (Cocaine) (JWH-073) (Ketamine) (Heroin) |z| < 2, satisfactory 84% 85% 87% 85% 2 ≤ |z| ≤ 3, questionable 7% 10% 4% 6% |z| > 3, unsatisfactory 9% 5% 9% 9%

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 2016/1 round of ICE, 17 laboratories obtained questionable z-scores with 2 ≤ |z| < 3. Twelve of these laboratories participated and performed quantification in the 2016/2 round with all laboratories improving their performance and obtaining acceptable z-scores with |z| < 2 for at least one substance. Three of these laboratories also obtained unsatisfactory z-scores and none of these laboratories obtained questionable z- scores in 2016/2.

22 laboratories obtained unsatisfactory z-scores in ICE 2016/1 with |z| ≥ 3. Of these laboratories, 17 participated in ICE 2016/2 and performed quantification, with 16 (94%) improving their performance in at least one substance. Ten (59%) of these laboratories also obtained an unsatisfactory z-score in the 2016/2 round and 4 (24%) obtained questionable z-scores.

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.

4 New Psychoactive Substances (NPS) reported by laboratories participating in the 2016/2 round of the ICE programme During the 2016/2 round of ICE, participating laboratories provided information on NPS that had been identified in their laboratories. In total there were 225 reports of 135 substances. The most commonly reported substances were equally from the groups of synthetic cathinones (32%) and synthetic cannabinoids (32%) as shown in figure 1.

Synthetic cannabinoids 2% 2% 1% 7% 4% Synthetic cathinones 32% Others

Phenethylamines

Ketamine and phencyclidine type substances 20% Tryptamines

Aminoindanes 32% Piperazines

Figure 1. NPS reported by ICE laboratories during the 2016/2 round of ICE

In terms of the mode of action of the NPS reported by ICE participants, the predominant substances reported were stimulants (42%), while 31% were synthetic cannabinoid receptor agonists (SCRA’s) and 9% were synthetic opioids (which included seven fentanyl derivatives) as shown in figure 2.

4% 6% 7%

42% Stimulants

9% SCRA's Opioids Hallucinogens Dissociatives Sedatives/Hypnotics

32%

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

NPS most commonly reported by laboratories participating in ICE 2016/2

The substances most often reported by ICE participants were the synthetic cannabinoid receptor agonists 5F-MDMB-PINACA (methyl 2-(1-(5-fluoropentyl)-1H-indazole-3-carboxamido)-3,3-dimethylbutanoate, AB- CHMINACA (N-(1-amino-3-methyl-1-oxobutan-2-yl)-1-(cyclohexylmethyl)-1H-indazole-3-carboxamide and the synthetic opioid furanylfentanyl (N-(1-phenethylpiperidin-4-yl)-N-phenylfuran-2-carboxamide. 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 0D11QZ cocaine 0HSVIE Cocaine 0LAKP0 Cocaine 0P0W03 COCAINE 10B0XJ Cocaine 1JJBJS cocaine 1YQDGQ cocain HCL 1ZKJHF Cocaine 211119 Cocaine 2PUPPP Cocaine 2QC44H Cocaine 2R20JW cocaine 33DUO3 cocaine 3PV3WL Cocaine 40HFEP Cocaine 4J4H44 Cocaine hydrochloride 55BR5Z cocaine 5MLCMA Cocaine 5ZDDX6 cocaine 7666AG cocaine 7IUIII cocaine 7JUSKK cocaine 7T7YHK Cocaine 8AHAJA cocain 8D1PTX COCAINE 8II46Y Cocaine 8J4DWT cocaine 8MV6V6 Cocaine 8Q8VEF Cocaine 8WEYGQ Cocaine 8Z8ZZZ cocaine 9994MR cocaine 9Q999K cocaine A33Q33 Cocaine A5GR55 Cocaine A7LUO7 COCAINE A8YSK1 cocaine AEDDRS cocaine APX4KD Cocaine ARZMMQ Cocaine HCl

Code Identified Substances ASLAA5 Cocaine AYNT4F Cocaina B3SNNC cocaine BARYZ2 cocaine BFIU0G cocaine BRVRR4 Cocaine hydrochloride C9CDOR cocaine CANEE8 cocaine CCIVVK cocaine CJWZIJ Cocaine CRSEZI cocaine CU6JGV COCAINE CWEOYI cocaine CZGHZZ cocaïne DMM5Z5 cocaine DNNSKS Cocaine DWRNDI cocaine E2OA5N cocaine E3MIHV cocaïne E5LDLX cocaine E66LY6 cocaine EHJ60F COCAINE 76.3 % EMJ8VM cocaine EXZYYP Cocaine HCl FK5BHB Cocaine FMFLFF cocaine G0B9NL COCAINE HYDROCHLORIDE G2GBDV cocaine GGA8CG Cocaine Hydrochloride GJIRPN Cocaine GKHDEM cocaine GNUILW cocaine GUDEBT COCAINE GV2PGK cocaine hydrochloride H13HRX COCAINE CHLORIDE HEHCMO Cocaine HF3FYI cocaine HJLSL6 Cocaine HRYNGY COCAINE IMVADS Cocaine IQYQE4 Cocaine IRWMIX Cocaine IWA0AA Cocaine IXUAHB Cocaine Hydrochloride

Code Identified Substances IZLLW0 cocaine JCUITV cocaine JEVX45 cocaine JKG5E5 cocaine JM2GKM cocaína JSZ6XW Cocaine K3S33Y Cocaine KBUURH cocaine hydrochloride KKKWIC cocaine KSQKKK cocaine L4444V COCAINE-HCl LDDCDD Cocaine LL8LML Cocaine LLL1RB Cocaine hydrochloride LNUUEI cocaine LQ8989 cocaine hydrochloride LVVWC7 cocaine M1XUWT Cocaine M72KOQ Cocaine MCCCCC Cocaine MDDETU Cocaine MDQMM4 Cocaine MMMMT5 Cocaine MOFYQQ cocaïne MOKSHS cocaine MWXNUW Cocaine MZMHCW Cocain N8BTCF Cocaine NWJDJI Cocaine NZOTC6 Cocaine O4KFNX cocaine O888ML Cocaine ODOOO2 cocaine hydrochloride OJFEOO cocaine OK66R6 cocaine OO9QOO Cocaine OQ4QQQ cocain ,benzoylecgonine OS838A cocaine OTSOQ9 cocaína P0FZ8V cocaine PHWNRB Cocaine PPLICW Cocaine PQQKLQ COCAINE QQQQJW cocaine

Code Identified Substances R7BBLB Cocaine RI3K33 cocaine HCl RJINCE Cocaine RJNRSN Cocaine RU8UQS cocaine RVP7VW cocaine SIFXH3 Cocaine SMYNNU Cocaine SUUW3G Cocaine SVGG03 Benzoylecognine, cocaine & ecognine methyl ester T2DI1R Cocaine T4VMD2 Cocaine TI22ZK Cocaine TQFFPF Cocaine TQMVZE Cocaine TRVLKK Cocaine TSSRQR Cocaine TSW3IE COCAINE TZOONA COCAINE hcl UFK6EF cocaine HCl UG88A8 COCAINE UJWYPY cocaine UMXXSY Cocaine UUUOU9 cocaine UWBOLU cocaine UXVVAC COCAINE UYFCCR COCAINE UYJBJJ Cocaine V011CO Cocaine VBEY7Y Cocaine VFC8CC cocaine VIFKAW cocaine VPHJRP COCAINE VVIRG4 Cocaine VVN4CQ cocain W0HPES &2&$ø1( WGZNNM Cocaine WMTTV7 Cocaine WQOZYA cocaine X0X444 cocaine XEE66N cocaine XNNNU1 Cocaíne (Hydrochloride) XXFX8D Cocaine YGQE84 Cocaine, Ecgonine methyl ester and Cinnamoylcocaine

Code Identified Substances YLHIIH COCAINE YQYLYY cocaine Z2BIDB cocaine Z8T8N1 cocaine ZCCQMZ Cocaine ZQHUPQ Cocaine hydrochloride ZWL0DM Cocaine ZXGCGG Cocaine

Statement of findings for Test Sample 1

Code Cocaine 0D11QZ + cocaine base 49% 0HSVIE +

0LAKP0 + The sample contains cocaine (73.9%) 0P0W03 + A color test (SCOTT-Cobalt thiocyanate TEST) with positive reaction to Cocaine, to the TLC was used as a solvent for the preparation of the samples the Dichloromethane and as eluent methanol, used an aluminum plate 20 × 20 cm. Confirmation of results were made on the equipment of THERMO SCIENTIFIC NICOLET Is 10 and NICOLET Is 50 FT-IR.In relation to 2016/2 sample/SM- 1, all tests are in compliance and the identified substance is cocaine. 10B0XJ + Confirmatory test (GCMS) shows test sample contains cocaine 1JJBJS +

1YQDGQ + impurites of cocain ( benzoylecgonin, cinnamoylcocain cis, trans, cocaethylen, ecgonine methyl ester, benzoic acid) 1ZKJHF + Examination revealed the presence of Cocaine 211119 + Results of screening test were positive for cocaine. Relation time and fragmentation pattern obtained with sample are equivalent to those obtained with cocaine. Cocaine was detected at 75.41 % by weight. 2PUPPP + Sample contains 78.7 ± 3.0 % (w/w) Cocaine base. 2QC44H + The sample obtains with positive result with Cobalt thiocyanate reagent. TLC : The Rf sample obtain with the same Rf Cocaine Standard. GC : The Rt sample obtain with the same Rt Cocaine Standard. 2R20JW + cocaine chloridrate 73.97% as base 33DUO3 + cocaine was as hydrochloride form. 3PV3WL + The sample SM1 contained 80,1 % of cocaine. Esthers of cocaine was in the sample SM1 identefied. 40HFEP + Mass spectrometry profile correlation between sample and reference material certified 4J4H44 + Cocaine hydrochloride confirmed in 1 unit tested of 1 unit received. 55BR5Z + ./. 5MLCMA + Sample 2016/2/SM-1 found to contain Cocaine 5ZDDX6 + the sample contain cis and trans cinnamoylcocaine, pseudoecgonine 7666AG +

Code Cocaine 7IUIII + The result of the sm 1 (123)tests received has confirmed that the mentioned simple contains cocaine with 70.95 percentage by weight 7JUSKK +

7T7YHK + On analysis, I found sample SM-1 to contain Cocaine. 8AHAJA +

8D1PTX +

8II46Y + Cocaine was identified by GC-MS. 8J4DWT + 82% +/-6 8MV6V6 + In the test sample 2016/2/SM-1 was detected cocaine 8Q8VEF +

8WEYGQ + White powder containing cocaine. 8Z8ZZZ +

9994MR + White powder, usual smell, totally soluble in water, precence of chloride ions 9Q999K + Sampel SM_1 was found to contain cocaine. A33Q33 + Cocaine confirmed A5GR55 + ecgonidine, methyl ester cinnamoylcocaine A7LUO7 + BY GC-MS AND FTIR A8YSK1 + Cocaine 80.1% AEDDRS + found cocaine with 77.7%ww APX4KD + The white powder was analysed and found to contain cocaine hydrochloride. ARZMMQ +

ASLAA5 + THE SAMPLE WAS FOUND TO CONTAIN COCAINE AYNT4F + De análisis realizados se concluye que la sustancia se trata de cocaina B3SNNC + The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule I 2. (2) Cocaine (benzoylmethylecgonine)

Code Cocaine BARYZ2 +

BFIU0G + The test sample number SM-1 containing a psycho narcotic drug cocaine. BRVRR4 + Examination and analyses performed on the white solid in SM1 showed it to contain cocaine hydrochloride (a central stimulant). Cocaine hydrochloride is a salt of cocaine. Assay SM1 = 82.6% cocaine hydrochloride C9CDOR +

CANEE8 +

CCIVVK + The sample contain cocaine. CJWZIJ + The sample contained 83.0% of cocaine. CRSEZI + ecgonine methyl ester cinnamoyl cocaine nor-cocaine CU6JGV +

CWEOYI + after chemical analysis was performed the sample was contain 93.8% cocaine CZGHZZ +

DMM5Z5 + Screeninhg test with cobaltthiocyanate test positive and confirmation with GCMS. DNNSKS + Ecgonine methyl ester, Ecgonine benzoylester, Cinnamoylcocaine DWRNDI + cocaine, benzoylecgonine E2OA5N +

E3MIHV + 142: apparition d'une coloration bleue (Réactif 1); Décoloration en Rose (réactif 2), apparition d'une coloration bleue foncés de la couche inférieure. 150: le rf du spot présent dans l'échantillon est non différentiable de celui du spot donné par le standard de cocaïne E5LDLX + cocaine: 75.1%ww E66LY6 +

EHJ60F +

EMJ8VM + Sample 2016/2/SM-1 contains cocaine, a dangerous drug. It also contains cinnamoylcocaine isomers, benzoyl ecgonine and methyl ecgonine.

Code Cocaine EXZYYP + The sample was performed by cobalt thioyanate test,then confirmed by TLC and GC/MS. Guantified by GCFID, the sample contained cocaine 78.1% as base.

FK5BHB + After analycing the simple with colorimetric tests, GC/MS confirmation and subsequent quantification by GC-FID we can say that this simple contains 82.38% in cocaine base FMFLFF + cocaine G0B9NL + Off-white powder 229 milligrams 1 package COCAINE HYDROCHLORIDE (88%) Class A [Note to UNODC we report salt form purities where salt form has been identified analytically] G2GBDV + cocaine is controlled by K.B. of 31/12/1930, changed by K.B. of 8/10/1963 GGA8CG + A sealed glass vial containing a white powder. This powder contained an average of 88% Cocaine Hydrochloride. GJIRPN + Cocaine is a Class A controlled drug subject to the provisions of the Misuse of Drugs Act 1971. GKHDEM + cocaine was detected by gc-ms screening and it was quantified by gc-fid using calibration curve GNUILW + List I of Single Convention on Narcotics drugs,1961. GUDEBT + Sample 2016/2/SM-1 a white powder gave a positive result for cocaine a controlled substance under national legislation on drugs. GV2PGK + Cocaine hydrochloride is present (75% w/w as base) with benzoylecgonine and cis-trans cinnamoylcocaine. H13HRX + ECGONIDINE METHYL ESTHER, ECGONINE METHYL ESTHER, CINNAMOYL COCAINE HEHCMO + A.p. of trans-cinnamoylcocaine and cis-cinnamoylcocaine HF3FYI + cocaine, concentration approx 80 % as free base HJLSL6 + Sample contained cocaine as hydrochloride, and small amounts of cis and trans cinnamoylcocaine. Identification of cocaine by FTIR and MS spectrum, quantification by GC/FID HRYNGY + POWDER IMVADS + SM-1 contains a drug: cocaine, 79,8% IQYQE4 +

IRWMIX + Sample 2016/2/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. IWA0AA + The sample contains cocaine which is listed as a controlled drug according to french order, appendix I of February 22nd 1990.

Code Cocaine IXUAHB + 229 milligrams - Cocaine Hydrochloride (91%) - Class A IZLLW0 + The sample contains a controlled substance as cocaine JCUITV +

JEVX45 + White powder containing 72.2%ww in cocaine JKG5E5 + cocaine hydrochloride JM2GKM + Pruebas colorimétricas con Marquis, Scott Prueba de Microcristales GC-MS y FT-IR JSZ6XW + The above article was examined and found to consist of a brown glass vial containing a quantity of white powder. The powder, which weighed 0.22 grams, was analysed and found to contain Cocaine. A sample of the powder was further analysed and found to contain 78% (weight for weight) Cocaine. Cocaine is a class A controlled drug within the provisions of the Misuse of Drugs Act 1971.

K3S33Y + The sample contains cocainehydrochloride. The content of cocainehydrochloride is determined to 95 %. Cocaine is a controlled substance in X. KBUURH + cocaine base 78,26 % KK6WBZ +

KKKWIC + 2016/2/SM-1 = Cocaine The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule I 2. (2) Cocaine (benzoylmethylecgonine) KSQKKK + In the sample was found cocaine L4444V + The sample fas found to contain COCAINE and : anhydrecgonine methyl ester - Methyl ecgonine - cinnamoylcocaine, as minor components LDDCDD + Blue colour by Cobalt Thiocyanate test indicates the possible presence of cocaine in sample 1.Then TLC result and GCMS result confirmed that the presence of cocaine in SM 1. LL8LML + Cocaine was detected with a purity of approximately 82% (as base) LLL1RB + One glass bottle containing 0.23 grammes of a powder containing 0.18 grammes of cocaine. LNUUEI + the powder is cocaine hydrochloride. The concentration of cocaine, as base, is 80.1% by weight LQ8989 + the item is powder containing cocaine hydrochloride 74.3% purity LVVWC7 +

Code Cocaine M1XUWT + Powder (sample) contains Cocaine M72KOQ + Traces of Cinnamoylcocaine. MCCCCC + From screening test using (CI) and ion scan and from confirmatory test using (GC-MS) the sample was found to contain the controlled drug cocaine. MDDETU + Sample contains 76,6 % of cocaine MDQMM4 + Methylecgonine cinnamoilcocaine MMMMT5 + The mixture contains cocaine and some form of sugar MOFYQQ + positive MOKSHS +

MWXNUW + The Test sample 2016/2/SM-1 was analyzed by Colour test and Thin Layer Chromatography technique and found to contain Cocaine. MZMHCW + It contains cocain in a purity of 75.1%. It also contains lactose N8BTCF + This sample contains cocaine and has no diluent. NWJDJI + Based on the above analysis, the sample was found to contain cocaine. NZOTC6 + - O4KFNX + White powder containing 81.0%ww cocaine O888ML + The test sample 2016/2/SM-1 was found to contain 70.5% controlled drug cocaine. ODOOO2 + The presence of drug was not as always confirmed by FTIR spectroscopy analysis because of equipment failure. OJFEOO + Cocaina is included in Table II Schedule I drugs (narcotics use by medicine) approved by Government Decision of Republic of Moldova no. 1088 of 05.10.2004 (Last Updated 5/13/2016) (Tables and lists of narcotic drugs,psychotropic substances and their precursors under control) OK66R6 + Only the cocaine can be identified. OO9QOO +

OQ4QQQ +

OS838A + The sample contains cocaine which is scheduled as illicit drug in France.

Code Cocaine OTSOQ9 + cocaína clorhidrato , polvo fino blanco. 83.31% P0FZ8V +

PHWNRB + The sample was found to contain 78.5% of cocaine (as base). PPLICW + The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule I 2. (2) Cocaine (benzoylmethylecgonine) PQQKLQ + THE SAMPLE 2016/2/SM-1 WAS FOUND TO CONTAIN COCAINE. QQQQJW +

R7BBLB + Cocaine (80 % w/w) in mixture with non-specified saccharides RI3K33 + Cocaine was identified in SM1. In addition Ecgonidine methyl ester, cis- and trans- cinnamoylcocaine and p-fluorococaine were identified. Analysis revealed that percentage of cocaine is 51.80%. RJINCE + Ergonidine,Cinnamoylcocaine RJNRSN + Cocaine detected in sample 2016/2/SM-1. Quantitative analysis not performed. RU8UQS + we have found results from swg-drug library, which the last version it, and we have studied for quantitative analysies with GC-FID. RVP7VW +

SIFXH3 + Sample 2016/2/SM-1 contains Cocaine. SMYNNU + The sample consist controlled drugs - Cocaine SUUW3G + ɫontained cocaine, cinnamoilcocaine, cis-cinnamoilcocaine and trace of methylecgonidine , methylecgonine SVGG03 + The sample cnotains 78.28 % cocaine & also it contains benzoylecgonine & ecognine methyl ester . T2DI1R + The chemical test and the coincidence in the retention time and mass fragmentogram with the reference material in the same conditions that the analyzed sample, indicate the cocaine presence. T4VMD2 + based on GC/MS analysis, cocaine had been identified TI22ZK + x grams of powder containing 75% cocaine. Class A TQFFPF + Analyses performed on Item # 1 revealed presence of Cocaine. TQMVZE + In the sample 1 we have faund cocaine. Cocaine is on the list of the drug in Montenegro.

Code Cocaine TRVLKK + SM1 contains Cocaine; Sample also contains benzoylecgonine, methylesterecgonine, cis/trans- cinnamoylcocaine and norcocaine as minor components TSSRQR +

TSW3IE + ANALYZED WHITE POWDER CONTAINS COCAINE TZOONA + COCAINE, ANHIDROMETHYLECGONINE, NORCOCAINE, CIS & TRANS CINNAMOILCOCAINE. BESE COCAINE 75,8 +/-2,7 UFK6EF + The sample contains cocaine. Cocaine is sheduled as illicit drug. UG88A8 + WHITE CRYSTALINE MATERIAL THAT CONTAINS DRUG COCAINE. UJWYPY +

UMXXSY + Cocaine, Ecgoninemethylester, Ecgonidine methylester, Cis-cinnamozlcocaine, Trans- cinnamozlcocaine, Norcocaine- GCMS - Compare massspectra with library retention time of reference sample and FTIR-Cocaine - compare with IR spectrum library UUUOU9 +

UWBOLU + the white powder contains cocaine (77.0%ww) wich is controlled by national law UXVVAC + Presence of cocaine hydrochloride was detected in the sample. The sample also contained multitude of trace level alkaloid impurities:(cis/trans)cinnamoylcocaine, benzoylecgonine, methylecgonine, norcocaine. UYFCCR + IN SAMPLE 2016/2/SM-1 COCAINE WAS FOUND. UYJBJJ + This sample is cocaine. V011CO + The high quality of measurement results (99%) proves the presence of cocaine in the sample. VBEY7Y + It is usually detected in our laboratory. High purity, characteristic of important seizures. VFC8CC +

VIFKAW + the sample contains cocaine. VPHJRP + The sample containing 74.5% cocaine base :also contain Benzoylecgonine VVIRG4 + Samples with high concentrations of Cocaine equivalent to the samples seized in Viet Nam VVN4CQ + cocain-HCL W0HPES + &2&$ø1(+&O

Code Cocaine WGZNNM +

WMTTV7 + The sample contains cocaine. WQOZYA + cinnamoylcocaine X0X444 + white powder containing cocaine and ecgonidine methylester, ecgonine methylester as cocaine impurities XEE66N + the sample is containing cocaine and percentage of pure cocaine in it is 77.9% XNNNU1 + Powder containing Cocaine Hydrochloride 64,7% Legal status: Illegal - Portuguese Drug law 15/93 XXFX8D + The sample found to contain Cocaine YGQE84 + Cobalt Thiocyanate (CT) positive. GC/MS Retention time and mass charge (m/z) similar characteristics with the substances used as standard or pattern YLHIIH + BENZOILECGONINE AND ECGONINE METYL ESTER YQYLYY + Presence of cocaine, 66.80% concentration, with traces of cinnamoylcocaine and benzoylecgonine Z2BIDB + On analysis, I found that the substances contain 77.9% w/w of cocaine. Z8T8N1 +

ZCCQMZ + Cocaine HCl ZQHUPQ + It has been detected the presence of cocaine hydrochloride in the sample ZWL0DM + not ZXGCGG + The identification was realized with prelimimary color test with cobalt thiocyanate and silver nitrate, the confirmative assay with FT-IR and CG-MS and the quantitative analysis was carried by GC-FID.

Identification methods for Test Sample 1

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

Analytical Technique Codes Code 140 141 142 150 160 161 170 171 172 180 190 200 211 220 230 231 210 0D11QZ SI I 0HSVIE SI 0LAKP0 S S S I I 0P0W03 S S I I 10B0XJ SI SI I SI Fast blue B salt 1JJBJS SI 1YQDGQ SI 1ZKJHF SI 211119 S S I 2PUPPP S I SI SI 2QC44H S S S I 2R20JW S S S I 33DUO3 SI I 3PV3WL SI I 40HFEP I I 4J4H44 I SI I 55BR5Z I SI SI 5MLCMA S I 5ZDDX6 S SI I I I I 7666AG I SI 7IUIII S S S I I 7JUSKK S S SI S fast blue B 7T7YHK S I I 8AHAJA S I I 8D1PTX SI SI I 8II46Y S S S I I 8J4DWT S I 8MV6V6 I 8Q8VEF I S 8WEYGQ S I SI 8Z8ZZZ S S I I 9994MR I SI 9Q999K S I A33Q33 S S SI I

Code 140 141 142 150 160 161 170 171 172 180 190 200 211 220 230 231 210 A5GR55 SI I A7LUO7 S S I I A8YSK1 S I AEDDRS SI APX4KD S I I ARZMMQ I SI ASLAA5 S S I I AYNT4F S S I I S Macroscopic B3SNNC SI I BARYZ2 SI I BFIU0G S S I I BRVRR4 S S S SI I I C9CDOR S I CANEE8 SI CCIVVK S SI I SI CJWZIJ SI I I UPLC-PDA CRSEZI I I SI I CU6JGV SI S SI I CWEOYI I S I CZGHZZ SI I DMM5Z5 S I I DNNSKS S I I I DWRNDI I SI I E2OA5N SI SI SI I E3MIHV S S S I E5LDLX I SI E66LY6 S S S I I S ac. nitrico EHJ60F S S S SI I SI EMJ8VM S S S I I I Duquenois-Levine Test EXZYYP S S S I I SI FK5BHB S S I I Duquenois FMFLFF SI I G0B9NL S S S I I I G2GBDV I S GGA8CG S S I I S Basic Cobalt thiocynanate (for ketamine) GJIRPN S S I GKHDEM SI GNUILW I SI GUDEBT S S I I

Code 140 141 142 150 160 161 170 171 172 180 190 200 211 220 230 231 210 GV2PGK I I H13HRX SI SI S SI I I S Benedict HEHCMO S S S SI I HF3FYI SI I HJLSL6 I I SI HRYNGY SI IMVADS S S S I I S IQYQE4 I I IRWMIX S S I I IWA0AA I I IXUAHB S S S I I IZLLW0 S I S S I JCUITV S S SI JEVX45 I I SI JKG5E5 SI S I SI JM2GKM S S S I I I JSZ6XW S I K3S33Y I I KBUURH SI I I KK6WBZ I SI KKKWIC SI I KSQKKK S S I I I L4444V S SI I LDDCDD S S SI I LL8LML S S I I LLL1RB S S I SI I I Raman Spectroscopy LNUUEI I I SI I LQ8989 I LVVWC7 S I SI I M1XUWT I M72KOQ I SI MCCCCC S S I MDDETU SI MDQMM4 I SI MMMMT5 S I I S MOFYQQ S I I S Drug Testing Kits MOKSHS I SI MWXNU S S SI S Fast Blue B Salt Test W MZMHCW S I

Code 140 141 142 150 160 161 170 171 172 180 190 200 211 220 230 231 210 N8BTCF I S I I NWJDJI S I I NZOTC6 SI O4KFNX I I SI O888ML S S S SI I ODOOO2 S I I I OJFEOO S S S I I I OK66R6 S I SI I OO9QOO SI SI OQ4QQQ S S I SI OS838A S S I OTSOQ9 S I I S P0FZ8V SI PHWNRB SI PPLICW SI I PQQKLQ S I SI QQQQJW I R7BBLB I SI I I S Raman RI3K33 S S I I I S Fast Blue B salt test RJINCE S S I I RJNRSN S SI I RU8UQS S S I SI RVP7VW SI SI SI I SIFXH3 S S S I I SMYNNU I SI I SUUW3G SI SVGG03 SI I T2DI1R S S I T4VMD2 S I TI22ZK S S I TQFFPF S S I I TQMVZE S S I I I TRVLKK I S TSSRQR SI I TSW3IE S S I I TZOONA S S S I I I I XRD UFK6EF I SI I UG88A8 SI S SI SI S Simon UJWYPY S SI SI I

Code 140 141 142 150 160 161 170 171 172 180 190 200 211 220 230 231 210 UMXXSY S S SI I UUUOU9 SI SI SI I UWBOLU I SI UXVVAC S I I I I UYFCCR I SI UYJBJJ S I I V011CO S S I I VBEY7Y SI S S I I I VFC8CC SI VIFKAW SI I VPHJRP S I I I I HPLC/RID VVIRG4 S I I I LC-MS-TOF VVN4CQ I SI SI W0HPES I SI I WGZNNM I SI WMTTV7 SI SI WQOZYA SI I X0X444 SI I XEE66N SI S S SI I XNNNU1 S S I XXFX8D S S I S Janovsky YGQE84 S S S I I YLHIIH I SI YQYLYY I Z2BIDB S S S I I I Raman Spectrometer Z8T8N1 SI I ZCCQMZ I SI I ZQHUPQ I S I ZWL0DM SI I ZXGCGG S S S I I

RESPONSE SUMMARY FOR TEST SAMPLE 1

Participants: 181

The response summary of all 181 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:

Substance Name Number of laboratories correctly identifying: Cocaine 181

False positives for Test Sample-1:

Round Code: Substance reported: Tech Code: 0

False negatives for Test Sample-1 (techniques(s) used for ANP):

Round Code: Substance Name: Tech Code: 0

Frequency of use of screening, identification and quantification techniques:

Response Summary Participants 181 Technique 140 141 142 150 160 161 170 171 172 180 190 200 210 211 220 230 231 Screening (No.) 54 75 62 19 0 3 0 4 0 72 19 1 13 0 1 2 0 (%) 29.8 41.4 34.3 10.5 0.0 1.7 0.0 2.2 0.0 39.8 10.5 0.6 7.2 0.0 0.6 1.1 0.0 Identification (No.) 13 6 5 34 5 12 1 35 1 168 79 4 8 3 0 7 4 (%) 7.2 3.3 2.8 18.8 2.8 6.6 0.6 19.3 0.6 92.8 43.6 2.2 4.4 1.7 0.0 3.9 2.2 Quantification (No.) 0 0 0 0 8 24 0 76 0 30 0 0 1 3 0 1 0 (%) 0.0 0.0 0.0 0.0 6.2 18.6 0.0 58.9 0.0 23.3 0.0 0.0 0.8 2.3 0.0 0.8 0.0

Round: 2016/2 Robust average = 77.3 % Substance: SM‐1; Cocaine UNODC value = 77.0 % 4.0 3.8 3.7 3.4

3.0 2.9 2.7 2.6 2.4 2.2

2.0 1.8 1.6 1.5 1.5 1.4 1.3 1.2 1.1 1.1 1.0 0.9

1.0 0.9 0.9 0.8 0.8 0.7 0.7 0.7 0.7 0.7 0.6 0.6 0.6 0.5 0.5 0.5 0.5 0.5 0.5 0.4 0.4 0.4 0.4 0.4 0.4 0.4 0.3 0.3 0.3 0.3 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.2 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.0 0.0 4.9 0.0 6.5 5.9 5.3 4.5 4.0 3.5 0.0 ‐ ‐ ‐ ‐ ‐ ‐ 0.1 0.1 0.1 0.1 0.1 13.3 ‐ ‐ ‐ ‐ ‐ ‐ 0.2 ‐ 0.2 ‐ 0.3 0.3 0.3 ‐ ‐ 0.4 ‐ 0.4 ‐ 0.5 ‐ 0.5 0.5 0.5 ‐ 0.5 0.5 0.5 ‐ ‐ ‐ 0.6 ‐ ‐ ‐ ‐ 0.6 0.7 ‐ 0.7 ‐ 0.7 0.7 ‐ ‐ ‐1.0 0.8 ‐ 0.8 0.8 ‐ 0.8 ‐ ‐ ‐ 0.9 ‐ 0.9 1.0 ‐ ‐ 1.1 ‐ 1.2 1.2 1.2 ‐ ‐ ‐ 1.3 ‐ 1.4 1.5 ‐ ‐ 1.5 1.6 1.6 1.6 ‐ ‐ ‐ ‐ 1.7

‐2.0 ‐ 2.2 ‐ 2.4 ‐ ‐3.0 2.8 ‐ 2.9 ‐

‐4.0 V 6JG 7IUIII UAHB 1JJBJS 8II46Y UYJBJJ TI22ZK CRSEZI HJLSL6 HF3FYI RJINCE JCUITV CJWZIJ LLL1RB RI3K33 8Z8ZZZ GJIRPN EHJ60F T2DI1R E66LY6 JEVX45 10B0XJ Z2BIDB EXZYYP JKG5E5 E5LDLX 4J4H44 IZLLW0 7JUSKK K3S33Y P0FZ8V A8YSK1 0LAKP0 211119 YQYLYY LL8LML UFK6EF X0X444 LNUUEI 55BR5Z IQYQE4 VPHJRP VVIRG4 VBEY7Y R7BBLB 40HFEP BARYZ2 LQ8989 VFC8CC Z8T8N1 JSZ6XW XEE66N TSSRQR IX CZGHZZ CU FK5BHB 8Q8VEF 2PUPPP OS838A KSQKKK 5ZDDX6 CANEE8 BRVRR4 G0B9NL 7666AG VIFKAW 2R20JW A5GR55 0D11QZ SVGG03 AEDDRS CWEOYI O4KFNX NZOTC6 A7LUO7 IMVADS DNNSKS H13HRX 8J4DWT GV2PGK IWA0AA C9CDOR E2OA5N 3PV3WL ZXGCGG UXVVAC HRYNGY 9994MR 33DUO3 KK6WBZ O888ML OTSOQ9 GNUILW LVVWC7 RU8UQS W0HPES GGA8CG 8MV6V6 KBUURH TZOONA G2GBDV ZCCQMZ TQMVZE DWRNDI ZQHUPQ RVP7VW MOKSHS 1YQDGQ XNNNU1 JM2GKM MDDETU UUUOU9 SMYNNU GKHDEM SUUW3G PHWNRB ZWL0DM ODOOO2 WQOZYA HEHCMO UWBOLU OO9QOO ARZMMQ WGZNNM MZMHCW MDQMM4

z‐scores can be interpreted by participants in line with ISO 13528:2005, secion 7.4.2 and ISO/IEC guide43‐1:1997(E) as follows: IzI < 2 = satisfactory 2 ≤ IzI ≤ 3 = questionable IzI > 3 = unsatisfactory According to the recommendations in ISO 13528:2005, an unsatisfactory z‐score is considered to give an action signal and a questionable z‐ score is considered to give a warning signal. A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occured that requires inverstigation.

28 Z‐Score Report per Sample per Substance

Round: 2016/2 Substance: SM‐1; Cocaine

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

0 z-score

-2

-4

-6

-8 HPLC GC‐FID GC‐MS

-10

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

Z-Scores for Test Sample 1 Cocaine Cocaine Deviation Code Concentration Deviation from Code Concentration z-score from robust z-score (mass%) robust average (mass%) average 5ZDDX6 19.6 -57.7 -13.3 ARZMMQ 77.0 -0.3 -0.1 0D11QZ 49.0 -28.3 -6.5 MOKSHS 77.0 -0.3 -0.1 RI3K33 51.8 -25.5 -5.9 T2DI1R 77.0 -0.3 -0.1 ZXGCGG 54.1 -23.2 -5.3 UWBOLU 77.0 -0.3 -0.1 XNNNU1 57.6 -19.7 -4.5 SMYNNU 77.2 -0.1 0.0 4J4H44 60.0 -17.3 -4.0 CRSEZI 77.3 0.0 0.0 7666AG 62.0 -15.3 -3.5 40HFEP 77.4 0.1 0.0 E66LY6 64.7 -12.7 -2.9 8Z8ZZZ 77.5 0.2 0.1 VFC8CC 65.2 -12.1 -2.8 P0FZ8V 77.5 0.2 0.1 YQYLYY 66.8 -10.5 -2.4 LVVWC7 77.6 0.3 0.1 W0HPES 67.6 -9.7 -2.2 AEDDRS 77.7 0.4 0.1 DWRNDI 70.0 -7.3 -1.7 1JJBJS 77.8 0.5 0.1 E2OA5N 70.5 -6.8 -1.6 UFK6EF 77.8 0.5 0.1 O888ML 70.5 -6.8 -1.6 X0X444 77.9 0.6 0.1 KSQKKK 70.5 -6.8 -1.6 XEE66N 77.9 0.6 0.1 IZLLW0 70.7 -6.6 -1.5 Z2BIDB 77.9 0.6 0.1 7IUIII 71.0 -6.3 -1.5 GGA8CG 78.0 0.7 0.2 HRYNGY 71.0 -6.3 -1.4 GNUILW 78.0 0.7 0.2 VVIRG4 71.5 -5.8 -1.3 JSZ6XW 78.0 0.7 0.2 GKHDEM 72.1 -5.2 -1.2 VIFKAW 78.0 0.7 0.2 JEVX45 72.2 -5.1 -1.2 8MV6V6 78.1 0.8 0.2 UXVVAC 72.2 -5.1 -1.2 EXZYYP 78.1 0.8 0.2 DNNSKS 72.5 -4.8 -1.1 HEHCMO 78.2 0.9 0.2 RU8UQS 73.0 -4.3 -1.0 KBUURH 78.3 1.0 0.2 33DUO3 73.2 -4.1 -0.9 SVGG03 78.3 1.0 0.2 JM2GKM 73.5 -3.8 -0.9 ZCCQMZ 78.4 1.1 0.3 BRVRR4 73.8 -3.5 -0.8 PHWNRB 78.5 1.2 0.3 0LAKP0 73.9 -3.4 -0.8 2PUPPP 78.7 1.4 0.3 JKG5E5 73.9 -3.4 -0.8 TSSRQR 78.7 1.4 0.3 2R20JW 74.0 -3.3 -0.8 BARYZ2 78.8 1.5 0.4 8II46Y 74.2 -3.1 -0.7 UYJBJJ 78.8 1.5 0.4 ZQHUPQ 74.2 -3.1 -0.7 G2GBDV 78.9 1.6 0.4 LQ8989 74.3 -3.0 -0.7 G0B9NL 79.0 1.7 0.4 RVP7VW 74.4 -2.9 -0.7 ZWL0DM 79.0 1.7 0.4 VPHJRP 74.5 -2.8 -0.6 55BR5Z 79.1 1.8 0.4 HJLSL6 74.8 -2.5 -0.6 WGZNNM 79.1 1.8 0.4 GV2PGK 75.0 -2.3 -0.5 RJINCE 79.3 2.0 0.5 OS838A 75.0 -2.3 -0.5 IQYQE4 79.3 2.0 0.5 TI22ZK 75.0 -2.3 -0.5 LLL1RB 79.4 2.1 0.5 ODOOO2 75.1 -2.2 -0.5 GJIRPN 79.6 2.3 0.5 E5LDLX 75.1 -2.2 -0.5 R7BBLB 79.6 2.3 0.5 MZMHCW 75.1 -2.2 -0.5 UUUOU9 79.7 2.4 0.5 C9CDOR 75.2 -2.1 -0.5 HF3FYI 79.7 2.4 0.6 211119.0 75.4 -1.9 -0.4 IMVADS 79.8 2.5 0.6 JCUITV 75.6 -1.7 -0.4 CANEE8 80.0 2.7 0.6 SUUW3G 75.8 -1.5 -0.3 3PV3WL 80.1 2.8 0.7 TZOONA 75.8 -1.5 -0.3 A8YSK1 80.1 2.8 0.7 KK6WBZ 76.0 -1.3 -0.3 LNUUEI 80.1 2.8 0.7 EHJ60F 76.3 -1.0 -0.2 OO9QOO 80.4 3.1 0.7 MDDETU 76.6 -0.7 -0.2 IWA0AA 80.5 3.2 0.7 A5GR55 77.0 -0.3 -0.1 CZGHZZ 80.6 3.3 0.8 30 2016/2-SM Copyright (c) 2017 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Cocaine Deviation Code Concentration from robust z-score (mass%) average CU6JGV 80.8 3.5 0.8 IXUAHB 81.0 3.7 0.9 O4KFNX 81.0 3.7 0.9 TQMVZE 81.3 4.0 0.9 VBEY7Y 81.4 4.1 1.0 8J4DWT 82.0 4.7 1.1 LL8LML 82.0 4.7 1.1 FK5BHB 82.4 5.1 1.2 CJWZIJ 83.0 5.7 1.3 OTSOQ9 83.3 6.0 1.4 1YQDGQ 83.6 6.3 1.5 7JUSKK 83.9 6.6 1.5 8Q8VEF 84.0 6.7 1.6 K3S33Y 84.9 7.6 1.8 NZOTC6 87.0 9.7 2.2 A7LUO7 87.5 10.2 2.4 MDQMM4 88.7 11.4 2.6 Z8T8N1 89.0 11.7 2.7 9994MR 89.9 12.6 2.9 WQOZYA 92.2 14.9 3.4 H13HRX 93.4 16.1 3.7 CWEOYI 93.8 16.5 3.8 10B0XJ 98.4 21.1 4.9

Sample 2 Analysis

Identified substances for Test Sample 2 Code Identified Substances 0D11QZ JWH073 0HSVIE JWH-073 0LAKP0 JWH073 0P0W03 JWH - 073 10B0XJ not able to identify 1JJBJS JWH-073 1YQDGQ JWH-073 1ZKJHF JWH-073 211119 JWH-073 2PUPPP JWH-073 2R20JW JWH-073 33DUO3 Naphtalen-1-yl-(1-butylandol-3-yl) methanone (JWH-073) 3PV3WL JWH 073 40HFEP JWH-073 4J4H44 JWH-073 55BR5Z JWH073 5MLCMA JWH-073 5ZDDX6 JHW-073 7IUIII JWH-073 7JUSKK JWH-073 7T7YHK JWH-073 8AHAJA JWH-073 8D1PTX JWH-073, LACTOSE 8II46Y JWH-073 8J4DWT JWH-073 8MV6V6 JWH-073 8Q8VEF JWH-073 8WEYGQ JWH-073 8Z8ZZZ JWH-073 9994MR jwh-073 9Q999K JWH-O73 A33Q33 JWH-073 A5GR55 JWH-073 A7LUO7 JWH-073 AND LACTOSE A8YSK1 JWH-073 AEDDRS JWH-073 APX4KD JWH-073 ARZMMQ JWH-073 ASLAA5 JWH-073 AYNT4F JWH-073

Code Identified Substances B3SNNC JWH-073 BARYZ2 JWH-073 C9CDOR JWH-73 CANEE8 JWH 073 CCIVVK JWH-073 CJWZIJ JWH-073 CRSEZI JWH 073 CU6JGV WE CAN´T IDENTIFY THESE DRUGS CWEOYI JWH-073 CZGHZZ JWH-073 DMM5Z5 JWH073 DWRNDI jwh-073 E2OA5N no investigado E3MIHV JWH-073 E5LDLX JWH-073 E66LY6 JWH-073 and Lactose EHJ60F JWH-073 EMJ8VM JWH 073 EXZYYP JWH-073 FK5BHB JWH-073 FMFLFF JWH073 G0B9NL 1-BUTYL-3-(1-NAPHTHOYL)INDOLE (JWH-073) G2GBDV JWH-073 GGA8CG JWH-073 GJIRPN JWH-073 GKHDEM jwh-073 GNUILW JWH-073 GV2PGK JWH 073 HEHCMO JVH-073 HF3FYI JWH-073 HJLSL6 JWH-073 HRYNGY JWH-073 IMVADS JWH-073 IQYQE4 JWH-073 IWA0AA JWH-073 IXUAHB JWH-073 IZLLW0 JWH-073 JEVX45 jwh-073 JKG5E5 JWH-073 JM2GKM JWH-073 JSZ6XW JWH-073 K3S33Y JWH-073 KBUURH JWH-073 KKKWIC JWH-073

Code Identified Substances KSQKKK JWH-073 L4444V JWH-073(synthetic cannabinoid) LDDCDD JWH LL8LML JWH-073 LLL1RB JWH-073 LNUUEI JWH-073 LQ8989 JWH 073 LVVWC7 JWH-073 M1XUWT JWH-073 M72KOQ Cocaine MCCCCC Napthalen-l-yl-(1-butylindol-3-yl) methanone (JWH-073) MDDETU JWH-073 MDQMM4 JWH-073 MMMMT5 JWH-073 MOKSHS JWH-073 MWXNUW JWH-073 and Lactose MZMHCW JWH-073 N8BTCF JWH-073 NWJDJI JWH-073 NZOTC6 JWH-073 O4KFNX JWH-073 O888ML JWH-073 ODOOO2 JWH073 OJFEOO Naphthalen-1-yl-(-butylindol-3-yl)methanone (JWH-073) OK66R6 JWH-073 OO9QOO JWH-073 OQ4QQQ The sample number two was analyzed with GCMS and yielded one pik at Rt= 18.9( dihydromethyl dioxo...),which is not recognize/readable by the library.The library is installed in 2008. OS838A JWH-073, lactose OTSOQ9 JWH-073 PHWNRB JWH-073 PPLICW JWH-073 PQQKLQ NIL R7BBLB JWH-073 RI3K33 Naphthalen-1 yl(1-butylindol-3-yl) methanone / JWH-073 RU8UQS jwh-073 SIFXH3 JWH-073 SMYNNU JWH-073 SUUW3G JWH-073 SVGG03 JWH-073 T2DI1R JWH-073 T4VMD2 JWH-073 TI22ZK JWH-073 TQMVZE JWH-073

Code Identified Substances TRVLKK JWH-073 TSSRQR JWH-073 TSW3IE JWH-073 TZOONA JWH-073 UFK6EF JWH-073 UG88A8 N/A UJWYPY JWH-073 UMXXSY JWH-073 UUUOU9 Benzodiazepine (possible) UWBOLU JWH-073 UXVVAC JWH-073 UYFCCR JWH-073 UYJBJJ JWH-073 V011CO JWH-073 VBEY7Y JWH-073 VFC8CC JWH-073 VIFKAW JWH-073 VPHJRP JWH 073 VVIRG4 JWH(073) VVN4CQ JWH-073 W0HPES JWH73 WGZNNM JWH-073 WMTTV7 JWH-073 WQOZYA JWH-073 X0X444 JWH-073 XEE66N jwh-73 XNNNU1 JWH-073 XXFX8D JWH-073 YGQE84 JWH-073 (Naphtalen-1-y1-(1-butylindol-3-y1)methanone and Lactose YLHIIH JWH-073 YQYLYY JWH-073 Z2BIDB JWH-073 Z8T8N1 JWH-073 ZCCQMZ JWH 073 ZQHUPQ JWH-073 ZWL0DM JWH073 ZXGCGG JWH-073

Statement of findings for Test Sample 2

Code JWH-073 Lactose 0D11QZ + ANP

0HSVIE + ANP

0LAKP0 + - The sample contains JWH073 (not quantified). 0P0W03 + + A color test (SCOTT-Cobalt thiocyanate TEST) with positive reaction to Cocaine, to the TLC was used as a solvent for the preparation of the samples the Dichloromethane and as eluent methanol, used an aluminum plate 20 × 20 cm. Confirmation of results were made on the equipment of THERMO SCIENTIFIC NICOLET Is 10 and NICOLET Is 50 FT-IR.For 2016/2 sample/SM-2 should stress that the preliminary test was not conclusive. With the FT-IR sensed the presence of LACTOSE and other substances which are not suitable to specify here. With the TLC was able to identify the substance JWH-073. 10B0XJ - - Could not be identified 1JJBJS + +

1YQDGQ + + LACTOSE 1ZKJHF + ANP Examination revealed the presence of synthetic cannabinoids JWH-073 211119 + ANP Results of screening test were positive for amphetamines type stimulants. Relation time and fragmentation pattern obtained with sample are equivalent to those obtained with JWH-073. 2PUPPP + + Sample contains 14.39 ± 0.79 % (w/w) JWH-073. The sample also contains lactose. 2QC44H - ANP

2R20JW + ANP JWH-073 34.08% 33DUO3 + ANP

3PV3WL + + The sample SM2 contained JWH 073. Quantification of JWH 073 our institute not performed. Lactose was in the sample SM2 identify. 40HFEP + + Mass spectrometry profile correlation between sample and reference material certified 4J4H44 + - JWH-073 confirmed in 1 unit tested of 1 unit received. 55BR5Z + + ./. 5MLCMA + ANP Sample 2016/2/SM-2 found to contain JWH-073 5ZDDX6 + + the sample also contains lactosa 7666AG + ANP JWH-073

Code JWH-073 Lactose 7IUIII + - The result of the sm 2 (117) tests received has confirmed that the mentioned simple contains JWH- 073 but we have not been able to give a cuantification result. 7JUSKK + ANP In Albanian is not in narcotic and psychotropic list 7T7YHK + + On analysis, I found sample SM-2 to contain JWH-073 and Lactose. 8AHAJA + +

8D1PTX + +

8II46Y + + JWH-073 was identified by GC-MS. 8J4DWT + ANP

8MV6V6 + ANP In the test sample 2016/2/SM-2 was detected JWH-073 8Q8VEF + -

8WEYGQ + ANP White powder containing JWH-073. 8Z8ZZZ + +

9994MR + +

9Q999K + ANP sample SM-2 was found to contain JWH-073 A33Q33 + ANP JWH-073 confirmed A5GR55 + + Lactose A7LUO7 + + BY GC-MS AND FTIR A8YSK1 + + JWH-073 and lactose AEDDRS + ANP

APX4KD + + The white powder was analysed and found to contain (1-butyl-1H-indol-3-yl)(naphthalen-1-yl) methanone (JWH-073). ARZMMQ + + additional substaces: lactose ASLAA5 + + The sample was found to contain JWH-073 and lactose AYNT4F + ANP De análisis realizados se concluye que la sustancia se trata del cannabionide sintético identificado como JWH-073

Code JWH-073 Lactose B3SNNC + ANP The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule II 2. (2) (ii) A synthetic cannabinoid receptor type I against namely, 1-butyl-3-(1-naphthoyl)indole (JWH-073) or an isomer there of. BARYZ2 + +

BFIU0G ANP ANP The test sample number SM-2 is not delivered. BRVRR4 - ANP Examination and analyses performed on SM2 did not reveal the presence of dangerous drugs. C9CDOR + +

CANEE8 + +

CCIVVK + + The sample contain JWH-073. CJWZIJ + + The sample contained 12.9% of JWH-073 and lactose. CRSEZI + + lactose CU6JGV - -

CWEOYI + + after chemical analysis was performed the sample was contain 2.566% JWH-073 & LACTOSE CZGHZZ + + reference missing DMM5Z5 + - Tested by GCMS DNNSKS - -

DWRNDI + - jwh-073 E2OA5N ANP ANP

E3MIHV + ANP 150: le Rf du spot donné par le standard est non identique avec le Rf obtenu avec la substance de référence JWH-073 (les deux uniquement, échantillon et standard ont été analysés par la suite sur la même plaque. E5LDLX + +

E66LY6 + +

EHJ60F + -

EMJ8VM + + Sample 2016/2/SM-2 contains JWH 073 and lactose. EXZYYP + ANP The sample gave negative result with Marquis' and Cobalt Thiocyanate reagents. Confirmed by GC/MS, and quantified by GCFID, the sample contained JWH-073 16.8%.

Code JWH-073 Lactose FK5BHB + - After analycing the simple with colorimetric tests, GC/MS confirmation we are able to say that this simple is JWH-073. It is not quantified because it does not have the righet stardands FMFLFF + ANP JWH073, synthetic cannabinoid G0B9NL + + White powder 228 milligrams 1 package 1-BUTYL-3-(1-NAPHTHOYL)-INDOLE (JWH-073) Class B G2GBDV + ANP JWH-073 is controlled by K.B. of 22/01/1998, changed by K.B. of 26/09/2011 GGA8CG + + A sealed glass vial containing a white powder. This powder contained 1-BUTYL-3-(1-NAPHTHOYL) INDOLE (JWH-073). GJIRPN + ANP JWH-073 is a Class B controlled drug subject to the provisions of the Misuse of Drugs Act 1971. GKHDEM + ANP JWH-073 was detected by gc-ms screening and it was quantified by gc-fid using response factor GNUILW + ANP JWH-073 belong to synthetic cannabinoid receptor agonists group, however, currently is not a controlled drug according to spanish legislation. GUDEBT + ANP Sample 2016/2/SM-2 a white powder gave a positive result for JWH-073. GV2PGK + + JWH073 is present with lactose. H13HRX - + LACTOSE HEHCMO + + No HF3FYI + ANP JWH-073, concentration approx 12% HJLSL6 + + Sample contained JWH-073 and lactose. Identification of JWH 073 by FTIR and MS spectrum, quantification by GC/FID HRYNGY + + POWDER IMVADS + ANP SM-2 contains a drug: JWH-073, 13.8% IQYQE4 + -

IRWMIX ANP + Sample 2016/2/SM-2 consists of white powder. No prohibited substances are detected in this sample. IWA0AA + + The sample contains JWH-073 which is listed as a controlled drug according to french order, appendix IV of February 22nd 1990. IXUAHB + + 225 milligrams - JWH-073 - Class B Lactose - Not Controlled IZLLW0 + ANP Non-controlled substance with effects similar to cannabis JCUITV ANP ANP

Code JWH-073 Lactose JEVX45 + ANP White powder containing jwh-073 not quantified JKG5E5 + - JWH-073 JM2GKM + + Marquis, Scott y Simon's GC-MS, FT-IR, UV JSZ6XW + - The above article was examined and found to consist of a brown glass vial containing a quantity of white powder. The powder, which weighed 0.21 grams, was analysed and found to contain JWH-073. JWH-073 is a compound structurally derived from 3–(1–naphthoyl)indole by substitution at the nitrogen atom of the indole ring by an alkyl substituent, and as such is a class B controlled drug within the provisions of the Misuse of Drugs Act 1971.

K3S33Y + + The sample contains JWH-073. JWH-073 is a controlled substance in X. KBUURH + + JWH 14.01 %, laktose KK6WBZ + -

KKKWIC + ANP The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule II 2. (2) (ii) A synthetic cannabinoid receptor type I against namely, 1-butyl-3-(1-naphthoyl)indole (JWH-073) or an isomer there of. KSQKKK + + JWH-073 was found in the sample

L4444V + + The sample was found to contain a SYNTHETIC CANNABINOID JWH-073(1-butyl-1H-indol-3YL) Naphtalen-1-YL, and LACTOSE LDDCDD + ANP No colour reaction with conventional reagents in our lab. But in TLC method (Toluene:Diethylamine system with Fast Blue B spray) Rf and colour of SM 2 is similar to Rf and colour of standard JWH. So SM 2 is JWH. LL8LML + ANP JWH-073 was detected. LLL1RB + + One glass bottle containing 0.23 grammes of a powder containing (1-butyl-1H-indol-3-yl)-1- naphthalenyl-methanone, being a compound structurally derived from 3-(1-naphthoyl)indole by substitution at the nitrogen atom of the indole ring with an alkyl substituent. LNUUEI + + The powder is a misture of lactose and JWH-073, a synthetic cannabinoid. The concentration of JWH-073 in the sample is 13.2% by weight. LQ8989 + ANP the item is powder containing JWH073 non quantified LVVWC7 + + The sample contains Lactose. M1XUWT + - Powder (sample) contains JWH-073 M72KOQ - + Lactose

Code JWH-073 Lactose MCCCCC + ANP From screening test using (MR) and ion scan and from confirmatory test using (GC-MS) the sample was found to contain the controlled drug JWH-073. MDDETU + - Sample contains JWH-073 MDQMM4 + ANP

MMMMT5 + ANP The mixture contains JWH-073 and some form of sugar MOFYQQ - - negative MOKSHS + - lactose MWXNUW + + The Test sample 2016/2/SM-2 was analyzed by Colour test and Thin Layer Chromatography technique and found to contain JWH-073 and Lactose. MZMHCW + + It contains JWH-073. It also contains lactose N8BTCF + + This sample contains JWH-073 and has lactose as diluent. NWJDJI + + Based on the above analysis, the sample was found to contain JWH-073 and lactose. NZOTC6 + ANP - O4KFNX + + White powder containing 12.1%ww JWH-073 and lactose O888ML + - The test sample 2016/2/SM-2 was found to contain the psychoactive substance Naphthalen-yl-(1- butylindol-3-yl) methanone (JWH-073). ODOOO2 + + Sample also contain lactose. The presence of lactose and JWH073 were not as always confirmed by FTIR spectroscopy analysis because of equipment failure. OJFEOO + - JWH-073 is included in Table I Schedule I drugs (narcotics-not use by medicine ) approved by Government Decision of Republic of Moldova no. 1088 of 05.10.2004 (Last Updated 5/13/2016) (tables and lists of narcotic, drugs, psychotropic substances and their precursors under control) OK66R6 + + The sample also contains lactose. OO9QOO + - lactose trace OQ4QQQ - ANP

OS838A + + The sample contains JWH-073 which is scheduled as illicit drug in France. The lactose is not scheduled as illicit drug in France. It's a cutting agent. OTSOQ9 + + cannabinoide sintetico P0FZ8V - ANP

Code JWH-073 Lactose PHWNRB + + The sample was found to contain JWH-073. PPLICW + ANP The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule II 2. (2) (ii) A synthetic cannabinoid receptor type I against namely, 1-butyl-3-(1-naphthoyl)indole (JWH-073) or an isomer there of. PQQKLQ ANP ANP THE SAMPLE 2016/2/SM-2 WAS NOT INCLUDED IN THE ICE PACKAGE. QQQQJW ANP ANP

R7BBLB + + JWH-073 (14.5 % w/w) and lactose RI3K33 + + Further analysis revealed that percentage of JWH-073 in sample is 1.20. In addition to JWH -073, lactose was also identified in the sample by FTIR. RJINCE + - JWH _073 RJNRSN + + JWH-073 and lactose were detected in sample 2016/2/SM-2. Quantitative analysis not performed. RU8UQS + ANP we have found results from swg-drug library, which the last version it, and we have studied for quantitative analysies with GC-FID. RVP7VW ANP ANP

SIFXH3 + ANP Sample 2016/2/SM-2 contains JWH-073. SMYNNU + - The sample consist controlled drugs - JWH-073 SUUW3G + ANP ɫontained JWH-073 SVGG03 + ANP The sample contains 13.88 % JWH-073 . T2DI1R + ANP The chemical test and the coincidence in the retention time and mass fragmentogram with the reference material in the same conditions that the analyzed sample, indicate the JWH-073 presence. T4VMD2 + ANP This sample yield yellow color during colorimetric analysis been performed by using Froehde and Marquis reagent. Based on GC/MS analysis, JWH-073 had been identified TI22ZK + ANP X grams of white powder containing JWH-073 (Naphthalen-1-yl(1-butylindol-3-yl)methanone. Class B TQFFPF + ANP Analyses performed on Item # 1 revealed presence of JWH-073 which is sintetic Canabinoid and which is not scheduled by the national Law on narcotics, psychotropic substances and precursors. TQMVZE + + In the sample 2 we have faund JWH 073. JWH 073 is on the list of the drug in Montenegro. TRVLKK + + SM2 contains JWH-073 and Lactose

Code JWH-073 Lactose TSSRQR + +

TSW3IE + + ANALYZED WHITE POWDER CONTAINS JWH-073 TZOONA + + JWH-073, LACTOSE UFK6EF + + The sample contains JWH-073 and lactose. JWH-073 is sheduled as illicit drug. UG88A8 ANP ANP N/A UJWYPY + + lactose UMXXSY + + JWH-073 - methanol extraction, alkaline solvent extraction (CHCl3) - GCMS - compare masspectra with library; Lactose - Extraction by ethanol - Residue - FTIR after evaporation to dryness under stream of Nitrogen - JWH-073 - compare IR spectra with library UUUOU9 - -

UWBOLU + ANP the white powder contains synthetic cannabinoid JWH-073 controlled by national law UXVVAC + + Presence of JWH-073 and lactose was detected in the sample. The sample also contained multitude of trace level impurities. UYFCCR + ANP IN SAMPLE 2016/2/SM-2 JWH-073 WAS FOUND. UYJBJJ + + This sample contains JWH-073 V011CO + - The high quality of measurement results (99%) proves the presence of JWH-073 in the sample. VBEY7Y + + Up to date it has never been detected in our laboratory. VFC8CC + +

VIFKAW + + the sample contains naphthalen-1-yl-(1-butylindol-3-yl)methanone and lactose. VPHJRP + + The sample containing 15.9% JWH073 and lactose. VVIRG4 + + Sample found to contain JWH(073) and lactose We do not conduct quantitative drug samples JWH(073) lost by standard sample plos VVN4CQ + + lactose W0HPES + - base WGZNNM + +

WMTTV7 + + The sample contains JWH-073, a sintetic cannabinoid and lactose

Code JWH-073 Lactose WQOZYA + ANP

X0X444 + + white powder containing JWH-073 and lactose as diluent XEE66N + + the sample is containing 8.9% pure jwh-73 XNNNU1 + ANP Powder containing JWH-073 Legal status: illegal - Portuguese NPS Law XXFX8D + ANP The sample found to contain JWH-073 YGQE84 + + Coloimetric reactions (CR) positive. GC/MS Retention time and mass charge (m/z) similar characteristics with the substances used as standard or pattern. FTIR absorption bands coincident with the substances used as pattern. YLHIIH + - NAPHTHALEN-1-y1-(1butylindol-3-yl)methanone (JWH-073) YQYLYY + ANP Presence of the synthetic cannabinoid JWH-073. Z2BIDB + + On analysis, I found that the substances contain JWH-073. Z8T8N1 + -

ZCCQMZ + + JWH 073 in lactose powder ZQHUPQ + + It has been detected the presence of JWH-073 in the sample. This substance appears in the European Database on New Drugs since March 2009. ZWL0DM + + LACTOSE ZXGCGG + + The identification was realized with prelimimary color test with Marquis Reagent the confirmative assay with FT-IR and CG-MS and also the quantitative analysis.

Identification methods for Test Sample 2

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

RESPONSE SUMMARY FOR TEST SAMPLE 2

Participants: 181

The response summary of all 181 participating laboratories for the identification off SM-2, frequency of use of screening and identification techniques and false positives and negatives:

Identificatiion of Test Sample-2:

Substance Name Number of laboratories correctly identtifying: JWH-073 162 Lactose 89

False positives for Test Sample-2:

Round Code: Substance reported: Tech Code: M72KOQ Cocaine 180 UUUOU9 Benzodiazepine (possible) 140/171 XNNNU1 Morphine 180

False negatives for Test Sample-2 (techniques(s) used for ANP):

Round Code: Answer Code: Tech Code: Round Code: Answer Code: Tech Code: CU6JGV - 171 QQQQJW ANP - P0FZ8V - 180/180 RVP7VW ANP - OQ4QQQ - 180/180 JCUITV ANP - 10B0XJ - 180 E2OA5N ANP - H13HRX - 150/180 IRWMIX ANP - BRVRR4 - 180 PQQKLQ ANP - MOFYQQ - 161/180 BFIU0G ANP - 2QC44H - 150 UG88A8 ANP - DNNSKS - 150/180 M72KOQ - 180 UUUOU9 - 180

Frequency of use of screening, identification and quantification techniques:

Response Summary Participants 181 Technique 140 141 142 150 160 161 170 171 172 180 190 200 210 211 220 230 231 Screening (No.) 54 75 62 19 030407219 1 13 0 120 (%) 29.8 41.4 34.3 10.5 0.0 1.7 0.0 2.2 0.0 39.8 10.5 0.6 7.2 0.0 0.6 1.1 0.0 Identification (No.) 13 6 534512135116879 4 83074 (%)7.23.3 2.8 18.8 2.8 6.6 0.6 19.3 0.6 92.8 43.6 2.2 4.4 1.7 0.0 3.9 2.2 Quantification (No.) 0 0 008240760300013010 (%)0.00.0 0.0 0.0 6.2 18.6 0.0 58.9 0.0 23.3 0.0 0.0 0.8 2.3 0.0 0.8 0.0

Robust average = 13.2 % Round: 2016/2 UNODC value = 14.5 % Substance: SM‐2; JWH‐073 4.00 3.0 3.00

2.00 1.8 1.8 1.4 1.3

1.00 0.8 0.7 0.7 0.6 0.6 0.6 0.5 0.4 0.4 0.3 0.3 0.3 0.1 0.1 0.1 0.0 10.6 0.00 5.4 ‐ 0.1 0.1 ‐ ‐ 0.1 0.2 ‐ ‐ 0.4 ‐ 0.4 ‐ 0.6 ‐1.00 ‐ 0.9 1.0 ‐ ‐ 1.1 ‐ 1.2 ‐ 1.5 ‐ 1.6 1.6 ‐2.00 ‐ ‐ 2.0 ‐ 2.1 ‐ 2.2 ‐

‐3.00

‐4.00 1JJBJS 8II46Y CRSEZI HJLSL6 CJWZIJ HF3FYI 4J4H44 EXZYYP LNUUEI R7BBLB VPHJRP Z8T8N1 VFC8CC TSSRQR XEE66N 5ZDDX6 2PUPPP 7666AG A5GR55 2R20JW NZOTC6 CWEOYI SVGG03 O4KFNX IMVADS UXVVAC ZXGCGG KK6WBZ 33DUO3 LVVWC7 W0HPES KBUURH MOKSHS SMYNNU GKHDEM ZWL0DM WQOZYA SUUW3G HEHCMO MDQMM4 z‐scores can be interpreted by participants in line with ISO 13528:2005, secion 7.4.2 and ISO/IEC guide43‐1:1997(E) as follows: IzI < 2 = satisfactory 2 ≤ IzI ≤ 3 = questionable IzI > 3 = unsatisfactory According to the recommendations in ISO 13528:2005, an unsatisfactory z‐score is considered to give an action signal and a questionable z‐ score is considered to give a warning signal. A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occured that requires inverstigation.

51 Z‐Score Report per Sample per Substance

Round: 2016/2 Substance: SM‐2; JWH‐073

Dispersion of z-scores using different analytical techniques for the quantification of JWH-073 in 2016/2 SM-2 10

0 z-score

-2

-4

-6

-8 HPLC GC‐FID GC‐MS NMR

-10

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

Z-Scores for Test Sample 2

JWH-073 Deviation Code Concentration from robust z-score (mass%) average CWEOYI 2.6 -10.6 -5.4 XEE66N 8.9 -4.3 -2.2 Z8T8N1 9.0 -4.2 -2.1 LVVWC7 9.2 -4.0 -2.0 MOKSHS 10.0 -3.2 -1.6 TSSRQR 10.0 -3.2 -1.6 W0HPES 10.3 -2.9 -1.5 MDQMM4 10.9 -2.3 -1.2 ZWL0DM 11.0 -2.2 -1.1 SMYNNU 11.3 -1.9 -1.0 5ZDDX6 11.3 -1.9 -0.9 KK6WBZ 12.0 -1.2 -0.6 WQOZYA 12.3 -0.9 -0.4 HF3FYI 12.4 -0.8 -0.4 NZOTC6 12.9 -0.3 -0.2 CJWZIJ 12.9 -0.3 -0.1 4J4H44 13.0 -0.2 -0.1 A5GR55 13.0 -0.2 -0.1 LNUUEI 13.2 0.0 0.0 CRSEZI 13.3 0.1 0.1 HEHCMO 13.4 0.2 0.1 SUUW3G 13.4 0.2 0.1 8II46Y 13.7 0.5 0.3 33DUO3 13.7 0.5 0.3 IMVADS 13.8 0.6 0.3 SVGG03 13.9 0.7 0.4 KBUURH 14.0 0.8 0.4 O4KFNX 14.1 0.9 0.5 UXVVAC 14.3 1.1 0.6 2PUPPP 14.4 1.2 0.6 1JJBJS 14.4 1.2 0.6 R7BBLB 14.5 1.3 0.7 7666AG 14.5 1.3 0.7 HJLSL6 14.8 1.6 0.8 GKHDEM 15.7 2.5 1.3 VPHJRP 15.9 2.7 1.4 VFC8CC 16.7 3.5 1.8 EXZYYP 16.8 3.6 1.8 ZXGCGG 19.1 5.9 3.0 2R20JW 34.1 20.9 10.6

Sample 3 Analysis

Identified substances for Test Sample 3 Code Identified Substances 0D11QZ ketamine 0HSVIE Ketamine 0LAKP0 Ketamine 0P0W03 KETAMINE 10B0XJ Ketamine 1JJBJS ketamine 1YQDGQ KETAMINE HCL 1ZKJHF Ketamine 211119 Ketamine 2PUPPP Ketamine 2QC44H Ketamine 2R20JW ketamine 33DUO3 Ketamin 3PV3WL Ketamine 40HFEP Ketamine 4J4H44 Ketamine hydrochloride 55BR5Z KETAMINE 5MLCMA Ketamine 5ZDDX6 ketamine 7666AG ketamine 7IUIII KETAMINE 7JUSKK ketamine 7T7YHK Ketamine 8AHAJA ketamine 8D1PTX KETAMINE, LACTOSE 8II46Y Ketamine 8J4DWT ketamine 8MV6V6 ketamine 8Q8VEF Ketamine 8WEYGQ Ketamine 8Z8ZZZ ketamine 9994MR ketamine 9Q999K ketamine A33Q33 Ketamine A5GR55 Ketamine A7LUO7 KETAMINE AND LACTOSE A8YSK1 Ketamine AEDDRS ketamine APX4KD Ketamine ARZMMQ ketamine

Code Identified Substances ASLAA5 Ketamine AYNT4F Ketamina B3SNNC Ketamine BARYZ2 ketamine BFIU0G ketamine C9CDOR ketamine + lactose CANEE8 Ketamin CCIVVK ketamine CJWZIJ Ketamine CRSEZI ketamine CU6JGV KETAMINE CWEOYI ketamine CZGHZZ kétamine DMM5Z5 Ketamine DNNSKS Ketamine DWRNDI ketamine E2OA5N ketamine E5LDLX ketamine E66LY6 Ketamine and Lactose EHJ60F KETAMINE EMJ8VM ketamine EXZYYP Ketamine HCl FK5BHB Ketamine FMFLFF ketamine G0B9NL KETAMINE HYDROCHLORIDE G2GBDV ketamine GGA8CG Ketamine Hydrochloride GJIRPN Ketamine GKHDEM ketamine GNUILW Ketamine GUDEBT KETAMINE GV2PGK ketamine hydrochloride H13HRX COCAINE, KETAMINE HEHCMO Ketamine HF3FYI ketamine HJLSL6 Ketamine HRYNGY KETAMINE IMVADS Ketamine IQYQE4 Ketamine IRWMIX Ketamine IWA0AA Ketamine IXUAHB Ketamine IZLLW0 Ketamine JCUITV KETAMINE

Code Identified Substances JEVX45 ketamine JKG5E5 ketamine JSZ6XW Ketamine KBUURH ketamine hydrochloride KKKWIC ketamine KSQKKK Ketamine L4444V KETAMINE (Anesthetic) LDDCDD Ketamine LL8LML Ketamine LLL1RB Ketamine LNUUEI ketamine LQ8989 Ketamine Hydrochloride LVVWC7 .(7$0ø1( M1XUWT Ketamine M72KOQ Ketamine MCCCCC Ketamine MDDETU Ketamine MDQMM4 Ketamine MMMMT5 ketamine MOFYQQ ketamine MOKSHS Ketamine MWXNUW Ketamine and Lactose N8BTCF Ketamine NWJDJI Ketamine NZOTC6 Ketamine O4KFNX ketamine O888ML Ketamine ODOOO2 Ketamine OJFEOO Ketamine OK66R6 ketamine OO9QOO Kétamine OQ4QQQ ketamin OS838A ketamine, lactose OTSOQ9 KETAMINA P0FZ8V ketamine PHWNRB Ketamine PPLICW Ketamine PQQKLQ KETAMINE QQQQJW ketamine R7BBLB Ketamine RI3K33 Ketamine RJINCE Ketamine RJNRSN Ketamine RU8UQS ketamine

Code Identified Substances RVP7VW ketamine SIFXH3 Ketamine SMYNNU Ketamine SUUW3G Ketamine SVGG03 Ketamine T2DI1R Ketamine T4VMD2 Ketamine TI22ZK Ketamine TQMVZE Ketamine TRVLKK Ketamine TSW3IE KETAMINE TZOONA KETAMINE hcl UFK6EF Ketamine UG88A8 KETAMINE UJWYPY ketamine UMXXSY Ketamine UUUOU9 ketamine UWBOLU ketamine UXVVAC Ketamine UYFCCR KETAMINE UYJBJJ Ketamine V011CO Ketamine VBEY7Y Ketamine VFC8CC Ketamine VIFKAW Ketamine VPHJRP Ketamine VVIRG4 Ketamine VVN4CQ ketamine W0HPES ketamine WGZNNM Ketamine WMTTV7 Ketamine WQOZYA ketamine X0X444 ketamine XEE66N ketamin XNNNU1 Ketamine XXFX8D Ketamine YGQE84 Ketamine YLHIIH KETAMINE YQYLYY katmine Z2BIDB ketamine Z8T8N1 ketamine ZCCQMZ Ketamine ZQHUPQ ketamine hydrochloride ZWL0DM KETAMINE

Code Identified Substances ZXGCGG Ketamine

Statement of findings for Test Sample 3

Code Ketamine Lactose 0D11QZ + ANP

0HSVIE + ANP

0LAKP0 + - The sample contains ketamine. 0P0W03 + + A color test (SCOTT-Cobalt thiocyanate TEST) with positive reaction to Cocaine, to the TLC was used as a solvent for the preparation of the samples the Dichloromethane and as eluent methanol, used an aluminum plate 20 × 20 cm. Confirmation of results were made on the equipment of THERMO SCIENTIFIC NICOLET Is 10 and NICOLET Is 50 FT-IR.For 2016/2 sample/SM-2 should stress that the preliminary test was not conclusive. With the FT-IR sensed the presence of LACTOSE and other substances which are not suitable to specify here. With the TLC was able to identify the substance KETAMINE. 10B0XJ + - Confirmatory test (GCMS) shows test sample contains ketamine 1JJBJS + +

1YQDGQ + + LACTOSE 1ZKJHF + ANP Examination revealed the presence of Ketamine 211119 + ANP Results of screening test were positive for cocaine. Relation time and fragmentation pattern obtained with sample are equivalent to those obtained with ketamine. 2PUPPP + + Sample contains 10.56 ± 0.59 % (w/w) Ketamine base. The sample also contains lactose. 2QC44H + ANP The sample obtains with positive result with Marquis reagent. TLC : The Rf sample obtain with the same Rf Ketamine Standard. GC : The Rt sample obtain with the same Rt Ketamine Standard. 2R20JW + ANP ketamine chloridrate 10,49% as base 33DUO3 + ANP

3PV3WL + + The sample SM3 contained 10,1 % of ketamine. Lactose was in this sample identify. 40HFEP + + Mass spectrometry profile correlation between sample and reference material certified 4J4H44 + + Ketamine hydrochloride and lactose confirmed in 1 unit tested of 1 unit received. 55BR5Z + + ./. 5MLCMA + ANP Sample 2016/2/SM-3 found to contain Ketamine 5ZDDX6 + + the sample also contains lactosa 7666AG + ANP

Code Ketamine Lactose 7IUIII + - The result of the sm 3 (25) tests received has confirmed that the mentioned simple contains ketamine but we have not been able to give a cuantification result. 7JUSKK + ANP

7T7YHK + + On analysis, I found sample SM-3 to contain Ketamine and Lactose. 8AHAJA + +

8D1PTX + +

8II46Y + + Ketamine was identified by GC-MS. 8J4DWT + ANP

8MV6V6 + ANP In the test sample 2016/2/SM-3 was detected ketamine 8Q8VEF + -

8WEYGQ + ANP White powder containing ketamine. 8Z8ZZZ + +

9994MR + + White powder, totally soluble in water, slightly soluble in chloroform 9Q999K + ANP sample SM-3 was found to contain 11.4% of ketamine. A33Q33 + ANP Ketamine confirmed A5GR55 + + Lactose A7LUO7 + + BY GC-MS AND FTIR A8YSK1 + + Ketamine and lactose AEDDRS + ANP

APX4KD + + The white powder was analysed and found to contain ketamine. ARZMMQ + + additional substaces: lactose ASLAA5 + + The sample was found to contain ketamine and lactose AYNT4F + ANP De análisis realizados se concluye que la sustancia se trata de ketamina B3SNNC + ANP The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule I 14. (1) Ketamine (2-(2-chlorophenyl)-2-(methylamino) cyclohexanone)

Code Ketamine Lactose BARYZ2 + +

BFIU0G + ANP The test sample number SM-3 containing a hallucinogenic narcotic drug ketamine. BRVRR4 + ANP Examination and analyses performed on SM3 revealed the presence of ketamine (an anaesthetic). C9CDOR + +

CANEE8 + -

CCIVVK + + The sample contain ketamine. CJWZIJ + + The sample contained 27.4% of ketamine and lactose. CRSEZI + + lactose CU6JGV + -

CWEOYI + + after chemical analysis was performed the sample was contain 4.897% ketamine & LACTOSE CZGHZZ + +

DMM5Z5 + - Mandelin reagent test positive and confirmation with GCMS DNNSKS + + Lactose DWRNDI + - ketamine, ketamine II(enol) E2OA5N + ANP

E3MIHV - ANP

E5LDLX + + ketamine: 13.0%ww E66LY6 + +

EHJ60F + -

EMJ8VM + + Sample 2016/2/SM-3 contains ketamine and lactose. EXZYYP + ANP The sample gave negative result with Marquis' and Cobalt Thiocyanate reagents. Confirmed by TLC and GC/MS, and quantified by GCFID, the sample contained Ketamine 10.7% as base. FK5BHB + - After analycing the simple with colorimetric tests, GC/MS confirmation and subsequent quantification by GC-FID we can say that this simple contains 10.41% in ketamine base FMFLFF + ANP ketamine

Code Ketamine Lactose G0B9NL + + White powder 228 milligrams 1 package KETAMINE HYDROCHLORIDE Class B G2GBDV + ANP ketamine is controlled by K.B. of 22/01/1998 GGA8CG + + A sealed glass vial containing a white powder. This powder contained Ketamine Hydrochloride. GJIRPN + ANP Ketamine is a Class B controlled drug subject to the provisions of the Misuse of Drugs Act 1971. GKHDEM + ANP ketamine was detected by gc-ms screening and it was quantified by gc-fid using calibration curve GNUILW + ANP Ketamine is a controlled drug in Spain under Anex I -List IV of RD 2829/1977 (National regulatory law for psychotropic substances). GUDEBT + ANP Sample 2016/2/SM-3 a white powder gave a positive result for ketamine a controlled substance under national legislation on drugs. GV2PGK + + ketamine hydrochloride is present (11%w/w as base) with lactose H13HRX + + LACTOSE HEHCMO + + No HF3FYI + ANP ketamine, concentration approx 10% HJLSL6 + + Sample contained ketamine and lactose. Identification of ketamine by FTIR and MS spectrum, quantification by GC/FID HRYNGY + + POWDER IMVADS + ANP SM-3 contains a drug: ketamine, 11.1% IQYQE4 + -

IRWMIX + + Sample 2016/2/SM-3 consists of white powder. Ketamine, a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. IWA0AA + + The sample contains ketamine which is listed as a controlled drug according to french order, appendix IV of February 22nd 1990. IXUAHB + + 228 milligrams - Ketamine - Class B Lactose - Not Controlled IZLLW0 + ANP The sample contains a controlled substance as ketamine JCUITV + ANP

JEVX45 + ANP White powdre containing 10.8%ww in ketamine JKG5E5 + + ketamine with lactose

Code Ketamine Lactose JM2GKM + + Tiocianato, marquis, Simon's GC-MS, FT-IR JSZ6XW + - The above article was examined and found to consist of a brown glass vial containing a quantity of white powder. The powder, which weighed 0.22 grams, was analysed and found to contain Ketamine. Ketamine is a class B controlled drug within the provisions of the Misuse of Drugs Act 1971.

K3S33Y + + The sample contains ketamine. Ketamine is not at controlled narcotic substance in X. Ketamine is subject of the pharmaceutical regulation. KBUURH + + ketamine base 11,27 %, laktose KK6WBZ + -

KKKWIC + ANP The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule I 14. (1) Ketamine (2-(2-chlorophenyl)-2-(methylamino) cyclohexanone) KSQKKK + + Ketamine and lactosa were found in the sample L4444V + + The sample was found to contain KETAMINE and LACTOSE LDDCDD + ANP Violet colour by cobalt Thiocyanate indicates the possible presence of ketamine in SM 3. TLC result and GCMS result confirmed the presence of ketamine. LL8LML + ANP Ketamine was detected. LLL1RB + + One glass bottle containing 0.22 grammes of a powder containing 0.02 grammes of ketamine. LNUUEI + + the powder is a mixture of lactose and ketamine. The concentration of ketamine, as base, is 10.4% by weight LQ8989 + ANP item is powder containing JWH073 non quantified LVVWC7 + + The sample contains Lactose. M1XUWT + - Powder (sample) contains Ketamine M72KOQ + + Lactose MCCCCC + ANP From screening test using (CI) and ion scan and from confirmatory test using (GC-MS) the sample was found to contain the controlled drug Ketamine. MDDETU + - Sample contains ketamine MDQMM4 + ANP

MMMMT5 + ANP The mixture contains Ketamine and some form of sugar

Code Ketamine Lactose MOFYQQ + - positive MOKSHS + - lactose MWXNUW + + The Test sample 2016/2/SM-3 was analyzed by Colour test and Thin Layer Chromatography technique and found to contain Ketamine and Lactose. MZMHCW + + It does not contain any controlled drugs according to the regulation of our country. It contains ketamine and lactose N8BTCF + + This sample contains ketamine and has lactose as diluent. NWJDJI + + Based on the above analysis, the sample was found to contain Ketamine and lactose. NZOTC6 + ANP - O4KFNX + + White powder containing 9.2%ww ketamine and lactose O888ML + - The test sample 2016/2/SM-3 was found to contain the hallucinogenic drug ketamine. ODOOO2 + + Sample also contain lactose. The presence of lactose and ketamine were not as always confirmed by FTIR spectroscopy analysis because of equipment failure. OJFEOO + - Ketamine is included in Table III Schedule I drugs (psychotropic substance-use by medicine) approved by Government Decision of Republic of Moldova no. 1088 of 05.10.2004 (Last Updated 5/13/2016) (tables and lists of narcotic drugs,psychotropic substances and their precursors under control) OK66R6 + + The sample also contains lactose. OO9QOO + - lactose OQ4QQQ + ANP

OS838A + + The sample contains ketamine which is scheduled as illicit drug in France. The lactose is not scheduled as illicit drug in France. It's a cutting agent. OTSOQ9 + + Ketamina P0FZ8V + ANP

PHWNRB + + The sample was found to contain 10.3% of ketamine (as base). PPLICW + ANP The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule I 14. (1) Ketamine (2-(2-chlorophenyl)-2-(methylamino) cyclohexanone) PQQKLQ + ANP THE SAMPLE 2016/2/SM-3 WAS FOUND TO CONTAIN KETAMINE

Code Ketamine Lactose QQQQJW + ANP

R7BBLB + + Ketamine (11.4 % w/w) and lactose RI3K33 + + Percentage of ketamine in SM3 is 11.66. In addition to ketamine, 2-chloro-7-methoxy-3- ethylquinoline, Bromotriphenyl methane and lactose were identified. RJINCE + - 1 Hexene.2 _p(chlorophenyl)4 methyl ketamine RJNRSN + + Sample 2016/2/SM-3 contained 11.5% Ketamine. The test sample also contained lactose. RU8UQS + ANP we have found results from swg-drug library, which the last version it, and we have studied for quantitative analysies with GC-FID. RVP7VW + ANP

SIFXH3 + ANP Sample 2016/2/SM-3 contains Ketamine. SMYNNU + - The sample consist controlled drugs - Ketamine SUUW3G + ANP ɫontained ketamine SVGG03 + ANP The sample contains 9.78 % ketamine . T2DI1R + ANP The chemical test and the coincidence in the retention time and mass fragmentogram with the reference material in the same conditions that the analyzed sample, indicate the ketamine presence. T4VMD2 + ANP Colorimetric analysis result in no color changes for all types of color test, but GC/MS analysis give result as ketamine detected in the sample TI22ZK + ANP x grams of white powder containing ketamine. Class B TQFFPF + ANP Analyses performed on Item # 1 revealed presence of Ketamine which is New Psycoactive Substance and which is not scheduled by the national Law on narcotics, psychotropic substances and precursors. TQMVZE + + Ketamine is not on the list of drug in Montenegro TRVLKK + + SM3 contains Ketamine and Lactose TSSRQR + +

TSW3IE + ANP ANALYZED WHITE POWDER CONTAINS KETAMINE TZOONA + + KETAMINE, LACTOSE UFK6EF + + The sample contains ketamine and lactose. Ketamine is sheduled as illicit drug.

Code Ketamine Lactose UG88A8 + ANP WHITE POWDER MATERIAL THAT CONTAINS PSYCHOTROPIC SUBSTANCE KETAMINE. UJWYPY + + lactose UMXXSY + + Ketamine - GCMS - compare massspectra with library, retention time of reference sample; Lactose- extraction by ethanol - Residue-FTIR, after evaporation to dryness under stream of Nitrogen - Ketamine - Compare IR spectra with library UUUOU9 + -

UWBOLU + ANP the white powder contains ketamine (23.3%ww) wich is controlled by national law UXVVAC + + Presence of ketamine hydrochloride and lactose was detected in the sample. UYFCCR + ANP IN SAMPLE 2016/2/SM-3 KETAMINE WAS FOUND. UYJBJJ + + This sample is ketamine. V011CO + - The high quality of measurement results (99%) proves the presence of ketamine in the sample. VBEY7Y + - It is usually detected in our laboratory. VFC8CC + +

VIFKAW + + the sample contains ketamine and lactose. VPHJRP + + The sample containing 10.3% of Ketamine and lactose VVIRG4 + + Ketamine existed in salt form Sample found to contain Ketamine and lactose VVN4CQ + + lactose W0HPES + + ketamine HCl WGZNNM + +

WMTTV7 + + The sample contains Ketamine and lactose. WQOZYA + ANP

X0X444 + + white powder containing ketamine and lactose XEE66N + + the sample is containing 11.3% pure ketamin XNNNU1 + ANP Powder containing Ketamine Legal status: illegal - Portuguses NPS Law

Code Ketamine Lactose XXFX8D + ANP The sample found to contain Ketamine YGQE84 + ANP CT (Cobalt thiocyanate) and MR (Marquis Reagent) Negative. GC/MS Retention time and mass charge (m/z) similar characteristics with the substances used as standard or pattern YLHIIH + - KETAMINE AND LACTOSA YQYLYY + ANP Presence of ketamine. Z2BIDB + + On analysis, I found that the substances contain 11.0% w/w of ketamine. Z8T8N1 + -

ZCCQMZ + + Ketamine in lactose powder ZQHUPQ + + It has been detected the presence of ketamine hydrochloride in the sample ZWL0DM + + LACTOSE ZXGCGG + + The sample correspond to a mixture of Ketamine and Lactose

Identification methods for Test Sample 3

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

RESPONSE SUMMARY FOR TEST SAMPLE 3

Participants: 181

The response summary of all 181 participating laboratories for the identification off SM-3, frequency of use of screening and identification techniques and false positives and negatives:

Identificatiion of Test Sample-3:

Substance Name Number of laboratories correctly identiffying: Ketamine 180 Lactose 89

False positives for Test Sample-3:

Round Code: Substance reported: Tech Code: H13HRX Cocaine 150/180 XNNNU1 1-(3-chhlorophenyl)piperazine 180

False negatives for Test Sample-3 (techniques(s) used for ANP):

Round Code: Substance Name: Tech Code: E3MIHV - 150

Frequency of use of screening, identification and quantification techniques:

Response Summary Participants 181 Technique 140 141 142 150 160 161 170 171 172 180 190 200 210 211 220 230 231 Screening (No.) 54 75 62 19 030407219 1 13 0 120 (%) 29.8 41.4 34.3 10.5 0.0 1.7 0.0 2.2 0.0 39.8 10.5 0.6 7.2 0.0 0.6 1.1 0.0 Identification (No.) 13 6 534512135116879 4 83074 (%)7.23.3 2.8 18.8 2.8 6.6 0.6 19.3 0.6 92.8 43.6 2.2 4.4 1.7 0.0 3.9 2.2 Quantification (No.) 0 0 008240760300013010 (%)0.00.0 0.0 0.0 6.2 18.6 0.0 58.9 0.0 23.3 0.0 0.0 0.8 2.3 0.0 0.8 0.0

Robust average = 10.5 % Round: 2016/2 UNODC value = 11.4 % Substance: SM‐3; Ketamine

4.00 3.6

3.00 2.5 2.3

2.00 1.7 1.5 1.5 1.3 1.2 1.2 1.2 1.0

1.00 0.9 0.9 0.8 0.8 0.8 0.7 0.6 0.6 0.6 0.5 0.5 0.5 0.5 0.4 0.4 0.4 0.3 0.3 0.3 0.3 0.2 0.2 0.1 0.1 0.0 13.0 79.5 0.00 5.7 4.5 4.1 3.5 0.0 0.0 0.0 ‐ ‐ ‐ ‐ 0.1 0.1 ‐ 0.1 0.1 0.1 ‐ ‐ ‐ ‐ 0.2 0.2 0.2 0.2 ‐ ‐ ‐ ‐ 0.3 0.3 0.3 ‐ ‐ ‐ 0.4 0.4 0.4 0.4 ‐ ‐ ‐ ‐ 0.6 ‐ 0.6 ‐ 0.7

‐1.00 0.8 ‐ ‐ 0.8 0.8 ‐ ‐ 0.9 ‐ 1.0 1.0 ‐ ‐ 1.2 ‐ 1.3 1.3 ‐ ‐ 1.4 1.4 ‐ ‐ 1.5 1.5 ‐ ‐ ‐2.00 2.6 ‐3.00 ‐

‐4.00 1JJBJS 8II46Y UYJBJJ CRSEZI HJLSL6 RJINCE CJWZIJ JCUITV HF3FYI RI3K33 LLL1RB 8Z8ZZZ 10B0XJ JEVX45 Z2BIDB IZLLW0 4J4H44 E5LDLX EXZYYP JKG5E5 X0X444 0LAKP0 VVIRG4 VBEY7Y IQYQE4 VPHJRP 40HFEP R7BBLB LNUUEI Z8T8N1 BARYZ2 VFC8CC XEE66N RJNRSN TSSRQR CZGHZZ 8Q8VEF FK5BHB 7666AG 2PUPPP 5ZDDX6 9Q999K 2R20JW A5GR55 O4KFNX NZOTC6 CWEOYI SVGG03 IMVADS DNNSKS GV2PGK C9CDOR UXVVAC 3PV3WL 9994MR ZXGCGG KK6WBZ 33DUO3 RU8UQS GNUILW W0HPES G2GBDV LVVWC7 KBUURH 8MV6V6 DWRNDI MOKSHS SMYNNU GKHDEM 5MLCMA WQOZYA SUUW3G ZWL0DM PHWNRB ODOOO2 HEHCMO UWBOLU MDQMM4 z‐scores can be interpreted by participants in line with ISO 13528:2005, secion 7.4.2 and ISO/IEC guide43‐1:1997(E) as follows: IzI < 2 = satisfactory 2 ≤ IzI ≤ 3 = questionable IzI > 3 = unsatisfactory According to the recommendations in ISO 13528:2005, an unsatisfactory z‐score is considered to give an action signal and a questionable z‐ score is considered to give a warning signal. A single action signal or warning signal in two successive rounds shall be taken that an anomaly has occured that requires inverstigation.

74 Z‐Score Report per Sample per Substance

Round: 2016/2 Substance: SM‐3; Ketamine

Dispersion of z-scores using different analytical techniques for the quantification of Ketamine in 2016/2 SM-3 10

0 z-score

-2

-4

-6

-8 HPLC GC‐FID GC‐MS NMR

-10

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

Z-Scores for Test Sample 3

ketamine Ketamine Deviation Code Concentration Deviation from Code Concentration z-score from robust z-score (mass%) robust average (mass%) average CWEOYI 4.9 -5.6 -5.7 9994MR 10.5 0.0 0.0 5ZDDX6 6.1 -4.5 -4.5 2PUPPP 10.6 0.1 0.0 RJINCE 6.5 -4.0 -4.1 0LAKP0 10.6 0.1 0.1 MDQMM4 7.1 -3.4 -3.5 VBEY7Y 10.6 0.1 0.1 CJWZIJ 8.0 -2.5 -2.6 EXZYYP 10.7 0.2 0.2 4J4H44 9.0 -1.5 -1.5 1JJBJS 10.7 0.2 0.2 DWRNDI 9.0 -1.5 -1.5 JEVX45 10.8 0.3 0.3 W0HPES 9.1 -1.4 -1.4 UXVVAC 10.8 0.3 0.3 IZLLW0 9.1 -1.4 -1.4 SUUW3G 10.8 0.3 0.3 O4KFNX 9.2 -1.3 -1.3 G2GBDV 10.8 0.3 0.3 VFC8CC 9.2 -1.3 -1.3 8Z8ZZZ 10.9 0.4 0.4 40HFEP 9.3 -1.2 -1.2 8II46Y 10.9 0.4 0.4 WQOZYA 9.5 -1.0 -1.0 C9CDOR 11.0 0.5 0.4 CZGHZZ 9.5 -1.0 -1.0 KK6WBZ 11.0 0.5 0.5 GNUILW 9.6 -0.9 -0.9 Z2BIDB 11.0 0.5 0.5 VVIRG4 9.7 -0.8 -0.8 GV2PGK 11.0 0.5 0.5 GKHDEM 9.7 -0.8 -0.8 CRSEZI 11.0 0.5 0.5 SVGG03 9.8 -0.7 -0.8 IMVADS 11.1 0.6 0.6 HF3FYI 9.8 -0.7 -0.7 HEHCMO 11.1 0.6 0.6 X0X444 9.9 -0.6 -0.6 DNNSKS 11.2 0.7 0.6 UYJBJJ 10.0 -0.5 -0.6 33DUO3 11.2 0.7 0.7 3PV3WL 10.1 -0.4 -0.4 KBUURH 11.3 0.8 0.8 BARYZ2 10.1 -0.4 -0.4 XEE66N 11.3 0.8 0.8 TSSRQR 10.1 -0.4 -0.4 HJLSL6 11.3 0.8 0.8 RU8UQS 10.1 -0.4 -0.4 9Q999K 11.4 0.9 0.9 LVVWC7 10.2 -0.3 -0.3 R7BBLB 11.4 0.9 0.9 5MLCMA 10.2 -0.3 -0.3 RJNRSN 11.5 1.0 1.0 LLL1RB 10.2 -0.3 -0.3 RI3K33 11.7 1.2 1.2 ZWL0DM 10.3 -0.2 -0.2 A5GR55 11.7 1.2 1.2 VPHJRP 10.3 -0.2 -0.2 7666AG 11.7 1.2 1.2 JKG5E5 10.3 -0.2 -0.2 JCUITV 11.8 1.3 1.3 PHWNRB 10.3 -0.2 -0.2 8Q8VEF 12.0 1.5 1.5 ODOOO2 10.4 -0.1 -0.1 MOKSHS 12.0 1.5 1.5 LNUUEI 10.4 -0.1 -0.1 IQYQE4 12.2 1.7 1.7 8MV6V6 10.4 -0.1 -0.1 ZXGCGG 12.8 2.3 2.3 FK5BHB 10.4 -0.1 -0.1 E5LDLX 13.0 2.5 2.5 NZOTC6 10.5 -0.1 -0.1 SMYNNU 14.1 3.6 3.6 2R20JW 10.5 0.0 0.0 UWBOLU 23.3 12.8 13.0 Z8T8N1 10.5 0.0 0.0 10B0XJ 88.9 78.4 79.5

Sample 4 Analysis

Identified substances for Test Sample 4 Code Identified Substances 0D11QZ heroine, 6-MAM, acetylcodein, papaverine and noscapine 0HSVIE Heroin 0LAKP0 Heroin 0P0W03 HEROINE 10B0XJ Heroine 1JJBJS heroin 1YQDGQ HEROIN BASE 1ZKJHF Heroin, Acetyl Codeine and Monoacetylmorphine 211119 Heroin 2PUPPP Heroin 2QC44H Heroin 2R20JW heroin 33DUO3 Diacetylmorphine, 6-aetcylcodeine, 6-monoacetzlmorphine, papaverine. 3PV3WL Heroine 40HFEP Heroin 4J4H44 Heroin 55BR5Z HEROIN 5MLCMA Heroin 5ZDDX6 heroin 7666AG heroin 7IUIII HEROINE 7JUSKK heroin 7T7YHK Heroin 8AHAJA heroin 8D1PTX HEROIN, MORPHINE, LACTOSE 8II46Y Heroin 8J4DWT heroin 8MV6V6 Heroin 8Q8VEF Heroin 8WEYGQ Heroin 8Z8ZZZ heroin 9994MR heroin 9Q999K heroin A33Q33 Heroin (Diacetylmorphine) A5GR55 Heroine A7LUO7 HEROIN AND 6-ACETYLCODEINE A8YSK1 Heroin AEDDRS heroin APX4KD Diamorphine ARZMMQ heroin base

Code Identified Substances ASLAA5 Heroin AYNT4F Heroína B3SNNC Heroin BARYZ2 heroine BFIU0G heroin BRVRR4 Heroin C9CDOR heroin+lactose CANEE8 heroin CCIVVK heroin CJWZIJ Heroin CRSEZI heroin CU6JGV HEROINE CWEOYI heroin CZGHZZ héroïne DMM5Z5 Morphine DNNSKS Heroin DWRNDI heroin E2OA5N heroina E3MIHV Héroïne E5LDLX heroin E66LY6 Heroin and Lactose EHJ60F HEROIN 25.1 % EMJ8VM heroin EXZYYP Heroin FK5BHB Heroine FMFLFF heroin G0B9NL DIAMORPHINE (commonly known as heroin) G2GBDV heroin GGA8CG Diamorphine GJIRPN Diamorphine GKHDEM heroin, morphine GNUILW Heroin GUDEBT HEROIN GV2PGK heroin H13HRX HEROINE HEHCMO Heroine HF3FYI heroine HJLSL6 Heroin, morphine HRYNGY HEROIN IMVADS Heroine IQYQE4 Heroine IRWMIX Heroin IWA0AA Heroin IXUAHB Diamorphine (Heroin)

Code Identified Substances IZLLW0 Heroine JCUITV HEROINE JEVX45 heroine, 6-MAM JKG5E5 heroin JM2GKM Heroina JSZ6XW Diamorphine K3S33Y Heroine KBUURH heroin base KK6WBZ Acetylcodeine炻ġmonoacetylmorphine KKKWIC Heroin KSQKKK Heorin L4444V HEROINE LDDCDD Heroin LL8LML Heroin LLL1RB Heroin LNUUEI heroin, 6-acetylmorphine LQ8989 Heroine LVVWC7 +(52ø1( M1XUWT Diamorphine (Heroin) M72KOQ Heroin MCCCCC Heroin MDDETU Heroine MDQMM4 Heroine MMMMT5 Heroin MOFYQQ heroïn,6MAM,6monoAetylcodeïne MOKSHS Heroin,6-MAM,Acetil Codein MWXNUW Heroin and Lactose MZMHCW Heroin N8BTCF Heroin NWJDJI Heroin and 6-Monoacetylmorphine NZOTC6 Heroin O4KFNX heroin O888ML Heroin ODOOO2 Heroine OJFEOO heroine OK66R6 heroine, 6-monoacetylmorphine OO9QOO Heroine OQ4QQQ heroin,morphin,acetylcodein,papaveri,noscapine OS838A heroin, noscapine, lactose OTSOQ9 Heroína P0FZ8V cocaine and morphine PHWNRB Diamorphine PPLICW Heroin PQQKLQ HEROIN

Code Identified Substances QQQQJW heroin R7BBLB Heroin RI3K33 Heroin RJINCE Diacetylmorphine RJNRSN Heroin RU8UQS heroin RVP7VW heroine SIFXH3 Heroin SMYNNU Heroin SUUW3G Heroine SVGG03 6-O-monoacetyl morphine , heroin , noscapine & papverine T2DI1R Heroine T4VMD2 Heroin TI22ZK Diamorphine TQFFPF Heroine TQMVZE Heroin TRVLKK Heroin TSSRQR Heroin, 6-MAM TSW3IE HEROINE (DIACETYL MORPHINE) TZOONA HEROIN base UFK6EF heroine base UG88A8 HEROIN UJWYPY heroine UMXXSY Heroin UUUOU9 Heroin UWBOLU heroin UXVVAC Heroin UYFCCR HEROIN UYJBJJ Heroin V011CO Heroin VBEY7Y Heroin VFC8CC Heroin VIFKAW heroin VPHJRP Heroine-Morphine VVIRG4 Heroin VVN4CQ heroin W0HPES heroin WGZNNM Heroin WMTTV7 Heroin WQOZYA heroin X0X444 heroine XEE66N eroin XNNNU1 Heroin XXFX8D Heroin

Code Identified Substances YGQE84 Heroin, acetylcodein, 6-MAM and Papaverine YLHIIH DIACETYLMORPHINE(HEROINE) YQYLYY heroin Z2BIDB heroin Z8T8N1 Heroin ZCCQMZ Heroin ZQHUPQ heroin and products of acetalization of morphine ZWL0DM HEROIN ZXGCGG Heroin

Statement of findings for Test Sample 4

Code Heroin Lactose Morphine minor comp. 0D11QZ + ANP ANP

0HSVIE + ANP ANP

0LAKP0 + - - The sample contains heroin. 0P0W03 + - - A color test (SCOTT-Cobalt thiocyanate TEST) with positive reaction to Cocaine, to the TLC was used as a solvent for the preparation of the samples the Dichloromethane and as eluent methanol, used an aluminum plate 20 × 20 cm. Confirmation of results were made on the equipment of THERMO SCIENTIFIC NICOLET Is 10 and NICOLET Is 50 FT-IR.In relation to 2016/2 sample/SM- 1, all tests are in compliance and the identified substance is Heroine.Even in this sample was detected another stain on the day of the TLC RF value of 0.85, probably DIAZEPAM 10B0XJ + - - Confirmatory test (GCMS) shows test sample contains Heroine 1JJBJS + + -

1YQDGQ + + - NOSCAPINE, ACETYLCODEINE, 06 MONOACETYLMORPHINE, LACTOSE 1ZKJHF + ANP - Examination revealed the presence of Heroin 211119 + ANP - Results of screening test were positive for opiates. Relation time and fragmentation pattern obtained with sample are equivalent to those obtained with heroin. Heroin was detected at 29.91 % by weight. 2PUPPP + + - Sample contains 27.8 ± 1.7 % (w/w) Heroin base. The sample also contains lactose, 6- monoacetylmorphine, acetylcodeine, noscapine and papaverine were also detected. 2QC44H + ANP - The sample obtains with positive result with Marquis reagent. TLC : The Rf sample obtain with the same Rf Heroin Standard. GC : The Rt sample obtain with the same Rt Heroin Standard. 2R20JW + ANP - heroin base 24.86 as base 33DUO3 + ANP - Heroin was as hydrochloride form. 3PV3WL + + - The sample SM4 contained 27,3 % of heroine. Acetyl codeine, acetyl morphine, heroine, noscapine was in this sample identify. 40HFEP + + - Mass spectrometry profile correlation between sample and reference material certified 4J4H44 + + - Heroin base and lactose confirmed in 1 unit tested of 1 unit received. 55BR5Z + + -

5MLCMA + ANP ANP Sample 2016/2/SM-4 found to contain Heroin 5ZDDX6 + + - the sample also contains acetycodein, 6mam, lactosa

Code Heroin Lactose Morphine minor comp. 7666AG + ANP -

7IUIII + - - The result of the sm 4 (124) tests received has confirmed that the mentioned simple contains cocaine with 24.86 percentage by weight 7JUSKK + ANP - The powder contain also acetylcodein, 6MAM, papaverine, noscapine. 7T7YHK + - - On analysis, I found sample SM-4 to contain Heroin, Acetylcodeine, 6-Monoacetylmorphine, Papaverine and Noscapine. 8AHAJA + + -

8D1PTX + + +

8II46Y + + - Heroin was identified by GC-MS. 8J4DWT + ANP - 26% +/-2 Also found acetilcodein and 6-monoacetilmorphine 8MV6V6 + ANP - In the test sample 2016/2/SM-4 was detected heroin, 6-monoacetylmorphine, acetylcodeine and noscapine. 8Q8VEF + - -

8WEYGQ + ANP - Light brown powder containing heroin. Also detected acetyl codeine and monoacetylmorphine. 8Z8ZZZ + + -

9994MR + + - brown powder, usual smell, slightly soluble in water, no chloride ions 9Q999K + ANP - sample SM-4 was found to contain 27.1% of heroin. A33Q33 + ANP - Heroin confirmed. Acetylcodeine, monoacetylmorphine, Papaverine and noscapine detected. A5GR55 + + - 6-monoacetylmorphine acetylcodein, lactose A7LUO7 + ANP ANP BY GC-MS AND FTIR A8YSK1 + + - heroin 26.3%, Monoacetylmorphine, Acetylcdeine and lactose AEDDRS + ANP - found diacetylmorphine (heroin) with 26.3%ww APX4KD + ANP - The brown powder was analysed and found to contain diamorphine (heroin). ARZMMQ + + - additional substaces: lactose ASLAA5 + - ANP The sample was found to contain heroin and acetylcodeine

Code Heroin Lactose Morphine minor comp. AYNT4F + ANP ANP De análisis realizados se concluye que la sustancia se trata de heroina B3SNNC + ANP ANP The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule I 1. (10) Diacetylmorphine (heroin) BARYZ2 + + -

BFIU0G + ANP ANP The test sample number SM-4 containing a psycho narcotic drug heroin. BRVRR4 + ANP - Examination and analyses performed on SM4 revealed the presence of heroin (a depressant). C9CDOR + + -

CANEE8 + - -

CCIVVK + + - The sample contain heroin. CJWZIJ + - - The sample contained 27.4% of heroin. CRSEZI + - - 6-monoacetylmorphine acetylcodeine narcotine CU6JGV + - -

CWEOYI + + ANP after chemical analysis was performed the sample was contain 65.98%heroin & LACTOSE CZGHZZ + ANP ANP

DMM5Z5 - - + Marquis reagent test positive and Confirmation with GCMS DNNSKS + - - Acethylcodeine, O6-MAM, Papaverine, Narcotine DWRNDI + - - heroin, acetylcodaine, 6mam, papaverine, noscapine E2OA5N + ANP ANP

E3MIHV + ANP - 141: apparition d'une coloration violé , orientant sur la présence possible d'opiacé. 150 : un des trois spots donnés par l'échantillon a un Rf identique à celui l’héroïne. E5LDLX + + - heroin: 24.9%ww E66LY6 + + - 6-monoacetylmorphine EHJ60F + - -

EMJ8VM + + - Sample 2016/2/SM-4 contains heroin and lactose. It also contains noscapine, papaverine, acetylcodeine, and O-6-monoacetylmorphine.

Code Heroin Lactose Morphine minor comp. EXZYYP + ANP - The sample positive result with Marquis' reagents. Confirmed by TLC and GC/MS, and quantified by GCFID, the sample contained Heroin 26.9% as base, and also contained 6-Monoacetylmorphine and Acetylcodeine. FK5BHB + - - After analycing the simple with colorimetric tests, GC/MS confirmation and subsequent quantification by GC-FID we can say that this simple contains 13.94% in heroine base FMFLFF + ANP - heroin G0B9NL + + ANP Pale brown powder 218 milligrams 1 package DIAMORPHINE (commonly known as heroin) (23%) Class A G2GBDV + ANP - cocaine is controlled by K.B. of 31/12/1930, changed by K.B. of 8/10/1963 GGA8CG + + - A sealed glass vial containing a brown powder. This powder contained an average of 24% Diamorphine (commonly known as Heroin). GJIRPN + ANP - Diamorphine is a Class A controlled drug subject to the provisions of the Misuse of Drugs Act 1971. GKHDEM + ANP + heroin was detected by gc-ms screening. The screening revealed some traces of morphine too. heroin was quantified by gc-fid using calibration curve. GNUILW + ANP - List I and IV of Single Convention on Narcotics drugs,1961. GUDEBT + ANP - Sample 2016/2/SM-4 a beige powder gave a positive result for heroin a controlled substance under national legislation on drugs. GV2PGK + + - heroin is present (23% as base) with lactose, acetyllcodeine, 06MAM,papaverine and noscapine. H13HRX + + - MONOACETYL MORPHINE, ACETYL CODEINE, LACTOSE HEHCMO + + - Acetylcodeine, 6-monoacetylmorphine,noscapine HF3FYI + ANP - heroine, concentration approx 18% as free base HJLSL6 + + + Sample contained heroin, monoacetylmorphine, acetylcodeine and small amounts of morphine and papaverine. Heroin identification by FTIR and MS spectrum, quantification by HPLC-DAD HRYNGY + - - POWDER IMVADS + ANP - SM-4 contains a drug: heroine, 27.6% IQYQE4 + - -

IRWMIX + + - Sample 2016/2/SM-4 consists of light brown powder. Heroin, a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. IWA0AA + + - The sample contains heroine which is listed as a controlled drug according to french order, appendix I of February 22nd 1990.

Code Heroin Lactose Morphine minor comp. IXUAHB + + - 214 milligrams - Diamorphine (commonly known as heroin) (25%) - Class A Lactose (indicated) - Not Controlled IZLLW0 + ANP ANP The sample contains a controlled substance as heroine JCUITV + ANP -

JEVX45 + ANP - beige powder containing 26.5%ww of heroin. 6-MAM has been also detected, below the LOQ (<1.48%ww) JKG5E5 + - - heroin JM2GKM + + ANP Marquis, Tiocianato GC-MS, FT-IR adicional se detectaron trazas de morfina JSZ6XW + - - The above article was examined and found to consist of a brown glass vial containing a quantity of brown powder. The powder, which weighed 0.20 grams, was analysed and found to contain Diamorphine. A sample of the powder was further analysed and found to contain 23% (weight for weight) Diamorphine. Diamorphine is a class A controlled drug within the provisions of the Misuse of Drugs Act 1971.

K3S33Y + - - The sample contains heroinehydrochloride. The content of heroinehydrochloride is determined to 30 %. Heroine is a controlled substance in X. KBUURH + + - heroine base 26,96 %, laktose KK6WBZ + - +

KKKWIC + ANP ANP The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule I 1. (10) Diacetylmorphine (heroin) KSQKKK + ANP - Heroin was found in the sample L4444V + - - The sample was found to conttain HEROINE and traces of: 6 monoacetylmorphine - Acetyl codeine - Noscapine - Papaverine, as minor components LDDCDD + ANP - Violet to reddish purple colour indicates the possible presence of morphine or codeine or heroin. But TLC and GCMS results confirmed that SM 4 is heroin. LL8LML + ANP ANP Diamorphine (heroin) was detected with a purity of approximately 21% (as base) LLL1RB + ANP - One glass bottle containing 0.22 grammes of a powder containing 0.05 grammes of heroin hydrochloride. LNUUEI + + - the powder is a mixture of lactose and heroin. the concentration of heroin in the sample is 27.5% by weight. LQ8989 + ANP ANP the item is powder containing heroin 25.55% purity

Code Heroin Lactose Morphine minor comp. LVVWC7 + - ANP

M1XUWT + - - Powder (sample) contains Diamorphine (Heroin) M72KOQ + - - Traces of Codeine, Morphine and 6-monoacetylmorphine. MCCCCC + ANP - From screening test using (MR) and ion scan and from confirmatory test using (GC-MS) the sample was found to contain the controlled drug Heroin. MDDETU + - - Sample contains 27,1 % of heroine MDQMM4 + ANP - acetylcodeine 6-monoacetylmorphine MMMMT5 + ANP ANP The mixture contains Heroin and additional substances such as narcotine and acetylcodeine MOFYQQ + - - positive MOKSHS + - - lactose MWXNUW + + - The Test sample 2016/2/SM-4 was analyzed by Colour test and Thin Layer Chromatography technique and found to contain Heroin and Lactose. MZMHCW + + - It contains heroin in purity of 15.1%. It also contains lactose N8BTCF + + - This sample contains heroin, 6-monoacetylmorphine and Acetylcodeine. AND it has lactose as diluent. NWJDJI + + - Based on the above analysis, the sample was found to contain heroin, 6-monoacetylmorphine, papaverine, noscapine, acetylcodeine and lactose. NZOTC6 + ANP ANP - O4KFNX + + - brown powder containing 26.9%ww diacetylmorphine (heroin). The sample als contains 6- monoacetylmorphine, acetylcodeine and lactose. O888ML + - - The test sample 2016/2/SM-4 was found to contain the controlled drug heroin (diacetylmorphine). ODOOO2 + + - Sample also contain lactose . The presence of lactose and heroin were not as always confirmed by FTIR spectroscopy analysis because of equipment failure. OJFEOO + - - Heroine is included in Table I Schedule I drugs (narcotics-not use by medicine ) approved by Government Decision of Republic of Moldova no. 1088 of 05.10.2004 (Last Updated 5/13/2016) (tables and lists of narcotic drugs,psychotropic substances and their precursors under control) OK66R6 + + - The sample also contains lactose, acetylcodeine, noscapine, papaverine. OO9QOO + - -

Code Heroin Lactose Morphine minor comp. OQ4QQQ + ANP +

OS838A + + - The sample contains heroin which is scheduled as illicit drug in France. The lactose is not scheduled as illicit drug in France. It's a cutting agent. The noscapine is an opium impurity. OTSOQ9 + - - Heroína + impurezas alcaloidales y 6- Monoacetylmorfina y acetil codeina. P0FZ8V + ANP +

PHWNRB + + - The sample was found to contain 24.2% of diamorphine (as base). PPLICW + ANP ANP The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule I 1. (10) Diacetylmorphine (heroin) PQQKLQ + ANP - THE SAMPLE 2016/2/SM-4 WAS FOUND TO CONTAIN HEROIN. QQQQJW + ANP ANP

R7BBLB + - - Heroin (24.5 % w/w) and other accompanying opioids: noscapine, 6-acetylmorphine a acetylcodeine RI3K33 + - - Percentage of Diacetyl morphine (heroin) in SM4 is 33.34. In addition to that 6-monoacetyl morphine and morphinan-6-ol,7,8 didehydro-4,5-epoxy-3-methoxy-17-methyl acetate (ester) were identified. RJINCE + - - 6 monoacetylmorphine,morphinan-6ol acetate RJNRSN + - - Sample 2016/2/SM-4 contained 25.7% Heroin. The test sample also contained acetylcodeine and 6 -monoacetylmorphine. RU8UQS + ANP ANP we have found results from swg-drug library, which the last version it, and we have studied for quantitative analysies with GC-FID. RVP7VW + ANP ANP

SIFXH3 + ANP - Sample 2016/2/SM-4 contains Heroin (Diamorphine). SMYNNU + + - The sample consist controlled drugs - Heroin SUUW3G + ANP - contained heroine and trace of acetylcodeine, 6-monoacetylmorphine, papaverine, noscapine SVGG03 + ANP - The sample contains 26.18 % heroin & also it contains 6-O-monoacetylmorphine , noscapine & papaverine . T2DI1R + ANP - The chemical test and the coincidence in the retention time and mass fragmentogram with the reference material in the same conditions that the analyzed sample, indicate the heroine presence. T4VMD2 + ANP ANP In colorimetric analysis purple color was observed for Froehde and Marquis reagent. GC/MS then identified Heroin to be found in the sample TI22ZK + ANP - x grams of brown powder containing 26% diamorphine. Class A

Code Heroin Lactose Morphine minor comp. TQFFPF + ANP ANP Analyses performed on Item # 4 revealed presence of Herione. TQMVZE + - - In the sample 4 we have faund Heroin. Heroin is on the list of the drug in Montenegro. TRVLKK + + - SM4 contains Heroin and Lactose; sample also contains Acetylcodeine, 6-Monoacetylmorphine, Papaverine and Noscapine TSSRQR + + -

TSW3IE + ANP - ANALYZED BEIGE POWDER CONTAINS HEROINE TZOONA + + - HEROIN, ACETILCODEINE, 6-MONOACETILMORPHINE, PAPAVERINE, NOSCAPINE, LACTOSE. BASE HEROIN 26,4+/-3,1 UFK6EF + + - The sample contains heroin and lactose. Heroine is sheduled as illicit drug. UG88A8 + ANP - LIGHT BROWN POWDER THAT CONTAINS DRUG HEROIN UJWYPY + + - lactose, AC-codiene, 6-MAM UMXXSY + + - Heroin, Papaverine, Noscapine, Acetylcodeine, 6-Monoacetylmorphine, Meconin -GCMS - compare massspectra with library; Lactose extraction by ethanol residue-FTIR, after evaporation to dryness under stream of Nitrogen - Heroin compare IR spectra with library. UUUOU9 + - -

UWBOLU + ANP - the light brown powder contains diacetylmorphine (23.2%ww) plus some traces of 6- monoacetylmorphine and acetylcodeine. These all are controlled by national law. UXVVAC + + + Presence of heroin hydrochloride and lactose was detected in the sample. The sample also contained acetylcodeine, 6-MAM, papaverine, noscapine and trace amount of meconine, morphine and acetylthebaol. UYFCCR + ANP - IN SAMPLE 2016/2/SM-1 HEROIN WAS FOUND. UYJBJJ + + - This sample is heroin. V011CO + + - The high quality of measurement results (99%) proves the presence of heroin in the sample. VBEY7Y + + - It is usually detected in our laboratory. VFC8CC + + -

VIFKAW + + - the sample contains heroin, 6-monoacetilmorphine, acetilcodeine and lactose. VPHJRP + + + The sample containing 56.1% of Heroine: 1.04% Morphine; also contain monoacetylcodeine and lactose VVIRG4 + + - Sample found to contain Heroin and lactose

Code Heroin Lactose Morphine minor comp. VVN4CQ + - - aceti-codeine, 6-MAM, noscapine W0HPES + + - heroin HCl WGZNNM + - -

WMTTV7 + + - The sample contains heroin and lactose. WQOZYA + ANP - 6-MAM, noscapine, acetylcodeine X0X444 + + - light brown powder containing heroine, others alkaloids - acetylcodeine, 6-monoacetylmorphine, meconine, papaverine, noscapine and lactose XEE66N + - - the sample is containing heroin and percentage of pure heroin in it is 29.1% XNNNU1 + ANP - Powder containing Heroin 28,2% Legal status: Illegal - Portuguese Drug law 15/93 XXFX8D + ANP - The sample found to contain Heroin YGQE84 + ANP ANP Marquis Reagent (MR) positive. GC/MS Retention time and mass charge (m/z) similar characteristics with the substances used as standard or pattern YLHIIH + - - 6 MONOACETYLMORPHINE, NOSCAPINE, PAPAVERINE , MORPHINE YQYLYY + ANP - Presence of heroin, 19.06 % concentration, with traces of 6-MAM, acetylcodeine, papaverine and noscapine Z2BIDB + - - On analysis, I found that the substances contain 25.5% w/w of heroin. Z8T8N1 + + ANP

ZCCQMZ + + + Heroin base and morphine traces in lactose powder ZQHUPQ + + - It has been detected the presence of heroin and subproducts of the acetalization of morphine in the sample ZWL0DM + + - SUGAR ZXGCGG + + ANP The sample correspond to a mixture of Heroin and Lactose

Identification methods for Test Sample 4

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

RESPONSE SUMMARY FOR TEST SAMPLE 4

Participants: 181

The response summary of all 181 participating laboratories for the identification off SM-4, frequency of use of screening and identification techniques and false positives and negatives:

Identificatiion of Test Sample-4:

Substance Name Number of laboratories correctly identiffying: Heroin 180 Lactose 67

False positives for Test Sample-4:

Round Code: Substance Name: Tech Code: UUUOU9 Nimetazepam 140/171

False negatives for Test Sample-4 (techniques(s) used for ANP):

Round Code: Substance Name: Tech Code: DMM5Z5 - 150/180

Frequency of use of screening, identification and quantification techniques:

Response Summary Participants 181 Technique 140 141 142 150 160 161 170 171 172 180 190 200 210 211 220 230 231 Screening (No.) 54 75 62 19 030407219 1 13 0 120 (%) 29.8 41.4 34.3 10.5 0.0 1.7 0.0 2.2 0.0 39.8 10.5 0.6 7.2 0.0 0.6 1.1 0.0 Identification (No.) 13 6 534512135116879 4 83074 (%)7.23.3 2.8 18.8 2.8 6.6 0.6 19.3 0.6 92.8 43.6 2.2 4.4 1.7 0.0 3.9 2.2 Quantification (No.) 0 0 008240760300013010 (%)0.00.0 0.0 0.0 6.2 18.6 0.0 58.9 0.0 23.3 0.0 0.0 0.8 2.3 0.0 0.8 0.0

Robust average = 25.9 % Round: 2016/2 UNODC value = 28.4 % Substance: SM‐4; Heroin

4.00

3.00 2.9 2.4 2.3 2.1

2.00 1.9 1.6 1.6 1.6 1.4 1.3 1.3 1.1 1.0 1.0 1.0 0.9 0.9 0.9

1.00 0.8 0.8 0.7 0.7 0.7 0.7 0.7 0.7 0.6 0.6 0.6 0.5 0.5 0.5 0.5 0.4 0.4 0.4 0.4 0.4 0.4 0.4 0.4 0.3 0.3 0.2 0.2 0.2 0.2 0.2 0.2 0.1 0.1 0.1 0.1 0.1 0.1 0.0 0.0 0.0 0.0 4.4 7.2 9.3 11.9 15.9 0.00 9.9 4.8 4.3 4.3 2 2 ‐ ‐ ‐ ‐ 0.1 0.1 0.1 0.1 ‐ ‐ ‐ ‐ 0.2 0.2 0. 0. ‐ 0.2 0.2 ‐ ‐ ‐ 0.2 ‐ ‐ 0.3 ‐ 0.3 ‐ 0.3 0.3 ‐ 0.4 0.4 0.4 ‐ ‐ 0.4 0.4 ‐ ‐ ‐ 0.4 0.4 ‐ ‐ ‐ ‐ 0.5 ‐ 0.6 0.6 0.6 0.6 ‐ ‐ ‐ ‐ 0.7 0.7 ‐ 0.7

‐1.00 ‐ ‐ 0.8 0.8 0.8 0.8 ‐ ‐ ‐ ‐ 0.9 ‐ 1.0 ‐ 1.0 1.1 1.1 ‐ ‐ ‐ 1.2 1.2 ‐ ‐ 1.3 ‐ 1.4 ‐

‐2.00 1.7 1.8 ‐ 1.8 ‐ 1.8 ‐ 1.9 ‐ 1.9 ‐ ‐ 2.0 2.0 ‐ ‐

‐3.00 2.7 ‐ 3.1 ‐ 3.3 ‐

‐4.00 0DM 7IUIII L 1JJBJS 8II46Y UYJBJJ TI22ZK HJLSL6 CRSEZI RJINCE CJWZIJ HF3FYI JCUITV RI3K33 8Z8ZZZ LLL1RB JEVX45 GJIRPN EHJ60F E66LY6 1ZKJHF 10B0XJ Z2BIDB EXZYYP JKG5E5 E5LDLX K3S33Y 4J4H44 IZLLW0 7JUSKK P0FZ8V 0LAKP0 YQYLYY LL8LML 211119 X0X444 55BR5Z LNUUEI A8YSK1 VVIRG4 IQYQE4 UFK6EF VBEY7Y VPHJRP VPHJRP Z8T8N1 40HFEP LQ8989 R7BBLB BARYZ2 IXUAHB RJNRSN XEE66N VFC8CC TSSRQR JSZ6XW CZGHZZ 8Q8VEF 2PUPPP OS838A 9Q999K KSQKKK CU6JGV FK5BHB CANEE8 G0B9NL 5ZDDX6 7666AG 2R20JW VIFKAW A5GR55 O4KFNX NZOTC6 IMVADS SVGG03 AEDDRS 8J4DWT CWEOYI DNNSKS GV2PGK E2OA5N C9CDOR IWA0AA 9994MR ZXGCGG UXVVAC HRYNGY 3PV3WL RU8UQS KK6WBZ 33DUO3 W0HPES GNUILW G2GBDV LVVWC7 KBUURH TZOONA 8MV6V6 GGA8CG ZCCQMZ TQMVZE DWRNDI XNNNU1 RVP7VW MOKSHS ZQHUPQ 1YQDGQ JM2GKM MDDETU GKHDEM UUUOU9 SMYNNU ZW ODOOO2 WQOZYA PHWNRB SUUW3G HEHCMO UWBOLU OO9QOO ARZMMQ WGZNNM MZMHCW MDQMM4 z‐scores can be interpreted by participants in line with ISO 13528:2005, secion 7.4.2 and ISO/IEC guide43‐1:1997(E) as follows: IzI < 2 = satisfactory 2 ≤ IzI ≤ 3 = questionable IzI > 3 = unsatisfactory Accordig 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 signal in two successive rounds shall be taken that an anomaly has occured that requires inverstigation.

97 Z‐Score Report per Sample per Substance

Round: 2016/2 Substance: SM‐4; Heroin

Dispersion of z-scores using different analytical techniques for the quantification of heroin in 2016/2 SM-4 10

0 z-score

-2

-4

-6

-8 HPLC GC‐FID GC‐MS/LC‐MS NMR -10

98 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Z-Scores for Test Sample 4

Heroin Heroin Deviation Code Concentration Deviation from Code Concentration z-score from robust z-score (mass%) robust average (mass%) average VPHJRP 1.04 -24.9 -9.9 Z2BIDB 25.5 -0.4 -0.2 FK5BHB 13.94 -12.0 -4.8 ZCCQMZ 25.5 -0.4 -0.2 VFC8CC 15 -10.9 -4.3 VBEY7Y 25.6 -0.3 -0.2 MZMHCW 15.1 -10.8 -4.3 IWA0AA 25.7 -0.2 -0.1 TQMVZE 17.64 -8.3 -3.3 RJNRSN 25.7 -0.2 -0.1 HF3FYI 18.2 -7.7 -3.1 JCUITV 25.8 -0.1 -0.1 YQYLYY 19.06 -6.8 -2.7 5ZDDX6 25.8 -0.1 -0.1 4J4H44 21 -4.9 -2.0 8J4DWT 26.0 0.1 0.0 LL8LML 21 -4.9 -2.0 ZQHUPQ 26.0 0.1 0.0 ODOOO2 21.14 -4.8 -1.9 VVIRG4 26.0 0.1 0.0 W0HPES 21.2 -4.7 -1.9 TI22ZK 26.0 0.1 0.0 RU8UQS 21.3 -4.6 -1.8 HJLSL6 26.1 0.2 0.1 GNUILW 21.4 -4.5 -1.8 SVGG03 26.2 0.3 0.1 1YQDGQ 21.5 -4.4 -1.8 1JJBJS 26.2 0.3 0.1 WQOZYA 21.6 -4.3 -1.7 K3S33Y 26.2 0.3 0.1 LLL1RB 22.4 -3.5 -1.4 AEDDRS 26.3 0.4 0.1 G0B9NL 22.6 -3.3 -1.3 A8YSK1 26.3 0.4 0.1 JSZ6XW 23 -2.9 -1.2 TZOONA 26.4 0.5 0.2 GV2PGK 23 -2.9 -1.2 8Z8ZZZ 26.4 0.5 0.2 UWBOLU 23.2 -2.7 -1.1 0LAKP0 26.4 0.5 0.2 IQYQE4 23.2 -2.7 -1.1 Z8T8N1 26.4 0.5 0.2 E2OA5N 23.3 -2.6 -1.0 JEVX45 26.5 0.6 0.2 C9CDOR 23.45 -2.5 -1.0 BARYZ2 26.5 0.6 0.2 G2GBDV 23.7 -2.2 -0.9 P0FZ8V 26.7 0.8 0.3 8MV6V6 23.9 -2.0 -0.8 GKHDEM 26.8 0.9 0.3 DWRNDI 24 -1.9 -0.8 O4KFNX 26.9 1.0 0.4 GGA8CG 24 -1.9 -0.8 EXZYYP 26.9 1.0 0.4 JM2GKM 24 -1.9 -0.8 KBUURH 27.0 1.1 0.4 ZXGCGG 24.16 -1.7 -0.7 8Q8VEF 27.0 1.1 0.4 PHWNRB 24.2 -1.7 -0.7 GJIRPN 27.0 1.1 0.4 VIFKAW 24.3 -1.6 -0.7 MOKSHS 27.0 1.1 0.4 UXVVAC 24.5 -1.4 -0.6 DNNSKS 27.0 1.1 0.4 R7BBLB 24.5 -1.4 -0.6 HRYNGY 27.0 1.1 0.4 55BR5Z 24.5 -1.4 -0.6 MDDETU 27.1 1.2 0.5 RVP7VW 24.51 -1.4 -0.6 9Q999K 27.1 1.2 0.5 JKG5E5 24.7 -1.2 -0.5 OO9QOO 27.1 1.2 0.5 2R20JW 24.86 -1.0 -0.4 3PV3WL 27.3 1.4 0.5 7IUIII 24.86 -1.0 -0.4 LNUUEI 27.4 1.5 0.6 E5LDLX 24.9 -1.0 -0.4 CJWZIJ 27.4 1.5 0.6 8II46Y 24.93 -1.0 -0.4 KSQKKK 27.6 1.7 0.6 WGZNNM 25 -0.9 -0.4 IMVADS 27.6 1.7 0.7 OS838A 25 -0.9 -0.4 KK6WBZ 27.6 1.7 0.7 IXUAHB 25 -0.9 -0.4 RJINCE 27.7 1.8 0.7 UYJBJJ 25.09 -0.8 -0.3 X0X444 27.7 1.8 0.7 EHJ60F 25.1 -0.8 -0.3 HEHCMO 27.8 1.9 0.7 40HFEP 25.13 -0.8 -0.3 2PUPPP 27.8 1.9 0.7 CU6JGV 25.24 -0.7 -0.3 UUUOU9 27.9 2.0 0.8 E66LY6 25.35 -0.5 -0.2 CANEE8 28.0 2.1 0.8 UFK6EF 25.4 -0.5 -0.2 TSSRQR 28.1 2.2 0.9 IZLLW0 25.4 -0.5 -0.2 XNNNU1 28.2 2.3 0.9 LQ8989 25.5 -0.4 -0.2 9994MR 28.3 2.4 0.9 99 2016/2-SM Copyright (c) 2017 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Z-Scores for Test Sample 4

Heroin Deviation Code Concentration from robust z-score (mass%) average NZOTC6 28.47 2.6 1.0 MDQMM4 28.49 2.6 1.0 ZWL0DM 28.5 2.6 1.0 A5GR55 28.75 2.9 1.1 LVVWC7 29.1 3.2 1.3 XEE66N 29.1 3.2 1.3 CRSEZI 29.5 3.6 1.4 211119 29.91 4.0 1.6 CZGHZZ 29.95 4.1 1.6 7JUSKK 30.02 4.1 1.6 33DUO3 30.8 4.9 1.9 SMYNNU 31.2 5.3 2.1 SUUW3G 31.7 5.8 2.3 ARZMMQ 32 6.1 2.4 RI3K33 33.34 7.4 2.9 7666AG 37 11.1 4.4 1ZKJHF 44 18.1 7.2 10B0XJ 49.35 23.5 9.3 VPHJRP 56.1 30.2 11.9 CWEOYI 65.98 40.1 15.9

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