INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report

INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP)

INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Summary Report

SEIZED MATERIALS 2017/1 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Table of contents Introduction Page 2 Comments from the International Panel of Forensic Experts Page 2 NPS reported by ICE participants Page 4 Codes and Abbreviations Page 6 Sample 1 Analysis Page 7 Identified substances Page 7 Statement of findings Page 12 Identification methods Page 23 Summary Page 29

Z- Scores Page 30 Sample 2 Analysis Page 33 Identified substances Page 33 Statement of findings Page 38 Identification methods Page 49 Summary Page 55

Z- Scores Page 56 Sample 3 Analysis Page 60 Identified substances Page 60 Statement of findings Page 66 Identification methods Page 77 Summary Page 83

Z- Scores Page 84 Sample 4 Analysis Page 88 Identified substances Page 88 Statement of findings Page 90 Identification methods Page 96 Summary Page 102 Test Samples Information

Samples Comments on samples Sample 1 SM-1 was prepared from a seizure containing 43.1 % (w/w) 3,4-methylenedioxypyrovalerone base. The test sample also contained lactose.

Sample 2 SM-2 was prepared from a seizure containing 23.7 % (w/w) Cocaine base. The test sample also contained lactose with methylecgonine, benzoylecgonine and cinnamoyl cocaine as minor components.

Sample 3 SM-3 was prepared from a seizure containing 55.7 % (w/w) MDMA. The test sample also contained lactose.

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

Samples Substances Concentrations Comments on substances Sample 1 3,4-Methylenedioxypyrovalerone 43.1 % Lactose 0 % Sample 2 Cocaine 23.7 % Lactose 0 % Sample 3 3,4-Methylenedioxymetamfetamine (MDMA) 55.7 % Lactose 0 % Sample 4 [blank sample]

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

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

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

Comments from the International Panel of Forensic Experts

Participation of Laboratories

In the 2017/1 round of the ICE programme, results were submitted within both the Seized Materials (SM) and Biological Specimens (BS) test groups by 238 laboratories in 76 countries. Within the SM test group, there were 204 participating laboratories from 71 countries and within the BS test group, results were submitted by 96 laboratories from 45 countries.

Qualitative Analysis

The analytical technique most commonly used for screening of test samples in the SM test group was the marquis reagent (42% of participants), while GC-MS (93%) was the most commonly used technique for identification/confirmation of the components in the test samples followed by FTIR (44%). The results for the qualitative identification of the controlled substances in the SM test group are shown in the table 1.

Table 1. Qualitative performance of participants in the 2017/1 round of ICE.

SM-1 SM-2 SM-3 SM-4 Test sample (MDPV) (Cocaine) (MDMA) (blank) Correct identification by 96% 99.5% 99% 99.5% participants Number of false 2 0 7 1 positives Number of false 3 1 1 - negatives Number of analysis not 6 0 0 0 performed

With regard to false negative results reported, there were a total of five (three for SM-1 and one each for SM-2 and SM-3). In total there were ten false positive results for substances in the ICE menu. The overall number of false positive/negative results reported by ICE participants is lower than in recent years and while this is encouraging,laboratories reporting false positive or false negative results should investigate the reasons for this andcorrective actions should be taken in order to continuously improve performance. There were only a totalof six analyses not performed, all of which were for SM-1 containing MDPV, (a new substance on the ICEmenu in the 2017/1round, which was placed under international control in 2015). ICE participants shouldnote that test samples can contain any of the substances in the ICE menu and screening and identificationcarried out should take this into account.

3 Quantitative Analysis

The proportion of participants who carried out quantitative analysis, 55 (27%) for SM-1, 144 (71%) for SM-2, and 122 (60%) for SM-3 continues to be encouraging, particularly the consistently high percentage of participants who quantifiy cocaine when present in test samples. It is also encouraging that 150 (74%) of participants in the SM test group performed quantitation and of these, 117 (78%) quantified more than one substance and 57 laboratories (38%) quantified the three test samples containing controlled substances. It is understood that quantitative analysis of controlled substances is often governed by local legislation and the requirements of prosecution. With regard to the analytical techniques used by participants performing quantitation, 52% used GC-FID, and 18% used either GC-MS or HPLC. z-scores obtained by participants in quantification are shown in table 2 below.

Table 2. Quantitative performance of participants in the 2017/1 round of ICE.

Test sample z-score SM-1 SM-2 SM-3 SM-4 (MDPV) (Cocaine) (MDMA) (Blank) |z| < 2, satisfactory 82% 82% 84% - 2 ≤ |z| ≤ 3, questionable 7% 8% 7% - |z| > 3, unsatisfactory 11% 10% 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 2016/2 round of ICE, twenty laboratories obtained questionable z-scores with 2 ≤ |z| < 3. Eighteen of these laboratories participated and performed quantification in the 2017/1 round with 15, (75%) improving their performance and obtaining acceptable z-scores with |z| < 2 for at least one substance. Three of these laboratories also obtained questionable z-scores and three laboratories also obtained unsatisfactory z- scores in 2017/1.

Twenty-three laboratories obtained unsatisfactory z-scores in ICE 2016/2 with |z| ≥ 3. Of these laboratories, twenty participated in ICE 2017/1 and performed quantification, with 18 (90%) improving their performance in at least one substance

The following laboratories obtained a single action signal or warning signal in the two successive rounds of 2016/2 and 20167/1 and shall take this as anomaly, which requires further investigation: CG1SCE, HXXSFV, YHAA5A, MQZPKC, IIIIXI, TTHTMU, EDCFFF, POEJXP, 1UUW16, HXXSFV, MQZPKC, POEJXP, G7772Y, A6YPWP, UFAT5C and 283GPP

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. 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 2017/1 round of the ICE programme.

During the 2017/1 round of ICE, participating laboratories provided information on NPS that had been identified in their laboratories. In total there were 148 reports of 93 substances. The most commonly reported substances were synthetic cathinones (36%) followed by synthetic cannabinoids (25%) as shown in figure 1.

5% 3% 25% 8% Synthetic cannabinoids

Synthetic cathinones

Others

Phenethylamines

Ketamine and phencyclidine type substances 23% Tryptamines

36%

Figure 1. NPS reported by ICE laboratories during the 2017/1round of ICE

In terms of the mode of action of the NPS reported by ICE participants, the predominant substances reported were stimulants (50%), while 16% were synthetic cannabinoid receptor agonists (SCRA’s) and 13% were synthetic opioids as shown in figure 2. 2% 8%

Stimulants

11% SCRA's

Opioids

Hallucinogens 50% Dissociatives 13% Sedatives/Hypnotics

16%

Figure 2. Mode of action of NPS most commonly reported by ICE participants in the 2017/1 round of ICE

NPS most commonly reported by laboratories participating in ICE 2017/1.

The substance most often reported by ICE participants was the synthetic cathinone ephylone (N- ethylpentylone) followed by the synthetic opioid U-47700 (3,4-dichloro-N-((1S,2S)-2- (dimethylamino)cyclohexyl)-N-methylbenzamide). This is the first time a synthetic opioid has been among the substances most reported by ICE participants. U-47700 was placed under International Control (Schedule I of the Single Convention on Narcotic Drugs of 1961) at the 2017 Meeting of the Commission on Narcotic Drugs. The decision became effective on 22 April 2017.

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. https://www.unodc.org/LSS/Home/BothAreas

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 0GK0Q0 3,4-Methylenedioxypyrovalerone and Lactose 0YYGT3 MDPV 100JU0 MDPV 1HAGZA FOUND 3,4-METHYLENEDIOXYPYROVALERONE (MDPV) 1S1T1G MDPV 1U0JGG 3,4-Methylenedioxypyrovalerone 1UUW16 MDPV 215ETZ 3,4-Methylenedioxypyrovalerone 283GPP MDPV (Methylenedioxypyrovalerone 2ACRDL 3,4METHYLENDIOXYPYROVALERONE 2B1A92 3,4-MDPV 2SI2CZ MDPV 2TYJEG MDPV 3AY738 MDPV 3OFVFV MDPV 3UI8PF 3,4-Methylenedioxypyrovalerone 3ZOPSC 3,4 MDPV 4FFKBN 3,4-Methylenedioxypyrovalerone (MDPV) 4PGMZO MDVP and Lactose 4WF099 MDPV 4X449Z Methylenedioxypyrovalerone(MDPV) 541LFZ MDPV hcl 58Y8FL MDPV 5A5855 3,4-MDPV 5G3N55 MDPV 5QMBSP MDPV 5QVQHW MDPV 5RTTW2 MDPV 5THFBN 3,4-Methylenedioxypyrovalerone 5X7UMS 3,4-Methylenedioxypyrovalerone 6A5NIA MDPV 6BUQUQ MDPV 7CW6XN MDPV 7MAM28 MDPV 88P8P5 Methyledioxypyrovalerone (MDPV) 8A4YUG 3,4-Methylenedioxypyrovalerone 8A5KSA MDPV 99U99A Methylenedioxypyrovalerone(MDPV) 99VFND 3,4-Methylenedioxypyrovalerone 9A8CUK 3,4-methylenedioxypyrovalerone

Code Identified Substances 9LR9YU Methylendioxypyrovalerone (MDPV) A3IH33 3,4Methylenedioxypyrovalerone A6YPWP MDPV AMECCZ MDPV AOGMWK 3,4-Methyedioxypyrovalerone AYJ22M MDPV HCl B6PUEJ 3,4-Methylenedioxypyrovalerone. BBXCFB 3,4-Methylenedioxypyrovalerone BFED5J 3,4-Methylenedioxypyrovalerone (MDPV) BJSGWA MDPV BMG4RM MDPV BPCSEV 3,4-Methylenedioxypyrovalerone BSN7V0 3,4-Methylenedioxypyrovalerone BSSEUS methylenedioxypyrovalerone(MDPV) BWALEI 3,4-methylenedioxypyrovalerone (MDPV) C9C8PA 3,4-Methylenedioxypyrovalerone CBC8TD MDPV CDDPDD MDPV CG1SCE MDPV CG43CR 3,4-Methylenedioxypyrovalerone CJ8TUV MDPV CSBOTS methylenedioxypyrovalerone (MDPV) DHIABX Methylenedioxipyrovalerone DINDT4 MDPV(3,4-Methylenedioxypyrovalerone ) DVAUDS MDPV E8EF88 3,4 methylenedixypyrovalerone (MDPV) EC0KNG MDPV EDCFFF 3,4-Methylenedioxypyrovalerone EEVV4K MDPV ELGLLX Methylenedioxyprovalone (MDPV) EWPSI1 3,4-Methylenedioxypyrovalerone EY4TQ0 3,4-MDPV F2RYW0 3,4-Methylenedioxypyrovalerone FCCEZJ MDPV FS5XU9 MDPV FVOURP coaine FZJOFH 3,4-Methylenedioxypyrovalerone G00C40 MDPV G7772Y 3,4-Methylenedioxypyrovalerone GDTQXP 3,4 MDPV GG0XXN 3,4-Methylenedioxypyrovalerone (MDPV) GTGG5G 3,4 MDPV HHHGBD Methyledioxypyrovalerone HHPRLM 3,4-Methylenedioxypyrovalerone

Code Identified Substances HWVVX1 MDPV HXXSFV Pyrovalerone IBADIN MDPV II3KTK 3,4-Methylenedioxypyrovalerone HCl IIIIXI MDPV IIORYA 3,4-methylenedioxypyrovalerone ILLLUA 3,4-MPDV IO2NIR MDPV IUAAMC 3,4-methylenedioxy pyrovalerone IUTURP 3,4-Methylenedioxypyrovalerone HCl IW9I29 MDPV J33P51 MDPV J7GZ5J MPDV J9A9TR MDPV JHT4NF MDPV JSZRBG MDPV JWJCVR 3,4- MDPV KFKKJK 3,4 Methylendioxypyrovalerone KNNBBF 3,4 Methylendioxypyrovalerone (MDPV) KORMOX MDPV L7MBHE MDPV L8TNQL Methylenedioxypyrovalerone LIGGG3 3,4-METHYLENEDIOXYPYROVALERONE, LACTOSE LJ1SES 3,4-Methylenedioxypyrovalerone (MDPV) LRNK4C MDPV MDJIDD unidentified MGUGGY Methylenedioxypyrovalerone (MDPV) MKKKKK 3,4-methylenedioxipirovalerone MQZPKC MDPV MXTSS3 MDPV MYMMDT MDPV N8QMXC MDPV(NPS) O0RMCH Methylenedioxypyrovalerone O5WQZI 3,4-Methylenedioxypyrovalerone OADJRA MDPV OBFIDR 3,4 MDPV ODVN18 MDPV OFRCFR MDPV(3,4-Methylenedioxypyrovalerone) OSZNWS 3,4-Methylenedioxypyrovalerone P0ADJ0 3,4-Methylenedioxypyrovalerone P3HHYE 3,4-Methylenedioxypyrovalerone P7LEGU No drugs P7PCPW 3,4-Methylenedioxypyrovalerone PBBITB MDPV

Code Identified Substances PKQQQQ 3,4 methylenedioxypyrovalerone(MDPV) POEJXP 3,4-Methylenedioxypyrovalerone (MDPV) PYTTET 3,4-Methylenedioxypyrovalerone (MDPV) Q4EE4E MDPV QGJYGY MDPV QI1JNX 3,4-Methylenedioxypyrovalerone QMZCMA Tramadol QOMHP5 3,4-methylenedioxypyrovalerone QRNQXH MDPV-Metilenedioxipirovalerona QXRKFZ MDPV R8T8AE 3,4-Methylenedioxypyrovalerone RHYD82 3,4-Methylenedioxypyrovalerone RNNNVK MDPV RPC9FU 3,4 Methylendioxypyrovalrone RPPFPC 3,4-Methylenedioxypyrovalerone RV66P1 MDPV RYB8ZA 3,4-Methylenedioxypyrovalerone S27VCS mpdv S97OK5 Methylenedioxipyrovalerone (MDPV) and Lactosa. SFHFBQ MPDV SGI5IO 3,4-Methylenedioxypyrovalerone SKSSPS 3,4-Methylenedioxypyrovalerone SKZHH0 Methyledioxypyrovalerone (MDPV) SSIHCS 3,4-Methylenedioxypyrovalerone SSSS3S MDPV SWSSOF MDPV TBUZWG Methylenedioxypyrovalerone (MDPV) TGCAAA Methyledioxypyrovalerone(MDPV) TTHTMU MDPV TTTTHT 3,4-MDPV TUVU7D Methylenedioxypyrovalerone (MDPV) UBTTQP 3,4-Methylenedioxypyrovalerone UDUUW5 MDPV (methylenedioxypyrovalerone) UDYUUU 3,4-Methylenedioxypyrovalerone UFAT5C 3,4-Methylenedioxypyrovalerone UHBHEQ MDPV UQYIVP 3,4-methylenedioxypyrovalerone(MDPV) UT2EIQ MDPV V3JVVY 3,4-Methylenedioxypyrovalerone V4QVVV 3,4-Methylenedioxypyrovalerone (MDPV) VGNZKV MDPV VTELFX MDPV HCL VVJVZV MPDV VVSOI6 Methylenedioxypyrovalerone

Code Identified Substances VVXRIZ 3,4-Methylenedioxypyrovalerone VYVVTU MDPV HCL W3O2KM 3,4-Methylenedioxypyrovalerone W7U77N 3,4-Methylenedioxypyrovalerone WAYGAS MDVP WDWUWW Methylenedioxypyrovalerone (MDPV) WTEPTR 3,4 MDPV WTVLQ8 3,4-Methylenedioxypyrovalerone XS2G6M MDPV XW94X4 MDPV XWBZZG MDPV XXYCLX not identified Y1FM12 3,4 MDPV YHAA5A 3,4Methylenedioxypyrovalerone MDPV YHNRNC MDPV ZDS0S1 MDPV - Methylenedioxypyrovalerone ZFBPKW Methylenedioxypyrovalerone (MDPV) ZIWYWS MDPV ZMVLHU 3,4-methylenedioxypyrovalerone ZNWNNS MDPV ZOSSZI methylenedioxypyrovalerone(MDPV) ZRVVPU MDPV ZWNZ3Z MPDV ZZVQGW MDPV

Statement of findings for Test Sample 1

Code 3,4- Methylenedioxypyr Lactose ovalerone 0GK0Q0 + + The sample 2017/1/SM-1 contains 3,4-Methylenedioxypyrovalerone and Lactose detected by GC/MS and FTIR. The percentage by weight of 3,4-Methylenedioxypyrovalerone is 44.8%. 0YYGT3 + -

100JU0 + ANP White powder that contains MDPV (methylenedioxypyrovalerone) that isn't under controlled substances. 1HAGZA + - 3,4-METHYLENEDIOXYPYROVALERONE (MDPV) IS LISTED IN THE THIRD SCHEDULE OF THE POISON ACT 1952. 1S1T1G + - The sample contains 3,4-methylenedioxypyrovalerone which is a cathinone. 1U0JGG + + Lactose 1UUW16 - + after analysis performed the sample contained MDPV +lactose 215ETZ + - The sample consist controlled drugs - 3,4-Methylenedioxypyrovalerone 283GPP + ANP On analysis of a representative sample of the powder methylenedioxypyrovalerone (MDPV) was detected. 2ACRDL + ANP

2B1A92 + - 3,4-MDPV confirmed by NMR structural analysis 2SI2CZ + + LACTOSE 2TYJEG + -

333HH3 ANP ANP

3AY738 + - The sample SM-1 contains MDPV, which is included in List F1 (List of narcotic substances banned in Brazil) of Annex I of SVS/MS 344, May 12, 1998. 3OFVFV + ANP That I examined and analysed the said sample and found it to contain: controlled substance(s) within the meaning of the Controlled Drugs and Substances Act: Schedule I 17 .1. Methylenedioxypyrovalerone (MDPV) 3UI8PF + + Lactose

Code 3,4- Methylenedioxypyr Lactose ovalerone 3ZOPSC + - Initially conducted a preliminary test to check in the presence of what kind of product we are. An intense blue reaction was found in the Incico And even came to wonder if the possibility of being a cocaine sample which came to contradict itself with the realization of other tests type TLC and FTIR. But later it did if a screening (TLC) where all the samples were prepared using as solvent the dichloromethane and how eluent methanol. A chromatographic Tina was used with the dimensions of 20cm × 20cm and the plate used for the purpose has the dimensions of 10cm × 20cm. In a 2 ml vial weighed 15 milligrams of the product and dissolved in 1.5 ml of the solvent (dichloromethane). With the help of a 5ȝl Micropipette, the specimens were placed on the chromatographic plate and left the same dry for a while. It placed about 80 ml of the solvent in Tina Chromatographic and left the same saturate for about 1 hour. Then the sample was placed in Tina Chromatographic with its lid and left the same elute about 25-30 minutes. At the end, the plate of Tina Chromatographic and left dry for 15 minutes. With the help of a chamber of UV a Ȝof 254 nn managed to visualize the stains on the plate and later do if the revelation of the plaque making use of the reagent of Dragendorf. In the sample 2017/1/SM1 was able to observe the presence of 3.4 Methyllenedioxypyrovalerone (3.4-MDPV). Subsequently, the equipment FTIR is 10 and is 50 in Transmitancia mode mixing the product with KBR and absorbance (ATR) and for sample 2017/1/SM1 was confirmed the presence of the 3.4 MDPV. 4FFKBN + + MDPV was identified by GCMS & quantified by GC analysis. 4PGMZO + + The Test sample 2017/1/SM-1 was analyzed by Thin Layer Chromatography technique and was found to contain MDVP and Lactose. 4WF099 + + Sample contained MDPV as hydrochloride and LACTOSE. Identification of MDPV by FTIR and GC/MS, quantification by GC/FID. Identification of LACTOSE by FTIR, HPLC/DIR and Colorimetric Reactions (Molish Test). 4X449Z + + 2017/1/SM-1 contains Methylenedioxypyrovalerone, a dangerous drug. It also contains Lactose. 541LFZ + + Base MDPV 43,81% (w/w) and Lactose 58Y8FL + ANP The powder contains MDPV. Methylenedioxypyrovalerone (MDPV) is a controlled drug under the Misuse of Drugs Act 1977 to 2016. This is because MDPV is structurally derived from 2-amino-1- phenyl-1-propanone by substitution in the phenyl ring with an alkylenedioxy group and by substitution at the 3-position of the propanone side-chain with an alkyl substituent and by inclusion of the nitrogen atom in a cyclic structure. (See paragraph 1A(b) of Schedule 1 to the Misuse of Drugs (Amendment) Act, 2015). 5A5855 + ANP 3,4-Methylenedioxypyrovalerone NPS 5G3N55 + ANP MDPV is controlled by law (Royal Decree 22/01/1998) 5QMBSP + - In the sample SM1 was identified MDPV by GC-MS.

5QVQHW + +

5RTTW2 + ANP MDPV is a Class B controlled drug subject to the provisions of the Misuse of Drugs Act 1971 - Amendment Order 2010 5THFBN + + 2017/1/SM-1contains drug (3,4-Methylenedioxypyrovalerone) and adulterant (lactose)

Code 3,4- Methylenedioxypyr Lactose ovalerone 5X7UMS + - analysis done by using GCMS 6A5NIA + ANP

6BUQUQ + ANP

7CW6XN + ANP MDPV was identified in the sample 2017/1/SM1. 7MAM28 + ANP De los análisis realizados se concluye que la sustancia se trata de metilendioxipirovalerona (MDPV) 88P8P5 + ANP LIST II OF THE CONVENTION ON PSYCHOTROPIC SUBSTANCES OF 1971 8A4YUG + - This substance was identified by colorimetric reaction, and using analytical techniques of Gas Chromatography / Mass Spectrometry and Fourier Transform Infrared Spectrometry. Quantification could not be performed due to the lack of methodologies 8A5KSA + + white powder containing 3,4-methylenedioxypyrovalerone and lactose 99U99A + - Using the techniques CR,TLC,GC-MS sample SM-1 was found to contain Methylenedioxypyrovalerone(MDPV). 99VFND + ANP

9A8CUK + ANP Sample 2017/1/SM-1 was found to contain 3,4-methylenedioxypyrovalerone (MDPV). Quantitative analysis was not carried out to determine the weight of the drug. 9LR9YU + + The tes sample also contained LACTOSE.

9T1OWI + - On analysis, i found that the substances contain 3,4-Metyhlenedioxypyrovalerone. A3IH33 + -

A6YPWP + ANP The sample contained 60.1% MDPV. AMECCZ + ANP Quantification not performed due to lack of analytical standard AOAPHK + +

AOGMWK + ANP The coincidence of the chemical test and the mass fragmentogram with the library compounds software , in the same conditions that the analysed sample, indicate the 3,4- Methyedioxypyrovalerone presence. AYJ22M + + The sample contain MDPV HCl (controlled substance) and lactose. B6PUEJ + ANP We did the respect tests and the substance identified was 3,4-Methylenedioxypyrovalerone.

Code 3,4- Methylenedioxypyr Lactose ovalerone BBXCFB + - The result of the tests of SM 1(35)received has confirmed that the mentioned simple contained 3,4- Methylenedioxypyrovalerone but we are not able to give a quantification result. BFED5J + + Presence of 3,4-Methylenedioxypyrovalerone hydrochloride and lactose was detected in the sample. BJSGWA + ANP

BMG4RM + +

BPCSEV + ANP The sample tested positive for MDPV, on screening and confirmation using GC-MS. The substance was not quantified as it is not included in the laboratory's validated procedure for drug quantification in seized materials. BSN7V0 + - Presence of MDPV BSSEUS + + MDPV existed in salt form. We also found lactose in the sample BWALEI + ANP The sample was found to contain 3,4-methylenedioxypyrovalerone (MDPV). C9C8PA + - the sample contains 3,4-MDPV CBC8TD + ANP The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule I 17.1 Methylenedioxypyrovalerone (MVPV) CDDPDD + ANP Lactose was also identified in trace amount. The analytical technique was GC-MS analysis of the silylated sample. CG1SCE + -

CG43CR + - SM-1 Contains 3,4-Methylenedioxypyrovalerone and lactose CJ8TUV + -

CSBOTS + ANP In the sample was found MDPV DHIABX + + Also it was detected lactose DINDT4 + + - QUANTITATIVE ANALYSIS CAN NOT BE OBTAINED WITHOUT STANDARD ARTICLE REFERENCE TO MDPV IN OUR LABORATORY - The sample contains Lactose. DVAUDS + + MDPPP, lactose E8EF88 + - Psychoactive drug with potent stimulating effects EC0KNG + ANP

EDCFFF + ANP 3,4-Methylenedioxypyrovalerone

Code 3,4- Methylenedioxypyr Lactose ovalerone EEVV4K + - Chlorhydrate ELGLLX + ANP The sample 2017/1/SM-1 was found to contain Methylenedioxyprovalone (MDPV). EWPSI1 + -

EY4TQ0 + + The sample contains 3,4-MDPV. 3,4-MDPV is sheduled as illicit drug.

F2RYW0 + ANP Retention time and fragmentation pattern obtained with sample are equivalent to those obtained with 3,4-Methylenedioxypyrovalerone. FCCEZJ + + The samples contains MDPV and lactose. MDPV is scheduled as illicit drug in France. FS5XU9 + ANP \\ FVOURP - - Analyse de l'échantillon révèle la présence de la cocaïne FZJOFH + ANP 3,4-Methylenedioxypyrovalerone G00C40 + + It contains MDPV (it is not quantified) and lactose G7772Y + ANP - GBKZCY ANP ANP RAS GDTQXP + ANP the sample was found to contain 3,4-Methylenedioxypyrovalerone GG0XXN + ANP It was detected the presence of 3,4-Methylenedioxypyrovalerone (MDPV) in the sample analysed. GTGG5G + - under control substance HHHGBD + ANP Methyledioxypyrovalerone was identified into material 2017/1/SM-1 by gas chromatography/mass spectrometry analysis. HHPRLM + ANP Lactose HWVVX1 + - MDPV HXXSFV + +

IBADIN + ANP THIS SAMPLE CONTAINS 3,4-MDPV CONFIRMED BY GC MS II3KTK + + A composite was formed from 1 unit for testing. 3,4-Methylenedioxypyrovalerone hydrochloride and lactose confirmed in the composite. IIIIXI + + MDPV is on the list of drugs

Code 3,4- Methylenedioxypyr Lactose ovalerone IIORYA + ANP

ILLLUA + + White powder containing MPDV and lactose IO2NIR + - We were able to identify the MDPV by comparing the mass spectrum obtained after injecting the SM1 sample to the GC/MS with that of our NIST08 database. This comparison gave us the pyrovalerone whose mass spectrum does not show the m/z 149 fragments and the molecular ion m/z 274 charasteristic of MDPV IUAAMC + + powder IUTURP + + 3,4-Methylenedioxypyrovalerone as base 46.36% and Lactose IW9I29 + ANP SM1 contained MDPV J33P51 + -

J7GZ5J + + White powder containing MPDV and lactose J9A9TR + ANP

JHT4NF + + SM1 contains 49% (w/w) MDPV base and lactose. JSZRBG + ANP Sample 2017/1/SM-1 a white powder gave a positive result for MDPV substance under national legislation on drugs JWJCVR + - NPS. Pyrovalerone ions sometimes interfere with ions of this substance. It is also difficult to differenciate it with 2,3-MDPV. compare. It was very helpful to have the standard provided by the UNODC. KFKKJK + - performed the physicochemical and instrumental analyzes it is concluded that sample number one contains 3.4 Methylendioxypyrovalerone KNNBBF + ANP In sample 2017/1/SM-1 was verified the presence of 3,4 Methylendioxypyrovalerone (MDPV) KORMOX + + The sample 1 containing MDPV and lactose. L7MBHE + - The sample contains MDPV (not quantified). L8TNQL + ANP White powder sample contains Methylenedioxypyrovalerone LIGGG3 + +

LJ1SES + - On analysis, I found the sample 'SM-1') containing 3,4-Methylenedioxypyrovalerone (MDPV). LRNK4C + ANP MDPV was detected by GC/MS but not quantified MDJIDD ANP ANP The sample was not completely analyzed.

Code 3,4- Methylenedioxypyr Lactose ovalerone MGUGGY + ANP The powder in this item was found to contain methylenedioxypyrovalerone (MDPV). MDPV is a Class B controlled substance under the provisions of the Misuse of Drugs Act 1971 (as amended). MKKKKK + ANP In the test sample 2017/1/SM-1 was detected 3,4-methylenedioxipirovalerone MQZPKC + + MDPV-LACTOSE MXTSS3 + -

MYMMDT + ANP

N8QMXC + - Sample 01 was found to contain Methyledioxypyrovalerone NRTTXK + ANP Based on the above analysis, the sample was found to contain methylenedioxypyrovalerone (MDPV). O0RMCH + ANP The sample contain illegal drug Methylenedioxypyrovalerone O5WQZI + + It has been detected the presence of 3,4-Methylenedioxypyrovalerone in the sample OADJRA + -

OBFIDR + ANP

ODVN18 + + Marquis reagent: negative result; Cobalt thiocyanate: negative result; GCMS: MDPV (compared with library MS spectrum of MDPV), FTIR: MDPV (compared to IR spectrum of MDVP), FTIR: lactose (spectrum of ethanol extract residue compared with IR spectrum of lactose); OFRCFR + + The substance contains MDPV (3,4-Methylenedioxypyrovalerone) and Lactose OSZNWS + +

P0ADJ0 + ANP Yellow colour with Zimmermann's test indicated the possible presence of MDPV. TLC and GC-MS results confirmed the presence of MDPV in SM-1. P3HHYE + ANP

P7LEGU + ANP From GCMSD analysis, the sample contained Methyledioxypyrovalerone (NPS) P7PCPW + + 49.9% 3,4-Methylenedioxypyrovalerone - The test sample also contained lactose PBBITB + ANP Controlled drug: MDPV Concentration: approx. 43 % PKQQQQ + - The sample correspond :3,4 methylenedioxypyrovalerone (MDPV) POEJXP + - MDPV was identified in SM1 and the percentage was 58.36.

Code 3,4- Methylenedioxypyr Lactose ovalerone PYTTET + ANP

Q4EE4E + + Se realizaron pruebas de color dando amarillo con el reactivo Marquis. Con el GC-MS se detectó MPDV QGJYGY + - SM 1 contains 3,4_Methylenedioxypyrovalerone. QI1JNX + ANP IN THE SAMPLE LABELED AS "2017/1/SM-1" WAS DETECTED 3,4-Methylenedioxypyrovalerone. QKD30L + - Sample was found to contain Methylenedioxypyrovalerone (MDPV) QMZCMA ANP ANP We did not have all the refrences drugs. According the TLC we found tramadol in the sample QOMHP5 + ANP

QRNQXH + + POSITIVA A MDPV Y LACTOSA QXRKFZ + ANP The sample SM-1 contains a drug 3,4-methylendioxypyrovalerone 41.8% R8T8AE + ANP The white powder was analysed and found to contain 3,4-Methylenedioxypyrovalerone (MDPV). RHYD82 + ANP The sample contains 3,4-Methylenedioxypyrovalerone. RNNNVK + + One glass bottle containing 0.23 grammes of a powder containing 0.10 grammes of 3,4- methylenedioxypyrovalerone, being a compound structurally derived from 2-amino-1-phenyl-1- propanone by substitution in the phenyl ring with an alkyenedioxy substituent and by substitution at the 3-position with an alkyl substituent and by inclusion of the nitrogen atom in a cyclic structure. RPC9FU + - Confirmed by GS/MS method, but the quantification analyses was not carried out because of not having relevant standard. substances RPPFPC + - Sample SM-1 was found to contain 3,4-Methylenedioxypyrovalerone. RV66P1 + ANP The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule I 17.1 Methylenedioxypyrovalerone (MDPV) RYB8ZA + + The sample contains 3,4-Methylenedioxypyrovalerone and lactose S27VCS + + -- S97OK5 + + Cobalt thiocyanate (CT) and Marquis reagent (MR) positive, CG/MS and mass charge ratio (M/Z) similar Characteristics with the substances used as standard or pattern. FTIR, absorption bands coincident with the substance used as standard. SFHFBQ + ANP

SGI5IO + + Sample also contain lactose. The presence of drug confirmed by GC-MS and FTIR spectroscopy analysis.The hydrochloride form of 3,4-Methylenedioxypyrovalerone was confirmed by the anion analysis and FTIR spectroscopy.

Code 3,4- Methylenedioxypyr Lactose ovalerone SKSSPS + ANP

SKZHH0 + + Sample 2017/1/SM-1 consists of white powder. Methyledioxypyrovalerone (MDPV), a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. SSIHCS + + lactose SSSS3S + ANP Item contained white powder, which was found to contain MDPV, a Class A drug. SWSSOF + ANP MASS SPECTRA TBUZWG + - The sample was found to contain Methylenedioxypyrovalerone (MDPV) TGCAAA + - We only used GCMS to detect MDVP.Rt2:21.521mins, Base peak:126. TTHTMU + ANP identified by GC-MS TTTTHT + - 47 % of 3,4-MDPV (free base) TUVU7D + - One brown glass vial with lid, labelled '2017/1/SM-1' and '15', which contained 228 milligrams of off- white powder. This powder contained methylenedioxypyrovalerone (MDPV). MDPV is a Class B controlled drug under the provisions of the Misuse of Drugs Act 1971 (as amended). UBTTQP + + 3,4-Methylenedioxypyrovalerone and lactose UDUUW5 + - Test sample 2017/1/SM-1 was confirmed to contain MDPV (methylenedioxypyrovalerone). MDPV is a DEA Schedule I controlled substance in the United States. UDYUUU + + LACTOSE.So we don't have standart of 3,4-Methylenedioxypyrovalerone we can't made quantative analys. UFAT5C + + contained 3,4-Methylenedioxypyrovalerone trace of artefact MDPV UHBHEQ + ANP The sample contains 44.1% MDPV as base UQYIVP + -

UT2EIQ + + LACTOSE V3JVVY + -

V4QVVV + ANP The sample contains 3,4-Methylenedioxypyrovalerone (MDPV). VGNZKV + + MDPV IN LACTOSE POWDER VTELFX + + LACTOSE

Code 3,4- Methylenedioxypyr Lactose ovalerone VVJVZV + ANP the White powder contains MPDV (45.1%w/w) which is controlled by national law VVSOI6 + - Examination of sample coded 2017/1/SM-1 revealed the presence of controlled drug methylenedioxypyrovalerone (MDPV) VVXRIZ + - Substance in Schedule II of Psychotropic Substances under International Control VYVVTU + + MDPV HCL, LACTOSA W3O2KM + + Item 2017/SM-1: a lumpy white powder which contained 3,4-Methylenedioxypyrovalerone (MDPV) and also indicated the presence of lactose. MDPV is a class B controlled drug under the provisions of the Misuse of Drugs Act 1971 (as amended). Lactose is not controlled under the provisions of the Misuse of Drugs Act 1971 (as amended). W7U77N + + 3,4-Methylenedioxypyrovalerone was identificated in the sample analyzed. WAYGAS + - Methylenedioxypyrovalerone (MDVP) detected within the sample submitted. WD6IRG ANP ANP

WDWUWW + + The substance is methylenedioxypyrovalerone (MDPV). WTEPTR + - We Found 3,4-Methylenedioxypyrovalerone. It is possible that it is the isomer 2,3 MDPV, since the technique does not allow to identify isomers. WTVLQ8 + + 3,4-Methylenedioxypyrovalerone +lactose XS2G6M + ANP white powder containing MDPV XW94X4 + ANP from screening test using (Marquis reagent(MR)) and ion scan, and from confirmation test using (Gc-Ms) the sample was found to contain the controlled drug (MDPV) XWBZZG + ANP MDVP was DETECTED in sample 2017/1/SM-1. XXYCLX - - we have found a peak but we can not identified it Y1FM12 + ANP We identified the sample by GC-MS, FTIR and we compared the results with the NIST library AND swgdrugs library. YHAA5A + + the sample is mixed with lactose YHNRNC + +

ZDS0S1 + - 231 milligrams of a white granular powder which was found to contain MDPV with a purity of 44% as base - Class B under the Misuse of Drugs Act 1971 (as amended) ZFBPKW + ANP Presence of MDPV was confirmed qualitatively. ZIWYWS + + ./.

Code 3,4- Methylenedioxypyr Lactose ovalerone ZMVLHU + ANP Sample 2017/1/SM-1 found to contain 3,4-methylenedioxypyrovalerone ZNWNNS + ANP The powder contains 46.4±2.3 % MDPV-base (by weight) ZOCUCZ ANP ANP

ZOSSZI + ANP Sample SM-1 found to contain methylenedioxypyrovalerone(MDPV) ZRVVPU + ANP

ZWNZ3Z + ANP White powder containing MPDV ZZVQGW + ANP

Identification methods for Test Sample 1

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

Analytical Technique Codes Code 140 141 142 150 160 161 171 172 180 190 200 211 220 230 231 210 0GK0Q0 I SI SI I 0YYGT3 I SI 100JU0 S S SI SI 1HAGZA S S SI 1S1T1G SI I 1U0JGG I SI I 1UUW16 S S I I 215ETZ I SI 283GPP S S S I I 2ACRDL S S I 2B1A92 SI I SI Raman 2SI2CZ I I I I SI I 2TYJEG S S S I I 333HH3 SI 3AY738 I SI I 3OFVFV SI I I GC-FTIR 3UI8PF SI SI I 3ZOPSC S S I I 4FFKBN S S S I I 4PGMZO S S SI S Fast Blue B Salt Test 4WF099 I SI I HPLC/DIR 4X449Z S S S I I GCMS/MS 541LFZ S S S I I I SI Duquenoise 58Y8FL I 5A5855 S S I I 5G3N55 I S 5QMBSP I 5QVQHW SI 5RTTW2 S S I 5THFBN S S I SI S microscopic examination 5X7UMS S S SI 6A5NIA SI 6BUQUQ I SI SI 7CW6XN S S I I S Tanred

Code 140 141 142 150 160 161 171 172 180 190 200 211 220 230 231 210 7MAM28 SI S I SI I Raman 88P8P5 I SI 8A4YUG S S S I I 8A5KSA SI I 99U99A S S S I I 99VFND S S S SI I SI 9A8CUK S I 9LR9YU S I I I 9T1OWI S S I I FTIR A3IH33 S I I A6YPWP I SI AMECCZ I I I AOAPHK I I SI I AOGMWK S S S I S Stereomicroscopic observation AYJ22M SI I SI B6PUEJ S S I S TANRED BBXCFB S S S I I BFED5J S I I I BJSGWA S S S I I BMG4RM S S SI SI I BPCSEV SI BSN7V0 S I I I BSSEUS S I I BWALEI SI I C9C8PA S S S I I CBC8TD I S I I CDDPDD S I SI I CG1SCE SI CG43CR S I I CJ8TUV SI CSBOTS S I I S Simon´s DHIABX S S S I I S Simon Reagent DINDT4 I S I SI I DVAUDS I SI I E8EF88 S S S I I EC0KNG SI S S I EDCFFF SI I EEVV4K SI SI ELGLLX S S S I

Code 140 141 142 150 160 161 171 172 180 190 200 211 220 230 231 210 EWPSI1 I I I SI I EY4TQ0 I SI I F2RYW0 S S S I FCCEZJ I I I FS5XU9 I S FVOURP S I FZJOFH SI G00C40 I G7772Y SI GBKZCY I I I I SI rapid test GDTQXP SI S S I I GG0XXN S S S I I GTGG5G SI I HHHGBD S I HHPRLM S I SI SI HWVVX1 SI SI SI SI I I SI HXXSFV SI IBADIN SI I II3KTK I SI I I IIIIXI S I I I IIORYA S I I ILLLUA I SI IO2NIR S I IUAAMC SI I IUTURP S S I I I IW9I29 S S I J33P51 SI J7GZ5J I SI I J9A9TR I S JHT4NF I I JSZRBG S S S I I JWJCVR S I I KFKKJK S I I KNNBBF SI S S SI I KORMOX S I I I I HPLC-R.I.D L7MBHE S S S I I L8TNQL SI SI I LIGGG3 SI SI I LJ1SES S I

Code 140 141 142 150 160 161 171 172 180 190 200 211 220 230 231 210 LRNK4C SI MDJIDD I SI MGUGGY S S I MKKKKK I MQZPKC S S S I I MXTSS3 S I MYMMDT SI I N8QMXC I I SI SI NRTTXK S I O0RMCH SI ASAP-TOF O5WQZI I S I OADJRA S I I OBFIDR S S I ODVN18 S S S SI I OFRCFR I S I I OSZNWS S S S SI I P0ADJ0 S S SI I I Mayer's Reagent P3HHYE I SI P7LEGU S I P7PCPW S S S I PBBITB SI I GC-IRD PKQQQQ SI I POEJXP S S I I I S fast blue salt test PYTTET SI Q4EE4E S S S I I QGJYGY S I SI I SI QI1JNX S S I QKD30L S S I I S Duquenois Levine Test (DLT) QMZCMA SI QOMHP5 SI QRNQXH SI I S S BENEDICT QXRKFZ S S S I I S R8T8AE S I I RHYD82 SI RNNNVK S S SI I RPC9FU SI RPPFPC SI RV66P1 S I I I GC-FTIR RYB8ZA SI I

Code 140 141 142 150 160 161 171 172 180 190 200 211 220 230 231 210 S27VCS I SI I S97OK5 S S S I I SFHFBQ SI SGI5IO S I I SKSSPS SI SKZHH0 S S I I SSIHCS SI I SSSS3S S S I I SWSSOF S S S I TBUZWG S S I I TGCAAA S S S I I TTHTMU S S I I I I TTTTHT SI I TUVU7D S S I I UBTTQP S I UDUUW5 S S S I UDYUUU I SI UFAT5C S I I UHBHEQ S S I S dugenois UQYIVP S I I UT2EIQ SI I V3JVVY S S I SI V4QVVV SI S S I I I VGNZKV SI I VTELFX SI VVJVZV I SI VVSOI6 SI I VVXRIZ S I I VYVVTU S S S I I I I W3O2KM S S SI SI W7U77N I SI I WAYGAS SI S S I I WD6IRG S S S I I WDWUW S I I I W WTEPTR S S I I WTVLQ8 SI I XS2G6M S I I SI XW94X4 S S I S Negms test XWBZZG SI SI I

Code 140 141 142 150 160 161 171 172 180 190 200 211 220 230 231 210 XXYCLX SI I I I Y1FM12 S SI I YHAA5A S S I I I I I YHNRNC SI I ZDS0S1 S S S I I ZFBPKW S SI I ZIWYWS I SI SI ZMVLHU S I ZNWNNS S I SI I ZOCUCZ S S S I ZOSSZI S I SI ZRVVPU S S S I I I ZWNZ3Z I SI ZZVQGW SI SI I

RESPONSE SUMMARY FOR TEST SAMPLE 1

Participants: 204

The response summary of all 204 participating laboratories for the identification of SM-1, frequency of use of screening and identification techniques and false positives and negatives:

Correct identification of Test Sample:

Substance Name Number of laboratories: 3,4-methylenedixypyrovalerone 195 Lactose 64

False positives for Test Sample-1:

Round Code: Substance reported: Tech Code: 1UUW16 Metamfetamine 180/160 FVOURP Cocaine 150

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

Round Code: Tech Code: FVOURP 150 XXYCLX 140/171 1UUW16 180 MDJIDD ANP QMZCMA ANP ZOCUCZ ANP 333HH3 ANP WD6IRG ANP GBKZCY ANP

Frequency of use of screening, identification and quantification techniques:

Response Summary Participants 204 Technique 140 141 142 150 160 161 170 171 172 180 190 200 210 211 220 230 231 Screening (No.) 74 85 68 19 0 3 0 5 0 75 22 1 15 1 1 1 0 (%) 36.3 41.7 33.3 9.3 0.0 1.5 0.0 2.5 0.0 36.8 10.8 0.5 7.4 0.5 0.5 0.5 0.0 Identification (No.) 19 7 4 43 6 12 0 31 2 190 90 3 13 5 0 5 6 (%) 9.3 3.4 2.0 21.1 2.9 5.9 0.0 15.2 1.0 93.1 44.1 1.5 6.4 2.5 0.0 2.5 2.9 Quantification (No.) 0 0 0 0 10 30 1 85 0 29 0 0 0 4 0 1 3 (%) 0.0 0.0 0.0 0.0 6.1 18.4 0.6 52.1 0.0 17.8 0.0 0.0 0.0 2.5 0.0 0.6 1.8

MDPV MDPV Deviation Code Concentration Deviation from Code Concentration z-score from robust z-score (mass%) robust average (mass%) average UQYIVP 30.4 -14.9 -4.8 WDWUWW 45.0 -0.3 -0.1 OSZNWS 39.7 -5.6 -1.8 5QVQHW 45.0 -0.3 -0.1 215ETZ 40.2 -5.1 -1.6 G7772Y 45.0 -0.3 -0.1 UFAT5C 40.6 -4.7 -1.5 VVJVZV 45.1 -0.2 -0.1 1UUW16 41.2 -4.1 -1.3 RYB8ZA 45.7 0.4 0.1 QXRKFZ 41.8 -3.5 -1.1 4WF099 46.1 0.8 0.3 BMG4RM 41.9 -3.4 -1.1 IUTURP 46.4 1.1 0.3 DVAUDS 42.1 -3.3 -1.1 ZNWNNS 46.4 1.1 0.3 SSIHCS 42.6 -2.7 -0.9 O5WQZI 46.7 1.4 0.4 II3KTK 43.0 -2.3 -0.7 MQZPKC 47.0 1.7 0.5 IUAAMC 43.0 -2.3 -0.7 BFED5J 47.0 1.7 0.5 9LR9YU 43.1 -2.2 -0.7 TTTTHT 47.0 1.7 0.5 PBBITB 43.3 -2.0 -0.7 2B1A92 47.3 2.0 0.6 88P8P5 43.3 -2.0 -0.7 HWVVX1 47.7 2.4 0.8 6A5NIA 43.3 -2.0 -0.7 2TYJEG 48.5 3.2 1.0 BSSEUS 43.7 -1.6 -0.5 YHAA5A 49.0 3.7 1.2 541LFZ 43.8 -1.5 -0.5 JHT4NF 49.0 3.7 1.2 3AY738 43.9 -1.4 -0.4 P7PCPW 49.9 4.6 1.5 JWJCVR 44.0 -1.3 -0.4 N8QMXC 52.5 7.2 2.3 2SI2CZ 44.0 -1.3 -0.4 SKSSPS 52.6 7.3 2.3 ZDS0S1 44.0 -1.3 -0.4 EDCFFF 52.6 7.3 2.3 UHBHEQ 44.1 -1.2 -0.4 W7U77N 52.9 7.6 2.4 RNNNVK 44.2 -1.1 -0.4 POEJXP 58.4 13.1 4.2 EC0KNG 44.6 -0.7 -0.2 OADJRA 58.5 13.2 4.2 ZZVQGW 44.6 -0.7 -0.2 A6YPWP 60.1 14.8 4.7 0GK0Q0 44.8 -0.5 -0.2 CG1SCE 72.2 26.9 8.6 4FFKBN 44.9 -0.4 -0.2 HXXSFV 78.6 33.3 10.7 AYJ22M 45.0 -0.3 -0.1

Round: 2017/1 Robust average = 45.3 % Substance: SM-1; MDPV UNODC value = 43.1 % 4.0

3.0 2.4 2.3 2.3 2.3

2.0 1.5 1.2 1.2 1.0 1.0 0.8 0.6 0.5 0.5 0.5 0.4 0.3 0.3 0.3 0.1 4.2 4.2 4.7 8.6 10.7 0.0 4.8 - 0.1 0.1 0.1 0.1 0.1 - 0.2 - - 0.2 - - - - 0.2 0.2 - - 0.4 0.4 - .5 0.4 0.4 0.4 0.4 - - - 0.5 - - 0 - - 0.7 0.7 0.7

-1.0 - - - 0.7 0.7 0.7 - - - 0.9 - 1.1 1.1 - 1.1 - - 1.3 - 1.5 - 1.6

-2.0 - 1.8 -

-3.0

-4.0 M FZ TZ CS TK 16 5C DS MC II3K 2SI2CZ SSIH PBBITB 541LFZ SKSSPS BFED5J 2TYJEG 215E ZDS0S1 EDCFFF POEJXP BSSEUS JHT4NF 88P8P5 6A5NIA VVJVZV TTTTHT 3AY738 IUTURP 9LR9YU UQYIVP 4FFKBN G7772Y RYB8ZA HXXSFV JWJCVR 2B1A92 CG1SCE QXRK UFAT AYJ22M OADJRA EC0KNG 0GK0Q0 YHAA5A 4WF099 IUAA O5WQZI DVAU P7PCPW A6YPWP RNNNVK MQZPKC OSZNWS UHBHEQ HWVVX1 1UUW ZZVQGW W7U77N N8QMXC ZNWNNS BMG4R 5QVQHW WDWUWW

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.

Round: 2017/1 Substance: SM-1; MDPV

Dispersion of z-scores using different analytical techniques for the quantification of MDPV in 2017/1 SM-1 10.0

8.0

6.0

4.0

2.0 re 0.0 sco - z

-2.0

-4.0

-6.0 HPLC GC-FID GC-MS NMR -8.0

-10.0

Sample 2 Analysis

Identified substances for Test Sample 2

Code Identified Substances 0GK0Q0 Cocaine and Lactose 0YYGT3 cocaine 100JU0 COCAINE 1HAGZA FOUND COCAINE 1S1T1G Cocaïne 1U0JGG Cocaine 1UUW16 cocaine 215ETZ Cocaine 283GPP Cocaine 2ACRDL COCAINE 2B1A92 Cocaine 2SI2CZ &2&$ø1( 2TYJEG cocaine 333HH3 Cocaine 3AY738 Cocaine 3OFVFV Cocaine 3UI8PF Cocaine 3ZOPSC COCAINE HCl and LACTOSE 4FFKBN Cocaine 4PGMZO Cocaine and Lactose 4WF099 COCAINE 4X449Z Cocaine 541LFZ cocaine hcl 58Y8FL Cocaine 5A5855 Cocaine 5G3N55 cocaine 5QMBSP Cocaine 5QVQHW cocaine 5RTTW2 Cocaine 25.2% purity 5THFBN Cocaine 5X7UMS Cocaine 6A5NIA Cocaine 6BUQUQ cocaine 7CW6XN Cocaine 7MAM28 Cocaine 88P8P5 COCAINE 8A4YUG COCAINE 8A5KSA cocaine 99U99A Cocaine 99VFND COCAINE 25.0%

Code Identified Substances 9A8CUK cocaine 9LR9YU Cocaine 9T1OWI Cocaine A3IH33 Cocaine A6YPWP Cocaine AMECCZ Cocaine AOGMWK Cocaine AYJ22M cocaine HCl B6PUEJ cocaine BBXCFB cocaine BFED5J Cocaine BJSGWA COCAIN BMG4RM Cocaine BPCSEV Cocaine BSN7V0 cocaine BSSEUS Cocaine BWALEI cocaine C9C8PA COCAINE CBC8TD Cocaine CDDPDD cocaine CG1SCE cocaine CG43CR Cocaine CJ8TUV COCAINE CSBOTS Cocaine DHIABX Cocaine DINDT4 &2&$ø1( DVAUDS Cocaine E8EF88 Cocaine EC0KNG cocaina EDCFFF Cocaine EEVV4K Cocaine ELGLLX Cocaine EWPSI1 Cocaine EY4TQ0 Cocaïne HCl F2RYW0 cocaine FCCEZJ cocaine FS5XU9 COCAINE FVOURP coaine FZJOFH cocaine G00C40 Cocaine G7772Y Cocaine GBKZCY cocaïne GDTQXP cocaine

Code Identified Substances GG0XXN Cocaine and minor components as cinnamoyl cocaine, methylecgonine esther and anydromethylecgonine esther GTGG5G Cocaine HHHGBD Cocaine HHPRLM cocaine HWVVX1 cocaine HXXSFV COCAINE IBADIN COCAINE II3KTK Cocaine HCl IIIIXI Cocaine IIORYA Cocaine ILLLUA cocaine IO2NIR Cocaine, Cinnamoylcocaine, Benzoylecgonine IUAAMC cocaine IUTURP Cocaine HCl IW9I29 Cocaine J33P51 Cocaine J7GZ5J cocaine J9A9TR Cocaine JHT4NF cocaine JSZRBG COCAINE JWJCVR Cocaine KFKKJK cocaine and lactose KNNBBF Cocaine KORMOX Cocaine L7MBHE Cocaine L8TNQL Cocaine LIGGG3 COCAINE, LACTOSE LJ1SES Cocaine LRNK4C cocaine MDJIDD Cocaine MGUGGY Cocaine MKKKKK cocaine MQZPKC COCAINE MXTSS3 COCAINE MYMMDT Cocaine N8QMXC Cocaine NRTTXK Cocaine O0RMCH Cocaine O5WQZI Cocaine HCl OADJRA COCAINE OBFIDR COCAINA ODVN18 Cocaine OFRCFR Cocaine

Code Identified Substances OSZNWS Cocaine P0ADJ0 Cocaine P3HHYE cocaine P7LEGU Cocaine P7PCPW cocaine PBBITB Cocaine PKQQQQ COCAINE HCL POEJXP Cocaine PYTTET cocaine; ecgonine methyl ester; anhydroecgonine methyl ester Q4EE4E Cocaína QGJYGY Cocaine QI1JNX Cocaine QKD30L Cocaine QMZCMA Cocaine QOMHP5 cocaine QRNQXH COCAINA CLORHIDRATO QXRKFZ Cocaine R8T8AE Cocaine RHYD82 Cocaine RNNNVK cocaine RPC9FU Cocaine RPPFPC Cocaine RV66P1 Cocaine RYB8ZA Cocaine S27VCS cocaine S97OK5 Cocaine and Lactose SFHFBQ cocaine SGI5IO cocaine hydrochloride SKSSPS Cocaine SKZHH0 Cocaine SSIHCS Cocaine SSSS3S COCAINE SWSSOF COCAINE TBUZWG Cocaine TGCAAA Cocaine TTHTMU cocaine (hydrochloride) TTTTHT Cocaine TUVU7D Cocaine hydrochloride UBTTQP Cocaine UDUUW5 Cocaine UDYUUU cocaine UFAT5C Cocaine UHBHEQ Cocaine UQYIVP Cocaine

Code Identified Substances UT2EIQ COCAIN V3JVVY cocaine V4QVVV Cocaine VGNZKV COCAINE VTELFX COCAIN HCL VVJVZV cocaine VVSOI6 Cocaine VVXRIZ Cocaine VYVVTU COCAINA HCL W3O2KM Cocaine Hydrochloride W7U77N Cocaine WAYGAS Cocaine WD6IRG Cocaine WDWUWW cocaine WTEPTR COCAINE WTVLQ8 cocaine XS2G6M COCAINE XW94X4 cocaine XWBZZG Cocaine XXYCLX cocaine Y1FM12 cocaine, lactose YHAA5A cocaine YHNRNC cocaine ZDS0S1 Cocaine Hydrochloride ZFBPKW Cocaine ZIWYWS Cocaine ZMVLHU Cocaine ZNWNNS cocaine ZOCUCZ cocaine ZOSSZI cocaine ZRVVPU cocaine ZWNZ3Z cocaine ZZVQGW cocaïne

Statement of findings for Test Sample 2

Code Cocaine Lactose 0GK0Q0 + + The sample 2017/1/SM-1 contains Cocaine and Lactose detected by GC/MS and FTIR. The percentage by weight of Cocaine is 28.2%. 0YYGT3 + - cocaine: 23.3%w/w 100JU0 + ANP Fine white powder that contains drug Cocaine. 1HAGZA + - COCAINE IS LISTED IN THE THIRD SCHEDULE OF THE DANGEROUS DRUGS ACT 1952. 1S1T1G + + The sample contains cocaïne 1U0JGG + + Lactose 1UUW16 - + after analysis performed the sample contained COCAINE + lactose 215ETZ + - The sample consist controlled drugs - Cocaine 283GPP + ANP On analysis of a representative sample of the powder cocaine was detected with a purity of approximately 29% calculated with reference to the base. 2ACRDL + ANP

2B1A92 + + Cocaine in mixture with mono- and disaccharides; lactose identified by Raman 2SI2CZ + + LACTOSE 2TYJEG + +

333HH3 + ANP

3AY738 + + The sample SM-2 contains Cocaine, which is included in List F1 (List of narcotic substances banned in Brazil) of Annex I of SVS/MS 344, May 12, 1998. 3OFVFV + ANP That I examined and analysed the said sample and found it to contain: controlled substance(s) within the meaning of the Controlled Drugs and 1 Substances Act: Schedule I 2. (2) Cocaine (benzoylmethylecgonine) 3UI8PF + + Ecgonine, Ecgonine methyl ester, trans-cinnamoylcocaine, benzoylecgonine, Lactose

Code Cocaine Lactose 3ZOPSC + + Initially conducted a preliminary test to check in the presence of what kind of product we are. An intense coloration was obtained using the test of Scott (Thiocyanate of cobalt) which came to confirm itself but later with the realization of other tests type TLC and FTIR. But later it did if a screening (TLC) where all the samples were prepared using as solvent the dichloromethane and how eluent methanol. A chromatographic Tina was used with the dimensions of 20cm × 20cm and the plate used for the purpose has the dimensions of 10cm × 20cm. In a 2 ml vial weighed 15 milligrams of the product and dissolved in 1.5 ml of the solvent (dichloromethane). With the help of a 5ȝl Micropipette, the specimens were placed on the chromatographic plate and left the same dry for a while. It placed about 80 ml of the solvent in Tina Chromatographic and left the same saturate for about 1 hour. Then the sample was placed in Tina Chromatographic with its lid and left the same elute about 25-30 minutes. At the end, the plate of Tina Chromatographic and left dry for 15 minutes. With the help of a chamber of UV a Ȝof 254 nn managed to visualize the stains on the plate and later do if the revelation of the plaque making use of the reagent of Dragendorf. In the sample 2017/1/SM2 was able to observe the presence of COCAÍNE. Subsequently, the equipment FTIR is 10 and is 50 in Transmitancia mode mixing the product with KBR and absorbance (ATR) and for sample 2017/1/SM2 was confirmed the presence of the COCAÍNE AND LACTOSE. 4FFKBN + + Cocaine was identified by GCMS & quantified by GC analysis. 4PGMZO + + The Test sample 2017/1/SM-2 was analyzed by Colour Test and Thin Layer Chromatography technique and was found to contain Cocaine and Lactose. 4WF099 + + Sample contained COCAINE as hydrochloride, LACTOSE, and small amounts of CIS and TRANS CINNAMOYLCOCAINE. Identification of COCAINE by FTIR and GC/MS, quantification by GC/FID. Identification of LACTOSE by FTIR, HPLC/DIR and Colorimetric Reactions (Molish Test). 4X449Z + + 2017/1/SM-2 contains Cocaine, a dangerous drug. It also contains Ecgonine Methyl Ester, cinnamoylcocaine isomers, Benzoylcocaine, and Lactose. 541LFZ + + Base Cocaine 24,19 +/- 2,8 % (w/w) and Lactose 58Y8FL + ANP The powder contains cocaine. Cocaine is a controlled drug under the Misuse of Drugs Acts, 1977 to 2016. The cocaine in this case is not exempt from control under subsection (1) of Section 3 of the Misuse of Drugs Act, 1977 under the terms of the Misuse of Drugs (Exemption) Order, 1988. The Exemption Order does not provide for an exemption in respect of Section 15 of the Misuse of Drugs Act, 1977. 5A5855 + ANP Cocaine 5G3N55 + ANP cocaine is controlled by law (Royal Decree 31/12/1930 changed by Royal Decree 8/10/1963) 5QMBSP + - In the sample SM2 was identified cocaine by GC-MS.

5QVQHW + +

5RTTW2 + ANP Cocaine is a Class A drug subject to the provisions of the Misuse of Drugs Act 1971 5THFBN + + 2017/1/SM-2 contains drug (cocaine) and adulterant (lactose) 5X7UMS + - analysis done by using GCMS 6A5NIA + ANP methylecgonine, cinnamoil cocaine

Code Cocaine Lactose 6BUQUQ + ANP

7CW6XN + ANP In the sample 2017/1/SM2 was detected the presence of cocaine as base in percentage by weight of 23.5 %. 7MAM28 + + De los análisis realizados se concluye que la sustancia se trata de cocaína. Se identifica adicionalmente lactosa. 88P8P5 + ANP LIST I OF SINGLE CONVENTION ON NARCOTICS DRUGS 1961 8A4YUG + - This substance was identified by Cobalt Thiocyanate test, and using analytical techniques of Gas Chromatography / Mass Spectrometry and Fourier Transform Infrared Spectrometry. And we obtained a quantification of 20.58% using HPLC-DAD techniques 8A5KSA + + white powder containing cocaine and lactose 99U99A + - 1.Using the techniques CR,TLC,GC-MS, FT-IR sample SM-2 was found to contain Cocaine. 2.Using technique GC-FID,quantification of SM-2 was done and found to contain Cocaine 3.0%. 99VFND + ANP

9A8CUK + ANP Sample 2017/1/SM-2 was found to contain cocaine. Quantitative analysis was not carried out to determine the weight of the drug. 9LR9YU + + The tes sample also contained LACTOSE, methylecgonine and cinnamoyl cocaine isomers (cis and trans) 9T1OWI + + On analysis, i found that the substances contain 23.1% w/w cocaine (base). A3IH33 + + The sample contains cocaine + lactose A6YPWP + ANP The sample contained 25.1% cocaine. Benzoyloecgonine and cinnamoyl cocaine were also detected as minor component. AMECCZ + ANP

AOAPHK + +

AOGMWK + ANP The chemical test and the coincidence in the retention time and mass fragmentogram with the reference material in the same conditions that the analysed sample, indicate the cocaine presence. AYJ22M + + The sample contain cocaine HCl (controlled substance) and lactose. B6PUEJ + ANP We did the respect tests and the substance identified was cocaine. BBXCFB + - The result of the tests of SM 1(35)received has confirmed that the mentioned simple contained cocaine with 21.7 percentage by weight

Code Cocaine Lactose BFED5J + + Presence of cocaine hydrochloride and lactose was detected in the sample. The sample also contaned multitude of trace level alkaloid impurities:(cis/trans)cinnamoylcocaine, norcocaine, benzoylecgonine, methylecgonine, ecgonine. BJSGWA + ANP

BMG4RM + +

BPCSEV + ANP The sample tested positive for Cocaine, on screening. Cocaine was confirmed and quantified. The percentage of cocaine by mass was 28%. BSN7V0 + + presence of cocaine with norcocaine,cynnamoylcocaine,ecgonine methyl ester cutted by lactose. BSSEUS + + Cocaine existed in salt form. We also found lactose in the sample BWALEI + ANP The sample was found to contain 26.0% of cocaine (as base). C9C8PA + + the sample contains cocaine CBC8TD + ANP 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) calculated on the hydrochloride as 16% w/w. CDDPDD + ANP Lactose was also identified in trace amount. The analytical technique was GC-MS analysis of the silylated sample. CG1SCE + -

CG43CR + - SM-2 Contains cocaine and lactose. CJ8TUV + -

CSBOTS + - In the sample was found cocaine DHIABX + + The sample contains cocaine HCl and lactose DINDT4 + + The sample contains Lactose. DVAUDS + + ekgonine methyl ester, cis-ciannamoyl cocaine, trans-ciannamoyl cocaine, metilekgonidin, lactose E8EF88 + -

EC0KNG + ANP

EDCFFF + ANP Cocaine EEVV4K + + chlorhydrate

Code Cocaine Lactose ELGLLX + ANP The sample 2017/1/SM-2 was found to contain Cocaine. EWPSI1 + -

EY4TQ0 + + The sample contains cocaïne HCl. Cocaïne HCl is sheduled as illicit drug. F2RYW0 + ANP Results of screening tests were positive for cocaine. Retention time and fragmentation pattern obtained with sample are equivalent to those obtained with cocaine. Cocaine was detected at 25.29% by weight. FCCEZJ + + The sample contains cocaine (25% as base) and lactose. Cocaine is scheduled as illicit drug in France. FS5XU9 + ANP \\ FVOURP + - Analyse de l'échantillon révèle la présence de la cocaïne FZJOFH + ANP cocaine G00C40 + + It contains cocaine at 22.7% and lactose G7772Y + ANP - GBKZCY + ANP RAS GDTQXP + ANP the sample was found to contain cocaine GG0XXN + ANP It was detected the presence of Cocaine as the major componet in the sample analysed. As minor components it was detected the presence of methylecgonine esther, cinnamoyl cocaine and anydroecgonine methyl esther. GTGG5G + - under control substance HHHGBD + ANP Cocaine was identified into material 2017/1/SM-2 by colorimetric reactions and gas chromatography/mass spectrometry analysis. HHPRLM + ANP Lactose HWVVX1 + + cocaine, lactose HXXSFV + +

IBADIN + ANP CONFIRMED BY GC MS AND QUANTIFIED BY GC FID AND HPTLC II3KTK + - A composite was formed from 1 unit for testing. Cocaine hydrochloride confirmed in the composite. IIIIXI + + Cocaine is on thre list of drugs.

Code Cocaine Lactose IIORYA + ANP

ILLLUA + + White powder containing cocaine and lactose IO2NIR + - We found in SM2 sample after injecting to the GC/MS cocaine, cinnamoylcocaine and benzoylecgonine. The major component is cocaine while cinnamoylcocaine and benzoylecgonine are in trace compared to cocaine. IUAAMC + + powder IUTURP + + Cocaine as base 25.31% and Lactose IW9I29 + ANP SM2 contained Cocaine J33P51 + -

J7GZ5J + + White powder containing 26,7%w/w cocaine and lactose J9A9TR + ANP

JHT4NF + + SM2 contains 25% (w/w) cocaine base and lactose. benzoylecgonine and cinnamoyl cocaine were also detected as minor components. JSZRBG + ANP Sample 2017/1/SM-2 a white powder gave a positive result for COCAINE substance under national legislation on drugs JWJCVR + - Common substance usually detected in the laboratory. KFKKJK + + performed the physicochemical and instrumental analyzes it is concluded that sample number two contains Cocaina KNNBBF + ANP In sample 2017/1/SM-2 was verified the presence of Cocaine, with a purity of 26.6% express as base (for each 100 grams of sample, 26.6 grams of cocaine) KORMOX + + The sample 2 containing 25,4% of Cocaïne and lactose, also the Benzoyelcgonine. L7MBHE + - The sample contains cocaine (25.8%). L8TNQL + ANP White powder sample contains Cocaine LIGGG3 + +

LJ1SES + - On analysis, I found the sample 'SM-2' containing Cocaine. LRNK4C + ANP cocaine was detected by GC/MS and quantified by GC/FID MDJIDD + + The sample contains cocaine base 25.50 % m/m. MGUGGY + ANP The powder in this item was found to contain cocaine at a concentration of 25%. Cocaine is a Class A controlled substance under the provisions of the Misuse of Drugs Act 1971 (as amended).

Code Cocaine Lactose MKKKKK + ANP In the test sample 2017/1/SM-2 was detected cocaine MQZPKC + + COCAINE-LACTOSE MXTSS3 + - 26% +/-3 MYMMDT + ANP

N8QMXC + + SM02 was found to contain Cocaine, lactose and trace amounts of anhydrecgonine methylester and transcinnamoylcocaine NRTTXK + ANP Based on the above analysis, the sample was found to contain cocaine. O0RMCH + ANP The sample contain cocaine O5WQZI + + It has been detected the presence of cocaine hydrochloride in the sample OADJRA + -

OBFIDR + ANP

ODVN18 + + Marquis reagent: negative result; Cobalt thiocyanate: cocaine positive result; GCMS: cocaine,ecgonidine methylester cis and trans-cinnamoylcocaine (compared with library MS spectrum) , FTIR: cocaine, lactose (compared to IR spectrum of cocaine:lactose 1:1 mixture), FTIR: lactose (see aboce - SM1); OFRCFR + + The substance contains %23 Cocaine and Lactose OSZNWS + + cis-cinnamoylcocaine, trans-cinnamoylcocaine, Methyl ecgonine P0ADJ0 + ANP Blue colour with Cobolt II thiocyanate test indicated the possible presence of cocaine. TLC and GC- MS results confirmed the presence of cocaine in SM-2. P3HHYE + ANP ECGONINE METHYL ESTHER also found P7LEGU + ANP From GCMS analysis, cocaine was detected P7PCPW + + 77.0 % Cocaine base - The test sample also contained lactose PBBITB + ANP Controlled drug: cocaine Concentration: approx. 24 % PKQQQQ + + The sample correspond: COCAINE HCL POEJXP + - The percentage of cocaine in SM2 was 24.00 PYTTET + ANP cocaine; ecgonine methyl ester; anhydroecgonine methyl ester Q4EE4E + + Se le realizaron pruebas de color y pruebas confirmativas como GC-MS, FT-IR

Code Cocaine Lactose QGJYGY + - SM 2 contains Cocaine. QI1JNX + ANP IN THE SAMPLE LABELED AS "2017/1/SM-2" WAS DETECTED Cocaine. QKD30L + - Sample was found to contain Cocaine QMZCMA + ANP

QOMHP5 + ANP

QRNQXH + + CONTIENE COCAÍNA Y LACTOSA QXRKFZ + ANP The sample SM-2 contains a drug cocaine 25.3% R8T8AE + ANP The white powder was analysed and found to contain cocaine hydrochloride. RHYD82 + ANP The sample contains cocaine. RNNNVK + + One glass bottle containing 0.21 grammes of a solid containing 0.05 grammes of cocaine. RPC9FU + - Confirmed by GS/MS method. Quantification analyses was performed by Gas Chromatography FID. RPPFPC + - Sample SM-2 was found to contain 31.9% cocaine base. RV66P1 + ANP 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) RYB8ZA + + The sample contains Cocaine and lactose S27VCS + + -- S97OK5 + + Cobalt thiocyanate (CT) positive, CG/MS and mass charge ratio (M/Z) similar Characteristics with the substances used as standard or pattern. FTIR, absorption bands coincident with the substance used as standard. SFHFBQ + ANP found cocaine: 25.8%w/w SGI5IO + + Sample also contain lactose. The presence of drug confirmed by GC-MS and FTIR spectroscopy analysis.The hydrochloride form of cocaine was confirmed by the anion analysis and FTIR spectroscopy. SKSSPS + ANP

SKZHH0 + + Sample 2017/1/SM-2 consists of white powder. Cocaine, a prohibited substance included in the National Law for Narcotics, is found to be present in this sample.

Code Cocaine Lactose SSIHCS + + ecgonidine, methyl ester; ecgonine methyl ester; cis-cinnamoylcocaine; lactose SSSS3S + ANP Item contained white powder, which was found to contain Cocaine, a Class A drug, at a purity of 23 per cent. SWSSOF + ANP SIZE MATERIAL COMPARATION SYNTESI INTERMEDIATES COMPOUNDS IDENTIFICATION (ECGONIDINE ME, ECGONINE ME, CINNAMOILCOCAINE) TBUZWG + - The sample was found to contain cocaine TGCAAA + - Cobalt Thiocyanate Test give blue colour.TLC and GCMS used for confirmation.In GCMS Rt:22.235mins,Base peak:182 TTHTMU + ANP Scott test positive, identified by GC-MS TTTTHT + - 23,5 % of Cocaine (free base) TUVU7D + + One brown glass vial with lid, labelled '2017/1/SM-2' and '16', which contained 225 milligrams of white powder. This powder contained an average of 28% cocaine hydrochloride. Cocaine is a Class A controlled drug under the provisions of the Misuse of Drugs Act 1971 (as amended). UBTTQP + + Cocaine 24.9% and lactose UDUUW5 + - Test Sample 2017/1/SM-2 was confirmed to contain cocaine. Cocaine is a DEA Schedule II controlled substance in the United States. UDYUUU + + LACTOSE UFAT5C + + contained cocaine trace cis-cinnamoilcocaine, methylecgonidine UHBHEQ + ANP The sample contains 30.8% Cocaine as base UQYIVP + -

UT2EIQ + + LACTOSE V3JVVY + +

V4QVVV + + The sample contains Cocaine. The seize material also contains Lactose. Cocaine Content (as base)=25.48% by weight VGNZKV + + COCAINE IN LACTOSE POWDER VTELFX + + LACTOSE, COCA LEAVES IMPURITIES VVJVZV + ANP the White powder contains cocaine (57.2%w/w) which is controlled by national law

Code Cocaine Lactose VVSOI6 + - Examination of the sample coded 2017/1/SM-2 revealed the presence of cocaine VVXRIZ + + The sample contains 23.6% ± 1 %. Also contain lactose. VYVVTU + + COCAINA HCL, LACTOSA W3O2KM + + Item 2017/SM-2: a white powder which contained Cocaine at a concentration of 26% (as base) and also indicated the presence of lactose. Cocaine is a class A controlled drug under the provisions of the Misuse of Drugs Act 1971 (as amended). Lactose is not controlled under the provisions of the Misuse of Drugs Act 1971 (as amended). W7U77N + + Cocaine was identificated in the sample analyzed. WAYGAS + - Cocaine confirmed in the sample submitted. WD6IRG + + The test sample 2017/1/SM-2 was found to contain 12.2% cocaine. The sample was also found to contain lactose. WDWUWW + + The substance is cocaine. WTEPTR + + We found cocaine 24.8% +-1.8. Was found too lactose. WTVLQ8 + + cocaine +lactose XS2G6M + ANP white powder containing cocaine XW94X4 + ANP from screening test using (Cobalt thiocyanate (CT)) and from confirmation test using (Gc-Ms) the sample was found to contain the controlled drug (Cocaine) XWBZZG + ANP Cocaine was DETECTED in sample 2017/1/SM-2. XXYCLX + -

Y1FM12 + + We identified the sample by GC-MS, FTIR and we compared the results with reference material, NIST library AND swgdrugs library. YHAA5A + + the sample is mixed with lactose YHNRNC + +

ZDS0S1 + + 221 milligrams of a white powder which was found to contain Cocaine Hydrochloride and Lactose. The purity of the cocaine is 24% in its base form - Class A controlled drug under the Misuse of Drugs Act 1971 (as amended) ZFBPKW + ANP Presence of Cocaine was confirmed qualitatively. ZIWYWS + + ./. ZMVLHU + ANP Sample 2017/1/SM-2 found to contain cocaine

Code Cocaine Lactose ZNWNNS + ANP The powder contains 25.3±1.0 % cocaine-base ZOCUCZ + ANP

ZOSSZI + ANP Sample SM-2 found to contain cocaine ZRVVPU + ANP

ZWNZ3Z + ANP White powder containing 26.8%w/w of cocaine ZZVQGW + ANP

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: 204

The response summary of all 204 participating laboratories for the identification of SM-2, frequency of use of screening and identification techniques and false positives and negatives:

Correct identification of Test Sample:

Substance Name Number of laboratories: Cocaine 203 Lactose 87

False positives for Test Sample-2:

There were no false positives reported for test sample 2

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

Round Code: Tech Code: 1UUW16 180

Frequency of use of screening, identification and quantification techniques:

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

Z-Scores for Test Sample 2

Cocaine Cocaine Deviation Code Concentration Deviation from Code Concentration z-score from robust z-score (mass%) robust average (mass%) average 99U99A 3.0 -22.1 -11.9 YHNRNC 24.4 -0.7 -0.4 1UUW16 5.0 -20.1 -10.8 QRNQXH 24.5 -0.6 -0.3 3AY738 11.2 -13.9 -7.5 BSSEUS 24.7 -0.4 -0.2 WD6IRG 12.2 -12.9 -6.9 WTEPTR 24.8 -0.3 -0.2 CBC8TD 14.2 -10.9 -5.9 UBTTQP 24.9 -0.2 -0.1 UQYIVP 19.4 -5.8 -3.1 ZOCUCZ 24.9 -0.2 -0.1 RHYD82 19.6 -5.5 -3.0 VVSOI6 24.9 -0.2 -0.1 Y1FM12 20.2 -4.9 -2.6 RNNNVK 24.9 -0.2 -0.1 EDCFFF 20.4 -4.7 -2.6 P3HHYE 25.0 -0.1 -0.1 8A4YUG 20.6 -4.5 -2.4 FS5XU9 25.0 -0.1 -0.1 TTHTMU 21.0 -4.1 -2.2 99VFND 25.0 -0.1 -0.1 BBXCFB 21.7 -3.4 -1.8 II3KTK 25.0 -0.1 -0.1 3OFVFV 22.3 -2.9 -1.5 MGUGGY 25.0 -0.1 -0.1 CJ8TUV 22.6 -2.5 -1.4 9LR9YU 25.0 -0.1 -0.1 G00C40 22.7 -2.4 -1.3 FCCEZJ 25.0 -0.1 -0.1 DINDT4 22.8 -2.3 -1.3 JHT4NF 25.0 -0.1 -0.1 QGJYGY 22.9 -2.3 -1.2 TUVU7D 25.0 -0.1 -0.1 AOAPHK 22.9 -2.2 -1.2 2TYJEG 25.1 0.0 0.0 SSIHCS 22.9 -2.2 -1.2 215ETZ 25.1 0.0 0.0 OFRCFR 23.0 -2.1 -1.1 A6YPWP 25.1 0.0 0.0 2SI2CZ 23.0 -2.1 -1.1 5RTTW2 25.2 0.1 0.0 SSSS3S 23.0 -2.1 -1.1 AYJ22M 25.2 0.1 0.1 9T1OWI 23.1 -2.0 -1.1 F2RYW0 25.3 0.2 0.1 88P8P5 23.1 -2.0 -1.1 5QVQHW 25.3 0.2 0.1 6A5NIA 23.1 -2.0 -1.1 QXRKFZ 25.3 0.2 0.1 IIIIXI 23.2 -1.9 -1.0 ZNWNNS 25.3 0.2 0.1 ILLLUA 23.3 -1.8 -1.0 IUTURP 25.3 0.2 0.1 0YYGT3 23.3 -1.8 -1.0 5QMBSP 25.4 0.3 0.1 DVAUDS 23.3 -1.8 -1.0 KORMOX 25.4 0.3 0.1 C9C8PA 23.4 -1.7 -0.9 VGNZKV 25.4 0.3 0.1 7CW6XN 23.5 -1.6 -0.9 V4QVVV 25.5 0.4 0.2 TTTTHT 23.5 -1.6 -0.9 JWJCVR 25.5 0.4 0.2 VVXRIZ 23.6 -1.5 -0.8 MDJIDD 25.5 0.4 0.2 OSZNWS 23.6 -1.5 -0.8 4WF099 25.5 0.4 0.2 5THFBN 23.7 -1.4 -0.8 SGI5IO 25.7 0.6 0.3 IUAAMC 23.8 -1.3 -0.7 1S1T1G 25.7 0.6 0.3 GTGG5G 23.9 -1.2 -0.7 UFAT5C 25.7 0.6 0.3 BMG4RM 23.9 -1.2 -0.6 O5WQZI 25.7 0.6 0.3 2ACRDL 24.0 -1.1 -0.6 UDYUUU 25.7 0.6 0.3 1U0JGG 24.0 -1.1 -0.6 SFHFBQ 25.8 0.7 0.4 POEJXP 24.0 -1.1 -0.6 VVJVZV 25.8 0.7 0.4 ZZVQGW 24.0 -1.1 -0.6 L7MBHE 25.8 0.7 0.4 ZDS0S1 24.0 -1.1 -0.6 RYB8ZA 25.9 0.8 0.4 CG43CR 24.1 -1.0 -0.6 P7PCPW 26.0 0.9 0.5 541LFZ 24.2 -0.9 -0.5 VYVVTU 26.0 0.9 0.5 PBBITB 24.2 -0.9 -0.5 MXTSS3 26.0 0.9 0.5 HWVVX1 24.2 -0.9 -0.5 58Y8FL 26.0 0.9 0.5 TBUZWG 24.2 -0.9 -0.5 BWALEI 26.0 0.9 0.5 8A5KSA 24.3 -0.8 -0.4 IBADIN 26.0 0.9 0.5 RV66P1 24.4 -0.7 -0.4 EEVV4K 26.0 0.9 0.5 EC0KNG 24.4 -0.7 -0.4 UT2EIQ 26.0 0.9 0.5 57 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE)

Z-Scores for Test Sample 2

Cocaine Deviation Code Concentration from robust z-score (mass%) average W3O2KM 26.0 0.9 0.5 VTELFX 26.0 0.9 0.5 EWPSI1 26.0 0.9 0.5 2B1A92 26.1 1.0 0.5 ZIWYWS 26.1 1.0 0.5 RPC9FU 26.1 1.0 0.5 EY4TQ0 26.2 1.1 0.6 AMECCZ 26.2 1.1 0.6 CSBOTS 26.3 1.2 0.6 LRNK4C 26.3 1.2 0.6 WDWUWW 26.4 1.3 0.7 333HH3 26.4 1.3 0.7 BFED5J 26.4 1.3 0.7 GBKZCY 26.4 1.3 0.7 4FFKBN 26.6 1.5 0.8 MKKKKK 26.6 1.5 0.8 KNNBBF 26.6 1.5 0.8 S27VCS 26.7 1.6 0.8 J7GZ5J 26.7 1.6 0.8 AOGMWK 26.7 1.6 0.8 ZWNZ3Z 26.8 1.7 0.9 OADJRA 26.8 1.7 0.9 5G3N55 27.1 2.0 1.1 3UI8PF 27.6 2.5 1.3 BPCSEV 28.0 2.9 1.5 0GK0Q0 28.2 3.1 1.7 J9A9TR 28.6 3.5 1.9 XXYCLX 28.8 3.7 2.0 MQZPKC 29.0 3.9 2.1 283GPP 29.0 3.9 2.1 PKQQQQ 30.0 4.9 2.6 YHAA5A 30.1 5.0 2.7 G7772Y 30.2 5.1 2.7 UHBHEQ 30.8 5.7 3.1 N8QMXC 31.1 6.0 3.2 RPPFPC 31.9 6.8 3.6 W7U77N 38.6 13.5 7.2 SKSSPS 39.2 14.1 7.6 CG1SCE 61.0 35.9 19.3 Q4EE4E 62.6 37.5 20.1 HXXSFV 83.7 58.6 31.5 5X7UMS 85.0 59.9 32.2

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

Z-Score Report per Sample per Substance

Robust average = 25.1 % Round: 2017/1 UNODC value = 23.7 % Substance: SM-2; Cocaine

4.00 3.7 3.2 3.1 3.00 2.7 2.7 2.6 2.1 2.1 2.0

2.00 1.9 1.7 1.6 1.3 1.1 0.9 0.9 0.9 0.9 0.9

1.00 0.8 0.8 0.8 0.7 0.7 0.7 0.6 0.6 0.6 0.6 0.6 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.5 0.4 0.4 0.4 0.4 0.3 0.3 0.3 0.3 0.3 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 0.0 0.0 7.3 7.6 19.3 20.1 31.5 0.00 7.5 6.9 5.9 0.0 - - - 0.1 0.1 0.1 0.1 0.1 0.1 0.1 0.1 11.9 10.8 ------0.1 0.1 0.1 0.1 ------0.2 - 0.2 - 0.3 - 0.4 0.4 0.4 - - 0.4 - - 0.5 0.5 0.5 0.5 - - - 0.5 - - 0.6 0.6 0.6 0.6 0.6 0.6 - - - - - 0.6 - - 0.7

-1.00 - 0.8 0.8 0.8 - - - 0.9 0.9 - - 0.9 0.9 - 1.0 1.0 - - 1.0 - - 1.1 1.1 1.1 - - - 1.1 1.1 1.1 - - - 1.2 1.2 1.2 - - 1.2 - - 1.3 - 1.3 - 1.5 - -2.00 1.8 - 2.2 - 2.4 - 2.5 - 2.6 -3.00 - 3.0 - 3.1 -

-4.00 IIIIXI II3KTK 2SI2CZ ILLLUA SSIHCS SGI5IO J7GZ5J SSSS3S FCCEZJ 541LFZ PBBITB 58Y8FL IBADIN 3UI8PF SKSSPS VVXRIZ 2TYJEG BFED5J 215ETZ VTELFX J9A9TR XXYCLX EDCFFF POEJXP ZDS0S1 VVSOI6 JHT4NF S27VCS CJ8TUV 88P8P5 6A5NIA TTTTHT BSSEUS IUTURP VVJVZV UT2EIQ 3AY738 DINDT4 0YYGT3 FS5XU9 9LR9YU 1S1T1G EWPSI1 BPCSEV RPPFPC UQYIVP BBXCFB 8A5KSA RV66P1 RYB8ZA EEVV4K 2B1A92 EY4TQ0 CSBOTS 4FFKBN G7772Y CG1SCE Q4EE4E HXXSFV G00C40 C9C8PA 2ACRDL QXRKFZ JWJCVR BWALEI LRNK4C 283GPP CBC8TD 3OFVFV QGJYGY OFRCFR UFAT5C SFHFBQ RPC9FU 99U99A 5THFBN 1U0JGG CG43CR AYJ22M MDJIDD RHYD82 9T1OWI ZOCUCZ 99VFND MXTSS3 333HH3 OADJRA 5G3N55 Y1FM12 EC0KNG VYVVTU 0GK0Q0 8A4YUG UBTTQP 4WF099 KNNBBF YHAA5A WTEPTR 5RTTW2 F2RYW0 VGNZKV WD6IRG IUAAMC TUVU7D V4QVVV O5WQZI L7MBHE ZIWYWS AMECCZ MKKKKK ZWNZ3Z AOAPHK DVAUDS YHNRNC A6YPWP P7PCPW GTGG5G RNNNVK 5QMBSP MQZPKC TTHTMU 7CW6XN OSZNWS UHBHEQ HWVVX1 TBUZWG QRNQXH UDYUUU 1UUW16 ZZVQGW W7U77N ZNWNNS PKQQQQ N8QMXC KORMOX MGUGGY BMG4RM 5QVQHW W3O2KM AOGMWK WDWUWW 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.

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

Z-Score Report per Sample per Substance

Round: 2017/1 Substance: SM-2; Cocaine

Dispersion of z-scores using different analytical techniques for the quantification of Cocaine in 2017/1 SM-2 10

0 score - z

-2

-4

-6

-8 HPLC GC-FID GC-MS NMR -10

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

Sample 3 Analysis

Identified substances for Test Sample 3

Code Identified Substances 0GK0Q0 MDMA and Lactose 0YYGT3 MDMA 100JU0 MDMA 1HAGZA 3,4-METHYLENEDIOXYMETAMFETAMINE (MDMA) 1S1T1G MDMA 1U0JGG 3,4-Methylenedioxymetamfetamine (MDMA) 1UUW16 MDMA 215ETZ 3,4-Methylenedioxymetamfetamine (MDMA) 283GPP MDMA (methylenedioxymethylamphetamine) 2ACRDL MDMA 2B1A92 MDMA 2SI2CZ MDMA 2TYJEG MDMA 333HH3 MDMA 3AY738 MDMA 3OFVFV MDMA 3UI8PF 3,4-Methylenedioxymetamfetamine (MDMA) 3ZOPSC MDMA Hcl and LACTOSE 4FFKBN 3,4-Methylenedioxymetamfetamine (MDMA) 4PGMZO MDMA and Lactose 4WF099 MDMA 4X449Z 3,4-Methylenedioxymetamfetamine(MDMA) 541LFZ MDMA hcl 58Y8FL MDMA 5A5855 3,4-MDMA 5G3N55 MDMA 5QMBSP MDMA 5QVQHW MDMA 5RTTW2 MDMA 5THFBN 3,4-Methylenedioxymetamfetamine (MDMA) 5X7UMS 3,4-Methylenedioxymetamfetamine (MDMA) 6A5NIA MDMA 6BUQUQ MDMA 7CW6XN MDMA 7MAM28 MDMA 88P8P5 3,4 Methylenedioxy-metamfetamine (MDMA) 8A4YUG 3,4-Methylenedioxymetamfetamine (MDMA) 8A5KSA MDMA 99U99A Methylenedioxymethamphetamine(MDMA) 99VFND 3,4-Methylenedioxymetamfetamine (MDMA) 54.6%

Code Identified Substances 9A8CUK 3,4-Methylenedioxymethamphetamine 9LR9YU 3,4-Methylenedioxymetamfetamine(MDMA) 9T1OWI 3,4-methylenedioxymethamphetamine (MDMA) A3IH33 MDMA A6YPWP MDMA AMECCZ MDMA AOGMWK 3,4 Methyedioxymethamfetamine AYJ22M MDMA HCl B6PUEJ 3,4-Methylenedioxymetamfetamine (MDMA) BBXCFB 3,4-Methylenedioxymetamfetamine (MDMA) BFED5J 3,4- Methylenedioxymetamfetamine BJSGWA MDMA BMG4RM MDMA BPCSEV 3,4-Methylenedioxymetamfetamine (MDMA) BSN7V0 MDMA ,methamfetamine BSSEUS 3,4-methylenedioxymethamphetamine (MDMA) BWALEI 3,4-methylenedioxymetamfetamine (MDMA) C9C8PA 3,4-Methylenedioxymetamfetamine (MDMA) CBC8TD MDMA CDDPDD MDMA CG1SCE MDMA CG43CR 3,4 Methylenedioxymethamphetamine CJ8TUV MDMA CSBOTS MDMA DHIABX MDMA DINDT4 3,4-Methylenedioxymetamfetamine (MDMA) DVAUDS MDMA E8EF88 3,4 methylenedioxymetamfetamine (MDMA) EC0KNG MDMA EDCFFF 3,4-Methylenedioxymetamfetamine (MDMA) EEVV4K MDMA ELGLLX 3,4-Methylenedioxymetafetamine (MDMA) EWPSI1 3,4-Methylenedioxymetamfetamine (MDMA) EY4TQ0 MDMA HCl F2RYW0 3,4-Methylenedioxymetamfetamine (MDMA) FCCEZJ MDMA FS5XU9 MDMA FVOURP heroin FZJOFH MDMA G00C40 MDMA G7772Y 3,4-Methylenedioxymetamfetamine (MDMA) GBKZCY mdea GDTQXP MDMA GG0XXN 3,4-Methylenedioxymetamfetamine (MDMA)

Code Identified Substances GTGG5G MDMA HHHGBD 3,4-Methylenedioxy-metamfetamine (MDMA) HHPRLM 3,4-Methylenedioxymetamfetamine (MDMA) HWVVX1 MDMA HXXSFV MDMA,MDEA IBADIN MDMA II3KTK 3,4-Methylenedioxymethamphetamine HCl IIIIXI MDMA IIORYA MDMA ILLLUA MDMA IO2NIR MDMA IUAAMC MDMA IUTURP 3,4-Methylenedioxymetamfetamine HCl IW9I29 MDMA J33P51 MDMA J7GZ5J MDMA J9A9TR MDMA JHT4NF MDMA JSZRBG MDMA JWJCVR MDMA KFKKJK 3,4 Methylenedioxymetamphetamine (MDMA) KNNBBF 3,4 Methylendioxymetamfetamine (MDMA) KORMOX MDMA L7MBHE MDMA L8TNQL 3,4-Methylenedioxy-metamfetamine (MDMA) LIGGG3 MDMA, LACTOSE LJ1SES 3,4-Methylenedioxymethamphetamine (MDMA) LRNK4C MDMA MDJIDD MDMA MGUGGY Methylenedioxymethylamphetamine (MDMA) MKKKKK MDMA MQZPKC MDMA MXTSS3 MDMA MYMMDT MDMA N8QMXC MDMA (XTC) NRTTXK 3,4-methylenedioxymetamfetamine (MDMA) O0RMCH MDMA O5WQZI 3,4-Methylenedioxymetamfetamine OADJRA MDMA OBFIDR MDMA ODVN18 MDMA OFRCFR MDMA OSZNWS 3,4-Methylenedioxymetamfetamine (MDMA) P0ADJ0 3,4-Methylenedioxymetamfetamine (MDMA)

Code Identified Substances P3HHYE 3,4-Methylenedioxymetamfetamine (MDMA) P7LEGU 3,4-Methylenedioxymetamfetamine (MDMA) P7PCPW MDMA PBBITB MDMA PKQQQQ 3,4-METHYLENDIOXYMETHAMPHETAMINE(MDMA) POEJXP N-methyl-3,4-methylenedioxymetamfetamine (MDMA) PYTTET 3,4-Methylenedioxymethamphetamine (MDMA) Q4EE4E 3,4-metilendioxianfetamina QGJYGY MDMA QI1JNX 3,4-Methylenedioxymetamfetamine (MDMA) QKD30L 3,4-Methylenedioxymethamphetamine (MDMA) QMZCMA Ecstasy QOMHP5 3,4-methylenedioxymethamphetamine QRNQXH 3,4-metilendioximetanfetamina (MDMA) QXRKFZ MDMA R8T8AE 3,4-Methylenedioxymetamfetamine RHYD82 3,4-Methylenedioxymetamfetamine (MDMA) RNNNVK 3,4-methylenedioxymethamphetamine RPC9FU MDMA RPPFPC MDMA RV66P1 MDMA RYB8ZA MDMA S27VCS mdma S97OK5 3,4-Methylenedioxi-metamfetamine (MDMA) SFHFBQ MDMA SGI5IO 3,4-Methylenedioxymetamfetamine (MDMA) SKSSPS 3,4-Methylenedioxymetamfetamine SKZHH0 3,4-Methylenedioxymetamfetamine (MDMA) SSIHCS 3,4-Methylenedioxymetamfetamine (MDMA) SSSS3S MDMA SWSSOF MDMA TBUZWG 3,4-Methylenedioxymetamfetamine (MDMA) TGCAAA 3,4-Methylenedioxymetamfetamine(MDMA) TTHTMU MDMA TTTTHT MDMA TUVU7D 3,4-Methylenedioxymethylamphetamine hydrochloride (MDMA) UBTTQP MDMA UDUUW5 MDMA (3,4-methylenedioxymethamphetamine) UDYUUU 3,4-Methylenedioxymetamfetamine (MDMA) UFAT5C MDMA UHBHEQ MDMA UQYIVP MDMA UT2EIQ MDMA V3JVVY MDMA

Code Identified Substances V4QVVV 3,4-Methylenedioxymetamfetamine (MDMA) VGNZKV MDMA VTELFX MDMA HCL VVJVZV MDMA (ecstasy) VVSOI6 Methylenedioxymetamfetamine VVXRIZ MDMA VYVVTU MDMA HCL W3O2KM 3,4-Methylenedioxymetamphetamine (MDMA) W7U77N 3,4-Methylenedioxymetamfetamine (MDMA) WAYGAS 3,4-Methylenedioxymethamphetamine WD6IRG MDMA WDWUWW MDMA WTEPTR MDMA WTVLQ8 3,4-Methylenedioxymetamfetamine XS2G6M MDMA XW94X4 MDMA XWBZZG MDMA XXYCLX mdma Y1FM12 MDMA, lactose YHAA5A MDMA YHNRNC MDMA ZDS0S1 MDMA HCL - 3,4, methylenedioxymethyl amphetamine hydrochloride ZFBPKW 3,4-Methylenedioxymetamfetamine (MDMA) ZIWYWS MDMA ZMVLHU 3,4-methylenedioxymetafetamine[MDMA] ZNWNNS MDMA ZOCUCZ MDMA ZOSSZI 3-4,methylenedioxymetamfetamine(MDMA) ZRVVPU MDMA ZWNZ3Z MDMA ZZVQGW MDMA

Statement of findings for Test Sample 3

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

0GK0Q0 + + The sample 2017/1/SM-1 contains MDMA and Lactose detected by GC/MS and FTIR. The percentage by weight of MDMA is 57.9%. 0YYGT3 + -

100JU0 + ANP Off white powder that contains drug MDMA. 1HAGZA + - 3,4-METHYLENEDIOXYMETAMFETAMINE (MDMA) IS LISTED IN THE FIRST SCHEDULE OF THE DANGEROUS DRUGS ACT 1952. 1S1T1G + - The sample contains 3,4-méthylènedioxy-méthamphétamine 1U0JGG + + Lactose 1UUW16 + + after analysis performed the sample contained MDMA + LACTOSE 215ETZ + - The sample consist controlled drugs - 3,4-Methylenedioxymetamfetamine (MDMA) 283GPP + ANP On analysis of a representative sample of the powder MDMA (Methylenedioxymethylamphetamine) was detected 2ACRDL + ANP

2B1A92 + - MDMA in mixture with mono- and disaccharides 2SI2CZ + + LACTOSE 2TYJEG + -

333HH3 + ANP

3AY738 + + The sample SM-3 contains MDMA, which is included in List F2 (List of psychotropic substances banned in Brazil) of Annex I of SVS/MS 344, May 12, 1998. 3OFVFV + ANP That I examined and analysed the said sample and found it to contain: controlled substance(s) within the meaning of the Controlled Drugs and Substances Act: Schedule I 19. (8) N-methyl-3,4-methylenedioxyamphetamine (MDMA) (N,Įdimethyl-1,3-benzodioxole-5-ethanamine) 3UI8PF + + Lactose

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

3ZOPSC + + Initially conducted a preliminary test to check in the presence of what kind of product we are. An intense dark color (black) appeared in the presence of the MARQUIS test (Sulfuric acid, formaldehyde) indicating the presence of MDMA, which came to confirm with the realization of TLC and the FTIR. But later it did if a screening (TLC) where all the samples were prepared using as solvent the dichloromethane and how eluent methanol. A chromatographic Tina was used with the dimensions of 20cm × 20cm and the plate used for the purpose has the dimensions of 10cm × 20cm. In a 2 ml vial weighed 15 milligrams of the product and dissolved in 1.5 ml of the solvent (dichloromethane). With the help of a 5ȝl Micropipette, the specimens were placed on the chromatographic plate and left the same dry for a while. It placed about 80 ml of the solvent in Tina Chromatographic and left the same saturate for about 1 hour. Then the sample was placed in Tina Chromatographic with its lid and left the same elute about 25-30 minutes. At the end, the plate of Tina Chromatographic and left dry for 15 minutes. With the help of a chamber of UV a Ȝof 254 nn managed to visualize the stains on the plate and later do if the revelation of the plaque making use of the reagent of Dragendorf. In the sample 2017/1/SM3 was able to observe the presence of 3.4 Methyllenedioxymetamfetamine (MDMA). Subsequently, the equipment FTIR is 10 and is 50 in Transmitancia mode mixing the product with KBR and absorbance (ATR) and for sample 2017/1/SM3 was confirmed the presence of the MDMA AND LACTOSE. 4FFKBN + + 3,4-Methylenedioxymetamfetamine (MDMA) was identified by GCMS & quantified by GC analysis. 4PGMZO + + The Test sample 2017/1/SM-3 was analyzed by Colour Test and Thin Layer Chromatography technique and was found to contain MDMA and Lactose. 4WF099 + + Sample contained MDMA as hydrochloride, and LACTOSE. Identification of MDMA by FTIR and GC/MS, quantification by GC/FID. Identification of LACTOSE by FTIR, HPLC/DIR and Colorimetric Reactions (Molish Test). 4X449Z + + 2017/1/SM-3 contains 3,4-Methylenedioxymetamfetamine, a dangerous drug. It also contains Lactose. 541LFZ + + BASE MDMA 55,21 +/-6,2 % (w/w) and Lactose 58Y8FL + ANP The powder contains MDMA. MDMA (also known as methylenedioxymethylamphetamine) is a controlled drug under the Misuse of Drugs Acts, 1977 to 2016. This is because methylenedioxymethylamphetamine is structurally derived from N-alkyl-alpha- methylphenethylamine, by substitution in the ring with an alkylenedioxy substituent. (See paragraph 1A(l) of Schedule 1 to the Misuse of Drugs (Amendment) Act, 2015). 5A5855 + ANP 3,4-Methylenedioxymethamphetamine 5G3N55 + ANP MDMA is controlled by law (Royal Decree 22/01/1998) 5QMBSP + - In the sample SM3 was identified MDMA (ecstasy) by GC-MS.

5QVQHW + +

5RTTW2 + ANP MDMA is a Class A drug subject to the provisions of the Misuse of Drugs Act 1971 5THFBN + + 2017/1/SM-3 contains drug (3,4-Methylenedioxymetamfetamine MDMA) and adulterant (lactose)

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

5X7UMS - - analysis done by using GCMS 6A5NIA + ANP

6BUQUQ + ANP

7CW6XN + ANP MDMA was identified in the sample 2017/1/SM3. First, colormietric test, then GC-MS, and Finally we made FTIR. 7MAM28 + ANP De los análisis realizados se concluye que la sustancia se trata de metilendioximetanfetamina (MDMA) 88P8P5 + ANP LIST II OF THE CONVENTION ON PSYCHOTROPIC SUBSTANCES OF 1971 8A4YUG + - This substance was identified by Marquis test, and using analytical techniques of Gas Chromatography / Mass Spectrometry and Fourier Transform Infrared Spectrometry. And we obtained a quantification of 60.53% using HPLC-DAD techniques 8A5KSA + + white powder containing 3,4-methylenedioxymetamfetamine and lactose 99U99A + - 1.Using the techniques CR,TLC,GC-MS,FT-IR sample SM-3 was found to contain Methylenedioxymethamphetamine(MDMA). 2.Using technique GC-FID,quantification of SM-3 was done and found to contain MDMA 7.2%.( As we do not do the quantification of MDMA in our Laboratory, we are not sure of the percentage).

99VFND + ANP

9A8CUK + ANP 2017/1/SM-3 was found to contain 58.16% of 3,4-Methylenedioxymethamphetamine (MDMA). 9LR9YU + + The tes sample also contained LACTOSE. 9T1OWI + - On analysis, i found that the substances contain 56.6% w/w 3,4-methylenedioxymethamphetamine (MDMA) (base). A3IH33 + -

A6YPWP + ANP The sample contained 56.2% MDMA. AMECCZ + ANP

AOAPHK + +

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

B6PUEJ + ANP We did the respect tests and the substance identified was 3,4-Methylenedioxymetamfetamine (MDMA). BBXCFB + - The result of the tests of SM 2(36)received has confirmed that the mentioned simple contained 3,4- Methylenedioxymetamfetamine (MDMA)but we are not able to give a quantification result. BFED5J + + Presence of 3,4-Methylenedioxymetamfetamine hydrochloride and lactose was detected in the sample. BJSGWA + ANP

BMG4RM + -

BPCSEV + ANP The sample tested positive for MDMA, on screening. MDMA was confirmed and quantified. The percentage of MDMA by mass was 58%. BSN7V0 + - Presence of MDMA with METHAMFETAMINE BSSEUS + + MDMA existed in salt form. We also found alpha-methyl-3,4-methylenedixyphenethylamine (MDA) and lactose in the sample BWALEI + ANP The sample was found to contain 55.0% of 3,4-methylenedioxymetamfetamine (MDMA) (as base). C9C8PA + + the sample contains MDMA CBC8TD + ANP The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule I 19. (8) N-methyl-3,4-methylenedioxyamphetamine (MDMA), N- alpha-dimethyl-1,3-benzodioxole-5-ethanamine calculated as the hydrochloride 63% w/w. CDDPDD + ANP Lactose was also identified in trace amount. The analytical technique was GC-MS analysis of the silylated sample. CG1SCE + -

CG43CR + - SM-3 Contains 3,4-Methylenedioxymethamphetamine and lactose. CJ8TUV + -

CSBOTS + ANP In the sample was found MDMA DHIABX + ANP Under the used methodology applied in the White poder received in the glass bottle, was detected the presence of 3,4 methylendioxymethamphetamineknown as MDMA, ecstasy o XTC DINDT4 + + The sample contains Lactose. DVAUDS + + MBDB, lactose E8EF88 + -

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

EC0KNG + ANP

EDCFFF + ANP 3,4-Methylenedioxymetamfetamine (MDMA) EEVV4K + - Chlorhydrate ELGLLX + ANP The sample 2017/1/SM-3 was found to contain 3,4-Methylenedioxymetafetamine (MDMA) EWPSI1 + -

EY4TQ0 + + The sample contains MDMA HCl. MDMA HCl is sheduled as illicit drug. F2RYW0 + ANP Retention time and fragmentation pattern obtained with sample are equivalent to those obtained with 3,4-Methylenedioxymetamfetamine (MDMA). FCCEZJ + + The sample contains MDMA (52% as base) and lactose. MDMA is scheduled as illicit drug in France. FS5XU9 + ANP \\ FVOURP - - Analyse de l'échantillon révèle la présence de l’héroïne FZJOFH + ANP MDMA G00C40 + + It contains MDMA at 57.2% and lactose G7772Y + ANP - GBKZCY - ANP RAS GDTQXP + ANP the sample was found to contain 3,4-Methylenedioxymetamfetamine (MDMA) GG0XXN + ANP It was detected the presence of 3,4-Methylenedioxymetamfetamine (MDMA) in the sample analysed. GTGG5G + - under control substance HHHGBD + ANP 3,4-Methylenedioxy-metamfetamine (MDMA) was identified into material 2017/1/SM-3 by colorimetric reactions and gas chromatography/mass spectrometry analysis. HHPRLM + ANP Lactose HWVVX1 + - MDMA HXXSFV + +

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

IBADIN + ANP CONFIRMED BY GC MS II3KTK + - A composite was formed from 1 unit for testing. 3,4-Methylenedioxymethamphetamine hydrochloride was confirmed in the composite. IIIIXI + + MDMA is on the list of drugs. IIORYA + ANP

ILLLUA + + White powder containing MDMA and lactose IO2NIR + - The major compound we found in the SM3 sample after GC/MS injection is MDMA. IUAAMC + + powder IUTURP + + 3,4-Methylenedioxymetamfetamine as base 58.36% and lactose IW9I29 + ANP SM3 contained MDMA J33P51 + -

J7GZ5J + + White powder containing 55.0%w/w MDMA and lactose J9A9TR + ANP

JHT4NF + + SM3 contains 59% (w/w) MDMA base and lactose. JSZRBG + ANP Sample 2017/1/SM-3 a white powder gave a positive result for MDMA substance under national legislation on drugs JWJCVR + - Frequently seized substance. KFKKJK + - performed the physicochemical and instrumental analyzes it is concluded that sample number three contains 3,4 Methylenedioxymetamphetamine (MDMA) KNNBBF + ANP In sample 2017/1/SM-3 was verified the presence of 3,4 Methylendioxymetamfetamine (MDMA) with a purity of 62.5% express as base (for each 100 grams of sample, 62.5 grams of MDMA) KORMOX + + The sample 3 containing 61,8% of MDMA and lactose. L7MBHE + - The sample contains MDMA (54.9%). L8TNQL + + White powder sample contains 3,4-Methylenedioxy-metamfetamine (MDMA)and lactose. LIGGG3 + +

LJ1SES + - On analysis, I found the sample 'SM-3' containing 3,4-Methylenedioxymethamphetamine (MDMA).

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

LRNK4C + ANP MDMA was detected by GC/MS and quantified by GC/FID MDJIDD + ANP The sample contains MDMA base 55.57 % m/m. MGUGGY + ANP The powder in this item was found to contain methylenedioxymethylamphetamine (MDMA) at a concentration of 60%. MDMA is a Class A controlled substance under the provisions of the Misuse of Drugs Act 1971 (as amended). MKKKKK + ANP In the test sample 2017/1/SM-3 was detected MDMA MQZPKC + + MDMA-LACTOSE MXTSS3 + -

MYMMDT + ANP

N8QMXC + - SM03 was found to contain MDMA, lactose and trace amounts of N,N dimethyl3,4methylenedioxyamphetamine NRTTXK + ANP Based on the above analysis, the sample was found to contain 3,4-methylenedioxymetamfetamine (MDMA) O0RMCH + ANP the sample contain MDMA O5WQZI + + It has been detected the presence of 3,4-Methylenedioxymetamfetamine in the sample OADJRA + -

OBFIDR + ANP

ODVN18 + + Marquis reagent: MDMA positive result; Cobalt thiocyanate: negative result; GCMS: MDMA (compared with library MS spectrum of MDMA + retention time of reference sample), FTIR: MDMA (compared to IR spectrum of MDMA <-library), FTIR: lactose (see above - SM1/SM2); OFRCFR + + The substance contains %53 MDMA and Lactose OSZNWS + -

P0ADJ0 + ANP Black colour with Marquist's test indicated the possible presence of MDMA. TLC and GC-MS results confirmed the presence of MDMA in SM-3. P3HHYE + ANP

P7LEGU + ANP From GCMS analysis, MDMA was detected P7PCPW + + 57.2% MDMA - - The test sample also contained lactose

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

PBBITB + ANP Controlled drug: MDMA Concentration: approx. 57 % PKQQQQ + - The sample correspond: 3,4-METHYLENDIOXYMETHAMPHETAMINE(MDMA) POEJXP + - MDMA was identified in SM3 and the percentage of MDMA as base was 60.00. PYTTET + ANP

Q4EE4E + + Se realizó pruebas cromáticas de marquis, tiocianato y Simon, pruebas instrumentales GC-MS y FT-IR QGJYGY + - SM 3 contains N_Methyl_3,4 methylenedioxyamphetamine. QI1JNX + ANP IN THE SAMPLE LABELED AS "2017/1/SM-3" WAS DETECTED 3,4- Methylenedioxymetamfetamine (MDMA). QKD30L + - Sample was found to contain 3,4-Methylenedioxymethamphetamine (MDMA) QMZCMA + ANP

QOMHP5 + ANP

QRNQXH + + La muestra es positiva a MDMA y Lactosa QXRKFZ + ANP The sample SM-3 contains a drug 3,4-methykendioxymetamfetamine 53% R8T8AE + ANP The off-white powder was analysed and found to contain 3,4-Methylenedioxymetamfetamine (MDMA). RHYD82 + ANP The sample contains 3,4-Methylenedioxymetamfetamine (MDMA). RNNNVK + ANP One glass bottle containing 0.27 grammes of a powder containing 0.15 grammes of 3,4- methylenedioxymethamphetamine being a compound structurally derived from N-alkyl-alpha- methylphenethylamine by substitution in the ring with an alkyl-enedioxy substituent. RPC9FU + - Confirmed by GS/MS method. Quantification analyses was performed by Gas Chromatography FID. RPPFPC + - Sample SM-3 was found to contain 69.7% MDMA base. RV66P1 + ANP The sample was found to contain a controlled substance within the meaning of the Controlled Drug and Substances Act: Schedule 1 19. (8) N-methyl-3,4-methylenedioxyamphetamine (MDMA) (N,Įdimethyl-1,3-benzodioxole-5-ethanamine) RYB8ZA + + The sample contains MDMA and lactose S27VCS + +

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

S97OK5 + ANP Marquis reagent (MR) positive, CG/MS and mass charge ratio (M/Z) similar Characteristics with the substances used as standard or pattern. SFHFBQ + ANP found MDMA: 58%w/w SGI5IO + + Sample also contain lactose. The presence of drug confirmed by GC-MS and FTIR spectroscopy analysis.The hydrochloride form of 3,4-Methylenedioxymetamfetamine (MDMA) was confirmed by the anion analysis and FTIR spectroscopy. SKSSPS + ANP

SKZHH0 + + Sample 2017/1/SM-3 consists of white powder. 3,4-Methylenedioxy-metamfetamine (MDMA), a prohibited substance included in the National Law for Narcotics, is found to be present in this sample. SSIHCS + + lactose SSSS3S + ANP Item contained a pale cream coloured powder, which was found to contain MDMA, a Class A drug, at a purity of 60 per cent. SWSSOF + ANP SIZE MATERIAL COMPARATION SYNTESI INTERMEDIATES COMPOUNDS IDENTIFICATION (DMMDA) TBUZWG + - The sample was found to contain 3,4-Methylenedioxymetamfetamine (MDMA) TGCAAA + - Marquis Test give black colour.TLC and GCMS used for confirmation.In GCMS Rt:15.379mis,Base peak:58 TTHTMU + ANP Marquis positive (black), Identified by GC-MS TTTTHT + - 59 % of MDMA (free base) TUVU7D + + One brown glass vial with lid, labelled '2017/1/SM-3' and '16', which contained 227 milligrams of off- white powder. This powder contained an average of 64% 3,4-methylenedioxymethylamphetamine hydrochloride (MDMA). MDMA is a Class A controlled drug under the provisions of the Misuse of Drugs Act 1971 (as amended). UBTTQP + + MDMA 64.2% and lactose UDUUW5 + - Test sample 2017/1/SM-3 was confirmed to contain MDMA (3,4- methylenedioxymethamphetamine). MDMA is a DEA Schedule I controlled substance in the United States. UDYUUU + + LACTOSE UFAT5C + - contained MDMA UHBHEQ + ANP The sample contains 66.0% MDMA as base

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

UQYIVP + -

UT2EIQ + + LACTOSE V3JVVY + ANP

V4QVVV + ANP The sample contains 3,4-Methylenedioxymetamfetamine (MDMA). 3,4-Methylenedioxymetamfetamine (MDMA) content (as base)=51.89% by weight VGNZKV + + MDMA IN LACTOSA POWDER VTELFX + + LACTOSE VVJVZV + ANP the White powder contains MDMA (57.2%w/w) which is controlled by national law VVSOI6 + - Examination of the sample coded 2017/1/SM-3 revealed the presence of methylenedioxymetamfetamine (MDMA) VVXRIZ + - (±)-N,Įdimethyl-3,4-(methylenedioxy)phenethylamine VYVVTU + + MDMA HCL, LACTOSA W3O2KM + + Item 2017/SM-3: a fine off white powder which contained 3,4-Methylenedioxymetamphetamine (MDMA) at a concentration of 54% (as base) and also indicated the presence of lactose. 3,4- Methylenedioxymetamphetamine (MDMA) is a class A controlled drug under the provisions of the Misuse of Drugs Act 1971 (as amended). Lactose is not controlled under the provisions of the Misuse of Drugs Act 1971 (as amended). W7U77N + + 3,4-Methylenedioxymetamfetamine (MDMA) was identificated in the sample analyzed. WAYGAS + - 3,4,-methylenedioxymethamphetamine (MDMA) confirmed in the specimen submitted. WD6IRG + - The test sample 2017/1/SM-3 was found to contain 76% MDMA (3,4- Methylenedioxymetamphetamine). WDWUWW + + The substance is MDMA. WTEPTR + + Was found MDMA and Lactose. WTVLQ8 + - 3,4-Methylenedioxymetamfetamine XS2G6M + ANP off-white powder containing MDMA XW94X4 + ANP from screening test using (Marquis reagent (MR)) and ion scan, and from confirmation test using (Gc-Ms) the sample was found to contain the controlled drug (MDMA) XWBZZG + ANP MDMA was DETECTED in sample 2017/1/SM-3.

Code 3,4- Methylenedioxymet Lactose amfetamine (MDMA)

XXYCLX + -

Y1FM12 + + We identified the sample by GC-MS, FTIR and we compared the results with reference material, NIST library AND swgdrugs library. YHAA5A + -

YHNRNC + +

ZDS0S1 + - 216 milligrams of an off-white powder which contained MDMA HCl with a purity of 55% in its base form - Class A controlled drug under the Misuse of Drugs Act 1971 (as amended) ZFBPKW + ANP Presence of MDMA was confirmed qualitatively. ZIWYWS + + ./. ZMVLHU + ANP Sample 2017/1/SM-3 found to contain 3,4-methylenedioxymetamfetamine[MDMA]. ZNWNNS + ANP The powder contains 50.7±2.9 % MDMA-base ZOCUCZ + ANP

ZOSSZI + ANP Sample SM-3 found to contain 56.7 % 3,4-methylenedioxymetamfetamine(MDMA) ZRVVPU + ANP

ZWNZ3Z + ANP White powder containing 59.2%w/w of MDMA ZZVQGW + ANP

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: 184

The response summary of all 204 participating laboratories for the identification of SM-3, frequency of use of screening and identification techniques and false positives and negatives:

Correct identification of Test Sample:

Substance Name Number of laboratories: 3,4-Methylenedioxymetamfetamine (MDMA): 201 Lactose: 62

False positives for Test Sample-3:

Round Code: Substance reported: Tech Code: BSN7V0 Metamfetamine 150/180 FVOURP Heroin 180 HXXSFV MDEA 180 VVJVZV MDEA 180 Q4EE4E MDA 180/190 GBKZCY MDEA 210 P3HHYE MDEA 190

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

Round Code: Tech Code: FVOURP 180

Frequency of use of screening, identification and quantification techniques:

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

Z-Scores for Test Sample 3

MDMA MDMA Deviation Code Concentration Deviation from Code Concentration z-score from robust z-score (mass%) robust average (mass%) average 3AY738 29.89 -26.1 -7.5 ZDS0S1 55 -1.0 -0.3 TTHTMU 36.5 -19.5 -5.6 5QVQHW 55.1 -0.9 -0.3 W7U77N 43.05 -13.0 -3.7 5G3N55 55.1 -0.9 -0.3 UQYIVP 45.37 -10.6 -3.0 5THFBN 55.2 -0.8 -0.2 4FFKBN 47.35 -8.7 -2.5 541LFZ 55.2 -0.8 -0.2 AMECCZ 47.5 -8.5 -2.4 P7LEGU 55.5 -0.5 -0.1 FS5XU9 49 -7.0 -2.0 1HAGZA 55.5 -0.5 -0.1 CJ8TUV 49.7 -6.3 -1.8 9LR9YU 55.5 -0.5 -0.1 ZNWNNS 50.7 -5.3 -1.5 TBUZWG 55.5 -0.5 -0.1 VVSOI6 50.8 -5.2 -1.5 4WF099 55.5 -0.5 -0.1 MKKKKK 51.8 -4.2 -1.2 MDJIDD 55.6 -0.4 -0.1 V4QVVV 51.89 -4.1 -1.2 J9A9TR 55.6 -0.4 -0.1 2SI2CZ 52 -4.0 -1.2 ILLLUA 55.6 -0.4 -0.1 FCCEZJ 52 -4.0 -1.2 IUAAMC 55.7 -0.3 -0.1 DINDT4 52.1 -3.9 -1.1 6A5NIA 55.8 -0.2 -0.1 ZMVLHU 52.2 -3.8 -1.1 AYJ22M 56.0 0.0 0.0 O5WQZI 52.5 -3.5 -1.0 1U0JGG 56.0 0.0 0.0 DVAUDS 52.5 -3.5 -1.0 2B1A92 56.1 0.1 0.0 ZZVQGW 52.56 -3.4 -1.0 A6YPWP 56.2 0.2 0.1 88P8P5 52.6 -3.4 -1.0 UDYUUU 56.3 0.3 0.1 XXYCLX 52.73 -3.3 -0.9 8A5KSA 56.4 0.4 0.1 1S1T1G 52.9 -3.1 -0.9 BSSEUS 56.5 0.5 0.1 CBC8TD 52.95 -3.1 -0.9 PBBITB 56.6 0.6 0.2 QXRKFZ 53 -3.0 -0.9 9T1OWI 56.6 0.6 0.2 OFRCFR 53 -3.0 -0.9 VGNZKV 56.6 0.6 0.2 QKD30L 53.03 -3.0 -0.9 ZOSSZI 56.7 0.7 0.2 AOAPHK 53.1 -2.9 -0.8 SGI5IO 57.0 1.0 0.3 2ACRDL 53.4 -2.6 -0.8 BFED5J 57.0 1.0 0.3 GTGG5G 53.4 -2.6 -0.8 RNNNVK 57.0 1.0 0.3 YHNRNC 53.4 -2.6 -0.8 SKSSPS 57.0 1.0 0.3 333HH3 53.8 -2.2 -0.6 G7772Y 57.2 1.2 0.3 EWPSI1 53.93 -2.1 -0.6 VVJVZV 57.2 1.2 0.3 II3KTK 54 -2.0 -0.6 P7PCPW 57.2 1.2 0.3 W3O2KM 54 -2.0 -0.6 G00C40 57.2 1.2 0.3 TUVU7D 54 -2.0 -0.6 RYB8ZA 57.3 1.3 0.4 SSIHCS 54.21 -1.8 -0.5 QGJYGY 57.3 1.3 0.4 WDWUWW 54.37 -1.6 -0.5 IIIIXI 57.4 1.4 0.4 EC0KNG 54.4 -1.6 -0.5 0GK0Q0 57.9 1.9 0.5 99VFND 54.6 -1.4 -0.4 SFHFBQ 58.0 2.0 0.6 BMG4RM 54.78 -1.2 -0.4 RPC9FU 58.0 2.0 0.6 215ETZ 54.8 -1.2 -0.4 BPCSEV 58.0 2.0 0.6 ZIWYWS 54.8 -1.2 -0.4 5QMBSP 58.1 2.1 0.6 ZOCUCZ 54.86 -1.1 -0.3 9A8CUK 58.2 2.2 0.6 L7MBHE 54.9 -1.1 -0.3 HWVVX1 58.2 2.2 0.6 S27VCS 55 -1.0 -0.3 IUTURP 58.4 2.4 0.7 J7GZ5J 55 -1.0 -0.3 LRNK4C 58.6 2.6 0.7 BWALEI 55 -1.0 -0.3 1UUW16 58.6 2.6 0.7 EEVV4K 55 -1.0 -0.3 TTTTHT 59.0 3.0 0.9

Z-Scores for Test Sample 3

MDMA Deviation Code Concentration from robust z-score (mass%) average JHT4NF 59.0 3.0 0.9 ZWNZ3Z 59.2 3.2 0.9 2TYJEG 59.3 3.3 0.9 EY4TQ0 59.7 3.7 1.1 MQZPKC 59.7 3.7 1.1 MGUGGY 60.0 4.0 1.1 POEJXP 60 4.0 1.1 SSSS3S 60 4.0 1.1 JWJCVR 60.28 4.3 1.2 8A4YUG 60.53 4.5 1.3 KORMOX 61.8 5.8 1.7 YHAA5A 62.47 6.5 1.8 KNNBBF 62.5 6.5 1.9 UBTTQP 64.2 8.2 2.3 OADJRA 64.2 8.2 2.3 UHBHEQ 66 10.0 2.9 N8QMXC 66.33 10.3 3.0 CG1SCE 68.67 12.7 3.6 UFAT5C 69.5 13.5 3.9 RPPFPC 69.73 13.7 3.9 OSZNWS 70.4 14.4 4.1 WD6IRG 76 20.0 5.7 RHYD82 76.65 20.7 5.9 EDCFFF 78 22.0 6.3 HXXSFV 87.63 31.6 9.0 5X7UMS 90.1 34.1 9.7

Robust average = 56.0 % Round: 2017/1 UNODC value = 55.7 % Substance: SM-3; MDMA

4.00 3.9 3.9 3.6 3.0

3.00 2.9 2.3 2.3 1.9 2.00 1.8 1.7 1.3 1.2 1.1 1.1 1.1 1.1 1.1 0.9 0.9

1.00 0.9 0.9 0.7 0.7 0.7 0.6 0.6 0.6 0.6 0.6 0.5 0.4 0.4 0.4 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.3 0.2 0.2 0.2 0.2 0.1 0.1 0.1 0.1 0.0 4.1 5.7 5.9 6.3 9.0 9.7 0.00 7.5 5.6 0.0 0.0 - - 0.1 0.1 - 0.1 0.1 0.1 - 0.1 0.1 0.1 0.1 0.1 ------0.2 0.2 0.3 0.3 - - 0.3 0.3 0.3 0.3 0.3 - - 0.3 0.3 - - - - - 0.4 0.4 0.4 - - - - - 0.4 - 0.5 0.5 - 0.5 - - 0.6 0.6 0.6 0.6 - - - 0.6 - -

-1.00 0.8 0.8 0.8 - - - 0.8 0.9 0.9 0.9 0.9 - 0.9 - - - - 0.9 - 1.0 - 1.0 1.0 1.0 - - - - 1.1 1.1 - 1.2 1.2 - 1.2 - - 1.2 - - 1.5 1.5 - - -2.00 1.8 - 2.0 - 2.4 2.5 - - -3.00 3.0 - 0.6 3.7

-4.00 - IIIIXI II3KTK 2SI2CZ ILLLUA J7GZ5J ZOSSZI SGI5IO FCCEZJ SSIHCS SSSS3S 541LFZ PBBITB SKSSPS BFED5J 2TYJEG 215ETZ J9A9TR XXYCLX VVSOI6 S27VCS ZDS0S1 JHT4NF POEJXP EDCFFF CJ8TUV 88P8P5 6A5NIA BSSEUS VVJVZV IUTURP TTTTHT 3AY738 FS5XU9 1S1T1G EWPSI1 9LR9YU BPCSEV RPPFPC UQYIVP 4FFKBN DINDT4 EEVV4K 2B1A92 8A5KSA G7772Y RYB8ZA EY4TQ0 CG1SCE HXXSFV QXRKFZ BWALEI G00C40 LRNK4C JWJCVR CBC8TD OFRCFR 2ACRDL P7LEGU QGJYGY SFHFBQ RPC9FU UFAT5C QKD30L 5THFBN MDJIDD AYJ22M 1U0JGG 333HH3 99VFND ZOCUCZ 5G3N55 9T1OWI 9A8CUK OADJRA RHYD82 EC0KNG 0GK0Q0 4WF099 8A4YUG YHAA5A KNNBBF UBTTQP 1HAGZA VGNZKV AMECCZ MKKKKK V4QVVV O5WQZI ZIWYWS L7MBHE IUAAMC ZWNZ3Z WD6IRG DVAUDS AOAPHK YHNRNC TUVU7D P7PCPW 5X7UMS GTGG5G A6YPWP RNNNVK 5QMBSP MQZPKC TTHTMU ZMVLHU UHBHEQ OSZNWS TBUZWG UDYUUU HWVVX1 W7U77N ZZVQGW 1UUW16 ZNWNNS N8QMXC KORMOX MGUGGY W3O2KM BMG4RM 5QVQHW WDWUWW

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

Z-Score Report per Sample per Substance

Round: 2017/1 Substance: SM-3; MDMA

Dispersion of z-scores using different analytical techniques for the quantification of MDMA in 2017/1 SM-3 10

2 e 0 scor - z

-2

-4

-6

-8 HPLC GC-FID GC-MS NMR

-10

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

Sample 4 Analysis

Identified substances for Test Sample 4

Code Identified Substances 100JU0 None 1HAGZA CAFFEINE 283GPP None 3ZOPSC No Drugs found 4WF099 No drug 4X449Z None 5A5855 No Controlled substance 5THFBN / 6BUQUQ blank 8A4YUG NOT FOUND 99U99A Not Applicable 9A8CUK No amphetamine type of stimulant/cocaine & no coca product AOGMWK None AYJ22M nothing B6PUEJ NA BBXCFB none BPCSEV No illegal substances detected CG43CR None EC0KNG ---- EDCFFF blank ELGLLX NIL EWPSI1 No found FCCEZJ none FVOURP - G7772Y - HHHGBD Not detected HWVVX1 - IIIIXI no drug IUTURP None JWJCVR None KORMOX none L7MBHE None LIGGG3 BLANK MDJIDD none MGUGGY N/A P0ADJ0 NIl P7LEGU No drug PBBITB - PKQQQQ NO FOUND ABUSE DRUGS QGJYGY No drugs

Code Identified Substances QI1JNX NONE RNNNVK - S97OK5 No controlled substance detected SGI5IO None SSSS3S No controlled drugs detected SWSSOF NO DRUGS FOUND TGCAAA Negative TTTTHT No drugs were found UDUUW5 Amphetamine UFAT5C does not contain controlled substances V3JVVY blank VTELFX No illicit substance W3O2KM Negative W7U77N No drugs were detected. WTEPTR NON DETECTED WTVLQ8 - XW94X4 None XWBZZG None Y1FM12 blank ZRVVPU -

Statement of findings for Test Sample 4

Code [blank sample] 0GK0Q0 The sample 2017/1/SM-4 does not contain any drug in the menu of ICE programme detected by GC/MS and FTIR. 0YYGT3 100JU0 Fine green powder that contains some sugar and no drugs under control. 1HAGZA CAFFEINE IS LISTED IN THE FIRST SCHEDULE OF THE POISON ACT 1952. 1S1T1G The sample contains no drugs 1U0JGG 1UUW16 215ETZ 283GPP A representative sample of the powder was analysed in order to detect the presence of a range of controlled drugs but none were found. 2ACRDL 2B1A92 Plant material 2SI2CZ LACTOSE 2TYJEG 333HH3 3AY738 No drugs were detected in the sample SM-4. 3OFVFV 3UI8PF 3ZOPSC Initially conducted a preliminary test to check in the presence of what kind of product we are.It was not possible to detect any drug using any of the prelimed tests. But later it did if a screening (TLC) where all the samples were prepared using as solvent the dichloromethane and how eluent methanol. A chromatographic Tina was used with the dimensions of 20cm × 20cm and the plate used for the purpose has the dimensions of 10cm × 20cm. In a 2 ml vial weighed 15 milligrams of the product and dissolved in 1.5 ml of the solvent (dichloromethane). With the help of a 5ȝl Micropipette, the specimens were placed on the chromatographic plate and left the same dry for a while. It placed about 80 ml of the solvent in Tina Chromatographic and left the same saturate for about 1 hour. Then the sample was placed in Tina Chromatographic with its lid and left the same elute about 25-30 minutes. At the end, the plate of Tina Chromatographic and left dry for 15 minutes. With the help of a chamber of UV a Ȝof 254 nn managed to visualize the stains on the plate and later do if the revelation of the plaque making use of the reagent of Dragendorf. In the sample 2017/1/SM4 It wasn't possible to sense any drugs. Subsequently, the equipment FTIR is 10 and is 50 in Transmitancia mode mixing the product with KBR and absorbance (ATR) and for sample 2017/1/SM4 It wasn't possible to sense any drugs. 4FFKBN 4PGMZO 4WF099 No drug detected by FTIR and GC/MS. 4X449Z 2017/1/SM-4 does not contain dangerous drug. However, it contains Glucose. 541LFZ 58Y8FL No controlled drugs detected. 5A5855 Does not contain controlled substance. 5G3N55 5QMBSP Without drugs 5QVQHW

Code [blank sample] 5RTTW2 No controlled drugs were detected. 5THFBN 2017/1/SM-4 does not contain any psychoactive substance, blank sample 5X7UMS couldnt detect any drug 6A5NIA 6BUQUQ 7CW6XN In the sample 2017/1/SM-4 was not found controlled substance. 7MAM28 No se detectó 88P8P5 8A4YUG 8A5KSA green herbal powder 99U99A NIL 99VFND 9A8CUK No amphetamine type of stimulant and no coca and coca product was detected in sample 2017/1/SM-4. 9LR9YU 9T1OWI On analysis, no controlled substances detected A3IH33 A6YPWP The sample doesn't contained controlled drugs. AMECCZ AOAPHK AOGMWK The chemical test, the stereomicroscopic observation and the no coincidence between the sample and the reference materials in the same conditions, indicate the non detection of cotrolled substances AYJ22M In the sample was not detected the presence of drugs, it is a unknown plant material. B6PUEJ We did the respect tests and there is not substance controlated. BBXCFB we have not found any controlled drug in SM 4 (44) BFED5J Presence of substances from the ICE menu was not detected in the sample. Blank test sample is plant powder. BJSGWA BMG4RM BPCSEV The sample tested negative for controlled drug screening targeted by the validated assays in our laboratory BSN7V0 BSSEUS BWALEI The sample was analysed and no common controlled drug was detected. C9C8PA NON-CONTROLLED SUBSTANCE CBC8TD I was unable to identify a substance within the meaning of the Controlled Drug and Substances Act or the Prescription Drug List as defined in section A.01.010 of the Food and Drug Regulations. CDDPDD CG1SCE CG43CR SM-4 does not contain any psychotropic substances. CJ8TUV SUGAR

Code [blank sample] CSBOTS It wasn¨t found any contrlled drug after screening, idetification and conformatio analysis. DHIABX The confirmation results were obtained by GC/MS analytical technique, including all the common drugs received in this lab. DINDT4 The sample contains Lactose. DVAUDS E8EF88 NO CONTROLLED DRUGS WERE IDENTIFIED EC0KNG EDCFFF blank EEVV4K ELGLLX The sample 2017/1/SM-4 was found to contain No narcotic drug. EWPSI1 EY4TQ0 F2RYW0 FCCEZJ The sample contains glucose, sucrose, inositol. It seems to be a powder made from a plant. FS5XU9 \\ FVOURP Recherche négative FZJOFH G00C40 It contains a mix of fructose, lactose, sucrose, inositol, maleic acid, L-threonic acid, glycerol G7772Y - GBKZCY RAS GDTQXP the sample was presumed to be a blank. however another confirmation technique is required. GG0XXN The substances that were tested for weren´t found to be present in the sample analysed. GTGG5G Lactose HHHGBD Drugs was not detected into material 2017/1/SM-4. HHPRLM HWVVX1 - HXXSFV IBADIN THIS SAMPLE WAS ANALYZED BY GC MS II3KTK No controlled substances confirmed in 1 unit tested of 1 unit received. IIIIXI There is no drug in the sample. IIORYA ILLLUA green powder containing malic acid, sugars, glycitol and trace of aminoacids IO2NIR We found no substances placed under control in the SM4 sample after GC/MS injection. No controlled drugs in this SM4 sample. IUAAMC powder IUTURP Sample gave negative results on Marquis and Cobalt Thiocyanate. No peak found on GCMS IW9I29 No dangerous drugs detected in SM4 J33P51 J7GZ5J green powder not containing any of the substances listed in Part 2 or 1 J9A9TR

Code [blank sample] JHT4NF JSZRBG Sample 2017/1/SM-4 a green powder gave a negative result for substances under national legislation on drugs JWJCVR Herbal matrix. KFKKJK carried out the physicochemical and instrumental analyzes it is concluded that sample number four does not contain controlled substances KNNBBF In sample 2017/1/SM-4 was not verified the presence of any of the substances listed in the ICE Programme menu KORMOX L7MBHE No controlled drugs detected. L8TNQL Green powder doesn't contain cannabinoids, opiates, cocaine, amphetamines, caffeine neither lidocaine. LIGGG3 LJ1SES LRNK4C MDJIDD The sample contains plant. MGUGGY No controlled substances were detected in the powder in this item. MKKKKK MQZPKC The green powder does not correspond to drugs MXTSS3 negative MYMMDT N8QMXC SM04 was found to be a blank sample free of any drugs or psychotropes NRTTXK Based on the above analysis, the sample was found to not contain any controlled drugs. O0RMCH The sample contain no illegal or controlled substances O5WQZI OADJRA NO substance detected OBFIDR NO SE IDENTIFICO SUSTANCIA CONTROLADA ODVN18 plant material, no substance of importance OFRCFR OSZNWS P0ADJ0 Nil P3HHYE P7LEGU From GCMS analysis, no interested peak was found P7PCPW PBBITB No findings of any controlled drug PKQQQQ TThe sample correspond : MANITOL, INOSITOL, ALBUTEROL, VITAMINE E POEJXP Controlled drugs were not identified. PYTTET Q4EE4E QGJYGY SM 4 contains no drug. QI1JNX IN THE SAMPLE LABELED AS "2017/1/SM-4" NO FORENSICS SUBSTANCES FOUND.

Code [blank sample] QKD30L No controlled drugs were found in the sample QMZCMA We test this sample with the refrence drugs that were available in TLC method and we can not find any drug QOMHP5 QRNQXH La muestra es material vegetal pulverizado QXRKFZ The sample SM-4 is a blank one R8T8AE The green material was analysed for controlled drugs with a negative result. RHYD82 RNNNVK One glass bottle containing 0.22 grammes of a powder, which did not contain any substances controlled under the Dangerous Drugs Ordinance (CAP.134). RPC9FU Performed by GS/MS method. RPPFPC No substance controlled in legislation was found. RV66P1 The sample was analysed and was unable to identify a substance within the meaning of the Controlled Drug and Substances Act or the Prescription Drug List as defined in section A.01.010 of the Food and Drug Regulations. RYB8ZA S27VCS S97OK5 Cobalt Thiocyanate (CT), Marquis Reagent (MR) and Colorimetric Reactions (CR) Negative. CG/MS Retention time and mass charge ratio (M/Z) no coincident with refernce material used as standard or pattern. SFHFBQ SGI5IO Probably blank. SKSSPS SKZHH0 Sample 2017/1/SM-4 consists of green powder. No prohibited substances are detected in this sample. SSIHCS SSSS3S Item contained a green coloured powder/material. No controlled drugs detected SWSSOF TBUZWG No drugs were found in sample TGCAAA Not found drugs in screening and confirmation test TTHTMU Every test and analitical methos gave negative results for drugs TTTTHT Sample doesn`t contain illegal substances TUVU7D One brown glass vial with lid, labelled '2017/1/SM-4' and '15', which contained 230 milligrams of green powder. No controlled drugs were detected in this powder. UBTTQP Inositol UDUUW5 Test sample 2017/1/SM-4 was confirmed to contain amphetamine. Amphetamine is a DEA Schedule II controlled substance in the United States. UDYUUU UFAT5C UHBHEQ No drug detected UQYIVP UT2EIQ SUGAR V3JVVY V4QVVV No controlled substance detected.

Code [blank sample] VGNZKV VTELFX SACCHAROSE, INOSITOL VVJVZV the green powder doesn't contain substances under control by national law VVSOI6 Examination of the sample coded 2017/1/SM-4 did not reveal the presence of any controlled drugs. VVXRIZ VYVVTU W3O2KM Item 2017/1/SM-4 a lumpy green powder was screened for the presence of controlled drugs with negative results- in relation to Misuse of Drugs Act 1971 (as amended). W7U77N No drugs were detected in the sample analyzed. WAYGAS Controlled drug substance not detected within the sample submitted. WD6IRG The test sample 2017/1/SM-4 do not found to contain any controlled drugs mentioned in the list of ICE 2017/1. WDWUWW In the substance no drugs were found. WTEPTR Using GCMS and FTIR, no substances were detected. WTVLQ8 D(+) Mannose XS2G6M green powder- no controlled substances detected XW94X4 no drugs were found XWBZZG No illicit drug was detected in 2017/1/SM-4. XXYCLX Y1FM12 we analyzed this sample by GC-MS, FTIR and colourimetric test YHAA5A the sample is consist of fine grinded herbal material YHNRNC ZDS0S1 230 milligrams of a green powder which was found to be negative. ZFBPKW No substance from ICE menu 2017/01/SM was detected. ZIWYWS ZMVLHU Sample 2017/1/SM-4 did not contain any drugs ZNWNNS ZOCUCZ ZOSSZI No controlled drug was found in the sample SM-4 ZRVVPU ZWNZ3Z green powder not containing any controlled drug ZZVQGW Te powder was supplementary tested on the presence of THC by UPLC-MS-MS(method to differentiate between fiber/drug type)

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: 204

The response summary of all 204 participating laboratories for the identification of SM-4, frequency of use of screening and identification techniques and false positives and negatives:

Identification of Test Sample-4:

Test sample 4 was a blank test sample prepared from damiana leaf

False positives for Test Sample-4:

Round Code: Substance Name: Tech Code: UDUUW5 Amphetamine 180

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

Frequency of use of screening, identification and quantification techniques:

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

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