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INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report

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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. 2017/1-SM 2 Copyright (c) 2017 UNODC Introduction An important element of the UNODC International Quality Assurance Programme (IQAP) is the implementation of the International Collaborative Exercises (ICE). The exercises allow laboratories, from both developing and developed countries, to continuously monitor their performance in drug testing on a truly global scale. This report provides information on analytical results of laboratories participating in the Seized Materials (SM) group. In order to maintain confidentiality, the participating laboratories have been assigned random “Web Codes”, which change every round. 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
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