INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report SEIZED MATERIALS 2016/1 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Table of contents Sample 1 Analysis Page 6 Identified substances Page 6 Statement of findings Page 11 Identification methods Page 20 False positives Page 26 Z-Scores Page 27 Sample 2 Analysis Page 31 Identified substances Page 31 Statement of findings Page 36 Identification methods Page 46 False positives Page 52 Z-Scores Page 53 Sample 3 Analysis Page 56 Identified substances Page 56 Statement of findings Page 61 Identification methods Page 70 False positives Page 76 Z-Scores Page 77 Sample 4 Analysis Page 80 Identified substances Page 80 Statement of findings Page 82 Identification methods Page 88 False positives Page 94 Z-Scores Page 95 Test Samples Information Samples Comments on samples Sample 1 SM-1 was prepared from a seizure containing 50.5 % (w/w) Cocaine base. The test sample also contained caffeine and levamisole. Benzoylecgonine and cinnamoyl cocaine were also detected as minor components. Sample 2 SM-2 was prepared from a seizure containing 13.8 % (w/w) MDMA. The test sample also contained lactose. Sample 3 SM-3 was prepared from a seizure containing 5.5 % (w/w) Amfetamine base. The test sample also contained caffeine and creatine. Sample 4 SM-4 wss a blank test sample prepared from plant material and contained no substances from the ICE menu Samples Substances Concentrations Comments on substances Sample 1 Caffeine - Quantification not required Cocaine 50.5 % Sample 2 3,4-Methylenedioxymetamfetamine (MDMA) 13.8 % Lactose - Quantification not required Sample 3 Amfetamine 5.5 % Caffeine - Quantification not required Sample 4 [blank sample] 2 2016/1-SM Copyright (c) 2016 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 2016/1 round of the ICE programme, results were submitted within both the Seized Materials (SM) and Biological Specimens (BS) test groups by 220 laboratories in 68 countries. Within the SM test group, there were 183 participating laboratories from 65 countries and within the BS test group, results were submitted by 92 laboratories from 46 countries. Qualitative Analysis The analytical technique most commonly used for screening of test samples in the SM test group was the marquis reagent (40% of participants), while GC-MS (91% of participants) was the most commonly used technique for identification/confirmation of the components in the test samples followed by FTIR (43% of participants). The results for the qualitative identification of the controlled substances in the SM test group, the number of false positive/negative results and the analyses not performed are shown in the table 1. Table 1. Performance of participants in the 2015/2 round of ICE. SM-1 SM-2 SM-3 Test sample SM-4 (blank) (Cocaine) (MDMA) (Amfetamine) Correct identification by 100% 98% 93% N/A participants Number of false positives 3 4 7 14 Number of false negatives 0 2 9 - Number of Analyses not performed 0 2 2 - While the overall number of false positive/negative results reported by ICE participants is encouragingly low, laboratories reporting false positive or false negative results should investigate the reasons for this and corrective actions should be taken in order to continuously improve performance. There were only a total of four analyses not performed. ICE participants should note that test samples can contain any of the substances in the ICE menu and screening and identification carried out should take this into account. Quantitative Analysis The number of participants who carried out quantitative analysis, 126 (69%) for SM-1, 107 (58%) for SM-2 and 94 (51%) for SM-3 continues to be encouraging, particularly the high percentage of participants who quantified the cocaine in SM-1. It is also encouraging that 130 (71%) of participants in the SM test group 3 performed quantitation and of these, 110 (84%) quantified more than one substance and 87 (67%) quantified all three test samples containing controlled substances. It is understood that quantitative analysis of controlled substances is often governed by local legislation and the requirements of prosecution. With regard to the analytical techniques used by participants performing quantitation, 53% used GC-FID, 29% used HPLC and 18% used mass spectrometry. z-scores obtained by participants in quantification are shown in table 2 below. Table 2. Quantitative performance of participants in the 2016/1 round of ICE. Test sample z-score SM-1 SM-2 SM-3 SM-4 (Cocaine) (MDMA) (Amfetamine) (Blank) |z| < 2, satisfactory 83% 87% 81% 2 ≤ |z| ≤ 3, questionable 6% 8% 9% |z| > 3, unsatisfactory 11% 5% 10% According to the recommendations in ISO 13528:2005, an unsatisfactory z-score is considered to give an action signal and a questionable z-score is considered to give a warning signal. A single action signal or warning signals in two successive rounds shall be taken that an anomaly has occurred that requires investigation. Participants with z-scores outside acceptable limits should review their quantification procedures. In the 2015/2 round of ICE, 16 laboratories obtained questionable z-scores with 2 ≤ |z| < 3. 13 of these laboratories participated and performed quantification in the 2016/1 round with 11, (84%) improving their performance and obtaining acceptable z-scores with |z| < 2 for at least one substance. Four of these laboratories also obtained questionable z-scores and five laboratories also obtained unsatisfactory z-scores in 2016/1. 25 laboratories obtained unsatisfactory z-scores in ICE 2015/2 with |z| ≥ 3. Of these laboratories, 15 participated in ICE 2016/1 and performed quantification, with 14 (93%) improving their performance in at least one substance. Seven (47%) of these laboratories also obtained an unsatisfactory z-score in the 2016/1 round of the ICE programme Laboratories that need to perform quantitation routinely are encouraged to participate regularly in external proficiency testing or collaborative exercises such as the ICE programme. This will enable laboratories to assess the quality of their quantitative methods through the z-score values obtained. In addition to the use of z-scores as a measure of performance in quantitation, participants are encouraged to compare their results with the assigned values provided in individual quantification reports, to assess the accuracy of their quantitative performance. Laboratories reporting false positive or false negative results should investigate the root causes and corrective actions taken promptly in order to continuously improve performance. Participation in the ICE programme also helps in monitoring the effect of corrective actions. UNODC would like to acknowledge the valuable contribution of the Chemical Metrology Laboratory of the Health Sciences Authority, Singapore, for the provision of specific software used for the quantitative statistical calculations in the ICE programme. New Psychoactive Substances (NPS) reported by laboratories participating in the 2016/1 round of the ICE programme During the 2016/1 round of ICE, participating laboratories provided information on NPS that had been identified in their laboratories. In total there were 214 reports of 136 substances. The most commonly reported substances were synthetic cathinones (33%) followed by synthetic cannabinoids (30%) as shown in figure 1. 4 Synthetic cannabinoids 5% 1% 1% 3% Synthetic cathinones 32% 15% Phenethylamines Others Piperazines 10% Ketamine and phencyclidine type substances Aminoindanes 33% Tryptamines Figure 1. NPS reported by ICE laboratories during the 2016/1 round of ICE In terms of the mechanism of action of the NPS reported by ICE participants, the predominant substances reported were stimulants (52%), while 30% were synthetic cannabinoid receptor agonists (SCRA’s) and 6% were dissociative substances as shown in figure 2. 3% 6% 4% 5% Stimulants 52% SCRAs Hallucinogens Sedatives/Hypnotics Dissociatives Opioids 30% Figure 2. Mode of action of NPS most commonly reported by ICE participants in the 2016/1 round of ICE 5 NPS most commonly reported by laboratories participating in ICE 2016/1 The substance most often reported by ICE participants was the stimulant ethylone followed by the dissociative ketamine and the