INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report
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INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report SEIZED MATERIALS 2015/1 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Table of contents Introduction Page 3 Comments from the International Panel of Forensic Experts Page 3 NPS reported by ICE participants Page 4 Codes and Abbreviations Page 7 Sample 1 Analysis Page 8 Identified substances Page 8 Statement of findings Page 12 Identification methods Page 21 Summary Page 26 Z-Scores Page 27 Sample 2 Analysis Page 31 Identified substances Page 31 Statement of findings Page 35 Identification methods Page 44 Summary Page 49 Z-Scores Page 50 Sample 3 Analysis Page 53 Identified substances Page 53 Statement of findings Page 55 Identification methods Page 60 Summary Page 65 Sample 4 Analysis Page 66 Identified substances Page 66 Statement of findings Page 71 Identification methods Page 80 Summary Page 85 Z-Scores Page 86 Full test Samples Information Samples Comments on samples Sample 1 SM-1 was prepared from a seizure containing 5.2 % (w/w) cocaine base. The test sample also contained glucose, caffeine, lidocaine, procaine and trace amounts of creatine and levamisole. Sample 2 SM-2 was prepared from a seizure containing 5.5 % (w/w) amfetamine base. The test sample also contained caffeine and creatine. Sample 3 SM-3 was a blank test sample containing no substances from the ICE menu. Sample 4 SM-4 was prepared from a seizure containing 72.2%(w/w) heroin base. the seizure also contained acetylcodeine, 6-monoacetylmorphine, papaverine, noscapine and trace amounts of morphine. Samples Substances to be identified from ICE menu Concentrations Comments on substances Sample 1 Caffeine 0 % quantification not required Cocaine 5.2 % Lidocaine (Lignocaine) 0 % quantification not required Procaine 0 % quantification not required Sample 2 Amfetamine 5.5 % Caffeine 0 % quantification not required Sample 3 [blank sample] Sample 4 Heroin 72.2 % Morphine minor component 0 % quantification not required 2 2015/1-SM Copyright (c) 2015 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 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 enables 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 2015/1 round of the ICE programme, results were submitted within both the Seized materials (SM) and Biological Specimens (BS) test groups by 207 laboratories in 66 countries. Within the SM test group, there were 177 participating laboratories from 65 countries and within the BS test group, results were submitted by 85 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 (41% of participants), while GC-MS (90%) was the most commonly used technique for identification/confirmation of the components in the test samples followed by FTIR (36%). The results for the qualitative identification of the controlled substances were excellent for all test samples in the SM group as shown in the table 1. Table 1. Performance of participants for the qualitative analysis in the 2015/1 round of ICE. SM-1 SM-2 SM-4 Test sample (Cocaine) (Amfetamine) SM-3 (Blank) (Heroin) Correct identification 98% 92% N/A 98% by participants With regard to the false positive results for controlled substances in the ICE menu there were a total of thirteen, (two each for SM-1 and SM-4, three for SM-2 and six for the blank test sample of plant material (SM-3). There were a total of eighteen false negative results in the three SM test samples containing controlled substances, 67% of which were for SM-2 where the amfetamine was not identified. 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. Quantitative Analysis The proportion of participants who carried out quantitative analysis, 127 (72%) for SM-1, 93 (53%) for SM-2 and 122 (69%) for SM-4 continues to be encouraging, particularly the high percentage of participants who quantified the cocaine in SM-1. It is also encouraging to note that 130 (73%) of participants in the SM test group performed quantitation and of these, 94 (72%) quantified all three test samples. It is understood that quantitative analysis of controlled substances is often governed by local legislation and the requirements of prosecution. With regard to the analytical techniques used by participants performing quantitation, 53% used GC-FID, 27% used HPLC and 19% used GC-MS. z-scores obtained by participants in quantification are shown in the table 2 (Percentage and number of laboratories are indicated). 3 Table 2. Performance of participants for quan titative analysis in the 2015/1 round of ICE . Test sample z-score SM-1 (Cocaine) SM-2 (Amfetamine) SM-4 (Heroin) |z| < 2, satisfactory 81% (103) 82% (76) 80% (98) 2 ≤ |z| ≤ 3, questionable 7% (9) 6% (6) 7% (7) |z| > 3, unsatisfactory 12% (15) 12% (11) 12% (12) 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 2014/2 round of ICE, nine laboratories obtained questionable z-scores with 2 ≤ |z| < 3. Of these laboratories, eight (100%) who performed quantification obtained acceptable z-scores with |z| < 2 in the current 2015/1 round of ICE for at least one substance. However, two of these laboratories still obtained questionable z-scores and two laboratories also obtained unsatisfactory z-scores in 2015/1. Fourteen laboratories obtained unsatisfactory z-scores in ICE 2014/2 with |z| ≥ 3, and of these, ten (71%) improved their performance in quantification in the current 2015/1 ICE round in at least one substance, although seven (50%) still obtained unsatisfactory z-scores in at least one substance in 2015/1. 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. New Psychoactive Substances (NPS) reported by laboratories participating in the 2015/1 round of the ICE programme During the 2015/1 round of ICE, participating laboratories provided information on NPS that had been identified in their laboratories. In total there were 246 reports of 118 substances. The most commonly reported substances were synthetic cannabinoids (33%) followed by synthetic cathinones (29%) and phenethylamine group substances (19%) as shown in figure 1. In general, this is the same trend that was reported in the 2014/2 round of ICE. 4 2% 2% 2% Synthetic cannabinoids 9% Phenethylamines 4% 33% Synthetic cathinones Tryptamines Others Piperazines 29% Ketamine and phencyclidine type substances 19% Aminoindanes Figure 1. NPS reported by ICE laboratories during the 2015/1 round of ICE NPS most commonly reported by laboratories participating in ICE 2015/1 The substance most often reported by ICE participants was the synthetic cathinone methylone followed by the phenethylamines DOC (2,5-Dimethoxy-4-chloroamphetamine) and 25I-NBOMe. These were followed by the synthetic cannabinoids, 5F-AKB-48 and AB-CHMINACA. All these are shown in table 3. Table 3. NPS most commonly reported by ICE participants in the 2015/1 round of ICE Substance IUPAC name Structure 1-(1,3-benzodioxol-5-yl)-2- Methylone (methylamino)propan-1-one 2-(4-iodo-2,5-dimethoxyphenyl)-N-(2- 25I-NBOMe methoxybenzyl)ethan-1-amine 1-(4-chloro-2,5-dimethoxyphenyl)propan-2- DOC amine 5 N-(adamantan-1-yl)-1-(5-fluoropentyl)-1H- 5F-AKB-48 indazole-3-carboxamide (S)-N-(1-amino-3-methyl-1-oxobutan-2-yl)-1- AB-CHMINACA (cyclohexylmethyl)-1H-indazole-3-carboxamide ICE participants can obtain further details of all the NPS reported to UNODC by logging on to the UNODC ICE portal and selecting the icon for the Early Warning Advisory on New Psychoactive Substances 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.