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International Collaborative Exercises (Ice) INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report SEIZED MATERIALS 2013/1 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 Codes and Abbreviations Page 5 Sample 1 Analysis Page 6 Identified substances Page 6 Statement of findings Page 10 Identification methods Page 19 Summary Page 23 Z-Scores Page 24 Sample 2 Analysis Page 27 Identified substances Page 27 Statement of findings Page 30 Identification methods Page 38 Summary Page 42 Z-Scores Page 43 Sample 3 Analysis Page 45 Identified substances Page 45 Statement of findings Page 48 Identification methods Page 56 Summary Page 60 Z-Scores Page 61 Sample 4 Analysis Page 63 Identified substances Page 63 Statement of findings Page 66 Identification methods Page 74 Summary Page 78 Z-Scores Page 79 Test Samples Information Samples Comments on samples Sample 1 SM-1 was prepared from a seizure containing 47.9% Heroin base. The seizure also contained 6- monoacetylmorphine, acetylcodeine, caffeine, papaverine, dextrometorphan and codeine. Trace amounts of morphine and noscapine could also be detected Sample 2 SM-2 was prepared from a seizure containing 68.7% Morphine base. The seizure also contained codeine and trace amounts of 6-monoacetylmorphine and heroin. Sample 3 SM-3 was prepared from a seizure containing 3.7% Nimetazepam. The seizure also contained lactose and glucose Sample 4 SM-4 was prepared from a seizure containing 10.3% Amfetamine base. The seizure also contained sucrose and trace amounts of methamphetamine and diphenylisopropylamine Samples Substances from the ICE Menu Concentrations Comments on substances Sample 1 Heroin 47.9 % Caffeine N/A Sample 2 Morphine 68.7 % Sample 3 Lactose N/A Nimetazepam 3.7 % Sample 4 Amfetamine 10.3 % 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. 2013/1-SM (2) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) 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. Two rounds are offered per year with each round presenting participants with four different test samples for analysis. 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 Samples within both the Seized materials (SM) and Biological Specimens (BS) test groups were sent to 165 laboratories in 57 countries. Within the SM test group, samples were sent to 139 laboratories and 132 laboratories (95%) submitted the results of their analysis in time for inclusion in the summary report, with 128 (97%) using the ICE portal for return of results. The almost universal usage of the ICE portal is a high endorsement of its utility. Some laboratories had difficulty in obtaining import authorization particularly for the new psychoactive substances included in the ICE menu and this resulted in an extension of the deadline for submission of results. It is hoped that these delays will be decreased in the future as both participants and competent authorities become more familiar with the international import/export requirements for these emerging substances. Qualitative Analysis The results for the qualitative identification of the controlled substances were good for all test samples in the SM group. In particular, with correct identification of the heroin in SM-1 and the morphine in SM-2 by 100% and 95% of participants respectively. SM-3 containing nimetazepam and SM-4 containing amphetamine were identified by 91% and 94% of participants respectively. Some 89.4% of participants overall used GC- MS for the qualitative analysis indicating access to this technique which is one of the most commonly used tandem techniques for the confirmation of controlled substances. It is encouraging to note that only six false positive results for controlled substances within the ICE menu were reported for the four test samples in the SM group, while there were a total of 24 false negative results. The seizure used for SM-1 contained at least nine components and 35 laboratories identified the trace amounts of morphine present. Participants who identified the morphine may have in error received a false positive result upon submission of results via the portal. As the amount of morphine present was low, those laboratories who did not identify it need not consider the result a false negative. For SM-4, five laboratories using GC/MS also identified trace amounts of methamphetamine present and similarly, this result need not be considered a false positive. The detection limits of the different analytical techniques shall be taken into consideration when ascribing false positive results in future ICE rounds. Quantitative Analysis A modified Z-score was used for the statistical examination of the quantitative results, as it is a robust method based on absolute deviations from the median of all participant values and is relatively insensitive to outliers. The proportion of participants who carried out quantitative analysis, 90 (68%) for SM-1, 54 (41%) for SM-2, 41 (31%) for SM-3 and 76 (58%) for SM-4 continues to be encouraging. The percentages of laboratories performing quantitative analysis for heroin has remained stable at 68% for ICE 2012/1, 70% for ICE 2012/2 and 68% for this current round. The percentages of laboratories performing quantitative analysis for morphine is also stable at 46% for ICE 2011/1 and 41% for the current round. Similarly, the percentages of laboratories performing quantitative analysis for amphetamine are comparable with 59% for (3) INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) both ICE 2011/2 and 2012/1, and 58% for the current round. Nimetazepam is a new substance on the ICE menu for this current round and it is encouraging to see 31% of laboratory already performing quantitative analysis for this drug. It is understood that quantitative analysis of controlled substances is often governed by local legislation and the prosecution requirements. Analysis of the Z-scores showed that 77 out of 90 (86%) of participants provided acceptable quantitative results with Z-scores within 3.5 for heroin in SM-1, 52 out of 54 (96%) for morphine in SM-2, 32 of 41 (78%) laboratories for nimetazepam in SM-3 and 68 of 76 (87%) for the amphetamine in SM-4. Participants with Z- scores outside acceptable limits should review their quantification procedures. 69% of participants in this round quantified at least one test sample and 30% quantified all four test samples. Z-score values obtained from quantitative analysis assist participating laboratories in evaluating their performance and Z-scores should be monitored over time as part of each laboratory’s quality assurance programme. (4) 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 2013/1-SM (5) Copyright (c) 2013 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Sample 1 Analysis Identified substances for
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