INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISE (ICE) Summary Report SEIZED MATERIAL 2011/2 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISE (ICE) Table of contents Introduction Page 4 Comments from the International Panel of Forensic Experts Page 4 Codes and Abbreviations Page 5 Sample 1 Analysis Page 6 Identified substances Page 6 Statement of findings Page 9 Identification methods Page 16 Summary Page 19 Z-Scores Page 20 Sample 2 Analysis Page 22 Identified substances Page 22 Statement of findings Page 23 Identification methods Page 29 Summary Page 32 Z-Scores Page 33 Sample 3 Analysis Page 34 Identified substances Page 34 Statement of findings Page 37 Identification methods Page 44 Summary Page 47 Z-Scores Page 48 Sample 4 Analysis Page 50 Identified substances Page 50 Statement of findings Page 53 Identification methods Page 59 Summary Page 62 Z-Scores Page 63 2011/2-SM (2) Copyright (c) 2012 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISE (ICE) Test Samples Information Samples Comments on samples Sample 1 SM1 was prepared from a seizure containing 6.9% w/w cocaine base. The sample also contained caffeine, lidocaine and procaine. Sample 2 SM2 was a blank test sample of glucose containing no substances in the ICE menu. Sample 3 SM3 was prepared from a seizure containing 5.5% w/w amfetamine base. The sample also contained caffeine and creatinine. Sample 4 SM4 was prepared from a sample containing 4.7% w/w ketamine base in glucose. Samples Substances Concentrations Comments on substances Sample 1 Caffeine 0 % Quantification not required. Cocaine 6.9 % Procaine 0 % Quantification not required. Lidocaine (Lignocaine) 0 % Quantification not required. Sample 2 [blank sample] Sample 3 Caffeine 0 % Quantification not required. Amfetamine 5.5 % Sample 4 Ketamine 4.7 % 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. 2011/2-SM (3) Copyright (c) 2012 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISE (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”. These codes will change in 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. 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 133 laboratories in 50 countries. Within the SM test group, samples were sent to 103 laboratories in 43 countries and 97 laboratories (94%) submitted the results of their analysis in time for inclusion in the summary report, with 95 (98%) 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 continue to have difficulty in obtaining import authorization and some delays in the preparation of test samples resulted in an extension of the deadline for submission of results. Qualitative Analysis The results for the qualitative identification of the controlled substances were excellent for SM-1, SM-3 and SM-4, with 98% correctly identifying cocaine in SM-1 and 93% of participants identifying amfetamine in SM-3 and ketamine in SM-4. Additionally, it is encouraging that a high percentage of laboratories identified the 3 additives: caffeine: 91%, lidocaine: 88% and procaine: 75% within SM-1. Within the blank test sample SM-2, there were no false positives for controlled substances on the ICE menu and 2 false positives for additives. Within SM-3 there were three false positive and 6 false negative results. Two false positives were reported for amfetamine in SM-4 and two additional false positive identifications were reported for substances not included in the ICE menu: methylphenidate (SM-3) and prazepam (SM-2), each of which was only reported once. 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, 72 (74%) for SM-1, 57 (59%) for SM-3 and 48 (50%) continues to be encouraging and some 91% of participants overall used GC-MS indicating the availability of a high level of technical expertise. Analysis of the Z-scores showed that 63 out of 72 (88%) of participants provided acceptable quantitative results with Z-scores within 3.5 for cocaine in SM-1, 50 out of 57 (88%) for amfetamine in SM-3 and 42 of 48 (88%) laboratories for ketamine in SM-4. Participants with Z-scores outside acceptable limits should review their quantification procedures. Overall, only 46% of participants carried out quantitation of all 3 samples, and encouragement should be given for those who do carry out quantitative analysis to do so on all samples as this allows them to get a better measure of their performance over time. Also, 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. Participation in ICE also helps in monitoring the effect of corrective actions. 2011/2-SM (4) Copyright (c) 2012 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISE (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 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 2011/2-SM (5) Copyright (c) 2012 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISE (ICE) Identified substances for Test Sample 1 Code Identified Substances 02RPHG Cocaïne 0H0JO1 caffeine, lidocaine, procaine, cocaine 1111NT Cocaine 1ZTSFT COCAINE 2JJ8HU cocaine 2XPJYP Cocaine 3TL3NN Cocaine 4FSWFF cocaïne 4GB444 Cocaine 4O1QQS Cocaine,Caffeine,Lidocaine and Procaine 4PBNK1 cocaine 4R4TLX cocaine 5IGXOG Cocaine Hydrochloride 666Q1T Cocaine, Lidocaine, Levamisol, Procaine, Caffeine 6GSCQF cocaine 6YRT1G Probably cocaine 73CCWP cocaine 76B77M cocaine 7WVOE5 cocaine 88XBE8 Cocaine 8GAURX cocaine hydrochloride 99V493 cocaine AOOEOD Cocaine AQADQV Cocaine AQZK6G Caffein, Cocaine, Lidocaine, Procaine B44PS4 Cocaine B4UUTU caffeine, cocaine and lidocaine BZCDP3 Cocaine CQSFOX Cocaine, lidocaine, procainamide CTMZ2M cocaine hidrochloride CTTOGT cocaine DL3VGI Cocaine (7%), Lidocaine(6%) DZ5DHD cocaine EAAA1A Cocaine EGILJI Cocaine, Procaine and Lidocaine F0XV9S Cocaine, Lidocaine, Procaine F2V4FT Procaïne et caféïne FFYCML Cocaine FGNTSP Cocaine FWFKFG Cocaine 2011/2-SM (6) Copyright (c) 2012 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISE (ICE) Code Identified Substances GBEILS cocaine GKMY4V cocaine GMTGGC cocaine hydrochloride GUBCXC Cocaine HHAPY1 COCAINE HHQBHO Cocaine HNNIXK Cocaine ICKQLL cocaine IKO7ZK Cocaine, Lidocaine, Procaine IYIISS cocaine, lidocaine, caffeine IYZIN8 Cocaine JETQUT cocaine JJIJLJ COCAINE KBBJUV cocaïne KSKMBO cocain KUUG6K cocaine L5OSY0 Cocaine L9SN4N Cocaine LCG7ZT Cocain LKB44Q cocaine LOO8O7 Cocaine, Lidocaine, Caffeine LUXVKH i found caffeine, cocaine, procaine and