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Iqap) International Collaborative Exercises (Ice INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report SEIZED MATERIALS 2014/1 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Table of contents Introduction Page 3 Comments from the International Panel of Forensic Experts Page 4 NPS reported by ICE participants Page 5 Codes and Abbreviations Page 11 Sample 1 Analysis Page 12 Identified substances Page 12 Statement of findings Page 15 Identification methods Page 23 Summary Page 27 Z-Scores Page 28 Sample 2 Analysis Page 30 Identified substances Page 30 Statement of findings Page 34 Identification methods Page 42 Summary Page 46 Z-Scores Page 47 Sample 3 Analysis Page 49 Identified substances Page 49 Statement of findings Page 53 Identification methods Page 61 Summary Page 65 Z-Scores Page 66 Sample 4 Analysis Page 68 Identified substances Page 68 Statement of findings Page 72 Identification methods Page 73 Summary Page 83 Z-Scores Page 84 Test Samples Information Samples Comments on samples Sample 1 SM-1 was prepared from a seizure containing 40.1% w/w 1-(3-chlorophenyl)piperazine base.The seizure also contained glucose. Trace amounts of codeine and morphine were detected upon analysis of a concentrated solution. If detected, the trace components present need not be considered a false positive result. Sample 2 SM-2 was prepared from a seizure containing 73.6% w/w Metamfetamine base.The samples also contain ed glucose and trace amounts of dimethylsulfone. Sample 3 SM-3 was prepared from a seizure containing 16.1% w/w Ketamine base. The seizure also contained lactose. Sample 4 SM-4 was prepared from a seizure containing 75.8% w/w cocaine base and trace amounts of benzoylecgonine and trans-cinnamoylcocaine. Samples Substances Concentrations Comments on substances Sample 1 1-(3-Chlorophenyl)piperazine 40.1 % sample also contained glucose Sample 2 Metamfetamine 73.6 % sample also contained glucose Sample 3 Ketamine 16.1 % Lactose - Sample 4 Cocaine 75.8 % 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. 2014/1-SM Copyright (c) 2014 UNODC 2 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. Revision of calculation of z-scores in ICE Following a recommendation from the International Panel of Forensic Experts and in order to allow ICE participants to interpret their z-scores in line with recommendations in ISO 13528:2005 and ISO/IEC guide 43-1:1997(E), UNODC have introduced an revision to the method used to calculate the z-scores. z-score is a statistical parameter used in proficiency tests and collaborative exercises as a measure of performance in quantitative analysis. They are calculated as: z = (x-X)/ σ̂ where x = result of participant, X = assigned value of component being quantified and σ̂ is the standard deviation for proficiency assessment (SDPA). One of the methods recommended in ISO 13528:2005 for determining the assigned value X is to use the consensus value from participants. Using this method, the SDPA is also calculated from the standard deviation of the results of participants. Initial estimates of X and σ known as x* and s* are calculated as: x* = median of xi (i = 1,2,……p) where p = number of participants s* = 1.483 median of │xi-x*│ Using these estimates, an iterative calculation (for details see ISO13528:2005, Annex C) is carried out to determine the final values of the robust average (x*) and robust standard deviation (s*) and the z-scores are calculated as z = (xi-x*)/s* Consequently z-scores can be interpreted by participants in line with ISO 13528:2005, section 7.4.2 and ISO/IEC guide43-1:1997(E) as follows: |z| < 2 = satisfactory 2 ≤ |z| ≤ 3 = questionable |z| > 3 = unsatisfactory 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. 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 3 Comments from the International Panel of Forensic Experts Participation of Laboratories In the 2014/1 round of the ICE programme, results were submitted within both the Seized Materials (SM) and Biological Specimens (BS) test groups by 182 laboratories in 59 countries. Within the SM test group, there were 151 participating laboratories from 57 countries, representing a 16% increase from the 2013/2 round. Within the BS test group, results were submitted by 72 laboratories from 38 countries, also corresponding to an increase of 16 % in the number of participants compared to the previous round. Qualitative Analysis The most commonly used technique for screening of test samples in the SM test group was the marquis reagent (42% of participants), while GC-MS (89%) was the most commonly used technique for identification/confirmation followed by FTIR (37%). The results for the qualitative identification of the controlled substances were excellent for all test samples in the SM group. 93% and 98% of participants correctly identified the 1-(3-chlorophenyl)piperazine and metamfetamine in SM-1 and SM-2 respectively. It is encouraging to note that 93% of participants identified the 1-(3-chlorophenyl)piperazine (94% identified this substance in 2013/2), indicating a continued excellent level of awareness of participants in the identification of this New Psychoactive Substance (NPS). 97% of participants correctly identified the ketamine in SM-3, an increase from 92% who correctly identified ketamine, when this was last used as a test sample in 2011/2. Finally, 99% of participants identified the cocaine in SM-4. 8 false positive results were reported for the four test samples in the SM group and there were only 7 false negative results. The detection limits of the different analytical techniques were taken into consideration when ascribing false positive results and as such laboratories who detected the trace amounts of Morphine and Codeine in SM-1 need not consider their results as false positives. Quantitative Analysis The proportion of participants who carried out quantitative analysis, 48 (32%) for SM-1, 83 (55%) for SM-2, 69 (46%) for SM-3 and 107 (71%) for SM-4 continues to be encouraging, particularly the high percentage of participants who quantified the cocaine in SM-4. 1-(3-chlorophenyl)piperazine is a relatively new substance In the ICE menu and there was a 5% increase in the number of laboratories who performed quantitative analysis for this drug compared to the previous round. It is also encouraging to note that 111 (74%) of participants in the SM test group performed quantitation. Of these, 38% quantified all test samples and 78% of laboratories quantified at least two of the 4 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, 50% used GC-FID, 24% used HPLC and 19% used GC-MS Analysis of the z-scores showed that 94% of participants provided acceptable quantitative results with |z| < 3 for 1-(3-chlorophenyl)piperazine in SM-1, 89% for metamphetamine in SM-2, 87% for ketamine in SM-3 and 87% for cocaine in SM-4. Laboratories are encouraged to carry out quantification as it can improve the quality of laboratory analyses and can be helpful in assessing the significance of the results. z-score values obtained assist participating laboratories in evaluating their performance and should be monitored over time as part of each laboratory’s quality assurance programme. Participants with z-scores outside acceptable limits should review their quantification procedures. 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 the ICE programme also helps in monitoring the effect of corrective actions. 4 New Psychoactive Substances (NPS) reported by laboratories participating in the 2014/1 round of the ICE programme During the 2014/1 round of ICE, participating laboratories provided information on NPS that had been identified in their laboratories.
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