INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Summary Report SEIZED MATERIALS 2017/2 INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Table of contents Introduction 3 Page Comments from the International Panel of Forensic Experts Page 3 NPS reported by ICE participants Page 5 Codes and Abbreviations Page 7 Sample 1 Analysis Page 8 Identified substances Page 8 Statement of findings Page 13 Identification methods Page 23 Summary Page 29 Z-Scores Page 30 Sample 2 Analysis Page 33 Identified substances Page 33 Statement of findings Page 38 Identification methods Page 48 Summary Page 54 Z-Scores Page 55 Sample 3 Analysis age P 58 Identified substances Page 58 Statement of findings Page 63 Identification methods Page 73 Summary Page 79 Z-Scores Page 80 Sample 4 Analysis Page 84 Identified substances Page 84 Statement of findings Page 86 Identification methods Page 92 Summary Page 98 Test Samples Information Samples Comments on samples Sample 1 SM-1 was prepared from a seizure containing 31.3 % (w/w) 3,4-methylenedioxypyrovalerone base. The test sample also contained lactose. Sample 2 SM-2 was prepared from a seizure containing 5.6 % (w/w) amfetamine base. The test sample also contained caffeine and creatine. Sample 3 SM-3 was prepared from a seizure containing 39.9 % (w/w) metamfetamine base. The test sample also contained lactose. Sample 4 SM-4 was a blank test sample of damiana leaf and contained no substances from the ICE menu Samples Substances Concentrations Comments on substances Sample 1 3,4-Methylenedioxypyrovalerone 31.3 % Lactose - Sample 2 Amfetamine 5.6 % Sample 3 Lactose - Metamfetamine 39.9 % Sample 4 [blank sample] - 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. 2017/2-SM 2 Copyright (c) 2018 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. 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. The ICE programme is a UNODC mandated activity and is implemented through regular budget funds and through the UNODC Global Scientific and Forensic Programme – Support Project (GLOU54), which operationalizes the forensic aspects of the UNODC Thematic Programme on Research, Trend Analysis and Forensics" Comments from the International Panel of Forensic Experts Participation of Laboratories In the 2017/2 round of the ICE programme, results were submitted within both the Seized Materials (SM) and Biological Specimens (BS) test groups by 241 laboratories in 74 countries. Within the SM test group, there were 200 participating laboratories from 68 countries and within the BS test group, results were submitted by 95 laboratories from 43 countries. Qualitative Analysis The analytical technique most commonly used for screening of test samples in the SM test group was the marquis reagent (39% of participants), while GC-MS (88% of participants) was the most commonly used technique for identification/confirmation of the components in the test samples followed by FTIR (39% 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 2017/2 round of ICE. SM-1 SM-2 SM-3 SM-4 Test sample (MDPV) (Amfetamine) (Metamfetamine) (Blank) Correct identification by 97% 94% 100% 99% participants Number of false 10 5 1 1 positives Number of false 3 11 0 1 negatives Number of Analyses not 3 3 0 0 performed With regard to false negative results reported, there were a total of fifteen (three for SM-1, eleven for SM-2 and one for SM-4). In total, there were seventeen false positive results for controlled substances or new psychoactive substances. The overall number of false positive/negative results reported by ICE participants continues to be low and while this is encouraging, 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. While there were only a total of six analyses not performed, ICE participants should notethat test samples can contain any of the substances in the ICE menu and screening and identificationcarried out should take this into account. 2017/2-SM 3 Copyright (c) 2018 UNODC INTERNATIONAL QUALITY ASSURANCE PROGRAMME (IQAP) INTERNATIONAL COLLABORATIVE EXERCISES (ICE) Quantitative Analysis The number of participants who carried out quantitative analysis, 49 (25%) for SM-1, 98 (50%) for SM-2 and 103 (53%) for SM-3 continues to be encouraging. It is also encouraging that 113 (58%) of participants in the SM test group performed quantitation and of these, 88 (78%) quantified more than one substance and 49 (43%) 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, 50% used GC-FID, 27% used HPLC and 21% used mass spectrometry. z-scores obtained by participants in quantification are shown in table 2 below. Table 2. Quantitative performance of participants in the 2017/2 round of ICE. Test sample z-score SM-1 SM-2 SM-3 SM-4 (MDPV) (Amfetamine) (Metamfetamine) (Blank) |z| < 2, satisfactory 80% 81% 83% - 2 ≤ |z| ≤ 3, questionable 2% 8% 7% - |z| > 3, unsatisfactory 18% 11% 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 2017/1 round of ICE, twenty one laboratories obtained questionable z-scores with 2 ≤ |z| < 3. Eleven of these laboratories participated and performed quantification in the 2017/2 round with ten (91%) laboratories improving their performance and obtaining acceptable z-scores with |z| < 2 for at least one substance. Six (55%) of these laboratories also obtained unsatisfactory z-scores and one (9%) laboratory obtained a questionable z-score in 2017/2. 23 laboratories obtained unsatisfactory z-scores in ICE 2017/1 with |z| ≥ 3. Of these laboratories, 11 participated in ICE 2017/2 and performed quantification, with seven (64%) improving their performance in at least one substance. Seven (64%) of these laboratories also obtained an unsatisfactory z-score in the 2017/2 round and three (27%) obtained questionable z-scores. The following laboratories obtained a single action signal or warning signal in the two successive rounds of 2017/1 and 2017/2 and shall take this as an anomaly, which requires further investigation: GLXRWX, VYHLIW, SSNSSS, RYT9EQ, UK1I4W, 6Y22ZW, TFIEH5, EP44XZ, 1M08A3, LDL46L, P9VJ99, 1M08A3, KR7NVL, VQI99W, ZM999M, BPKXUS, WWT4QM. Of the laboratories that obtained a single action or warning signal in ICE rounds 2016/2 and 2017/1, the following also obtained an action or warning signal in 2017/2 GLXRWX, KR7NVL, 6Y22ZW, TFIEH5, BPKXUS. 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