Lock Eric, Aalberg Laura, Andersson Kjell, Dahlén Johan, Cole Michael D, Finnon Yvonne, Huizer Henk, Jalava Kaisa, Kaa Elisabet, Lopes Alvaro, Poortman-van der Meer Anneke, Sippola Erkki
Institut de Police Scientifique, University of Lausanne, Bâtiment de Chimie, CH-1015 Lausanne-Dorigny, Switzerland.
Forensic Sci Int. 2007 Jun 14;169(1):77-85. doi: 10.1016/j.forsciint.2006.10.019. Epub 2006 Dec 18.
This paper is the fifth in a series of six in relation to the development of a harmonised method for the profiling of amphetamine [L. Aalberg, K. Andersson, C. Bertler, H. Borén, M.D. Cole, J. Dahlén, Y. Finnon, H. Huizer, K. Jalava, E. Kaa, E. Lock, A. Lopes, A. Poortman-van der Meer, E. Sippola, Development of a harmonised method for the profiling of amphetamines I. Synthesis of standards and compilation of analytical data, Forensic Sci. Int. 149 (2005) 219-229; L. Aalberg, K. Andersson, C. Bertler, M.D. Cole, Y. Finnon, H. Huizer, K. Jalava, E. Kaa, E. Lock, A. Lopes, A. Poortman-van der Meer, E. Sippola, J. Dahlén, Development of a harmonised method for the profiling of amphetamines II. Stability of impurities in organic solvents, Forensic Sci. Int. 149 (2005) 231-241]. The third paper [K. Andersson, K. Jalava, E. Lock, L. Aalberg, Y. Finnon, H. Huizer, E. Kaa, A. Lopes, A. Poortman-van der Meer, M.D. Cole, J. Dahlén, E. Sippola, Development of a harmonised method for the profiling of amphetamines III. Development of the gas chromatographic method, Forensic Sci. Int., in press] dealt with the optimisation of the gas chromatographic and detection methods whereas the fourth paper [K. Andersson, K. Jalava, E. Lock, Y. Finnon, S. Stevenson, L. Aalberg, H. Huizer, E. Kaa, A. Lopes, A. Poortman-van der Meer, M.D. Cole, J. Dahlén, E. Sippola, Development of a harmonised method for the profiling of amphetamines IV. Optimisation of sample preparation, Forensic Sci. Int., in press] concerned the optimisation of the extraction method prior to GC analysis. This paper is a study of the optimised method in order to determine its stability. Investigations of within and between day variations were carried out in four laboratories. Moreover, variations between laboratories were also determined. Both flame ionisation detector (FID) and MS detection were used. One laboratory studied nitrogen-phosphorous detector (NPD) detection as well. For this task, 12 batches of amphetamine were prepared. Six of them were synthesised via the Leuckart route, three via the nitrostyrene route and three via the reductive amination route [A.M.A. Verweij, Impurities in illicit drug preparations: amphetamine and methamphetamine, Forensic Sci. Rev. 1 (1989) 2-11]. Taking into account all studied target compounds and the average results from four laboratories, the within day variation was around 6% for FID and 5% for MS, the between days variation was around 10% for FID and 8% for MS. For NPD detection, within day variation was 5% and between days variation 9% (only one laboratory). Finally, the inter-laboratory variation was about 12% for FID (four laboratories) and 10% for MS (three laboratories).
本文是关于苯丙胺剖析统一方法开发的六篇系列论文中的第五篇[L. 阿尔贝格、K. 安德森、C. 贝特勒、H. 博伦、M.D. 科尔、J. 达伦、Y. 芬农、H. 胡伊泽、K. 亚拉瓦、E. 卡阿、E. 洛克、A. 洛佩斯、A. 波特曼 - 范德米尔、E. 西波拉，苯丙胺剖析统一方法的开发I. 标准品的合成与分析数据的汇编，《法医学国际》149 (2005) 219 - 229；L. 阿尔贝格、K. 安德森、C. 贝特勒、M.D. 科尔、Y. 芬农、H. 胡伊泽、K. 亚拉瓦、E. 卡阿、E. 洛克、A. 洛佩斯、A. 波特曼 - 范德米尔、E. 西波拉、J. 达伦，苯丙胺剖析统一方法的开发II. 有机溶剂中杂质的稳定性，《法医学国际》149 (2005) 231 - 241]。第三篇论文[K. 安德森、K. 亚拉瓦、E. 洛克、L. 阿尔贝格、Y. 芬农、H. 胡伊泽、E. 卡阿、A. 洛佩斯、A. 波特曼 - 范德米尔、M.D. 科尔、J. 达伦、E. 西波拉，苯丙胺剖析统一方法的开发III. 气相色谱法的开发，《法医学国际》，待发表]论述了气相色谱和检测方法的优化，而第四篇论文[K. 安德森、K. 亚拉瓦、E. 洛克、Y. 芬农、S. 史蒂文森、L. 阿尔贝格、H. 胡伊泽、E. 卡阿、A. 洛佩斯、A. 波特曼 - 范德米尔、M.D. 科尔、J. 达伦、E. 西波拉，苯丙胺剖析统一方法的开发IV. 样品前处理的优化，《法医学国际》，待发表]关注的是气相色谱分析之前萃取方法的优化。本文是对该优化方法稳定性的一项研究。在四个实验室进行了日内和日间变化的调查。此外，还测定了实验室间的差异。同时使用了火焰离子化检测器（FID）和质谱检测。有一个实验室还研究了氮磷检测器（NPD）检测。为此任务，制备了12批苯丙胺。其中6批通过勒卡特路线合成，3批通过硝基苯乙烯路线合成，3批通过还原胺化路线合成[A.M.A. 韦尔韦伊，非法药物制剂中的杂质：苯丙胺和甲基苯丙胺，《法医学评论》1 (1989) 2 - 11]。考虑到所有研究的目标化合物以及四个实验室的平均结果，FID的日内变化约为6%，MS的日内变化约为5%；FID的日间变化约为10%，MS的日间变化约为8%。对于NPD检测，日内变化为5%，日间变化为9%（仅一个实验室）。最后，FID的实验室间差异约为12%（四个实验室），MS的实验室间差异约为10%（三个实验室）。
