Weinmann W, Renz M, Vogt S, Pollak S
Institut für Rechtsmedizin, Klinikum der Albert-Ludwigs-Universität, Freiburg, Germany.
Int J Legal Med. 2000;113(4):229-35. doi: 10.1007/s004149900098.
A combination of automated solid-phase extraction (SPE) and subsequent two-step derivatisation has been developed for the simultaneous analysis of basic drugs of abuse and cocaine metabolites in serum samples. Substances included in this procedure are morphine, codeine, methadone, cocaine, benzoylecgonine, methylecgonine, amphetamine, methamphetamine, MDMA, MDEA and MDA. SPE with mixed-mode cartridges (RP-C8 and cation-exchange) was fully automated with a Zymark RapidTrace SPE robot. GC/MS analysis was performed after derivatisation with a new two-step reaction by trifluoroacetic anhydride and 2,2,3,3,3-pentafluoropropanol. High recoveries (> 85%) with high reproducibility (CV 1.1-3.8%) were found for all drugs. High correlation coefficients (r > 0.998) were obtained due to the addition of deuterated standards prior to extraction. Experience obtained over 2 years of applying this method to drug analysis in serum is discussed.
已开发出一种将自动化固相萃取（SPE）与后续两步衍生化相结合的方法，用于同时分析血清样本中滥用的碱性药物和可卡因代谢物。该方法所涵盖的物质有吗啡、可待因、美沙酮、可卡因、苯甲酰爱康宁、甲基爱康宁、苯丙胺、甲基苯丙胺、摇头丸、3,4-亚甲基二氧基-N-乙基苯丙胺和3,4-亚甲基二氧基苯丙胺。使用Zymark RapidTrace SPE机器人实现了混合模式柱（反相C8和阳离子交换）的SPE完全自动化。在用三氟乙酸酐和2,2,3,3,3-五氟丙醇进行新的两步反应衍生化后，进行气相色谱/质谱分析。所有药物的回收率均很高（> 85%），重现性也很高（变异系数为1.1 - 3.8%）。由于在萃取前添加了氘代标准品，获得了高相关系数（r > 0.998）。文中讨论了将该方法应用于血清药物分析的两年多来所获得的经验。
