Heinl Sonja, Lerch Oliver, Erdmann Freidoon
Department of Forensic Toxicology, University Hospital Giessen and Marburg GmbH, Institute of Legal Medicine Giessen, Frankfurter Strasse 58a, 35392 Giessen, Germany
Gerstel GmbH & Co. KG, Eberhard-Gerstel-Platz 1, 45473 Muelheim an der Ruhr, Germany.
J Anal Toxicol. 2016 Sep;40(7):498-503. doi: 10.1093/jat/bkw047. Epub 2016 Jun 25.
The determination of Δ(9)-tetrahydrocannabinol (THC), cannabinol (CBN) and cannabidiol (CBD) in hair is a major routine task in forensic laboratories worldwide. A comprehensively automated liquid-liquid extraction (LLE) method has been developed. The automation was carried out by an x-y-z sample robot equipped with modules capable of shaking, centrifugation and solvent evaporation. It comprises digestion of hair in sodium hydroxide solution, LLE, extract evaporation, reconstitution in silylation reagent, inlet derivatization and GC-MS analysis. Method validation guidelines of the Society for Toxicological and Forensic Chemistry were fulfilled. The limit of quantification (LOQ) was 0.01 ng/mg for THC, 0.06 ng/mg for CBN and 0.03 ng/mg for CBD. This is below the required LOQ for THC (0.02 ng/mg) in medical psychological assessments in Germany. Also it is far below the required LOQ of the Society of Hair Testing of 0.1 ng/mg for THC. Four-round robin tests were passed successfully and several post- and ante-mortem samples were analyzed. To date the method is routinely employed at the Institute of Legal Medicine in Giessen, Germany. To the best of our knowledge, this is the first publication on a comprehensively automated classical LLE workflow in the field of hair analysis.
测定毛发中的Δ(9)-四氢大麻酚(THC)、大麻酚(CBN)和大麻二酚(CBD)是全球法医实验室的一项主要日常工作。现已开发出一种全面自动化的液液萃取(LLE)方法。自动化操作通过配备有能够进行振荡、离心和溶剂蒸发模块的x-y-z样本机器人来完成。该方法包括在氢氧化钠溶液中对毛发进行消解、液液萃取、提取物蒸发、在硅烷化试剂中复溶、进样衍生化以及气相色谱-质谱联用(GC-MS)分析。该方法符合毒理与法医化学协会的方法验证指南。THC的定量限(LOQ)为0.01 ng/mg,CBN为0.06 ng/mg,CBD为0.03 ng/mg。这低于德国医学心理评估中对THC要求的LOQ(0.02 ng/mg)。同时也远低于毛发检测协会对THC要求的LOQ 0.1 ng/mg。成功通过了四轮循环试验,并对多个生前和死后样本进行了分析。迄今为止,该方法已在德国吉森法医学研究所常规使用。据我们所知,这是毛发分析领域关于全面自动化经典液液萃取工作流程的首次发表。