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液相色谱-高分辨率质谱法测定人发中三种大麻素、两种(-)-反式-Δ-四氢大麻酚代谢物和六种苯丙胺类兴奋剂。

Liquid chromatography-high resolution mass spectrometry for the determination of three cannabinoids, two (-)-trans-Δ-tetrahydrocannabinol metabolites, and six amphetamine-type stimulants in human hair.

机构信息

BK21 PLUS Team for Creative Leader Program for Pharmacomics-based Future Pharmacy and Drug Metabolism and Bioanalysis Laboratory, College of Pharmacy, The Catholic University of Korea, Bucheon 14662, Republic of Korea.

Forensic Chemistry Laboratory, Forensic Science Division, Supreme Prosecutor's Office, Seoul 06590, Republic of Korea.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2020 Jul 15;1149:122157. doi: 10.1016/j.jchromb.2020.122157. Epub 2020 May 19.

Abstract

Since cannabis and amphetamine-type stimulants (ATS) are drugs of abuse used alone and concurrently worldwide, it is important to analyze them simultaneously. However, there are no reports of analytical method for the simultaneous extraction of these compounds and metabolites in hair samples of suspected drug abusers, due to the different chemical properties of acidic and lipophilic cannabinoids, and basic and hydrophilic ATS. We developed a liquid chromatography-high resolution mass spectrometry (LC-HRMS) method for the quantification of cannabidiol (CBD), cannabinol (CBN), (-)-trans-Δ-tetrahydrocannabinol (THC), THC metabolites such as 11-nor-9-carboxy-Δ-tetrahydrocannabinol (THC-COOH) and THC-COOH-glucuronide (THC-COOH-glu), and six ATS of amphetamine, methamphetamine, phentermine, methylenedioxyamphetamine, methylenedioxymethamphetamine, and methylenedioxyethylamphetamine in the least amounts of human hair samples. The pulverized hair samples (10 mg) were extracted with 1 mL of 0.5% formic acid in methanol three times, and the supernatants were evaporated in a stream of nitrogen gas. The residue was dissolved and the aliquot was analyzed by LC-HRMS using positive electrospray ionization and the parallel reaction monitoring mode. The lower limits of quantitation were 0.1 pg mg for THC-COOH and THC-COOH-glu, 4 pg mg for CBD, CBN, and THC, and 10 pg mg for the six ATS. Linearity, accuracy, precision, matrix effect, recovery, and post-preparation stability for the 11 analytes were fully validated. The present method was successfully applied to the determination of 11 analytes in hair samples of 10 suspected drug abusers.

摘要

由于大麻和苯丙胺类兴奋剂(ATS)在全球范围内被单独和同时滥用,因此同时分析它们非常重要。然而,由于酸性和亲脂性大麻素和碱性和亲水性 ATS 的不同化学性质,目前尚无关于同时提取这些化合物和代谢物在疑似药物滥用者头发样本中的分析方法的报道。我们开发了一种液相色谱-高分辨质谱(LC-HRMS)方法,用于定量分析大麻二酚(CBD)、大麻酚(CBN)、(-)-反式-Δ-四氢大麻酚(THC)、THC 代谢物如 11-去甲-9-羧基-Δ-四氢大麻酚(THC-COOH)和 THC-COOH-葡糖苷酸(THC-COOH-glu)以及六种 ATS 安非他命、甲基苯丙胺、苯丁胺、亚甲二氧基苯丙胺、亚甲二氧基甲基苯丙胺和亚甲二氧基乙基苯丙胺。将研磨的头发样本(10 mg)用 1 mL 0.5%甲酸甲醇提取三次,将上清液在氮气流中蒸发。将残渣溶解并等分,通过正电喷雾电离和并行反应监测模式的 LC-HRMS 进行分析。THC-COOH 和 THC-COOH-glu 的定量下限为 0.1 pg mg,CBD、CBN 和 THC 的定量下限为 4 pg mg,六种 ATS 的定量下限为 10 pg mg。11 种分析物的线性、准确性、精密度、基质效应、回收率和制备后稳定性均得到充分验证。该方法成功应用于 10 名疑似药物滥用者头发样本中 11 种分析物的测定。

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