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UPLC-MS-MS 检测死后全血案例中的 JWH-018 和 JWH-073。

Detection of JWH-018 and JWH-073 by UPLC-MS-MS in postmortem whole blood casework.

机构信息

AIT Laboratories, Indianapolis, IN 46241, USA.

出版信息

J Anal Toxicol. 2012 Apr;36(3):145-52. doi: 10.1093/jat/bks013.

Abstract

Synthetic cannabinoids have been detected in various herbal blends sold legally in convenience stores, smoke shops, and on the Internet. Many of these compounds have extreme forensic significance. We developed and validated a rapid ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of trace concentrations of two of these compounds, JWH-018 and JWH-073, in human blood. Samples underwent liquid-liquid extraction at pH 10.2 into ethyl ether. Tandem mass spectrometry was performed in positive electrospray ionization mode with multiple reaction monitoring using two transitions and one calculated ion transition ratio for each analyte. Deuterated analogs were used as internal standards. Total run time was 2.6 min. The linear dynamic range was 0.05-50 ng/mL with a limit of detection of 0.01 ng/mL for each analyte. Intra-run imprecision (at two different concentration levels, 2 and 8 ng/mL) was 3.9-10.3% for JWH-018 and 3.5-6.2% for JWH-073. Inter-run imprecision was 6.5-7.2% for JWH-018 and 4.8-5.5% for JWH-073. Intra-run accuracy was 95.9-112.7% for JWH-018 and 92.6-104.7% for JWH-073. Inter-run accuracy was 99.1-107.0% for JWH-018 and 97.7-102.0% for JWH-073. Carryover, exogenous drug interferences, ion suppression and matrix selectivity were also assessed. The method has been applied to postmortem forensic casework received by the laboratory and has proven to be robust and reliable. Concentrations of authentic samples have ranged from 0.1-199 ng/mL for JWH-018 and 0.1-68.3 ng/mL for JWH-073.

摘要

合成大麻素已在便利店、烟店和互联网上销售的各种草药混合物中被检测到。其中许多化合物具有极端的法医学意义。我们开发并验证了一种快速超高效液相色谱-串联质谱法,用于测定人血中两种化合物 JWH-018 和 JWH-073 的痕量浓度。样品在 pH 10.2 下用乙醚进行液-液萃取。串联质谱在正电喷雾电离模式下进行,使用两种过渡和每个分析物的一个计算离子过渡比进行多反应监测。氘代类似物用作内标。总运行时间为 2.6 分钟。线性动态范围为 0.05-50ng/mL,每个分析物的检测限为 0.01ng/mL。JWH-018 的批内精密度(在两个不同浓度水平,2 和 8ng/mL 时)为 3.9-10.3%,JWH-073 的批内精密度为 3.5-6.2%。JWH-018 的批间精密度为 6.5-7.2%,JWH-073 的批间精密度为 4.8-5.5%。JWH-018 的批内准确度为 95.9-112.7%,JWH-073 的批内准确度为 92.6-104.7%。JWH-018 的批间准确度为 99.1-107.0%,JWH-073 的批间准确度为 97.7-102.0%。交叉污染、外源性药物干扰、离子抑制和基质选择性也进行了评估。该方法已应用于实验室收到的法医死后案例,结果证明该方法具有稳健性和可靠性。JWH-018 的真实样品浓度范围为 0.1-199ng/mL,JWH-073 的浓度范围为 0.1-68.3ng/mL。

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