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尿液中61种合成大麻素代谢物定性分析的固相萃取-液相色谱-串联质谱法

Solid-phase extraction-liquid chromatography-tandem mass spectrometry method for the qualitative analysis of 61 synthetic cannabinoid metabolites in urine.

作者信息

Gaunitz Franziska, Kieliba Tobias, Thevis Mario, Mercer-Chalmers-Bender Katja

机构信息

Institute of Legal Medicine, Faculty of Medicine, University of Cologne, Cologne, Germany.

Institute of Biochemistry, German Sport University Cologne, Cologne, Germany.

出版信息

Drug Test Anal. 2020 Jan;12(1):27-40. doi: 10.1002/dta.2680. Epub 2019 Oct 18.

Abstract

This article comprises the development and validation of a protocol for the qualitative analysis of 61 phase I synthetic cannabinoid metabolites in urine originating from 29 synthetic cannabinoids, combining solid-phase extraction (SPE) utilizing a reversed phase silica-based sorbent (phenyl) with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Validation was performed according to the guidelines of the German Society of Toxicological and Forensic Chemistry. Sufficient chromatographic separation was achieved within a total runtime of 12.3 minutes. Validation included specificity and selectivity, limit of detection (LOD), recovery and matrix effects, as well as auto-sampler stability of processed urine samples. LOD ranged between 0.025 ng/mL and 0.5 ng/mL in urine. Recovery ranged between 43% and 97%, with only two analytes exhibiting recoveries below 50%. However, for those two analytes, the LODs were 0.05 ng/mL in urine. In addition, matrix effects between 81% and 185% were determined, whereby matrix effects over 125% were observed for 10 non-first-generation synthetic cannabinoid metabolites. The developed method enables the rapid and sensitive detection of synthetic cannabinoid metabolites in urine, complementing the spectrum of existing analytical tools in forensic case work. Finally, application to 61 urine samples from both routine and autopsy case work yielded one urine sample that tested positive for ADB-PINACA N-pentanoic acid.

摘要

本文介绍了一种用于定性分析源自29种合成大麻素的尿液中61种I期合成大麻素代谢物的方法的开发与验证,该方法将使用反相硅胶基吸附剂(苯基)的固相萃取(SPE)与液相色谱-串联质谱(LC-MS/MS)相结合。验证是根据德国毒理学和法医化学学会的指南进行的。在12.3分钟的总运行时间内实现了充分的色谱分离。验证包括特异性和选择性、检测限(LOD)、回收率和基质效应,以及处理后尿液样本的自动进样器稳定性。尿液中的LOD在0.025 ng/mL至0.5 ng/mL之间。回收率在43%至97%之间,只有两种分析物的回收率低于50%。然而,对于这两种分析物,尿液中的LOD为0.05 ng/mL。此外,还测定了81%至185%的基质效应,其中10种非第一代合成大麻素代谢物的基质效应超过125%。所开发的方法能够快速、灵敏地检测尿液中的合成大麻素代谢物,补充了法医案件工作中现有分析工具的范围。最后,将该方法应用于61份来自常规和尸检案件工作的尿液样本,发现有一份尿液样本检测出ADB-PINACA N-戊酸呈阳性。

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