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一种通过液相色谱-串联质谱法筛查血液中64种新型精神活性物质和5种苯丙胺类物质的新方法及其在实际案例中的应用。

A novel screening method for 64 new psychoactive substances and 5 amphetamines in blood by LC-MS/MS and application to real cases.

作者信息

Vaiano Fabio, Busardò Francesco P, Palumbo Diego, Kyriakou Chrystalla, Fioravanti Alessia, Catalani Valeria, Mari Francesco, Bertol Elisabetta

机构信息

Department of Health Science, University of Florence, Italy.

Unit of Forensic Toxicology (UoFT) - Department of Anatomical Histological, Forensic and Orthopaedic Sciences, Sapienza University of Rome, Italy.

出版信息

J Pharm Biomed Anal. 2016 Sep 10;129:441-449. doi: 10.1016/j.jpba.2016.07.009. Epub 2016 Jul 7.

Abstract

Identification and quantification of new psychoactive substances (NPS), both in biological and non-biological samples, represent a hard challenge for forensic toxicologists. NPS are increasingly emerging on illegal drug market. Many cases of co-consumption of NPS and other substances have also been reported. Hence, the development of analytical methods aiming at the detection of a broad-spectrum of compounds (NPS and "traditional" drugs) could be helpful. In this paper, a fully validated screening method in blood for the simultaneous detection of 69 substances, including 64 NPS (28 synthetic cannabinoids, 19 synthetic cathinones, 5 phenethylamines, 3 indanes, 2 piperazines, 2 tryptamines, 2 phencyclidine, methoxetamine, ketamine and its metabolite) and 5 amphetamines (amphetamine, methamphetamine, MDMA, MDA, 3,4-methylenedioxy-N-ethylamphetamine - MDEA-) by a dynamic multiple reaction monitoring analysis through liquid chromatography - tandem mass spectrometry (LC-MS/MS) is described. This method is very fast, easy to perform and cheap as it only requires the deproteinization of 200μL of blood sample with acetonitrile. The chromatographic separation is achieved with a C18 column. The analysis is very sensitive, with limits of quantification ranging from 0.1 to 0.5ng/mL. The method is linear from 1 to 100ng/mL and the coefficient of determination (R(2)) was always above 0.9900. Precision and accuracy were acceptable at any quality control level and recovery efficiency range was 72-110%. Matrix effects did not negatively affect the analytical sensitivity. This method was successfully applied to three real cases, allowing identification and quantification of: mephedrone and methamphetamine (post-mortem); ketamine, MDMA and MDA (post-mortem); AB-FUBINACA (ante-mortem).

摘要

在生物和非生物样本中识别和定量新型精神活性物质(NPS),对法医毒理学家来说是一项艰巨的挑战。NPS在非法毒品市场上日益涌现。也有许多NPS与其他物质共同使用的案例报道。因此,开发旨在检测广谱化合物(NPS和“传统”毒品)的分析方法可能会有所帮助。本文描述了一种经过全面验证的血液筛查方法,通过液相色谱-串联质谱(LC-MS/MS)的动态多反应监测分析同时检测69种物质,包括64种NPS(28种合成大麻素、19种合成卡西酮、5种苯乙胺、3种茚满、2种哌嗪、2种色胺、2种苯环己哌啶、甲氧基苯丙胺、氯胺酮及其代谢物)和5种苯丙胺类药物(苯丙胺、甲基苯丙胺、摇头丸、MDA、3,4-亚甲基二氧基-N-乙基苯丙胺 - MDEA-)。该方法非常快速、易于操作且成本低廉,因为它只需要用乙腈对200μL血液样本进行去蛋白处理。使用C18柱实现色谱分离。该分析非常灵敏,定量限范围为0.1至0.5ng/mL。该方法在1至100ng/mL范围内呈线性,测定系数(R²)始终高于0.9900。在任何质量控制水平下,精密度和准确度均可接受,回收率范围为72-110%。基质效应未对分析灵敏度产生负面影响。该方法成功应用于三个实际案例,实现了以下物质的识别和定量:甲氧麻黄酮和甲基苯丙胺(死后);氯胺酮、摇头丸和MDA(死后);AB-FUBINACA(生前)。

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