Vaiano Fabio, Busardò Francesco P, Palumbo Diego, Kyriakou Chrystalla, Fioravanti Alessia, Catalani Valeria, Mari Francesco, Bertol Elisabetta
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.
J Pharm Biomed Anal. 2016 Sep 10;129:441-449. doi: 10.1016/j.jpba.2016.07.009. Epub 2016 Jul 7.
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).
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)。