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一种用于筛查和定量毛发中16种合成卡西酮的多分析物液相色谱-串联质谱法:应用于死后案例。

A multi-analyte LC-MS/MS method for screening and quantification of 16 synthetic cathinones in hair: Application to postmortem cases.

作者信息

Freni Francesca, Bianco Sara, Vignali Claudia, Groppi Angelo, Moretti Matteo, Osculati Antonio Marco Maria, Morini Luca

机构信息

Department of Public Health, Experimental and Forensic Medicine, University of Pavia, via Forlanini 12, 27100, Pavia, Italy.

Department of Public Health, Experimental and Forensic Medicine, University of Pavia, via Forlanini 12, 27100, Pavia, Italy.

出版信息

Forensic Sci Int. 2019 May;298:115-120. doi: 10.1016/j.forsciint.2019.02.036. Epub 2019 Feb 28.

DOI:10.1016/j.forsciint.2019.02.036
PMID:30897447
Abstract

A multi-analyte method for detection and quantification of 16 synthetic cathinones (known also as "bath salts") in human hair has been developed and fully validated using liquid chromatography-tandem mass spectrometry system. About 20 mg of hair samples, previously washed and homogenized, were ultrasonicated with 1 mL HCl 0.1 M solution. Samples were then extracted using a solid phase extraction procedure (SPE), taken to dryness and reconstituted in 100 μL mobile phase. Finally, they were directly injected into a liquid chromatographic system, coupled with tandem mass spectrometer detector. The validation criteria parameters were satisfactory according with the international guidelines. A LOQ of 5 pg/mg was obtained for 4-fluoromethcathinone (4-FMC), buphedrone, ethcathinone, methcathinone, mephedrone and naphyrone, while the method proved to be more sensitive for 4-methylethcathinone (4-MEC), methedrone, alpha-pyrrolidinopentiophenone (α-PVP), alpha-pyrrolidinohexiophenone (α-PHP), methylenedioxypyrovalerone (MDPV), butylone, ethylone, 3,4-dimethylmethcathinone (3,4-DMMC), pentedrone and pentylone, reaching a LOQ of 1 pg/mg. Potential use of bath salts was investigated in postmortem cases of young subjects previously tested positive at least to one traditional drug of abuse. Two samples out of 17 cases analyzed provided positive results for synthetic cathinones. One sample has been divided in two segments of 2.5 cm length each. Both segments were positive for 8 different cathinone derivatives, namely: 3,4-DMMC, 4-FMC, 4-MEC, α-PHP, α-PVP, methcathinone, methedrone and pentedrone. The second case provided positive results for ethcathinone.

摘要

已开发出一种用于检测和定量人发中16种合成卡西酮(也称为“浴盐”)的多分析物方法,并使用液相色谱 - 串联质谱系统进行了全面验证。将约20毫克预先洗涤并匀化的头发样品用1毫升0.1 M盐酸溶液超声处理。然后使用固相萃取程序(SPE)提取样品,干燥后再用100微升流动相复溶。最后,将它们直接注入液相色谱系统,并与串联质谱检测器联用。验证标准参数符合国际指南要求。4-氟甲基卡西酮(4-FMC)、丁丙诺啡、乙卡西酮、甲基卡西酮、甲麻黄碱和萘黄酮的定量限为5 pg/mg,而该方法对4-甲基乙卡西酮(4-MEC)、甲基麻黄碱、α-吡咯烷戊酮(α-PVP)、α-吡咯烷己酮(α-PHP)、亚甲基二氧吡咯戊酮(MDPV)、丁酮、乙酮、3,4-二甲基甲基卡西酮(3,4-DMMC)、戊酮和戊基酮更为灵敏,定量限达到1 pg/mg。在先前至少对一种传统滥用药物检测呈阳性的年轻受试者的死后案例中,对浴盐的潜在用途进行了研究。在分析的17个案例中,有2个样本的合成卡西酮检测呈阳性。一个样本被分成两段,每段长2.5厘米。两段均对8种不同的卡西酮衍生物呈阳性,即:3,4-DMMC、4-FMC、4-MEC、α-PHP、α-PVP、甲基卡西酮、甲基麻黄碱和戊酮。第二个案例中乙卡西酮检测呈阳性。

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