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高效液相色谱-串联质谱法分析毛发中的甲基苯丙胺和苯丙胺手性对映体

[Analysis of methamphetamine and amphetamine chiral enantiomers in hair by high performance liquid chromatography-tandem mass spectrometry].

作者信息

Zhang Yingyi, Li Liang, Xing Xuqin, Zhou Zhengzheng, Ma Ande

机构信息

Department of Hygiene Inspection & Quarantine Science, School of Public Health, Southern Medical University, Guangzhou 510515, China.

Faculty of Forensic Medicine, Zhongshan School of Medicine, Sun Yat-sen University, Guangzhou 510080, China.

出版信息

Se Pu. 2018 Dec 8;36(12):1290-1296. doi: 10.3724/SP.J.1123.2018.08040.

Abstract

A chiral separation method was developed for the analysis of methamphetamine (METH) and amphetamine (AM) in hair by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The samples were extracted using methanol by ultrasonication in a high-temperature water bath. The chromatographic separation was performed on a SUPELCO Astec CHIROIOTIC V2 column with the mobile phase of methanol-20 mmol/L ammonium acetate aqueous solution containing 0.1% (v/v) formic acid (99:1, v/v). All the compounds showed linear relationship in the range of 15-300 ng/mg (>0.99). The limits of detection (LODs) of METH and AM were 0.1 ng/mg and 0.15 ng/mg, respectively. The limits of quantification (LOQs) of METH and AM were 0.4 ng/mg and 0.5 ng/mg, respectively. The inter-day precisions were all ≤ 6.8%, and the intra-day precisions were all ≤ 11.4%. Fifty drug abuse samples were determined by this method. Up to 70% of the cases were determined as -(+)-METH and -(+)-AM, while 18% of the cases were -(+)-METH, -(+)-AM, -(-)-METH and -(-)-AM. The proposed method is rapid, simple, and provides technical support and a scientific basis for the chiral analysis in actual hair samples for forensic toxicant identification.

摘要

建立了一种手性分离方法,用于通过高效液相色谱-串联质谱法(HPLC-MS/MS)分析毛发中的甲基苯丙胺(METH)和苯丙胺(AM)。样品在高温水浴中用甲醇超声提取。色谱分离在SUPELCO Astec CHIROIOTIC V2柱上进行,流动相为含0.1%(v/v)甲酸的甲醇-20 mmol/L醋酸铵水溶液(99:1,v/v)。所有化合物在15 - 300 ng/mg范围内呈线性关系(>0.99)。METH和AM的检测限(LOD)分别为0.1 ng/mg和0.15 ng/mg。METH和AM的定量限(LOQ)分别为0.4 ng/mg和0.5 ng/mg。日间精密度均≤6.8%,日内精密度均≤11.4%。用该方法测定了50份药物滥用样品。高达70%的案例被确定为-(+)-METH和-(+)-AM,而18%的案例为-(+)-METH、-(+)-AM、-(-)-METH和-(-)-AM。该方法快速、简便,为实际毛发样品中用于法医毒物鉴定的手性分析提供了技术支持和科学依据。

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