色谱

色谱 ›› 2018, Vol. 36 ›› Issue (12): 1290-1296.DOI: 10.3724/SP.J.1123.2018.08040

• 研究论文 • 上一篇    下一篇

高效液相色谱-串联质谱法分析毛发中甲基苯丙胺和苯丙胺手性对映异构体

张颖怡1, 李良2, 邢旭琴1, 周政政1, 马安德1   

  1. 1. 南方医科大学公共卫生学院卫生检验检疫系, 广东 广州 510515;
    2. 中山大学中山医学院法医学系, 广东 广州 510080
  • 收稿日期:2018-08-27 出版日期:2018-12-08 发布日期:2014-11-06
  • 通讯作者: 马安德,Tel:(020)61648562,E-mail:mandmy@smu.edu.cn
  • 基金资助:

    国家自然科学基金资助项目（81501629）；广东省自然科学基金资助项目（2017A030310051）.

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

ZHANG Yingyi1, LI Liang2, XING Xuqin1, ZHOU Zhengzheng1, MA Ande1   

  1. 1. Department of Hygiene Inspection & Quarantine Science, School of Public Health, Southern Medical University, Guangzhou 510515, China;
    2. Faculty of Forensic Medicine, Zhongshan School of Medicine, Sun Yat-sen University, Guangzhou 510080, China
  • Received:2018-08-27 Online:2018-12-08 Published:2014-11-06
  • Supported by:

    National Natural Science Foundation of China (No. 81501629); National Natural Science Foundation of Guangdong, China (No. 2017A030310051).

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摘要：

建立了高效液相色谱-串联质谱（HPLC-MS/MS）分析毛发中甲基苯丙胺与苯丙胺对映异构体的手性分离方法。采用SUPELCO Astec CHIROBIOTIC® V2手性液相色谱柱，以甲醇-含0.1%（v/v）甲酸的20 mmol/L乙酸铵水溶液（99：1，v/v）为流动相进行手性分离。结果表明，甲醇高温水浴超声法能较好地提取苯丙胺类化合物，且峰形较好（拖尾因子>0.95）。S-（+）-甲基苯丙胺、R-（-）-甲基苯丙胺、S-（+）-苯丙胺和R-（-）-苯丙胺在15~300 ng/mg范围内线性关系良好，相关系数均大于0.99；甲基苯丙胺和苯丙胺的检出限分别为0.1 ng/mg和0.15 ng/mg，定量限分别为0.4 ng/mg和0.5 ng/mg；日内精密度均≤6.8%，日间精密度均≤11.4%。采用所建方法对50余嫌疑人毛发进行手性分析，检出单一S-（+）-甲基苯丙胺和S-（+）-苯丙胺的占70%，同时检出S-（+）-甲基苯丙胺、R-（-）-甲基苯丙胺、S-（+）-苯丙胺和R-（-）-苯丙胺的占18%。该法简单快速，精密度好，可为实际法医毒物鉴定案例中的毛发手性分析提供技术支持与科学依据。

关键词: 苯丙胺, 对映异构体, 高效液相色谱-串联质谱, 甲基苯丙胺, 毛发

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 (r>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 S-(+)-METH and S-(+)-AM, while 18% of the cases were S-(+)-METH, S-(+)-AM, R-(-)-METH and R-(-)-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.

Key words: amphetamine (AM), enantiomers, hair, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), methamphetamine (METH)

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