法医学杂志

法医学杂志 ›› 2017, Vol. 33 ›› Issue (6): 619-621.DOI: 10.3969/j.issn.1004-5619.2017.06.011

• 技术与应用 • 上一篇    下一篇

GC-MS法测定血中1-甲基海因含量及其法医学应用

高利娜，袁慧雅，徐恩宇，刘俊亭   

  1. （中国医科大学法医学院，辽宁 沈阳 110013）
  • 发布日期:2017-12-25 出版日期:2017-12-28
  • 通讯作者: 刘俊亭，男，教授，博士研究生导师，主要从事体内药毒物分析研究；E-mail：liujunting8@163.com
  • 作者简介:高利娜（1983—），女，博士，副教授，主要从事体内药毒物分析研究；E-mail：gaolina0114@sina.com
  • 基金资助:

    辽宁省教育厅科学研究一般项目（L2015570）

Determination of 1-methylhydantoin Concentration in Blood by GC-MS Method and Its Application in Forensic Medicine

GAO LI-NA, YUAN HUI-YA, XU EN-YU, LIU JUN-TING   

  1. （School of Forensic Medicine, China Medical University, Shenyang 110013, China）
  • Online:2017-12-25 Published:2017-12-28

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摘要： 目的 建立全血中1-甲基海因的气相色谱-质谱（GC-MS）分析方法，为1-甲基海因相关法医学鉴定案件提供技术支持。 方法 取0.5 mL血样，加入500 ng内标盐酸双苯戊二氨酯（SKF525A）、0.01 mol/L稀盐酸溶液2 mL，加入碳酸铵0.5 g调节pH值为9，加入乙酸乙酯2 mL，然后离心，取有机溶剂层，吹干后进行GC-MS分析。 结果 血液中1-甲基海因在0.5～50 ng/mL范围内线性关系良好，线性回归方程为y=0.015 51 x+0.007 26（R2=0.999 7），最低检出限为0.1 ng/mL，回收率为93.02%～108.12%，日内、日间精密度分别小于6.07%和13.37%。 结论 本方法测定所得结果准确，重现性好，可用于血样中1-甲基海因含量的测定。

关键词: 法医毒理学, 气相色谱-质谱法, 血液, 1-甲基海因, 代谢物

Abstract: Objective To establish a gas chromatographic-mass spectrometric （GC-MS） analysis method for quantifying 1-methylhydantoin concentration in whole blood. To provide technical support to forensic identification related cases of 1-methylhydantoin. Methods As an internal standard, 500 ng SKF525A was added to 0.5 mL blood sample, and then 2 mL 0.01 mol/L dilute hydrochloric acid and 0.5 g ammonium carbonate were added in order to buffer the pH value to 9, and following 2 mL ethyl acetate. The organic solvent layer was obtained after centrifuge and then analysed by GC-MS after drying. Results Good linear relationship of 1-methylhydantoin in blood was obtained in the range of 0.5-50 ng/mL. The equation of linear regression was y=0.015 51 x+0.007 26（R2=0.999 7） with 0.1 ng/mL detection limit, and the recovery was 93.02%-108.12%. The intra-day and inter-day precision were less than 6.07% and 13.37%, respectively. Conclusion The results gotten by this method is accurate and reproducible, which can be used for the determination of 1-methylhydantoin concentration in blood samples.

Key words: forensic toxicology, gas chromatography-mass spectrometry, blood, 1-methylhydantoin, metabolite

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