法医学杂志

法医学杂志 ›› 2021, Vol. 37 ›› Issue (3): 378-381.DOI: 10.12116/j.issn.1004-5619.2020.300304

• 论著 • 上一篇    下一篇

五氟苄基衍生化GC-MS法检测血液中叠氮离子

李茂盛1， 郑水庆1， 盛振海1， 何思阳1， 邓乾亚1， 梁晨1， 吴忠平1， 曹芳琦2， 杜猛3   

  1. 1. 上海市公安局物证鉴定中心 上海市现场物证重点实验室，上海 200083； 2. 上海市刑事科学技术研究院 上海市现场物证重点实验室，上海 200083； 3. 上海市公安局嘉定分局刑事科学技术研究所，上海 201800
  • 发布日期:2021-06-25 出版日期:2021-06-28
  • 通讯作者: 吴忠平，男，高级工程师，主要从事毒品毒物检验鉴定；E-mail：15575907@qq.com 曹芳琦，女，副研究员，主要从事毒品毒物分析与快速检测研究；E-mail：frankie-cao@163.com
  • 作者简介:李茂盛（1983—），男，工程师，主要从事毒品毒物检验鉴定；E-mail：greedy198365@sina.com

Determination of Azide Ions in Blood by Pentafluorobenzyl Derivation Followed by GC-MS

LI Mao-sheng1, ZHENG Shui-qing1, SHENG Zhen-hai1, HE Si-yang1, DENG Qian-ya1, LIANG Chen1, WU Zhong-ping1, CAO Fang-qi2, DU Meng3   

  1. 1. Shanghai Key Laboratory of Crime Scene Evidence, Institute of Forensic Science of Shanghai Public Security Bureau, Shanghai 200083, China; 2. Shanghai Key Laboratory of Crime Scene Evidence, Shanghai Research Institute of Criminal Science and Technology, Shanghai 200083, China; 3. Institute of Criminal Science, Jiading Branch of Shanghai Public Security Bureau, Shanghai 201800, China
  • Online:2021-06-25 Published:2021-06-28

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摘要： 目的 建立血液中叠氮离子的五氟苄基衍生化气相色谱-质谱（gas chromatography-mass spectrometry，GC-MS）法。 方法 取血液检材0.2 mL置于10 mL玻璃试管中，依次加入内标物氰化钠、衍生化试剂五氟苄基溴和催化剂十四烷基二甲基苄基氯化铵，涡旋混合后，微波炉低火档加热3 min，离心后取有机相进行GC-MS分析。 结果 血液中叠氮离子在0.5~20 μg/mL质量浓度范围内的线性关系良好，最低检测限为0.25 μg/mL，相对回收率为91.36%~94.58%，并成功应用于1例叠氮化钠中毒死亡案件，死者血液中叠氮离子质量浓度为11.11 μg/mL。 结论 本研究建立的方法专属性强，操作简便，适用于血液中叠氮离子的快速检测。

关键词: 法医毒物化学, 气相色谱-质谱法, 五氟苄基衍生化, 叠氮离子, 氰离子

Abstract: Objective To establish a method for determination of the azide ions in blood by gas chromatography-mass spectrometry （GC-MS） following pentafluorobenzyl derivatization. Methods A blood sample of 0.2 mL was placed into a 10 mL glass test tube, and the internal standard sodium cyanide, derivatization reagent pentafluorobenzyl bromide and catalyst tetradecyl benzyl dimethyl ammonium chloride were added in turn. After vortex mixing, the mixture was heated with low-power microwave for 3 min. After centrifugation, the organic phase was taken for GC-MS analysis. Results The azide ions in blood had a good linear relationship in the mass concentration range of 0.5 to 20 μg/mL. The lowest detection limit was 0.25 μg/mL and the relative recovery was 91.36%-94.58%. The method was successfully applied to a case of death from sodium azide poisoning. The mass concentration of azide ions in the blood of the dead was 11.11 μg/mL. Conclusion The method developed in this paper has strong specificity and is easy to operate, which is suitable for the rapid detection of azide ions in blood.

Key words: forensic toxicology, gas chromatography-mass spectrometry, pentafluorobenzyl derivatization, azide ion, cyanide ion

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