五氟苄基衍生化GC-MS法检测血液中叠氮离子  

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

作　　者：李茂盛[1] 郑水庆[1] 盛振海 何思阳[1] 邓乾亚 梁晨[1] 吴忠平[1] 曹芳琦 杜猛[3] LI Mao-sheng;ZHENG Shui-qing;SHENG Zhen-hai;HE Si-yang;DENG Qian-ya;LIANG Chen;WU Zhong-ping;CAO Fang-qi;DU Meng(Shanghai Key Laboratory of Crime Scene Evidence,Institute of Forensic Science of Shanghai Public Se-curity Bureau,Shanghai 200083,China;Shanghai Key Laboratory of Crime Scene Evidence,Shanghai Research Institute of Criminal Science and Technology,Shanghai 200083,China;Institute of Criminal Science,Jiading Branch of Shanghai Public Security Bureau,Shanghai 201800,China)

机构地区：[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

出　　处：《法医学杂志》2021年第3期378-381,共4页Journal of Forensic Medicine

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 spec⁃trometry,GC-MS)法。方法取血液检材0.2mL置于10mL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3min,离心后取有机相进行GC-MS分析。结果血液中叠氮离子在0.5~20μg/mL质量浓度范围内的线性关系良好,最低检测限为0.25μg/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11.11μg/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。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 20μg/mL.The lowest detection limit was 0.25μg/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 11.11μg/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.

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 

分 类 号：DF795.1[医药卫生—法医学]