顶空气相色谱/质谱联用法测定人全血中的无机氰化物  

Determination of Inorganic Cyanide in Human Blood by HS-GC/MS

作　　者：魏春明[1] 宋歌[1] 杜鸿雁[1] 于忠山[1] 常靖[1] 侯小平[1] 马华成[2] 陈建旭[2] 张延春[2] 王炯[1] WEI Chunming;SONG Ge;DU Hongyan;YU Zhongshan;CHANG Jing;HOU Xiaoping;MA Huacheng;CHEN Jianxu;ZHANG Yanchun;WANG Jiong(Institute of Forensic Science, Ministry of Public Security & Beijing Engineering Research Center of Crime Scene Evidence Examination, Beijing 100038, China;Institute of Forensic Science and Technology, Henan Provincial Public Security Bureau, Zhengzhou 450003, China)

机构地区：[1]公安部物证鉴定中心北京市现场物证检验工程技术研究中心,北京100038 [2]河南省公安厅刑科所,郑州450003

出　　处：《刑事技术》2017年第4期294-297,共4页Forensic Science and Technology

基　　金：中央级公益性科研院所基本科研业务费专项资金项目(No.2017JB001)

摘　　要：目的建立一种简便的测定人全血中无机氰化物的顶空气相色谱-质谱联用方法。方法样品前处理采用1m L全血,放入10m L顶空瓶中,加入1m L去离子水稀释后,加入0.5m L浓磷酸,立即封盖,60℃加热15min,进行HS-GC/MS分析。色谱分析采用Agilent GS-GASPRO(30m×0.32mm)色谱柱,质谱分析采用SIM模式采集数据。结果氰化物在0.1~100μg/m L浓度范围内线性良好(R^2>0.998),精密度(n=6)<10%,回收率>80%,最低检出限为0.05μg/m L。结论本方法简单、高效,可准确测定人全血中无机氰化物的浓度。Objective To establish a convenient method to determine the inorganic cyanide in human blood by headspace-gas chromatography/mass spectrometry(HS-GC/MS).Methods1mL whole blood was used as the sample to be pretreated,then put into a10mL headspace vial where to dilute with1mL deionized water.After addition of0.5mL phosphoric acid(≥85%),the vial was sealed immediately and heated at60℃for15min,being kept ready for analysis by HS-GC/MS.An Agilent?GS-GASPRO chromatographic column(30m×0.32mm)was chosen to separate the sample under the mass spectrum scanning mode as the selected ion monitoring(SIM).Results The linearity of the inorganic cyanide determined among0.1-100μg/mL is good(R2>0.998)with an RSD(n=6)<10%and recovery>80%.The limit of detection(LOD)is0.05μg/mL.Conclusion This method is simple,efficient,able to accurately determine the inorganic cyanide in human blood.

关 键 词：法医毒物分析 顶空气相色谱/质谱联用法 无机氰化物 全血 

分 类 号：DF795.1[医药卫生—法医学]