铁灭克的检验  

Studies on the examination of temik in the poisonous cases

作　　者：张银华[1] 喻晓[1] 孙凤梅[1] 

机构地区：[1]湖北省公安厅刑侦总队,武汉430070

出　　处：《刑事技术》2003年第2期21-23,共3页Forensic Science and Technology

基　　金：公安部资助科研项目(No.C20004223101)

摘　　要：目的建立生物检材中铁灭克农药的定性、定量分析方法;方法利用溶剂苯萃取生物检材中的铁灭克农药,应用薄层色谱(TLC)、气相色谱(GC)两种方法进行定性分析,应用气相色谱-质谱-选择离子监测(GC-MS-SIM)分析方法进行定性定量分析,并测定了该方法的检测限、线性回归方程和回收率。结果应用TLC、GC、GC-MS、GC-MS-SIM等分析方法成功地在两个实际案例中检出了铁灭克农药,利用GC-MS联用技术获得了铁灭克热解产物涕灭威腈的质谱图,GC-MS-SIM分析方法分析涕灭威的检测限是0.02ng,获得了m/z68、m/z100和m/z115三个特征离子定量分析的线性回归方程,样品添加标样回收率为99.0至103.5%。结论铁灭克热不稳定,受热易分解。获得了铁灭克热分解产物涕灭威腈的质谱图。GC-MS-SIM分析方法检测铁灭克具有灵敏度高、回收率高等优点。Objective To establish a method for qualitative and quantitative analyzing aldicarb pesticide.Methods Extracting the aldicarb pesticide with benzene solvent in the biological samples,qualitative analyzing aldicarb pesticide by thin layer chromatography(TLC)and gas chromatography(GC),qualitative and quantitative analyzing aldicarb pesticide by gas chromatography-mass spectrometry(GC-MS ),The limit of detection,linearity regression equation and recoveries of this method are determined.Results The aldicarb pesticide was successfully detected in the two cases by GC-MS ,and the mass spectrum of aldicarb nitrile which thermal decomposition from aldicarb was acquired.The limit of detection of analyzing aldicarb pesticide by GC-MS in the model selective ion monitor was0.02ng,three linearity regression equation of the characteristics ion m/z68,m/z100and m/z115of aldicarb nitrile were acquired with correlation coefficients0.9963～0.9981.the recovery of standard added to the samples is vary from99.0%to103.5%.Conclusion temik is thermal labile and easy decomposd by heat.The mass spectrum of aldicarb nitrile which thermal decomposed from aldicarb was acquired.The selective ion monitor analysis method by GC-MS is of advantage of high sensitivity and high recovery.

关 键 词：铁灭克农药 溶剂苯萃取 生物检材 GC-MS-SIM分析方法 案例分析 

分 类 号：D918.93[政治法律—法学]