开展了卷烟和烟叶中有机氯、有机磷和拟除虫菊酯3类29种农药残留的气相色谱-电子轰击离子源质谱(gC-EI/MS)的分析方法研究。优化与选择了卷烟和烟叶样品的前处理条件,样品经正己烷-丙酮(体积比为1∶1)混合提取剂超声提取、flOrISIl硅土和中性氧化铝双净化剂固相萃取柱净化、二氯甲烷-正己烷(体积比为95∶5)混合洗脱剂洗脱和浓缩后,以磷酸三苯酯(TPP)为内标物,采用gC-EI/MS的选择离子监测方式(SIM)进行定性和定量分析。当样品的加标水平为20,50,100μg/kg时,加标回收率为70%--110%,相对标准偏差在2%--8%之间;除了甲氰菊酯、氯菊酯和溴氰菊酯的方法检出限(lOd)分别为1.85,1.74与2.54μg/kg外,其余的26种农药的lOd均小于0.8μg/kg;线性范围为5.0--500.0μg/kg,相关系数都大于等于0.999 4。此分析方法已成功地应用于卷烟和烟叶样品中3类29种痕量农药残留的分析。A method was developed for rapid determination of 29 pesticide residues in tobacco based on gas chromatography coupled with electron impact ionization mass spectrometric detection(GC-EI/MS).After the optimization of different parameters,such as the extraction solvent,elution solvent,purificant,pesticides were extracted from tobacco with hexane-acetone(1∶1,v/v) in an ultrasonic bath,cleaned-up on a column,packed with Florisil and neutral alumina,eluted with dichloromethane-hexane(95∶5,v/v),and then determined by GC-EI/MS in the selected ion monitoring mode(SIM) with triphenyl phosphate(TPP) as internal standard.The recoveries were performed at 20,50 and 100 μg/kg fortification levels for each pesticide,and the recoveries ranged from 70% to 110% with the relative standard deviations between 2% and 8%.The detection limits were less than 0.8 μg/kg for 26 pesticides except for the fenpropathrin,deltamethrin and permethrin.The method was linear over the range of 5.0-500.0 μg/kg with the correlation coefficients between 0.9994 to 0.9999.The method was successfully applied to the analysis of these pesticides in tobacco.国家基础科学人才培养基金项目(J0630429
