气相色谱-串联质谱技术分析烟草中的132种农药残留

利用气相色谱-串联质谱(GC-MS/MS)检测技术,建立了检测烟草中的132种农药残留的高灵敏度方法。分析过程中考察了不同萃取溶剂、不同缓冲盐体系、不同净化剂对目标物回收率的影响。最终确定烟草样品以乙腈进行提取,以N-丙基乙二胺(PSA)与碳18(C18E)的混合净化剂进行净化,氮气吹近干后用正己烷-丙酮(9:1, v/v)复溶,过有机滤膜后进行GC-MS/MS测定,内标法定量。132种农药在20～2000 μg/kg之间线性关系良好(r2 ＞0.99);所有农药的方法定量限(LOQ, S/N=10)均低于20 μg/kg;在50、200、500 μg/kg的加标水平下,除灭蚁灵及六氯苯回收率稍低外,其他农药的平均回收率为68.10%～123.15%,相对标准偏差(RSD)为1.79%～19.88%。对国际烟草科学研究合作中心(CORESTA)2012年共同实验的烟草样品进行检测,对比本方法与已有的标准方法,其结果一致性较好。该方法准确、可靠,灵敏度好,适用于烟草中132种农药残留的快速筛查与定性、定量分析。

Determination of 132 pesticide residues in tobacco by gas chromatography-tandem mass spectrometry

A simple method for the determination of 132 pesticide residues in tobacco by gas chromatography-triple quadrupole tandem mass spectrometry (GC-MS/MS) was established. The influences of different extraction solvents, different buffer systems and different purifying agents on the recoveries of pesticides were investigated. The tobacco sample was extracted with acetonitrile, then cleaned up by the mixed sorbents of primary secondary amine (PSA) and octadecylsilane (C18E). After dried by nitrogen, the extract residue was reconstituted with n-hexane-acetone (9:1, v/v). GC-MS/MS in multi-reaction monitoring (MRM) mode was used as the detection method and triphenyl phosphate (TPP) as the internal standard. All of the 132 pesticides had good linear relationships (r2 ＞0.99) between 20 μg/kg and 2000 μg/kg. At the three spiked levels of 50, 200 and 500 μg/kg in the tobacco extract, the average recoveries of all the pesticides were in the range of 68.10% to 123.15% except for mirex and hexachlorobenzene; moreover, the relative standard deviations (RSDs) of them were between 1.79% and 19.88%. We participated in the CORESTA (Cooperation Centre for Scientific Research Relative to Tobacco) 2012’s co-experiment. The results of our method and the existed standard methods had good consistency. The accurate, reliable and sensitive method can be applied to the determination of the 132 pesticide residues in tobacco for rapid screening and quantitative analysis.