气相色谱-串联质谱技术分析烟草中49种农药残留  

Determination of 49 pesticide residues in tobacco by gas chromatography-tandem mass spectrometry

作　　者：李玮[1] 卢春山[2] 李华 屠海云 周敏[1] 

机构地区：[1]杭州市质量技术监督检测院,浙江杭州310019 [2]浙江工业大学绿色化学合成技术国家重点实验室培育基地,浙江杭州310032 [3]常州亚邦申联化工有限公司,江苏常州213127

出　　处：《色谱》2010年第11期1048-1055,共8页Chinese Journal of Chromatography

摘　　要：采用改进的QuEChERS(quick,easy,cheap,effective,rugged and safe)前处理法,结合气相色谱-串联质谱(GC-MS/MS)技术建立了检测烟草中49种农药残留的分析方法。样品用含0.1%乙酸的乙腈溶液提取,提取液被氮吹至干后,残渣用乙腈-乙酸乙酯(1:1,v/v)溶液溶解,溶解液经N-丙基乙二胺(PSA)吸附剂、无水MgSO4、C18吸附剂净化后,直接进行GC-MS/MS测定,内标法定量。实验结果表明,49种农药在低质量浓度(0.05μg/L)的加标水平下的平均加标回收率为60.4%～104.8%,高质量浓度(5μg/L)的平均加标回收率为70%～115%,相对标准偏差均小于15%;其中16种农药的方法检出限(LOD)分别为0.01～0.03μg/kg,其余33种农药的LOD均小于0.01μg/kg;相关系数都大于或等于0.991。该方法样品前处理简单、分析时间短、灵敏度和精密度均符合农药多残留痕量检测技术的要求,适用于烟草中多种农药残留的检测。A method was developed for rapid determination of 49 pesticide residues in tobacco based on gas chromatography-tandem mass spectrometry（GC-MS/MS）.Tobacco was extracted with 0.1% acetic acid-acetonitrile solution.The supernatant was quantitatively transferred and dried with nitrogen.The concentrated extract was dissolved with acetonitrile-ethyl acetate（1：1,v/v）solution and cleaned up by primary secondary amine（PSA）sorbents,MgSO4and C18 sorbents,then determined by GC-MS/MS with mirex as internal standard.The ranges of spiked recoveries of 49 pesticides at 0.05μg/L and 5μg/L were 60.4%-104.8%and 70%-115%,respectively.The relative standard deviations were below15%.The detection limits of 16 pesticides were 0.01-0.03μg/kg and those of the other 33 pesticides were less than0.01μg/kg;the correlation coefficients were larger than 0.991.This method is simple,rapid and characterized with acceptable sensitivity and accuracy to meet the requirements for the analysis of multiple pesticide residues in tobacco.

关 键 词：气相色谱-串联质谱 农药残留 烟草 

分 类 号：O658[理学—分析化学]