QuEChERS结合质谱法测定食用菌中13种农药残留

Determination of 13 kinds of pesticide residues in edible fungi by QuEChERS combined with mass spectrometry

目的建立QuEChERS前处理结合气相色谱-串联质谱法(gaschromatography-tandemmass spectrometry,GC-MS/MS)和液相色谱-串联质谱法(liquidchromatography-tandemmassspectrometry,LC-MS/MS)测定食用菌中13种农药残留的分析方法。方法冬菇、草菇和金针菇3种食用菌分别以乙腈提取,改良的QuEChERS方法净化,气相色谱-串联质谱法采用AgilentHP-5MSultralnert柱(30.0m×250μm,0.25μm)分离,液相色谱-串联质谱法采用农残色谱柱ACQUITY UPLC?BEH C18(2.1 mm×50 mm,1.7μm)分离,气相色谱-串联质谱仪和液相色谱-串联质谱仪外标法测定。结果本方法在5~500μg/L范围内线性关系良好,相关系数大于0.99,在3个水平下13种农药的回收率为68.2%~119.8%,相对标准偏差(relative standard deviation,RSD)为0.7%~12.5%。结论此方法适用但不限用于食用菌中13种农药残留的测定。

Objective To establish an analytical method for the determination of 13 kinds of pesticide residues in edible fungi by QuEChERS(quick,easy,cheap,effective,rugged and safe)pretreatment,gas chromatography-tandem mass spectrometry(GC-MS/MS)and liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods Three kinds of edible fungi,including Volvariella edodes,Volvariella volvacea and Flammulina velutipes,were extracted with acetonitrile and purified by improved QuEChERS method,GC-MS/MS was performed on an Agilent HP-5 MS ultralner column(30.0 m×250μm,0.25μm),LC-MS/MS was performed on acquity UPLC column?BEH C18(2.1 mm×50 mm,1.7μm)separation.GC-MS/MS and LC-MS/MS were used for external standard determination.Results The linear relationship was good in the range of 5-500μg/L,and the correlation coefficients were greater than 0.99.Under 3 levels,the recoveries of 13 pesticides were 68.2%-119.8%,and the relative standard deviations(RSD)were 0.7%-12.5%.Conclusion This method is applicable,which is not limited to the determination of 13 kinds of pesticide residues in edible fungi.