分散固相萃取/高效液相色谱-串联质谱法检测大葱中虫酰肼、涕灭威及其衍生物的农药残留

Determination of Tebufenozide,Aldicarb,Aldicarb-sulfoxide and Aldicarb-sulfone in Scallion Using Dispersive Solid Phase Extraction Liquid Chromatography-Tandem Mass Spectrometry

采用分散固相萃取法净化（DSPE），高效液相色谱-串联质谱法（HPLC—MS／MS）在分时段多反应监测模式下对大葱中的虫酰肼、涕灭威及其衍生物进行测定，外标法定量，并对比了乙酸乙酯和乙腈作为提取剂的提取效果。结果表明，采用乙腈为提取剂时，4种农药在10—120μg/L范围内线性关系良好，且方法的定量下限（LOQ）均低于10μg/kg；在10μg/kg的加标水平下，大葱基质中4种农药的平均回收率为60％～110％，相对标准偏差（RSD）小于5．0％。该方法操作简便快速，定量准确，干扰小，能用于大葱基质中虫酰肼、涕灭威及其衍生物等农药残留的检测。

A liquid chromatography - tandem mass spectrometric （ LC - MS/MS） method was estab- lished for the determination of tebufenozide, aldicarb, aldicarb-sulfoxide and aldicarb-sulfone in scallion. The samples were extracted with acetonitrile and ethyl acetate, respectively. It was found that the extraction efficiencies of 4 pesticides with acetonitrile were better than those with ethyl ace- tate. Co-extractives were removed from the acetonitrile extracts using dispersive solid phase extraction （DSPE）. The calibration curves were linear in the range of 10 - 120 μg/L with correlation coeffi- cients（r2） more than 0. 995. The limits of quantitation（LOQs） of 4 pesticides were all less than 10 μg/kg^-1, and the average recoveries at the spiked level of 10 μg/kg^-1 in scallion samples from 60% to 110% with RSDs less than 5.0%. The results showed that this method was rapid sitive and specific, and was appropriate for the simultaneous identification and quantification of ticides in scallion. ranged , sen- 4 pesticides in scallion.