QuEChERS/HPLC-MS/MS法同时测定果蔬中17种农药残留

Determination of 17 Pesticide Residues in Fruits and Vegetables by QuEChERS Method Coupled with High Performance Liquid Chromatography Tandem Mass Spectrometry

[目的]利用高效液相色谱-串联质谱(HPLC-MS/MS)检测技术,建立了果蔬中同时测定17种农药残留的分析方法。[方法]采用QuEChERS前处理方法,用含1%(V/V)乙酸的乙腈溶液提取样品,以无水硫酸镁(MgSO_4)作为脱水剂,经N-丙基乙二胺(PSA)和石墨化碳黑(GCB)混合净化剂净化,C_(18)色谱柱分离,高分辨质谱在正离子模式下选用多重反应监测(MRM)扫描测定,基质匹配标准曲线外标法定量。[结果]17种农药在150 ng/mL范围内线性关系良好,相关系数均在0.99以上。分别对黄瓜、苹果进行3个加标水平的回收试验(1.0、2.0、5.0μg/kg),17种目标物的回收率为60.2%117.7%,相对标准偏差低于12.8%。检出限(S/N≥3)为0.2μg/kg,定量限(S/N≥10)为1.0μg/kg。[结论]该方法简单、快速、灵敏、精确,能够同时准确测定果蔬样品中17种农药残留。

[Objective] A rapid and effective method was established for the simultaneous determination of 17 pesticide residues in fruits and vegetables by high performance liquid chromatography tandem mass（HPLC-MS/MS）.[Method] Using modified QuEChERS method,the samples was extracted with acetonitrile containing 1%（V/V） acetic acid,purified by a mixed sorbent of MgSO_4,primary secondary amine（PSA） and graphitized carbon black（GCB）,separated on a C_（18） column and analyzed by postitive electrospray ionization tandomd method.[Result]The results showed that the 17 pesticide residues were linear in the range of 1-50 ng/mL with correlation mass spectrometry under multiple reactions monitoring（MRM） mode.The quantitative analysis was used by external standarcoefficients（r） over 0.99.The recoveries at spiked levels of 1.0,2.0 and 5.0 μg/kg for all target compounds in the samples were in the range of 60.2%-117.7%,with relative standard deviations less than 12.8%.The limits of detection（LOD,S/N≥3） was 0.2 μg/kg;the limits of quantitation（LOQ,S/N≥10）was 1.0 μg/kg.[Conclusion] A simple,rapid,sensitive and accurate method was developed,which was suitable for the determination of 17 pesticide residues in fruits and vegetables simultaneously.