UPLC-MS/MS检测3种蔬菜中的11种农药

Determination of 11 pesticide residues in three vegetables by UPLC-MS /MS

建立了使用超高效液相色谱-串联质谱（ UPLC-MS/MS）快速有效测定甘蓝、豇豆以及菠菜三种蔬菜中11种常见农药残留的方法。蔬菜样品经乙腈提取,Cleanert-NH2固相萃取柱净化后,采用ACQUITY UPLC·BEH C18色谱柱分离,以电喷雾电离、多反应监测模式检测。考察了不同配比的甲醇-水组成的流动相对电离效率、分辨率和灵敏度的影响,研究了不同蔬菜样品中的基质效应。通过基质匹配标准曲线进行定量,11种农药在5-100μg·L-1范围内线性良好,线性相关系数r〉0．99,目标农药的检出限在0．05-0．5μg·kg-1之间,11种农药在0．01 mg·kg-1,0．05 mg·kg-1和0．10 mg·kg-1三个加标水平下的回收率为80%-120%,相对标准偏差为2．7%-16．3%。

This paper described a method for the determination of 11 pesticides residues in cabbage,cowpea and spinach by ultra-high-performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. The samples were extracted with acetonitrile and cleaned-up with Cleanert-NH2 . The separation was performed on ACQUITY UPLC ABEH C18 column. The methanol-water with different proportion was used as mobile phase and the ionization efficiency,resolution and sensitivity were compared. 11 pesticides were determined in the modes of electrospray ionization and multiple reaction monitoring. The analytes were quantified by matrix-matched internal standard method. The calibration curves show good linearity in 5-100 μg·L-1 for each pesticide（R〉0. 99）. The limits of detection（LODs）were in the range of 0. 05-0. 5 μg·kg-1. The recoveries of all the pesticides varied from 80%to 120%with the relative standard deviations of 2. 7% -16. 3%at the spiked levels 0. 01,0. 05,0. 10 mg·kg-1 for all pesticides.