QuEChERS结合GC-MS/MS检测果蔬中13种农药残留

Determination of 13 Pesticide Residues in Fruits and Vegetables by QuEChERS Combined with GC-MS/MS

目的:基于QuEChERS方法结合气相色谱串联质谱(Gas Chromatography-Tandem Mass Spectrometry,GC-MS/MS)技术,建立一种简单、快速检测果蔬中农药残留的方法。方法:果蔬样品匀浆后,先用乙腈和乙酸缓冲盐包提取,再用m-PFC小柱净化,最后用GC-MS/MS测定,外标法定量。结果:13种农药在10~500μg·L^(-1)浓度范围内线性关系良好,相关系数(R2)均大于0.994,检出限为0.35~0.92μg·kg^(-1),定量限为1.0~2.8μg·kg^(-1);13种农药在3个水平下的加标回收率为82.4%~110.1%,相对标准偏差为2.9%~9.3%。结论:所建立的方法可操作性强,具有较高的精密度和准确度,可用于果蔬中农药残留的定性和定量检测。

Objective:To establish a simple and rapid method for the detection of pesticide residues in fruits and vegetables based on the QuEChERS method combined with gas chromatography-tandem mass spectrometry(GC-MS/MS)technology.Method:After homogenization,the fruit and vegetable samples were first extracted with acetonitrile and acetic acid buffer,then cleaned up with m-PFC cartridges,and finally determined by GC-MS/MS and quantified by external standard method.Result:The 13 pesticides had good linear relationships in the concentration range of 10~500μg·L^(-1),and the correlation coefficients(R2)were all greater than 0.994.The limits of detection were 0.35~0.92μg·kg^(-1),and the limits of quantification were 1.0~2.8μg·kg^(-1).The recoveries of the 13 pesticides at three levels were 82.4%~110.1%,and the relative standard deviation were 2.9%~9.3%.Conclusion:The established method is highly operable,has high precision and accuracy,and can be used for the qualitative and quantitative determination of pesticide residues in fruits and vegetables.