液相色谱-质谱联用法测定蔬菜中氟虫腈及其代谢物的残留量

Determination of Fipronil and Its Metabolites Residues in Vegetables by Liquid Chromatography-Mass Spectrometry

本文建立了蔬菜中氟虫腈及其代谢物残留量的QuECHERS-高效液相色谱串联质谱分析方法。样品经乙腈提取,氯化钠、硫酸镁盐析,以乙腈-水为流动相梯度洗脱,C18色谱柱分离,采用电喷雾负离子模式,基质配制标准溶液,外标法定量。氟虫腈及其代谢物在10 min内完好分离。在0.005~0.5 mg·L^(-1)浓度范围内,线性关系良好(R2>0.999),对黄瓜、韭菜、芹菜、番茄、茄子进行3个添加水平回收试验,回收率为92%~118%。相对标准偏差为1.7%~7.4%。该方法简便快捷,适用于蔬菜中农药残留的测定。

A method for the determination of fipronil and its metabolite residues in vegetables by QuEChERS high performance liquid chromatography tandem mass spectrometry was established.Samples were extracted by acetonitrile,salted out by sodium chloride and Magnesium Sulfate,separated by acetonitrile water as mobile phase and separated by C18 column.The standard solution was prepared by electro spray negative ion mode and quantified by external standard method.Fipronil and its metabolites were well separated within 10 minutes.In the range of 0.005~0.5 mg·L^(-1),the linear relationship is good(R2>0.999).The recovery tests of cucumber,leek,celery,tomato and eggplant are carried out at three addition levels,and the recovery range is 92%~118%.The relative standard deviation is 1.7%~7.4%.The method is simple,rapid and suitable for the determination of pesticide residues in vegetables.