气相色谱-三重四极杆质谱法测定鸡蛋中氟虫氰及其代谢残留

Determination of fipronil and metabolites in eggs by GC-MS/MS method

建立了QuEChERS快速提取和净化样品,气相色谱-三重四级杆质谱联用法测定鸡蛋中氟虫腈及其代谢物氟甲腈、氟虫腈砜、氟虫腈亚砜的方法。水和乙腈萃取、C_(18)和PSA净化样品,气相色谱分离,多反应离子监测模式测定。氟虫腈及其3种代谢物在5~400μg/L范围内线性关系良好,方法的检出限为1.0~2.5μg/kg;定量限为3.0~7.5μg/kg。在两个浓度水平进行加标,上述4种测定物的回收率为72.5%~95.3%,相对标准偏差为3.7%~7.5%。本方法可满足鸡蛋中氟虫腈及其代谢物氟甲腈、氟虫腈砜、氟虫腈亚砜残留检测的实际需要。

A QuEChERS method was developed for the extraction and purification of egg samples,the determination of fipronil and metabolites in the samples by gas chromatography-triple quadrupole mass spectrometry（GC-MS/MS）.The samples were extracted by acetonitrile-water,then purified by C18 and PSA.The target compounds were separated by gas chromatography,and mass spectrometric acquisition was carried out by multiple reaction monitoring（MRM）.The linearities of the four pesticide residues were in the range of 5 ～ 400 μg/L,with good correlation coefficient,and the limits of the detection were 1.0 ～ 2.5 μg/kg.Then the limits of quantification were 3.0 ～ 7.5 μg/kg,which meets the domestic and international requirements for the detection of fenvalerate in eggs.The recoveries of the four insecticides were 72.5 % ～ 95.3% and the relative standard deviations were 3.7% ～ 7.5% spiked at two levels of concentration.This method has the advantages of low consumption of organic reagents and high efficiency,which can meet the actual needs for detection of fenvalerate and its metabolites fluorosilane,fipronil sulfone and fipronil sulfoxide residues in eggs.