摘要
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.
作者
曾凯
余文婷
杨亚宣
罗明标
ZENG Kai;YU Wen-ting;YANG Ya-xuan;LUO Ming-biao(Jiangxi Key Laboratory for Mass Spectrometry and Instrumentation, East China University of Technology, Nanchang 330013;Nanchang Key Laboratory of Quality and Safety Evaluation of Traditional Chinese Medicine, Nanchang Institute for Food and Drug Control, Nanchang 330012)
出处
《分析试验室》
CAS
CSCD
北大核心
2018年第6期677-680,共4页
Chinese Journal of Analysis Laboratory
基金
江西省质谱科学与仪器重点实验室开放基金项目(JXMS201503)
长江学者和创新团队发展计划资助(IRT13054)
南昌市指导性科技计划项目(洪科字96号第123项)资助