摘要
本研究以尖椒、苹果、鸡蛋、茶叶等 9 种食品为分析对象,建立了氟虫腈及其代谢物的液相色谱-串联质谱检测方法.采用基质固相分散萃取技术(QuEChERS),试样经提取、盐析萃取和净化后,以水和乙腈为流动相,用BEH C18 色谱柱进行分离,在电喷雾负离子模式(ESI-)下,用多反应监测(MRM)进行采集,使用外标法定量.氟虫腈及其代谢物在 0.5～20 μg/kg(尖椒、芒果、苹果)、1.0～40 μg/kg(大米、牛肉、猪肝、虾、鸡蛋)和 2.5～100 μg/kg(茶叶)各个加标浓度范围内线性相关性良好,r2≥0.9978;检测尖椒、芒果、苹果的定量限为0.50 μg/kg;检测大米、鸡蛋、虾、牛肉、猪肝的定量限为 1.0 μg/kg;检测茶叶的定量限为 2.5 μg/kg;9 种食品中氟虫腈及其代谢物的各个浓度水平加标回收率为 70.0%～115.1%,相对标准偏差为 0.7%～13.6%.该方法快速、灵敏、高效、安全,适用于多类食品中氟虫腈及其代谢物残留量的测定.
Abstract
In this study,9 kinds of food such as bell pepper,apple,egg and tea were analyzed,and a liquid chromatography-tandem mass spectrometry method for detection of fipronil and its metabolites was constructed.The specimens were extracted,salted extracted and purified using matrix solid-phase dispersive extraction(QuEChERS),separated on a BEH C18 column with water and acetonitrile as mobile phases,collected in electrospray anionic mode(ESI-)with multiple reaction monitoring(MRM),and quantified using external standard methods.Fipronil and its metabolites showed good linear correlations in the spiked concentration ranges of 0.5-20 μg/kg(pepper,mango,apple),1.0-40 μg/kg(rice,beef,pig liver,shrimp,egg),and 2.5-100 μg/kg(tea),with r2≥0.9978.The method quantitative limit was 0.50 μg/kg to detect pepper,mango and apple,1.0 μg/kg to detect rice,egg,shrimp,beef and pork liver,and 2.5 μg/kg to detect tea.The recoveries of fipronil and its metabolites spiked in nine foods at their corresponding concentration levels ranged from 70.0%to 115.1%with the relative standard deviations(RSDs)of 0.7%to 13.6%.The method,with the advantage of rapid,sensitive,efficient and safe,is suitable for the determination of the residues of fipronil and its metabolites in various types of food.
基金项目
南宁市科学研究与技术开发计划项目(20212148)
NETL
NSTL
万方数据