Determination of Fipronil and Its Metabolite Residues in Foods by QuEChERS-Liquid Chromatography-Tandem Mass Spectrometry
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.
QuEChERSliquid chromatography-tandem mass spectrometryeggsteafipronil and its metabolites
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