Rapid determination of fipronil and its metabolite residues in eggs using ultra performance liquid chromatography-tandem mass spectrometry

Abstract

A method was developed for the rapid simultaneous determination of fipronil and its metabolite residues in eggs using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The egg samples (2 g) with 2 mL water were extracted with 4 mL acetonitrile. After adding 1 g sodium chloride, the mixture was centrifuged at 9000 r/min for 10 min at 4℃. The suspension was diluted and filtered through a 0.22 μm organic membrane. The analytes were separated on a C18 column (100 mm×2.1 mm, 1.7 μm), and detected under the multiple reaction monitoring (MRM) mode with a negative ESI source. The average recoveries of fipronil and its metabolites varied from 77.4% to 112.1%, and the relative standard deviations were between 4.0% and 13.6% at three spiked levels. The limits of detection (LODs) ranged from 0.10 μg/kg to 0.43 μg/kg. The method is simple, effective, and can be applied to real samples.