Analysis of fipronil and metabolites of fipronil in eggs by LC-MS/MS

Abstract

A simple, sensitive and reliable method was developed and applied to determine fipronil and its metabolites in chicken egg by means of liquid chromatography-tandem mass spectrometry (LC-MS/MS). Chicken egg samples were extracted with water and acetonitrile, added with DisQuE salt, shaken and then centrifuged. The extracts were purified by Oasis cartridge prior to analysis by LC-MS/MS. The calibration curve showed good linearity within the concentrations from 0.5 to 10.0 µg/kg (R2 > 0.99). The average recovery rates of fipronil and its metabolites at three spiked levels of 2.0; 5.0 and 10.0 µg/kg ranged from 93.24 % to 107.89 % and the relative standard deviations were less than 9.2 %. The LOQ of this method was of 0.6 µg/kg and LOD was of 0.2 µg/kg. The method has also been successfully applied to analyze fipronil and its metabolites in the real samples.