Analytical Method for Fipronil and Fipronil Sulfone in Livestock Products Using LC-MS/MS

A rapid and sensitive method for the simultaneous determination of fipronil and fipronil sulfone (metabolite B) in livestock products was developed. The analytes were extracted from samples with acidic acetonitrile. The crude extracts were subjected to clean-up step using neutral alumina cartridge column. The HPLC separation was performed on a C18 column with isocratic elution of acetonitrile and ammonium formate solution. For the determination of the analytes, a tandem mass spectrometry with negative ion electrospray ionization was used. In the recovery tests using 6 livestock products fortified with MRLs levels of analytes, the truenesses for fipronil and fipronil sulfone were 95 to 115 and 94 to 101% with the repeatabilities of 0.8 to 4.1 and 0.9 to 5.1 RSD%, respectively. The limits of quantification for both analytes were estimated to be 0.001 mg/kg. The developed method is considered suitable for regulatory analysis of fipronil and fipronil sulfone.