Development and validation of modified QuEChERS methods for the analysis of fipronil and its metabolites in chicken meat

Abstract

A sensitive method for the precisely and accurate determining the presents of fipronil and its metabolites in chicken meat was developed and validated using a modified quick, easy, cheap, effective, rugged and safe approach coupled with gas chromatography-mass spectrometry analysis. The solvent acetonitrile was used for the extraction of the samples with the salt phases composed of sodium chloride and magnesium sulphate, and then in the second phase used C18 and anhydrous magnesium sulphate. The linearity of the analytical response across the studied range of concentrations (0.005-0.050 mg kg-1) was excellent, obtaining correlation coefficients higher than 0.99. The average recoveries of the pesticide ranged from 75 to 106% for fortification levels of 0.005, 0.01 and 0.05 mg kg-1. The precision values associated with the analytical method, expressed as RSD values, were less than 11.15%. Matrix-matched solutions were also prepared by serially diluting the intermediate solution with blank chicken meat sample extracts containing none of the tested analytes to perform matrix-matched calibration with the same concentrations as in the solvent. The validated method was used to analyse the target compounds in 30 real samples imported from European countries. The present of fipronil-desulfinyl metabolite was confirmed in four samples.