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Determination of fipronil and its major metabolites in vegetables, fruit and soil using QuEChERS and gas chromatography-mass spectrometry

A rapid, simple and selective gas chromatography with mass spectrometric detection (GC-MS) method was developed and validated for simultaneously determining fipronil and its three major metabolites in vegetables, fruit and soil. The fipronil residues were extracted using QuEChERS technique with ethyl acetate and then were purified by dispersive solid phase extraction (d-SPE) cleanup for cabbage, cauliflower, okra, tomato, grapes and soil. The linearity of the analytical response across the studied range of concentrations (0.01–0.5 µg mL−1) was excellent, obtaining correlation coefficients higher than 0.999. The average recoveries of the pesticide from all matrixes ranged from 86 to 112%, for fortification levels of 0.01, 0.05 and 0.1 µg g−1. The precision values associated with the analytical method, expressed as RSD values, were less than 10.15% for the pesticide in all matrixes. This method can be used to evaluate environmental residues and the safety of agricultural products.