Simultaneous Determination of Flupyradifurone and Its Metabolites in Citrus Samples Using Ultrahigh Performance Liquid Chromatography-Tandem Mass Spectrometry

KeyWord:pesticide residue  flupyradifurone  metabolites  citrus  ultrahigh performance liquid chromatography-tandem mass spectrometry£¨UPLC-MS/MS£©

Abstract:

      An analytical method was developed for the simultaneous detection of flupyradifurone and its three metabolites iª±e.difluoroacetic acid£¨DFA£©£¬6-chloronicotinic acid£¨6-CNA£© and difluoroethylaminofuranone£¨DFEA£© in citruses by ultrahigh performance liquid chromatography tandem mass spectrometry£¨UPLC-MS/MS£©.Citrus samples were extracted with acetonitrile£¬and cleaned up by dispersive solid phase extraction£¨PSA£©.The analytes were detected in multiple reaction monitoring£¨MRM£© mode under alternate positive/negative electrospray ionization£¨ESI+/ESI- £© mode£¬and quantified by the external standard method.The results showed that there were good linearities for flupyradifurone and its metabolites in their respective concentration ranges with correlation coefficients of 0.997 9-0.999 6.The limits of detection were 0.001 mg/L.The average recoveries for the analytes in the whole citrus fruit and fruit pulp at spiked levels of 0.05£¬0.3 and 2 mg/kg ranged from 71.9%to 106%with relative standard deviations£¨RSDs£© of 0.8%-9.1%.The average recoveries of the analytes in citrus fruit peel at spiked levels of 0.1£¬0.3 and 3 mg/kg ranged from 77.9%to 100%with relative standard deviations£¨RSDs£© of 1.2%-6.5%.The limits of quantitation£¨LOQs£© for flupyradifurone and its metabolites in the whole citrus fruit£¬fruit pulp and peel were 0.05£¬0.05 and 0.1 mg/kg£¬respectively.The method is simple£¬stable£¬rapid and sensitive£¬and is suitable for the determination of flupyradifurone and its metabolites in citrus samples.