Determination of Fipronil and Its Metabolites in Fresh Jujube by Low Temperature Liquid-Liquid Extraction/Ultra High Liquid Chromatography-Tandem Mass Spectrometry
Determination of Fipronil and Its Metabolites in Fresh Jujube by Low Temperature Liquid-Liquid Extraction/Ultra High Liquid Chromatography-Tandem Mass Spectrometry[J]. 2015,34(12):1360-1365.
Determination of Fipronil and Its Metabolites in Fresh Jujube by Low Temperature Liquid-Liquid Extraction/Ultra High Liquid Chromatography-Tandem Mass Spectrometry[J]. 2015,34(12):1360-1365.DOI:
An analytical method for the qualitative and quantitative analyses of fipronil and its metabolites residues in fresh jujube was developed by using low temperature liquid-liquid extraction and ultra high liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). The fresh jujube sample was extracted with acetonitrile,followed by liquid-liquid extraction at -25 ℃. The analysis of fipronil and its metabolites was performed under negative ion mode and multiple reaction monitoring(MRM),quantified by the external standard method. Under the optimized conditions,the fipronil and its metabolites showed good linearities in the range of 0.02 - 10 μg/L,with correlation coefficients(r2) higher than 0.999. The limits of detection of the method were in the range of 0.005-0.02 μg/kg. The average recoveries of fipronil and its metabolites in fresh jujube matrices were in the range of 78.5%-95.8% with relative standard deviations of 3.4%-6.9%. The method is simple and highly sensitive,and is suitable for the rapid determination of fipronil and its metabolites in fresh jujube.
关键词
低温液液萃取超高效液相色谱-串联质谱(UPLC-MS/MS)鲜枣氟虫腈及其代谢物
Keywords
low temperature liquid-liquid extractionultra high liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)fresh jujubefipronil and its metabolites