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CUI Xiangyong, MU Jiaojiao, WANG Yansong, CHEN Xuehui, LIU Pengyu, ZHANG Fengqing, WANG Dongyan, ZHU Jun. LC-MS/MS Determination of Fipronil and Its 3 Metabolites in Eggs[J]. PHYSICAL TESTING AND CHEMICAL ANALYSIS PART B:CHEMICAL ANALYSIS, 2018, 54(5): 601-605. DOI: 10.11973/lhjy-hx201805024
Citation: CUI Xiangyong, MU Jiaojiao, WANG Yansong, CHEN Xuehui, LIU Pengyu, ZHANG Fengqing, WANG Dongyan, ZHU Jun. LC-MS/MS Determination of Fipronil and Its 3 Metabolites in Eggs[J]. PHYSICAL TESTING AND CHEMICAL ANALYSIS PART B:CHEMICAL ANALYSIS, 2018, 54(5): 601-605. DOI: 10.11973/lhjy-hx201805024

LC-MS/MS Determination of Fipronil and Its 3 Metabolites in Eggs

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  • Received Date: October 18, 2017
  • LC-MS/MS was applied to the determination of fipronil and its 3 metabolites in eggs. The egg sample was extracted with acetonitrile. After centrifugation, the supernatant was evaporated to near dryness by N2-blowing. The residue was taken up with water and then purified with HLB solid phase extraction column. Shim-pack XR-ODS C18 chromatographic column was used as stationary phase, and the mixture of 4 mmol·L-1 ammonium acetate solution and methanol mixed in different ratios was used as mobile phase in gradient elution. ESI- and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass fraction of fipronil and its 3 metabolites were kept in the same range of 1-50 μg·kg-1, with same detection limit (3S/N) of 0.3 μg·kg-1. Tests for recovery were made by standard addition method at the concentration levels of 1, 5, 20 μg·kg-1, giving values of recovery and RSD's (n=6) in the ranges of 89.9%-96.1% and 1.6%-3.3% respectively.
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