Citation: NING Xiao, JIN Shao-Ming, GAO Wen-Chao, CAO Jin, DING Hong. Determination of Fipronil and Its Metabolites in Vegetative Foods by QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2018, 46(8): 1297-1305. doi: 10.11895/j.issn.0253-3820.171530 shu

Determination of Fipronil and Its Metabolites in Vegetative Foods by QuEChERS-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

National Institutes for Food and Drug Control, Beijing 100050, China

Received Date: 27 December 2017
Revised Date: 14 May 2018

A method was developed for the determination of fipronil and its metabolites fipronil-desulfinyl, fipronil-sulfone and fipronil-sulfide in eggs, animal muscle, viscera and egg products by ultra liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). On the basis of QuEChERS method, the extraction solvent, extraction times and sorbents were optimized to ensure the extraction efficiency and the purification of extraction. Finally, the samples were extracted with acetonitrile, followed by centrifugation in the presence of anhydrous magnesium sulfate and sodium chloride. The upper solvent was then cleaned-up by PSA and C₁₈, detected with UPLC MS/MS and quantified with external matrix standards. The result indicated that the average spiked recoveries of fipronil, fipronil-desulfinyl, fipronil-sulfone and fipronil-sulfide in vegetative foods samples were 75.7%-104.5% with relative standard deviations (RSDs) of 1.3%-10.4%, the LODs were 0.5-1.6 μg/kg, and the LOQs were 5.0 μg/kg. This method was simple, sensitive and accurate, and could be used for the routine analysis of fipronil and its three metabolites residues in eggs, animal muscle, viscera and egg products.
- Ultra high performance liquid chromatography-tandem mass spectrometry,
- QuEChERS,
- Vegetative foods,
- Fipronil,
- Fipronil-desulfinyl,
- Fipronil-sulfone,
- Fipronil-sulfide
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