Determination of fipronil and its metabolites in chicken egg, muscle and cake by a modified QuEChERS method coupled with LC-MS/MS

作者：Qiaozhen Guo, Shan Zhao, Jing Zhang, Kailun Qi, Zhenxia Du, Bing Shao · 发表于：Food Additives & Contaminants Part A · 年份：2018 · DOI：10.1080/19440049.2018.1472395 · 被引用次数：65 · 研究领域：Pesticide Residue Analysis and Safety、Insect and Pesticide Research、Pharmacological Effects and Assays

An easy-to-use method for determining the levels of fipronil and its metabolites (fipronil-desulfinyl, fipronil-sulfone and fipronil-sulfide) in chicken egg, muscle and cake was developed and validated using a modified quick, easy, cheap, effective, rugged and safe (QuEChERS) approach coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. The samples were extracted using acetonitrile, salted out with sodium chloride at -20°C, and then purified by combined PSA and C18 phases and anhydrous magnesium sulphate. The recoveries were 80.4-119% with relative standard deviations (RSDs) < 10% for the different matrixes. The validated method was used to analyse the target compounds in 214 real samples collected in Beijing. The metabolite fipronil-sulfone was detected in most of the samples and was identified as the main residue in the egg and cake. The method was validated using a proficiency test for fipronil in products of animal origin published by Wageningen University & Research in 2017.