QuEChERS-超高效液相色谱-串联质谱法测定动物源性食品中氟虫腈及其代谢物残留

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

建立了禽蛋、动物肌肉、内脏和蛋制品中氟虫腈及其代谢物氟甲腈、氟虫腈砜、氟虫腈亚砜的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。在QuEChERS方法基础上,针对目标物化学性质和样品杂质情况,对提取溶液的种类、提取次数、净化材料等参数进行了优化。最终样品经乙腈提取,NaCl、无水MgSO_4盐析分层,提取液经PSA结合C_(18)进行分散固相萃取净化,以UPLC-MS/MS进行测定,基质外标法进行定量分析。结果表明,动物源性食品中氟虫腈、氟甲腈、氟虫腈砜、氟虫腈亚的平均加标回收率在75.7%~104.5%之间,相对标准偏差在1.3%~10.4%之间,检出限在0.5~1.6μg/kg之间,定量限为5.0μg/kg。此方法快速、简便、灵敏度高、准确,可用于禽蛋、动物肌肉、内脏和蛋制品中氟虫腈及其3种代谢物残留的同时测定。

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 Qu ECh ERS 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.