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Citation: ZHANG Aizhi, LI Xiangjiang, WANG Zhiqing, ZHANG Shufen, SONG Yue, CAO Lili, CAI Juemei, CHEN Linji. Rapid determination of fipronil and its metabolite residues in eggs using ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, ;2018, 36(8): 745-751. doi: 10.3724/SP.J.1123.2018.03012 shu

Rapid determination of fipronil and its metabolite residues in eggs using ultra performance liquid chromatography-tandem mass spectrometry

Ningbo Institute for Food Control, Ningbo 315048, China

Received Date: 12 March 2018

A method was developed for the rapid simultaneous determination of fipronil and its metabolite residues in eggs using ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The egg samples (2 g) with 2 mL water were extracted with 4 mL acetonitrile. After adding 1 g sodium chloride, the mixture was centrifuged at 9000 r/min for 10 min at 4℃. The suspension was diluted and filtered through a 0.22 μm organic membrane. The analytes were separated on a C18 column (100 mm×2.1 mm, 1.7 μm), and detected under the multiple reaction monitoring (MRM) mode with a negative ESI source. The average recoveries of fipronil and its metabolites varied from 77.4% to 112.1%, and the relative standard deviations were between 4.0% and 13.6% at three spiked levels. The limits of detection (LODs) ranged from 0.10 μg/kg to 0.43 μg/kg. The method is simple, effective, and can be applied to real samples.
- ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS),
- QuEChERS,
- fipronil and its metabolites,
- eggs,
- matrix effects
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