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| Determination of Fipronil and Its Metabolites in Animal Derived Foods by QuEChERS Method Combined with Ultra Performance Liquid Chromatography-High-resolution Benchtop Q Exactive Mass Spectrometry |
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| DOI： |
| KeyWord:fipronil animal derived food QuEChERS high resolution mass spectrometry metabolites |
| Author | Institution |
| L? Bing,YIN Shuai-xing,CHEN Da-wei,FANG Cong-rong,ZHOU Shuang,ZHAO Yun-feng |
1.国家食品安全风险评估中心/卫生部食品安全风险评估重点实验室;2.岛津技迩上海商贸有限公司 |
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| Abstract: |
| Based on cryogenic treatment and QuEChERS method,an ultra performance liquid chromatography-high resolution benchtop Q-Exactive mass spectrometry method for the determination of fipronil and its metabolites in animal derived foods was established.The samples were extracted with acetonitrile,and cleaned up by the cryogenic treatment and dispersive solid phase extraction(d-SPE)with the N-propylethlene diamine(PSA)and C18.The chromatographic analysis was performed on a BEH C18 column with 0.1% acetic acid and acetonitrile as mobile phase by gradient elution,and the external standard calibration was used for quantification.The negative ion acquisition mode was applied,and the quantitative analysis was carried out by high resolution mass spectrometry using parallel reaction monitoring(PRM)mode.Fipronil and its metabolites showed good linearities in the concentration ranges of 0.02-2 μg/L and 0.2-20 μg/L,with the correlation coefficients(r2)above 0.992.For liquid or semi-liquid samples(such as milk and eggs)and the solid samples(such as chicken)，the limits of quantification(LOQs)for 4 analytes were between 0.1 μg/kg and 0.2 μg/kg.At different spiked levels,the average recoveries of fipronil and its metabolites in eggs,chicken and milk were in the ranges of 81.6%-96.9%,81.2%-96.0% and 79.1%-100.1%,with the relative standard deviations(RSDs)of 1.3%-11.5%,3.4%-11.4% and 1.5%-10.7%,respectively.The method was simple,sensitive and accurate,and was suitable for the rapid screening and quantitative analysis of fipronil and its metabolites in animal derived foods,and the sensitivity of the method could meet the requirement for residual limitation of EU. |
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