超高效液相色谱-串联质谱法快速测定鸡蛋中氟虫腈及其代谢物残留

建立了超高效液相色谱-串联质谱(UPLC-MS/MS)快速测定鸡蛋中氟虫腈及其代谢物的方法。在2 g鸡蛋中加入2 m L水后,用4 m L乙腈提取,然后加入1 g NaCl,于4℃以9 000 r/min离心10 min,稀释后过有机膜。采用C18色谱柱(100 m m×2.1 m m,1.7μm)分离,在电喷雾电离源、负离子模式下进行多反应监测(MRM)采集。结果表明,氟虫腈及其代谢物在3个添加水平下的回收率为77.4%~112.1%,相对标准偏差为4.0%~13.6%,检出限为0.10~0.43μg/kg。该法简单、高效,可用于实际样品检测。

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

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.