液相色谱-四极杆-静电场轨道阱高分辨质谱测定鸡蛋及鸡肉中氟虫腈及其代谢物残留的研究

Determination of fipronil and its metabolites residues in chicken egg and muscle by liquid chromatography quadrupole-orbitrap-high resolution mass spectrometry

关键词:  氟虫腈及其代谢物  鸡蛋  鸡肉  液相色谱-高分辨质谱

摘要:

建立了一种测定鸡蛋与鸡肉中氟虫腈及其3种代谢物(氟甲腈、氟虫腈硫醚及氟虫腈砜)的液相色谱-四极杆-静电场轨道阱高分辨质谱方法。样品经提取和盐析后,由PRiME HLB净化柱快速净化,经液相色谱分离后,四极杆/静电场轨道阱质谱准确定性并定量,平行反应监测模式检测。4种待测组分均获得足够的色谱保留和分离,各药物在 0.1-5.0 μg/kg范围内呈现良好的线性关系,日内日间精密度小于20 %,方法回收率在75~115 %之间,方法的定量限为0.1 μg/kg。此方法快速、准确且灵敏度高,为目前国际上爆发的“毒鸡蛋”事件提供了准确有效的技术手段。

Abstract:

Abstracts： A method was established for the determination of fipronil and its metabolites (fipronil-desulfiny, fipronil sulfide and fipronil sulfone) residues in chicken egg and muscle by LC-quadrupole-Orbitrap MS. Chicken egg and muscle samples was exacted with acetonitrile, salted out by sodium chloride and anhydrous magnesium sulfate. Then the supernatant was quickly purified by PRiME HLB solid phase extraction prior to analysis by LC-HRMS. The matrix-matched calibration curve showed a good linear within the concentration range from 0.1-5.0 μg/kg. The average recoveries of fipronil and its metabolites at 3 levels of 0.1, 0.2 and 1.0 μg/kg ranged from 75% to 115%, and the relative standard deviations were less than 20%. The method was rapid and high sensitive, which provided an accurate and effective solution for the international incident of “poisonous eggs”.