基于平行反应监测模式的液相色谱-四极杆-静电场轨道阱质谱测定生鲜牛乳中氟虫腈及其代谢物残留

目的：建立一种测定生鲜牛乳中氟虫腈及其3种代谢物（氟甲腈、氟虫腈硫醚及氟虫腈砜）残留的液相色谱-四极杆-静电场轨道阱质谱方法。方法：样品经乙腈提取后，经Captiva ND lipids净化柱去除基质中的脂质干扰物，液相色谱分离，四极杆-静电场轨道阱质谱定性定量测定，平行反应监测模式检测。结果：4种待测组分均获得足够的色谱保留和分离，各化合物在0.5~10.0 μg·kg^-1范围内呈现良好的线性关系，日内日间精密度小于15%，方法回收率在85%~115%之间，方法的定量下限为0.5 μg·kg^-1。结论：此方法快速、准确且灵敏度高，为监测生鲜牛乳中的氟虫腈提供了有效的技术手段。

Objective: To establish a quantitative method of LC-quadrupole-Orbitrap MS for the determination of fipronil and its metabolites(fipronil-desulfinyl, fipronil sulfide, and fipronil sulfone) residues in raw milk. Methods: Milk samples were exacted with acetonitrile. Then the supernatant was purified by Captiva ND lipids solid phase extraction prior to being separated by liquid chromatography and analyzed by quadrupole-orbitrap mass spectrometry. The analytes were determined with parallel reaction monitoring mode. Results: The four analytes had sufficiently chromatography retention and separation. The calibration curve of each object showed a good linear within the concentration range from 0.5-10.0 μg·kg^-1. The intra-and inter-day precisions were less than 15%. The average recoveries ranged from 85% to 115%. And the limit of detection was 0.5 μg·kg^-1. Conclusion: The method is rapid and highly sensitive,which provides an accurate and effective solution for the determination of fipronil in raw milk.

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