液相色谱-串联质谱法测定猪肉中氟虫腈及其代谢物残留

Quantitative determination of fipronil and its metabolites residues in pork by liquid chromatography-tandem mass spectrometry

中文关键词:  氟虫腈及其代谢物  猪肉  液相色谱-串联质谱法  残留

英文关键词:fipronil and its metabolites  pork  liquid chromatography-tandem mass spectrometry  residue

中文摘要:

      目的 建立一种测定猪肉中氟虫腈及其3种代谢产物(氟甲腈、氟虫腈硫醚及氟虫腈砜)的液相色谱-串联质谱方法。方法 样品经乙腈提取后, 经固相萃取柱去除基质中的脂质干扰物, 液相色谱分离, 串联四极杆质谱定量测定, 选择性反应监测模式检测。结果 4种待测组分均获得足够的色谱保留和分离, 各药物在0.5~10.0 μg/kg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 的定量限为0.5 μg/kg。结论 此方法快速、准确且灵敏度高, 为监测猪肉中的氟虫腈提供了准确有效的技术手段。

英文摘要:

      Objective To establish a quantitative method for determination of fipronil and its metabolites (fipronil-desulfiny, fipronil sulfide and fipronil sulfone) residues in pork by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Pork samples were exacted with acetonitrile. Then the supernatant was purified by solid phase extraction prior to analysis by LC-MS/MS. The analytes were determined by selective reaction monitoring mode. Results The matrix-matched calibration curve showed a good linear within the concentration range of 0.5-10.0 μg/kg. The average recoveries of fipronil and its metabolites at 3 spiked levels of 0.5, 1.0 and 5.0 μg/kg ranged from 85% to 115%, and the relative standard deviations were less than 15%. The limit of quantitation was 0.5 μg/kg. Conclusion The method is rapid, accurate and sensitive, which provides an accurate and effective solution for the monitoring of fipronil in pork.