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

作　　者：曲斌[1] 刘善菁 刘雨昕 陆桂萍[1] 耿士伟[1] QU Bin;LIU Shan-Jing;LIU Yu-Xin;LU Gui-Ping;GENG Shi-Wei(Jiangsu Quality Inspection and Testing Center for Animal Products, Nanjing 210036, China)

机构地区：[1]江苏省畜产品质量检验测试中心,南京210036

出　　处：《食品安全质量检测学报》2018年第6期1332-1337,共6页Journal of Food Safety and Quality

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0.5~10.0μg/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0.5μg/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。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 supematant 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 0.5-10.0μg/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 0.5μg/kg. Conclusion The method is rapid, accurate and sensitive, which provides an accurate and effective solution for the monitoring of fipronil in pork.

关 键 词：氟虫腈及其代谢物 猪肉 液相色谱-串联质谱法 残留 

分 类 号：O657.63[理学—分析化学]