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QuEChERS-固相萃取-UHPLC-MS/MS法快速检测猪肾中氟虫腈及其代谢物残留量
作者姓名:丁宁  吕飞  刘敏慧  赵旭伟  伍和平  沈鸿  蒋小良
作者单位:河源海关;惠州海关;江门海关;河源市农产品质量监督检验检测中心
基金项目:广东省科技发展专项资金项目(河科P001);广州海关科技计划项目(2018GDK24)。
摘    要:利用Qu ECh ERS-固相萃取法结合高效液相色谱—串联质谱法检测猪肾中氟虫腈及其3个代谢物残留量。样品用甲酸乙腈和商品化多兽残Qu ECh ERS盐包提取,采用固相萃取净化,外标法定量。在不同浓度的加标水平下,氟虫腈及其代谢物在猪肾中的平均回收率为95.3%~105.7%,相对标准偏差为2.68%~7.58%,方法检出限在0.0033μg/kg~0.50μg/kg,定量限在0.011μg/kg~1.50μg/kg范围内。该方法高效、简单、准确、灵敏,适用于对猪肾样品氟虫腈及其3种代谢物的快速定量分析。

关 键 词:QUECHERS  UHPLC-MS/MS  猪肾  氟虫腈及其代谢物

Rapid Detection of Fipronil and its Metabolite Residues in Pid Kidney by solid Phase Extraction-QuEChERS-combined with high Performance Liquid Chromatography-tandem mass Spectrometry
Authors:DING Ning  LV Fei  LIU Min-Hui  ZHAO Xu-Wei  WU He-Ping  SHEN Hong  JIANG Xiao-Liang
Institution:(Heyuan Customs,Heyuan 517000;Huizhou Customs,Huizhou 516001;Jiangmen Customs,Jiangmen 529000;Heyuan agricultural product quality supervision inspection and Testing Center,Heyuan 517000)
Abstract:The QuEChERS-solid phase extraction(SPE) combined with high performance liquid chromatography tandem mass spectrometry was used to detect the residues of fipronil and its three metabolites in pig kidney. The samples were extracted with methane acetonitrile and QuEChERS Salt package, purified by SPE, quantified by external standard method. At different concentrations, the average recoveries of fipronil and its metabolites in pig kidney were in range of 95.3%~105.7%,with RSD in the range of 2.68%~7.58%, the LOD was in the range of 0.0033μg/kg~0.50μg/kg, and LOQ was in the range of 0.011μg/kg~1.50μg/kg. The method is efficient, simple, accurate and sensitive, which is suitable for rapid quantitative detection of fipronil and its three metabolites in pig kidney.
Keywords:QuEChERS  UHPLC-MS/MS  pig kidney  fipronil and its metabolites
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