液相色谱-质谱法测定蔬菜中氟虫腈及代谢物残留与氟虫腈砜的来源探究  

Determination of Fipronil and Its Metabolites in Vegetables by Liquid Chromatography-Tandem Mass Spectrometry and the Investigation of Fipronil Sulfone Sources

作　　者：黄江鹏 孙雯雯 陈少敏 陈慧冰 吴海军 HUANG Jiang-peng;SUN Wen-wen;CHEN Shao-min;CHEN Hui-bing;WU Hai-jun(Guangzhou Huadu District Agricultural Technology Management Center,Guangzhou 510800,China;Shanghai AB Sciex Analytical Instrument Trading Co.,Ltd,Guangzhou 510320,China;Guangzhou Customs Technology Center,Guangzhou 510000,China;Guangzhou Nansha Mingxi Detection Service Co.,Ltd.,Guangzhou 511464,China)

机构地区：[1]广州市花都区农业技术管理中心,广东广州510800 [2]上海爱博才思分析仪器贸易有限公司,广东广州510320 [3]广州海关技术中心,广东广州510000 [4]广州南沙明曦检测服务有限公司,广东广州511464

出　　处：《分析测试学报》2025年第2期342-348,共7页Journal of Instrumental Analysis

摘　　要：建立了液相色谱-串联质谱同时测定蔬菜中氟虫腈及代谢物氟甲腈、氟虫腈砜、氟虫腈硫醚残留的方法。样品经乙腈提取后稀释,过微孔滤膜后,在多反应监测模式下进行检测。结果表明:4种目标组分的线性范围为1~100μg/L,相关系数均大于0.998,回收率为96.0%~117%,相对标准偏差为1.7%~5.3%,定量下限为0.005 mg/kg。该方法操作简便,回收率和重复性良好。使用该方法测定抽样蔬菜样品,检出氟虫腈砜残留,但未检出氟虫腈。针对检测出的氟虫腈砜进行了深入调查和来源研究,采用气相色谱-质谱法测定农户施用的农药,发现农药中添加氟虫腈砜。A method was established for the determination of fipronil and its metabolites fipronil de⁃sulfinyl,fipronil sulfone and fipronil sulfide in vegetables by liquid chromatography-tandem mass spectrometry.The sample was extracted with acetonitrile and diluted,then filtered through millipore filter and multiple reaction monitoring(MRM)mode was selected for the determination.The results showed that the linear range for four analytes was 1-100μg/L,with the correlation coefficients(r2)larger than 0.998.The limit of quantification was 0.005 mg/kg.The recoveries were ranged from 96.0%to 117%,and the relative standard deviations(RSDs)were between 1.7%-5.3%.This meth⁃od proves to be simple,fast and accurate,and has relative better recoveries and repeatability.Fipro⁃nil sulfone was detected in the market sampling vegetable samples,while fipronil was not detected.In-depth investigation and source research on the detected fipronil sulfone was conducted by gas chro⁃matography-mass spectrometry method,and the results showed that fipronil sulfone was found to be added in pesticides.

关 键 词：液相色谱-串联质谱法 气相色谱-质谱法 蔬菜 农药残留 氟虫腈及代谢物 

分 类 号：O657.7[理学—分析化学] TS207.3[理学—化学]