超高效液相色谱-质谱联用法测定山野菜中5种农药的残留  

Determination of five pesticides residues in wild vegetables by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：符群[1] 赵红华[1] 刘峰[2] 任红波[2] 魏俊青[2] 陈国峰[2] 

机构地区：[1]东北林业大学林学院,黑龙江哈尔滨150040 [2]黑龙江省农业科学院农产品质量安全研究所,农业部农产品质量安全风险评估实验室(哈尔滨),黑龙江哈尔滨150086

出　　处：《食品工业科技》2017年第15期238-243,共6页Science and Technology of Food Industry

基　　金：2016全国粮油蔬菜质量安全风险评估项目(GJFP20160010002)

摘　　要：建立超高效液相色谱-质谱联用法[ACQUITY UPLC/Xevo TQ-S]测定人工栽培山野菜中啶虫脒、吡虫啉、多菌灵、嘧霉胺、苯醚甲环唑5种农药残留。以乙腈为提取溶剂,采用多重反应离子监测(MRM)模式,ACQUITY UPLC BEH C18为分析色谱柱、0.1%甲酸乙酸铵-乙腈为流动相,对样品进行检测分析。结果表明:5种农药在0.0005~2.0000 mg/L范围内与峰面积呈良好线性关系,相关系数在0.9947~0.9999之间。在农药混合标准溶液0.005~0.200 mg/kg的水平下,添加回收率均在73.43%~115.84%之间,相对标准偏差为2.04%~18.19%。检出限在0.020~0.510μg/kg范围内;定量限在0.066~1.699μg/kg范围内。本方法操作简单、快捷、准确度和精密度高,可应用于山野菜中5种农药残留测定。A method was established for determining acetamiprid, imidacloprid, carbendazim, pyrimethanil, difenoconazole residues in wild vegetables by ultra- high performance liquid chromatography- mass spectrometry （ ACQUITY UPLC/Xevo TQ-S）. Residues in samples were extracted with acetonitrile, and separated by C18 column with gradient elution using a mobile phase made up of acetonitrile and 0.1% formic acid ammonium acetate and detected.The results showed the linear range of 0.0005-2.0000 mg/L with the correlation coefficients from 0.9947 to 0.9999.The recoveries rates at 0.005~0.200 mg/kg levels were in the range of 73.43%- 115.84% .The relative standard deviation（ RSD ）was 2.04%- 18.19% .The limits of detection were 0.020-0.510 t,g/kg and the limits of quantitation were 0.066-1.699 μg/kg.The method proved to be simple, sensitive, rapid, accurate and precise for the determination of five kinds of pesticide residues in wild vegetables.

关 键 词：超高效液相色谱-质谱 山野菜 农药残留 检测 

分 类 号：TS207.3[轻工技术与工程—食品科学]