郑和辉, 于建, 查玉娥, 卞战强, 田向红, 张娟. 液相色谱质谱法直接进样测定饮用水中6种常用农药残留[J]. 环境卫生学杂志, 2016, 6(1): 60-63. DOI: 10.13421/j.cnki.hjwsxzz.2016.01.014
    引用本文: 郑和辉, 于建, 查玉娥, 卞战强, 田向红, 张娟. 液相色谱质谱法直接进样测定饮用水中6种常用农药残留[J]. 环境卫生学杂志, 2016, 6(1): 60-63. DOI: 10.13421/j.cnki.hjwsxzz.2016.01.014
    ZHENG Hehui, YU Jian, ZHA Yu, BIAN Zhanqiang, TIAN Xianghong, ZHANG Juan. Determination of 6 Pesticides Simultaneously in Drinking Water by Liquid Chromatography-Mass Spectrometry[J]. Journal of Environmental Hygiene, 2016, 6(1): 60-63. DOI: 10.13421/j.cnki.hjwsxzz.2016.01.014
    Citation: ZHENG Hehui, YU Jian, ZHA Yu, BIAN Zhanqiang, TIAN Xianghong, ZHANG Juan. Determination of 6 Pesticides Simultaneously in Drinking Water by Liquid Chromatography-Mass Spectrometry[J]. Journal of Environmental Hygiene, 2016, 6(1): 60-63. DOI: 10.13421/j.cnki.hjwsxzz.2016.01.014

    液相色谱质谱法直接进样测定饮用水中6种常用农药残留

    Determination of 6 Pesticides Simultaneously in Drinking Water by Liquid Chromatography-Mass Spectrometry

    • 摘要: 目的 建立同时测定生活饮用水中毒死蜱、丁草胺、乙草胺、敌敌畏、莠去津和多菌灵6种常用农药的超高效液相色谱串联质谱(UPLC-MS/MS)分析方法。方法 采用Waters公司Acquity UPLC BEH C18柱(2.1 mm×50 mm),以乙腈/甲醇和0.1%甲酸水溶液为流动相,进行梯度洗脱分离。经正离子电喷雾(ESI+)电离及多反应监测(MRM)模式检测。结果 毒死蜱和敌敌畏的质量浓度在2.5~100 μg/L,丁草胺和乙草胺的质量浓度在0.5~20 μg/L,莠去津的质量浓度在0.125~5 μg/L,多菌灵的质量浓度在0.05~2 μg/L范围时,线性相关系数r ≥ 0.999;毒死蜱、丁草胺、乙草胺、敌敌畏、莠去津和多菌灵的最低检测质量浓度分别为7,21,10,5和1 ng/L。平均回收率为84.7%~105.0%,相对标准偏差为1.5%~6.1%。用该分析方法检测了7个地下水样品,都检出了莠去津残留,浓度在0.01~0.03 μg/L。结论 该方法具有操作简便、灵敏度高、抗干扰能力强、样品分析时间短等特点,可用于饮用水中6种农药残留水平和残留动态的日常监测。

       

      Abstract: Objectives An ultra-performance liquid chromatography-tandem mass spectrometric method (UPLC-MS/MS)was established for the simultaneous determination of chlorpyrifos, butachlor, acetochlor, dichlorvos, atrazine and carbendazim residues in drinking water.Methods Water samples were separated by a Acquity UPLC BEH(2.1mm×50 mm)C18 column with a gradient elution of acetonitrile/methanol and 0.1% formic acid, and detected by UPLC-MS/MS. The identification was achieved by eletrospray ionization (ESI+)in multiple reactions monitoring (MRM)mode.Results There was a good linear relationship while the levels of chlorpyrifos and dichlorvos were 2.5~100 μg/L, the levels of butachlor and acetochlor were 0.5~20 μg/L, the levels of atrazine were 0.125~5 μg/L and that of carbendazim were 0.05~2 μg/L in tested samples; the correlation coefficients were not less than 0.999. The detection limits were 7, 21, 10, 5 and 1 ng/L for chlorpyrifos, butachlor, acetochlor, dichlorvos, atrazine and carbendazim, respectively. The recoveries were in the ranged of 84.7%~105.0% with relative standard deviations of 1.5%~6.1%. The results indicated that the method was easy, rapid, efficient, and suitable for simultaneous determination of six pesticide residues in drinking water. Atrazine was detected in all 7 underground water samples by the method, and the concentration was 0.01~0.03μg/L.Conclusions The method was simple and rapid with good accuracy and high sensitivity. The method could meet the needs for the determination of these 6 pesticides in drinking water.

       

    /

    返回文章
    返回