液相色谱质谱法直接进样测定水中的4种农药-wsyj修改稿.docVIP

液相色谱串联质谱法直接进样测定水中的呋喃丹、草甘膦、灭草松和2,4－D 郑和辉，李洁，魏建荣，吴大南，王萍 北京市疾病预防控制中心环境卫生所，北京 100013 摘要：目的 建立直接进样测定饮用水和水源水中的草甘膦和呋喃丹的液相色谱质谱的分析方法。方法 水样直接过0.22μm滤膜，用高效液相色谱带串联质谱分析检测，色谱柱：Atlantis C18 2.1mm× 50 mm。进行两个添加水平的测定，每个水平5个重复。结果 草甘膦、呋喃丹、灭草松和2，4－D在水中水平的添加，通过测定和工作曲线的计算，得到的回收率在％～10％相对标准偏差在0.8%～5.0％；草甘膦μg/mL，呋喃丹灭草松和2，4－D。在自来水和水源水中分别添加草甘膦、呋喃丹、灭草松和2，4－D，以倍信噪比（S/N）计算，在进样量20μL时；得到的本方法最低检测质量浓度分别是：草甘膦0.04μg/mL；呋喃丹0.ng/mL；灭草松0.10ng/mL和2，4－D 0.40ng/mL。结果表明该方法简单，速度快，准确度和灵敏度高，满足测定日常饮用水中新增的这四种农药检测项目的需要by Liquid Chromatography Electrospray Ionization Tandem Mass Spectrometry ZHENG Hehui, Li Jie,WU Danan ,WANG Ping Beijing Center for Disease Prevention and Control， Beijing 100013， China Abstract: Objective To setup the method for determination of carbofuran, glyphosate, bentazone, and 2,4-D in drinking water by liquid chromatography with tandem mass spectrometry. Methods Chromatographic column: Atlantis C18 2.1mm?50 mm; After passing 0.22nμm filter membrane, samples were detected by LC-MS-MS. Results At two spiked level, the average recoveries for glyphosate and carbofuran in drinking water were 99.0％～105.0％. Relative standard deviations were 0.8％～5.0％. The concentration of glyphosate at 0.2~4.0μg/mL, carbofuran at 0.1~2.0ng/mL, bentazone, and 2,4-D at 0.5~10.0 ng/mL, their linear regression values were greater than 0.9998 r≥0.9998 . The limits of detection S/N 10 for carbofuran 0.04ng/mL; glyphosate 0.04μg/mL; bentazone 0.10ng/mL; 2,4-D 0.40ng/mL. Conclusion Results showed that the method was simple and fast, had a good accuracy and high sensitivity. So it can meet the need for determination of carbofuran, glyphosate, bentazone, and 2,4－D in drinking water. Keywords: Glyphosate, Carbofuran, Bentazone, 2,4-D, Mass Spectrometry, Drinking Water 新制定的《生活饮用水卫生标准》[1]中，新增加了呋喃丹、草甘膦、灭草松和2，4－D四个农药检测项目，给出的呋喃丹和草甘膦的分析方法是样品浓缩后用液相色谱分离，再进行柱后衍生化，用莹光检测器检测，前处理较复杂，对柱后反应试剂和设备有特殊的要求。灭草松和2，4－D的分析方法也需要先进行预浓缩，再在碱性条件下用碘甲烷溶液酯化，生成易挥发的甲基化衍生物，再用GC-ECD测定，该方法的前处理复杂，对衍生化条件要求高。在以往的文献中，也有液相色谱质谱测定呋喃丹[2-3]、灭草松和2，4－D[3]的方法