超高效液相色谱串联质谱法快速测定生活饮用水中草铵膦、草甘膦及其代谢物氨甲基膦酸残留

Determination of glufosinate, glyphosate and their metabolites aminomethyl phosphonic acid residues in drinking water by ultra performance liquid chromatography triple quadrupole mass spectrometry

中文关键词:  超高效液相色谱串联质谱法  草铵膦  草甘膦  氨甲基膦酸  生活饮用水

英文关键词:ultra performance liquid chromatography triple quadrupole mass spectrometry  glufosinate  glyphosate  aminomethyl phosphonic acid  drinking water

中文摘要:

      目的 建立了一种非衍生-超高效液相色谱-串联质谱快速检测生活饮用水中的草铵膦、草甘膦及其代谢物氨甲基膦酸残留的方法。方法 以5 mmol/L的乙酸铵-氨水溶液(pH 12.0)和乙腈为流动相, 梯度洗脱, Dikma Polyamino 氨基柱(2.0 mm×150 mm, 5 μm)色谱分离, 采用电喷雾离子源负离子模式多反应监测(MRM)进行质谱测定, 采用外标法定量。结果 草铵膦、草甘膦、氨甲基膦酸分别在2.5~100, 5~200, 5~200 μg/L的浓度范围内线性关系良好, 相关系数(r2)均大于0.999。方法的检出限分别为1.0、2.0、2.0 μg/L, 定量限为2.5、5.0、5.0 μg/L。草铵膦、草甘膦、氨甲基膦酸在3档加标水平下的回收率为93.6%~102%, 相对标准偏差(relative standard deviation, RSD)为4.47%~7.15%。结论 本方法的样品无需衍生, 简便、准确可靠, 可用于生活饮用水中草铵膦、草甘膦及其代谢物氨甲基膦酸残留的快速检测。

英文摘要:

      Objective To establish a rapid method for determination of glufosinate, glyphosate, and its metabolites aminomethyl phosphonic acid residues in drinking water by ultra performance liquid chromatography triple quadrupole mass spectrometry (UPLC-MS/MS). Methods The analytes were separated on the Dikma Polyamino column (2.0 mm×150 mm, 5 μm) using acetonitrile and5 mmol/L ammonium acetate -ammonia solution (pH12.0) as a mobile phase for gradient elution, and then determined by tandem mass spectrometry in negative electrospray ion source mode under multiple reaction monitoring. The quantitative determination was performed by external standard method. Results Glyphosate, glyphosate, and aminomethylphosphonic acid had good linear relationships in the concentration ranges of 2.5100 μg/L, 5200 μg/L, and 5200 μg/L, respectively, and the correlation coefficients (r2) were all greater than 0.999. The limits of detection were 1.0, 2.0, 2.0 μg/L, and the limits of quantitation were 2.5, 5.0, 5.0 μg/L, respectively. The recoveries of glufosinate, glyphosate and aminomethyl phosphonic acid at the 3 standard levels were 93.6%-102%, and the relative standard deviation (RSD) was 4.47%7.15%. Conclusion The sample of this method does not require derivation. Itis simple, accurate and reliable, and can be used for the rapid detection of glufosinate, glyphosate, and their amino acid metabolite residues in drinking water.