高效液相色谱-柱前衍生法测定水中有机磷除草剂.PDFVIP

高效液相色谱-柱前衍生法测定水中有机磷除草剂 1 2 1 1 刘铮铮 ，李立 ，王 静 ，潘荷芳 （1：浙江省环境监测中心，浙江 杭州 310012；2 ：树人大学生物与环境学院，浙江 杭州 310015 ） 摘 要：建立了水样中痕量草甘膦，草铵膦和氨甲基磷酸的FMOC 柱前衍生-高效液相色谱-荧光检测分析方 法。草甘膦，草铵膦和氨甲基磷酸的平均加标回收率分别为 94.2%、90.8%、98.6%；相对标准偏差分别为 4.8% 、0.68%、2.8% ；方法的定性下限和定量下限分别为：0.05、0.04、0.009μg/L 和 0.16、0.12、0.03μg/L。 水样放置两天后，水样中的草甘膦，草铵膦分别降解了 17.8%和 19.5%，而水样经过衍生后在 5 天内是稳 定的。 关键词：草甘膦；草铵膦；氨甲基磷酸；高效液相色谱；荧光；衍生。 中图分类号：X832 文献标识码：A Determination of organophosphorus herbicide in water by high performance liquid chromatography-pre- column derivatization LIU Zheng-zheng, et al (Zhejiang Environmental Monitoring Center, Hangzhou 310012, China) Abstracts: A method is proposed that allows the simultaneous determination of residue glyphosate, glufosinate and aminomethylphosphonic acid (AMPA) in water samples. The method involves pre-column derivatization step with 9-fluorenylmethylchloroformate (FMOC) in borate buffer and detection based on high performance liquid chromatography (HPLC) coupled with fluorophotomeric detectior. The method produces satisfactory reliability, sensitivity, and accuracy. The mean recovery values are 94.2%, 90.8%, 98.6% for glyphosate, glufosinate and AMPA, respectively, and the relative standard deviation are 4.8% ，0.68%，2.8%, respectively. Limits of detection and quantitative lower limits are 0.05, 0.04, 0.009μg/L and 0.16, 0.12, 0.03μg/L for the three compounds. The degradation rate of glyphosate, glufosinate in water are 17.8% and 19.5% after 2 days. The derivatization of these compounds are stable in 5 days. Key woods: Glyphosate; Glufosinate; Aminomethylphosphonic acid; High performance liquid chromatography; Fluorophotomeric; Derivatization 草甘膦（Glyphosate ）是一种优良的灭生性高效除草剂，也是现在国际上使用最广泛的 有机磷除草剂。草铵膦（Glufosinate ）是继草甘膦之后又一性能优良的灭生性除草剂，其不 但可以灭生除草，还可以作为转基因技术研究的筛选剂 [1] 。而氨甲基磷酸