柱后加碱-高效阴离子交换色谱-脉冲安培检测法测定农田土中草铵膦、氨甲基膦酸和草甘膦残留

doi:10.3724/SP.J.1123.2019.03025

色谱 ›› 2019, Vol. 37 ›› Issue (9): 1004-1010.DOI: 10.3724/SP.J.1123.2019.03025

柱后加碱-高效阴离子交换色谱-脉冲安培检测法测定农田土中草铵膦、氨甲基膦酸和草甘膦残留

陶雪梅¹, 朱红霞², 高立红³, 李仁勇⁴

1. 甘肃省环境监测中心, 甘肃兰州 730030;
2. 中国环境监测总站, 北京 100012;
3. 赛默飞世尔科技(中国)有限公司应用研发中心, 北京 100085;
4. 中科谱研(北京)科技有限公司, 北京 100027

收稿日期:2019-03-20 出版日期:2019-09-08 发布日期:2015-07-30
通讯作者: 朱红霞

Determination of glufosinate, aminomethylphosphonic acid, and glyphosate residues in farmland soil by post-column addition of alkali using high performance anion exchange chromatography-pulse amperometric detection

TAO Xuemei¹, ZHU Hongxia², GAO Lihong³, LI Renyong⁴

1. Gansu Province Environmental Monitoring Centre, Gansu, Lanzhou 730030, China;
2. China National Environmental Monitoring Centre, Beijing 100012, China;
3. Application Development Center, Thermo Fisher Scientific, Beijing 100085, China;
4. Zhongke PUYAN(Beijing) Science and Technology Co., Ltd., Beijing 100027, China

Received:2019-03-20 Online:2019-09-08 Published:2015-07-30

摘要/Abstract

摘要： 应用柱后加碱-高效阴离子交换色谱-脉冲安培检测法同时测定了农田土中草铵膦、氨甲基膦酸和草甘膦的残留。土壤样品用2 mmol/L氢氧化钠振荡提取，混匀后依次用0.22 μm滤膜、IC-C₁₈和IC-Na柱处理。滤液中的3种目标物和共存离子经IonPacAS11-HC离子色谱柱分离，柱后加碱-脉冲安培检测器检测。结果表明，草铵膦和草甘膦质量浓度在20.0~1000 μg/L、氨甲基膦酸质量浓度在5.0~400 μg/L范围内线性关系良好，相关系数均大于0.999。草铵膦、氨甲基膦酸和草甘膦的检出限分别为0.08、0.02和0.04 mg/kg，回收率为80.2%~106%，相对标准偏差为0.7%~5.0%（n=6）。该方法抗干扰性强、灵敏度和准确度高，操作简便快捷，适用于农田土中草铵膦，氨甲基膦酸和草甘膦残留量的检测。

关键词: 氨甲基膦酸, 草铵膦, 草甘膦, 高效阴离子交换色谱, 脉冲安培检测, 农田土, 柱后加碱

Abstract: A chromatographic method was developed for the determination of glufosinate (GLUF), aminomethylphosphonic acid (AMPA), and glyphosate (GLY) in farmland soil by the post-column addition of alkali using high performance anion exchange chromatography-pulse amperometric detection. Samples were extracted with 2 mmol/L sodium hydroxide solution, then filtered through a 0.22 μm membrane, and purified by a IC-C₁₈ column and IC-Na column. Three target compounds and coexisting ions in the filtered solution were separated on an IonPacAS11-HC anion exchange column (250 mm×4 mm), and were detected by the post-column addition of alkali using pulse amperometric detection. Results showed that GLUF and GLY had good linearity in the range of 20.0-1000 μg/L, and AMPA had good linearity in the range of 5.0-400 μg/L, with correlation coefficients above 0.999. The limits of detection of GLUF, AMPA, and GLY were 0.08, 0.02, and 0.04 mg/kg, respectively, and the recoveries were in the range of 80.2%-106% with RSDs of 0.7%-5.0% (n=6). The method provides strong anti-interference, high sensitivity, and accuracy, and can be adopted simply and quickly; therefore, it is suitable for detecting the residues of GLUF, AMPA, and GLY in farmland soil.

Key words: aminomethylphosphonic acid (AMPA), farmland soil, glufosinate (GLUF), glyphosate (GLY), high-performance anion exchange chromatography, post-column addition of alkali, pulse amperometric detection

中图分类号:

O658

陶雪梅, 朱红霞, 高立红, 李仁勇. 柱后加碱-高效阴离子交换色谱-脉冲安培检测法测定农田土中草铵膦、氨甲基膦酸和草甘膦残留[J]. 色谱, 2019, 37(9): 1004-1010.

TAO Xuemei, ZHU Hongxia, GAO Lihong, LI Renyong. Determination of glufosinate, aminomethylphosphonic acid, and glyphosate residues in farmland soil by post-column addition of alkali using high performance anion exchange chromatography-pulse amperometric detection[J]. Chinese Journal of Chromatography, 2019, 37(9): 1004-1010.

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柱后加碱-高效阴离子交换色谱-脉冲安培检测法测定农田土中草铵膦、氨甲基膦酸和草甘膦残留

Determination of glufosinate, aminomethylphosphonic acid, and glyphosate residues in farmland soil by post-column addition of alkali using high performance anion exchange chromatography-pulse amperometric detection

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