| NBD-Cl柱前衍生-高效液相色谱法测定土壤中草甘膦残留 |
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| 引用本文： | 吴文静,林燕.NBD-Cl柱前衍生-高效液相色谱法测定土壤中草甘膦残留[J].农药学学报,2020,22(6):1027-1032. |
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| 作者姓名： | 吴文静 林燕 |
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| 作者单位： | 中国农业大学 理学院 应用化学系 农药创新中心,北京 100193;中国农业大学 理学院 应用化学系 农药创新中心,北京 100193 |
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| 基金项目： | 国家重点研发计划 (2016YFD0200208-4) |
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| 摘 要： | 建立了以4-氯-7-硝基苯并呋喃 (NBD-Cl) 柱前衍生为基础测定土壤中草甘膦残留的高效液相色谱法。土壤样品经0.6 mol/L KOH溶液提取，加入NBD-Cl衍生剂，在0.125 mol/L (pH = 9.0~10.5) 硼酸盐缓冲液介质中、60 ℃水浴条件下反应80 min。以0.02 mol/L V (磷酸氢二钠水溶液) : V (甲醇) = 70 : 30的混合溶液为流动相，经C18反相色谱柱分离后，采用二极管阵列检测器在500 nm波长处进行检测，外标法定量。结果表明:草甘膦在0.01~2.0 mg/L 范围内线性关系良好，相关系数为0.9999，定量限 (LOQ) 为0.02 mg/kg；向空白土壤样品中添加0.02、0.1和10 mg/kg 3个水平的草甘膦标准溶液，平均回收率在82%~93%之间，相对标准偏差 (RSD) 为2.5%~3.9%。该方法简便高效，适用于土壤样品中草甘膦的残留分析。
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| 关 键 词： | 4-氯-7-硝基苯并呋喃 柱前衍生化 草甘膦 高效液相色谱 土壤 残留分析 |
| 收稿时间： | 2020-02-15 |
Determination of glyphosate in soils by HPLC with pre-column derivatization using 4-chloro-7-nitro-1,2,3-benzoxadiazole |
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| Institution: | Innovation Center of Pesticide Research, Department of Applied Chemistry, College of Science, China Agricultural University, Beijing 100193, China |
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| Abstract: | A simple selective high-performance liquid chromatography (HPLC) method has been developed for the determination of glyphosate residue in soil samples based on a pre-column derivatization with 4-chloro-7-nitro-1,2,3-benzoxadiazole (NBD-Cl). Soil samples were extracted by 0.6 mol/L KOH solution. Glyphosate was derivatized with NBD-Cl in 0.125 mol/L sodium tetraborate medium (pH = 9.0-10.5). The reaction was completed after 80 min at 60 ℃. A elution consisting of a mixture of 0.02 mol/L Na2HPO4 solution and methanol (70 : 30, V/V) was used to separate the amine derivatives in a C18 column at room temperature. Diode array detector was applied at 500 nm. The correlation coefficient for the method was 0.9999 at the concentration ranging from 0.01 to 2.0 mg/L. The limits of quantification was 0.02 mg/kg. The average recoveries of glyphosate spiked at 0.02, 0.1and 10 mg/kg levels in soil samples were between 82% and 93%, and the relative standard deviations (RSD) were between 2.5% and 3.9%.The method is simple, rapid and suitable for the confirmation and quantification of GLUF in soil. |
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