液相色谱法研究超高效除草剂水解反应动力学

论文编号:SW199  论文字数:9352,页数:24

摘要： 本文采用高效液相色谱法研究了新型超高效除草剂N－(2－溴苯基)－2－(4，6－二甲氧基嘧啶－2－基氧)苄胺（ZJ0777）的水解反应。测定的最佳分析条件为： C18反相色谱柱，流动相甲醇:水为0.6：0.4，紫外检测波长245.8nm，线性范围5～100mg.L-1，相关系数为0.9998，峰面积变异系数为3.77％，回收率为97.9％～103.6％，检出限为2.5mg.L-1。研究结果表明：ZJ0777在酸性、中性条件下比较稳定，不易水解，而在碱性条件下随温度升高水解速度加快。本研究的目的在于探索ZJ0777的水化学降解行为，作为环境安全性评价的科学依据。

关键词：高效液相色谱；水解；温度效应；ZJ0777；除草剂

Abstract: The hydrolysis of a highly active herbicide N-(2-bromophenyl)-2- (4,6-dimethoxypyrimidin- 2-yloxy)benzylamine (ZJ0777) in distilled water was studied by HPLC analysis in the paper. RP-HPLC was adopted with C18 column, methanol-water (60:40) as the mobile phase, detecting wavelength was at 240 nm, The calibnation curves were linear with a rang of 5~100 mg. L-1 for ZJ0777, r=0.9998. RSD was 3.77%. Average recovery rate was 97.9~103.6%. The detection limit was 2.5 mg.L-1. The experimental results indicated that ZJ0777 was relative stable in acidic or neutral condition, while the hydrolysis rate increased in basic medium. The study explored the hydrolysis behavior of ZJ0777 as the scientific evidence for environmental evaluation.

Keywords:  HPLC; Hydrolysis; Temperature effect; ZJ0777; Herbicide

目   录
中文摘要...................................................................Ⅰ
英文摘要...................................................................Ⅱ
目录.......................................................................Ⅲ
1  前言..................................................................... 1
 1.1 长残效除草剂使用概况.................................................. 1
 1.2 嘧啶苄胺类除草剂简介.................................................. 2
 1.3 新除草剂ZJ0777介绍................................................... 2
 1.4 农药水解动力学规律.................................................... 3
 1.5 水解速率的影响因素.................................................... 4
 1.6 农药的水解机理........................................................ 4
 1.7 农药水解的研究方法.................................................... 5
    1.7.1 预备实验.......................................................... 5
    1.7.2 不稳定化合物的水解................................................ 5
   1.7.3 水解分析方法...................................................... 6
2  实验部分 ................................................................ 6
  2.1 主要仪器与试剂........................................................ 6
    2.1.1 仪器.............................................................. 6
    2.1.2 试剂.............................................................. 6
  2.2 实验准备.............................................................. 6
    2.2.1 实验器皿的处理.................................................... 6
   2.2.2缓冲溶液的配制 .....................................................7
    2.2.3 ZJ0777储备溶液的配制...............................................7
    2.2.4 ZJ0777储备溶液与水的配比实验.......................................7
  2.3 水解实验操作.......................................................... 7
  2.4 水解体系的PH检测......................................................8
  2.5 分析方法.............................................................. 8
    2.5.1 HPLC操作条件的选择 ............................................... 8
 2.5.2 操作条件.......................................................... 9
 2.5.3 方法回收率........................................................ 9
 2.5.4 方法精密度....................................................... 10
 2.5.5 方法线性关系测定................................................. 10
3  结果与讨论.............................................................. 11
 3.1 PH对ZJ0777水解速率的影响............................................ 12
 3.2 温度对ZJ0777水解速率的影响.......................................... 13
 3.3 ZJ0777水解转化率..................................................... 15
4  总结与展望.............................................................. 16
致谢....................................................................... 17
参考文献................................................................... 18