嘧啶苄胺类化合物的水解反应研究

范文编号:ZY097    范文字数:9838,页数:22

摘要：本文通过高效液相色谱法研究了嘧啶苄胺类化合物的水解反应。建立8个嘧啶苄胺类化合物的最佳液相色谱条件：Diamonsil(TM)钻石-C18反相色谱柱（150mmX4.6mm,不锈钢柱）；ZJ0777的流动相为甲醇：水=0.6:0.4(V/V)；另外7种化合物为甲醇：水=0.9:0.1(V/V)，柱温25℃，它们的工作曲线的线性相关系数均接近于1，该分析方法的回收率为95.47%～104.93%。实验表明其水解符合一级反应动力学方程，并得出各水解反应的动力学参数。结果显示随着反应温度升高以及溶液pH值增大有利于水解反应的进行。
关键词：嘧啶苄胺类化合物；高效液相色谱法；水解反应；动力学方程

Abstract: The hydrolysis of pyrimidinbenzylamine derivatives were studied by HPLC analysis in the paper. The best analysis method was adopted with C18 column (150 mm×4.6 mm, the stainless steel pillar, diamonsil (TM) diamond-type) for 8 pyrimidinbenzylamine derivatives. The methanol-water (60:40, V/V) as the mobile phase is for ZJ0777, while methanol-water (90:10, V/V) for the other compounds. Average recovery rate was 98.5~104%, The column temperature was 25℃. The calibnation curves were linear, r=0.9998. Average recovery rate was 95.47~104.93%. The kinetics process can be described by the fist-order reaction law, and the hydrolytic reaction parameters have been obtained. The experimental results show that it is helpful to the hydrolytic process via rising pH value and temperature.
Keyword: Pyrimidinyloxybenzylamine；HPLC；Hydrolysis；Kinetics

目 录
中文摘要Ⅰ
英文摘要Ⅱ
目录·Ⅲ
1．绪论·1
 1.1前言1
 1.2农药的水解动力学规律1
 1.3影响水解速率的因素2
 1.4农药的水解机理2
 1.5农药水解研究方法3
 1.6农药水解分析方法3
2．实验部分·5
 2.1仪器和试剂5
 2.1.1仪器·5
 2.1.2试剂·5
 2.2实验设计5
 2.2.1实验器皿处理·5
 2.2.2缓冲溶液的配制·5
 2.2.3储备液溶剂的选择·5
 2.2.4储备溶液的配制·6
 2.3水解实验操作6
 2.3.1水解溶液的配制·6
 2.3.2水解样预处理·6
 2.3.3测试实验·6
 2.3.4水解体系的检测·6
 2.4分离条件的选择6
 2.4.1检测波长的选择·6
 2.4.2流动相比例的选择·7
 2.4.3最佳液相条件的确定·8
3．结果与讨论·9
 3.1方法的建立9
 3.1.1线性关系·9
 3.1.2灵敏度的测定10
 3.1.3精密度的测定10
 3.1.4回收率的测定10
 3.2嘧啶苄胺类化合物的水解反应·12
 3.2.1水解反应半衰期13
 3.2.1水解反应转化率13
4．结论与展望15
致谢·16
参考文献·17

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