嘧啶芐胺類化合物的水解反應研究

制藥工程論文編號:ZY097    論文字數:9838,頁數:22

目 錄
中文摘要Ⅰ
英文摘要Ⅱ
目錄·Ⅲ
1．緒論·1
 1.1前言1
 1.2農藥的水解動力學規律1
 1.3影響水解速率的因素2
 1.4農藥的水解機理2
 1.5農藥水解研究方法3
 1.6農藥水解分析方法3
2．實驗部分·5
 2.1儀器和試劑5
 2.1.1儀器·5
 2.1.2試劑·5
 2.2實驗設計5
 2.2.1實驗器皿處理·5
 2.2.2緩沖溶液的配制·5
 2.2.3儲備液溶劑的選擇·5
 2.2.4儲備溶液的配制·6
 2.3水解實驗操作6
 2.3.1水解溶液的配制·6
 2.3.2水解樣預處理·6
 2.3.3測試實驗·6
 2.3.4水解體系的檢測·6
 2.4分離條件的選擇6
 2.4.1檢測波長的選擇·6
 2.4.2流動相比例的選擇·7
 2.4.3最佳液相條件的確定·8
3．結果與討論·9
 3.1方法的建立9
 3.1.1線性關系·9
 3.1.2靈敏度的測定10
 3.1.3精密度的測定10
 3.1.4回收率的測定10
 3.2嘧啶芐胺類化合物的水解反應·12
 3.2.1水解反應半衰期13
 3.2.1水解反應轉化率13
4．結論與展望15
致謝·16
參考文獻·17

摘要：本文通過高效液相色譜法研究了嘧啶芐胺類化合物的水解反應。建立8個嘧啶芐胺類化合物的最佳液相色譜條件：Diamonsil(TM)鉆石-C18反相色譜柱（150mmX4.6mm,不銹鋼柱）；ZJ0777的流動相為甲醇：水=0.6:0.4(V/V)；另外7種化合物為甲醇：水=0.9:0.1(V/V)，柱溫25℃，它們的工作曲線的線性相關系數均接近于1，該分析方法的回收率為95.47%～104.93%。實驗表明其水解符合一級反應動力學方程，并得出各水解反應的動力學參數。結果顯示隨著反應溫度升高以及溶液pH值增大有利于水解反應的進行。
關鍵詞：嘧啶芐胺類化合物；高效液相色譜法；水解反應；動力學方程

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