柱层析分离甲基托布津粗品中杂质的研究

Separation of Thiophanate-Methyl by Column Chromatography

利用硅胶柱层析和薄层层析分离甲基托布津合成产物中的微量杂质。柱层析分离杂质的适宜条件:0.5mL的粗品上硅胶(80-100目)的层析柱,流动相为乙酸乙酯∶石油醚(3∶2,V/V),流速为0.9mL·min-1,并通过高效液相色谱及时测定结果,经过多次富集得到杂质纯品,并由液质联用仪和核磁共振分析杂质结构,得出杂质是因为反应过程中发生副反应(水解或者氧化),所以应创造无氧的反应条件。

In this paper,trace impurity in synthetic thiophanate-methy1 was separated and purified by thin layer chromatography and silica gel column chromatography. The optimum condition for silica gel column were confirmed： 0. 5mL of crude reaction produce was applied to silica gel column（ gel 80-100 mesh） while mixture of ethyl acetate： petroleum ether（ 3∶ 2,V / V） was used as mobile phase and the flow rate was 0. 9mL /min,thereby separating impurities and Thiophanate-Methy1 were measured by HPLC at any time. After several rounds of enrichment to obtain impurity pure,the structure of impurities was analyzed by liquid chromatography-mass spectrometry and nuclear magnetic,so it＇s concluded that the impurity was the result of hydrolysis or oxidation,and anaerobic reaction conditions should be created.