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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
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摘要 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.
出处 《扬州职业大学学报》 2014年第2期30-33,共4页 Journal of Yangzhou Polytechnic College
关键词 柱层析 分离 甲基托布津 column chromatography separation thiophanate-methyl
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