4-苯基噁唑烷-2-硫酮对映体的模拟移动床色谱分离  

Separation of 4-phenyloxazolidine-2-thione enantiomers by simulated moving bed chromatography

作　　者：王绍艳[1] 李守江 洪鹤员 魏伯峰[1] 

机构地区：[1]辽宁科技大学化学工程学院,辽宁鞍山114051

出　　处：《中国科技论文》2017年第12期1346-1349,共4页China Sciencepaper

基　　金：国家自然科学基金资助项目(21576127);高等学校博士学科点专项科研基金资助项目(20132120110002);鞍山市科委基金资助项目(3126)

摘　　要：为了实现4-苯基噁唑烷-2-硫酮对映体的拆分,采用三带模拟移动床(simulated moving bed,SMB)色谱体系。该体系以甲醇为流动相,单键合β-环糊精手性填料为固定相,色谱柱规格为长100mm,直径10mm,设置洗脱带Ⅰ:2根色谱柱;精制带Ⅱ:1根色谱柱;吸附带Ⅲ:1根色谱柱,Ⅰ带独立。用线性理想模型描述4-苯基噁唑烷-2-硫酮对映体在色谱单柱的色谱行为。将单柱理想模型与2-1-1模式的结点模型结合,建立SMB色谱模型,用SMB色谱模型描述连续进样时4-苯基噁唑烷-2-硫酮对映体在SMB体系的分离情况。模型计算与实验结果表明:连续进样下,通过调整切换时间不能同时得到高纯度的2个对映体。实验中选择间歇进样,可以同时获得实际纯度大于98.0%的2个对映体。To realize the separation of 4-phenyloxazolidine-2-thione enantiomers, three-zone simulated moving bed （SMB） chroma-tography system was employed. In this SMB system, /5-cyclodextrin-bonded chiral silica gels was used as the stationary phase, methanol as the mobile phase, the size of a column was 100 mm in length and 10 mm in diameter, and the three zones included the independent eluting zone Ⅰ with two columns , the refining zone Ⅱ with one column and the desorbing zone Ⅲ with one column The ideal model based on the linear adsorption isotherm was used to describe the chromatographic behaviors of 4-phenyloxazoli- dine-2-thione enantiomers. SMB chromatographic model established by the combination of the ideal model of the single column and the node model of 2-1-1 mode was used to describe SMB separation process of 4-phenyloxazolidine-2-thione enantiomers. The results of model calculation and experiment showed that under the condition of continuous feeding, it was unable to obtain the two enantiomers with higher purities at same time by adjusting the switching time. When intermittent feeding was done, the obtained purities of the two products were more than 98. 0% simultaneously.

关 键 词：模拟移动床 分离 4-苯基噁唑烷-2-硫酮对映体 色谱模型 

分 类 号：O652.6[理学—分析化学]