高效液相色谱手性固定相法分离R基-3-吡啶基亚砜对映体  

Separation of Racemic R-3-Pyridyl Sulfoxide on Chiral Stationary Phase by High Performance Liquid Chromatography

作　　者：谢昆[1] 李劲[1] 刘有成[1] 陈小春[1] 

机构地区：[1]中国科学技术大学化学系,合肥230026

出　　处：《分析化学》2005年第9期1295-1297,共3页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.20332020);国家教育部高等学校博士学科点专项科研基金(No.200358055);安徽省教育厅重点科研计划(No.2003kj050zd)资助项目

摘　　要：利用正相高效液相色谱法在一种纤维素衍生物手性固定相(OB-H)上成功分离了一系列(7个)的R基-3-吡啶基亚砜的对映异构体。通过考察流动相中异丙醇的含量和温度对手性分离的影响,优化色谱分离条件。随着流动相中异丙醇含量的增加,除了带有支链的化合物Ⅲ外,其他6个化合物对映体的容量因子k′和分离度Rs都会减少。柱温变化对分离度的影响不大。长的碳链和支链都会使溶质与固定相的作用减弱,因此,容量因子k′和分离度Rs也会减小。所有测试结果显示:该固定相对这类化合物有较好的分离效果。最佳分离条件是流动相中含有30%的异丙醇,柱温为25℃。A series of racemic R-3-pyridyl sulfoxides were successfully separated by a cellulose derivative based chiral stationary phase （OB-H） under normal -phase high performance liquid chromatography （HPLC） conditions. Through investigation on the influence of the percentage of iso-propanol in the mobile phase and the column temperature on the resolution, the chromatographic conditions were optimized. As the percentage of iso-propanol in the mobile phase increased, the capacity factors k＇and the resolution factors Rs of the series of racemic sulfoxides all decreased except for compound Ⅲ which had a branched chain. The influence of temperature on resolution was not obvious. As far as the solutes were considered, a long carbon chain or a branched chain both can decrease the interaction of solutes with the stationary phase, so the capacity factors k＇ and the resolution factors Rs of the enantiomers would decrease, too. The results show that this chiral stationary phase exhibits good stereoselectivity to the series of racemic sulfoxide enantiomers. And the best resolution condition is 30% iso-propanol in the mobile phase and the column temperature at 25℃.

关 键 词：高效液相色谱 手性固定相 亚砜 色谱分离 高效液相色谱法 手性分离 对映体 吡啶基 纤维素衍生物 分离条件 

分 类 号：O657.72[理学—分析化学] O657.8[理学—化学]