色谱

色谱

• 技术与应用 • 上一篇    

高效液相色谱使用两种类型的纤维素-三(对甲基苯甲酸酯)固定相手性拆分非洛地平的比较

徐丽芳1, 鲁耀1, 李奕2, 许旭1,2*   

  1. 1. 上海应用技术学院化学与环境工程学院, 上海 200235; 2. 中国科学院上海有机化学研究所, 上海 200032
  • 收稿日期:2009-10-09 修回日期:2009-12-09 出版日期:2010-04-28 发布日期:1980-12-25
  • 通讯作者: 许旭

Comparison of chiral separations of felodipine by high performance liquid chromatography using two cellulose tris(4-methyl benzoate) stationary phases

XU Lifang1, LU Yao1, LI Yi2, XU Xu1,2*   

  1. 1. School of Chemical and Environmental Engineering, Shanghai Institute of Technology, Shanghai 200235, China; 2. Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai 200032, China
  • Received:2009-10-09 Revised:2009-12-09 Online:2010-04-28 Published:1980-12-25
  • Contact: XU Xu

PDF

590

被引次数

25

摘要： 以高效液相色谱手性固定相法对非洛地平(FEL)进行手性拆分。分别采用两种类型的纤维素-三(对甲基苯甲酸酯)手性柱Chiralcel OJ-R和Chiralcel OJ-H进行比较实验,以正己烷-异丙醇(90:10, v/v)为流动相,考察了流动相、柱温对保留及手性拆分的影响。实验显示,两柱拆分FEL的van’t Hoff图均发生了转折,在高温区域为焓驱动,在低温区域为熵驱动。两柱在温度升高时拆分FEL的分离度均提高,其中OJ-H的分离度优于OJ-R。两种手性柱对FEL具有相似的拆分机理。

关键词: 非洛地平 , 高效液相色谱, 手性拆分, 手性固定相

Abstract: Chiral resolutions of felodipine (FEL) were compared using two cellulose tris(4-methyl benzoate) stationary phases, Chiralcel OJ-R and Chiralcel OJ-H. The effects of the mobile phase and the column temperature on the retention and separation were compared. Using n-hexane/2-propanol (90:10, v/v) as mobile phase, the FEL can be enantioseparated. There are transition temperatures in the van’t Hoff plots of the two columns. In the higher temperature region the enantioseparation was enthalpy controlled, and in the lower temperature region it was entropy controlled. The higher temperature was good for the resolution of FEL enantiomers even though the selectivity was change with maximum value at 19 ℃ for OJ-R and 14 ℃ for OJ-H. The two columns showed similar mechanism in the FEL chiral separation.

Key words: chiral separation, chiral stationary phase, felodipine , high performance liquid chromatography (HPLC)