色谱

色谱 ›› 2016, Vol. 34 ›› Issue (8): 739-744.DOI: 10.3724/SP.J.1123.2016.04026

• 研究论文 • 上一篇    下一篇

键合型邻乙酰水杨酸纤维素酯手性固定相的合成及应用

李杨1, 封华2, 蒋登高3   

  1. 1. 河南省食品药品检验所, 河南 郑州 450003;
    2. 郑州市妇幼保健院, 河南 郑州 450003;
    3. 郑州大学化工与能源学院, 河南 郑州 450001
  • 收稿日期:2016-04-15 出版日期:2016-08-08 发布日期:2016-07-26
  • 通讯作者: 李杨

Preparation and application of covalently bonded cellulose acetylsalicylate chiral stationary phases

LI Yang1, FENG Hua2, JIANG Denggao3   

  1. 1. Henan Institute for Food and Drug Control, Zhengzhou 450003, China;
    2. Women and Infants Hospital of Zhengzhou, Zhengzhou 450003, China;
    3. School of Chemical Engineering and Energy, Zhengzhou University, Zhengzhou 450001, China
  • Received:2016-04-15 Online:2016-08-08 Published:2016-07-26

PDF

96

被引次数

1

摘要：

将邻乙酰水杨酸纤维素酯通过间隔臂——2-（3，4-环氧环己基）乙基三甲氧基硅烷键合于硅胶之上，制得键合型手性固定相CSP1，考察了其与同类纤维素衍生物制得的涂敷型手性固定相在拆分效果方面的异同，并探讨了其差异的原因与机理。为了印证间隔臂中环己基对于手性拆分的作用，本文又将CSP1与间隔臂中不具有环己基的键合型手性固定相CSP2进行了拆分对比，进一步证实了间隔臂中环己基的作用。结果表明，键合型手性固定相相比涂敷型固定相在拆分咪唑类药物方面具有优势，这种优势一方面来自于流动相范围的扩大，另一方面是由于间隔臂中环己基对纤维素表面结构的修饰作用。

关键词: 间隔臂, 键合, 邻乙酰水杨酸纤维素酯, 手性固定相

Abstract:

The chemical bonded cellulose acetylsalicylate chiral stationary phase (CSP1) was obtained by fixing cellulose derivative on silica gel with beta-(3, 4-epoxycyclohexyl) ethyl trimethoxy silane as space arm. The resolution mechanism and feasibility of CSP1 were studied by comparing CSP1 with coated chiral stationary phase prepared by cellulose acetylsalicylate. The role of cyclohexyl group in the space arm was also verified by comparing CSP1 with CSP2 which had no cyclohexyl group in the space arm. Based on the chromatographic results, the immobilized chiral stationary phase exhibited better chiral resolving abilities than coated stationary phase for imidazoles. It is due to, on the one hand, more types of mobile phases used, on the other hand, the modified cellulose by cyclohexyl group.

Key words: bond, cellulose acetylsalicylate, chiral stationary phase, space arm

中图分类号: