高等学校化学学报

高等学校化学学报 ›› 2000, Vol. 21 ›› Issue (12): 1828.

• 论文 • 上一篇    下一篇

〆,β-联苯双酯对映体在纤维素类手性固定相上的高效液相色谱法直接拆分——流动相改性剂对保留时间和立体选择性的影响

刘月启1, 葛永辉1, 蔡青松1, 蒋生祥1, 陈立仁1, 常俊标2   

  1. 1. 中国科学院兰州化学物理研究所, 兰州 730000;
    2. 河南省化学研究所, 郑州 450003
  • 收稿日期:1999-11-11 出版日期:2000-12-24 发布日期:2000-12-24
  • 通讯作者: 陈立仁(1937年出生),男,研究员,主要从事高效液相色谱研究.
  • 基金资助:

    中国科学院重点基金(批准号:KY95-S1-205)资助

Directly Resolution of Enantiomeric 〆,β-Biphenyl Dialkyl Dicarboxylates by HPLC on a Cellulose-Based Chiral Stationary Phase --Mobile Phase Modifier Effects on Retention and Stereoselectivity

LIU Yue-Qi1, GE Yong-Hui1, CAI Qing-Song1, JIANG Sheng-Xiang1, CHEN Li-Ren1   

  1. 1. Lanzhou Institute of Chemical Physics, the Chinese Academy of Sciences, Lanzhou 730000, China;
    2. Institute of Chemistry of Henan Province, Zheng zhou 450003, China
  • Received:1999-11-11 Online:2000-12-24 Published:2000-12-24

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摘要： 涂敷纤维素-三(3,5-二甲基苯基氨基甲酸酯)(CDMPC)于自制的球形氨丙基硅胶上,制备了手性固定相.用该固定相首次直接拆分了一系列外消旋联苯双酯类保肝药物.考察了伯醇(甲醇/乙醇、乙醇、正丙醇、正丁醇和正戊醇)和仲醇(2-丙醇、2-丁醇和2-戊醇)及叔丁醇等流动相改性剂对保留时间和立体选择性的影响.结果表明,流动相中不同醇对各样品的保留时间和立体选择性有不同程度的影响,理想的手性拆分可通过改变流动相中醇类改性剂来实现

关键词: 手性拆分, 醇类改性剂, 纤维素类手性固定相, 联苯双酯

Abstract: Achiral stationary phase(CSP) was prepared by coating cellulose tris(3,5-dimethylphenylcarbamate) onto aminopropylated spherical silica gel.The enantioselective separation of a series of biphenyl dialkyl dicarboxylates(DDBs) with antihepatitis activity was chromatographed for the first time on the CSpOf the six DDBs investigated, five could be directly resolved via normal phase mode HPLC.The effect of alcohol modifiers in mobile phase was investigated.The mobile phases used in the study were composed of hexane modified with two homologous series of alcohols: methanol ethanol mixtures(1:1, molar ratio), ethanol, 1-propanol, 1-butanol, 1-pentanol and 2-propanol,2-butanol,2-pentanol, and tert butanol.It was found that the retention time and the separation factors of DDBs on the CSPwere dramatically influenced by the kinds of alcohols in mobile phase.The results of the study indicate that alcohol in the mobile phase not only competes for chiral bondings sites with chiral solutes but can also alter the steric environment of the chiral cavities on the CSPby binding to achiral sites at or near the chiral cavity.The purpose of this paper is to demonstrate that better chiral resolution can be obtained via a change of alcohol modifiers in mobile phase

Key words: Enantiomer separation, Alcoholic modifier, Cellulose based CSP, Biphenyl dialkyl dicarboxylates

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