化学学报 ›› 2000, Vol. 58 ›› Issue (11): 1424-1428. 上一篇    下一篇

研究论文

联苯类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

刘月启;刘霞;蒋生祥;陈立仁;常俊标   

  1. 中国科学院兰州化学物理研究所.兰州(730000);河南省化学工业研究所.郑州( )
  • 出版日期:2000-11-15 发布日期:2000-11-15

Direct optical resolution of the enantiomers of biphenyl compounds by high-performance liquid chromatography on cellulose tris-(3,5- dimethylphenylcarbamate) stationary phase

Liu Yueqi;Liu Xia;Jiang Shengxiang;Chen Liren;Chang Junbiao   

  1. Lanzhou Inst Chem Phys, CAS.Lanzhou(730000);Henan Inst of Chem Ind. Zhengzhou
  • Online:2000-11-15 Published:2000-11-15

涂敷纤维素-三(3,5-二甲基苯基氨基甲酸酯)于自制的球形氨丙基硅胶上,制备了手性固定相。用该固定相直接拆分了一系列外消旋联苯类保肝药物。考察了柱温和流动相中乙醇含量对样品的保留和立体选择性的影响,升高柱温或增大流动相中乙醇含量都会使对映体的保留因子和分离因子降低。氨考察榈的分离因子的对数与温度的倒数成线性关系。确定了对映体从流动相传递到固定相的吉布斯自由能变之差值、焓变之差值及熵变之差值。

关键词: 联苯P, 纤维素, 固定相, 高速液体色谱, 手性拆分

A chiral 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 compounds with antihepatitis activity was achieved for the first time on the CSP, using the normalphase mode. The effects of temperature and concentration of ethanol in the mobile phase on the chiral separation were studied. the retention factors and separation factors for the enantiomers of all investigated compounds decreased with increasing temperature or increasing ethanol concentration in the eluent. The natural logarithms of the separation factors (lnα) of the investigated compounds depended linearly on the reciprocal of temperature (1/T). The thermodynamic parameters, such as the difference in enthalpy △(△H°), entropy △(△S°) and Gibbs free energy △(△G°) for the transfer of analyte from the mobile phase to the CSP were calculated.

Key words: DIPHENYL P, CELLULOSE, STATIONARY PHASE, HIGH SPEED LIQUID CHROMATOGRAPHY

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