高效液相色谱手性固定相法直接拆分4种吲哚类衍生物

将纤维素-三(3,5-二甲基苯基氨基甲酸酯)(CDMPC)涂敷于自制的球形氨丙基硅胶上,制备成了纤维素-三(3,5-二甲基苯基氨基甲酸酯)手性固定相(CDMPC-CSP)。利用正相高效液相色谱,在该固定相上对新合成的4种吲哚类衍生物对映体进行了手性拆分。通过选择不同结构和浓度的醇类改性剂,优化了色谱分离条件,同时探讨了醇的结构和浓度对于对映体拆分和保留的影响。结果表明,适合Ⅱ~Ⅳ号样品拆分的醇类改性剂分别为正丁醇、乙醇和乙醇,而适合Ⅰ号样品的醇类改性剂为乙醇和正丙醇组成的混合体系。在优化的各流动相体系下,4种吲哚类衍生物的对映体都得到了很好的分离。在此基础上计算了它们的对映体过量值(e.e.值)。实验结果令人满意,表明高效液相色谱手性固定相法是拆分这类化合物的一种理想方法。

Direct Chiral Separation of Four Indole Derivatives by High Performance Liquid Chromatography with Chiral Stationary Phase

A chiral stationary phase (CSP) was prepared by coating cellulose-tris(3,5-dimethylphenyl carbamate) (CDMPC) onto spherical silica gel. Four newly synthesized chiral indole derivatives were directly resolved on the CDMPC-CSP by a normal-phase system. The influences of structure and proportion of the alcohol in mobile phases on the separation by high-performance liquid chromatography with chiral stationary phase (HPLC) were investigated to optimize the chromatographic conditions. N-butano1, ethanol and ethanol were suitable for the separation of sample I, III, and IV as the modifiers, respectively, whereas the mixture of ethanol and n-propanol was suitable for sample I. Under the optimal conditions, excellent enantioseparation was achieved and the enantiomer excess values of all the four samples were determined. The satisfactory results indicated that the method of HPLC is ideal for the separation of indole derivatives.