表层二氧化锆/硅基－CDMPC手性固定相的制备及联苯双酯类保肝药的直接拆分

用分子自组装的方法制备了表层纳米氧化锆包覆多孔微米硅球，得到的氧化锆 /硅胶微球用作高效液相色谱担体，本方法制备的担体具有氧化锆的表面特性并保 持了硅胶的颗粒均匀、表面积大、渗透性好的优点，可以制备大涂敷量的手性固定 相，以增加固定相的手性识别能力，以涂敷量为20%的纤维素－三（3，5-二甲基苯 基氨基甲酸酯）－氧化锆/硅胶手性固定相（CDMPC-coated ZrO_2/SiO_2）上，对 联苯双酯类保肝药物进行直接拆分，考察了流动相极性、第二种极性改性剂对样品 保留和拆分的影响；并对手性拆分机理进行了阐述，结果表明：CDMPC- ZrO_2/SiO_2手性固定相比CDMPC-ZrO_2具有更好的手性拆分能力。

Preparation of Derivatized Cellulose Coated ZrO_2/SiO_2 and Direct Chiral Resolution of a-Biphenyl Dicarboxylate Compounds by HPLC

A novel HPLC support material was prepared by the Layer-by-Layer (LbL) self-assembly technique. Fabrication of multilayers of nanometer- scale zirconia particles on 5μm silica spheres via sequential electrostatic adsorption of surfactant and zirconia sol from dilute aqueous solution was described. The support prepared by this method is of larger surface area, lower density, better permeability, less background pressure for chiral separation. The larger specific surface area of the material permits higher level amount of chiral polymer coated on the support, increasing the enantioselectivity and chiral resolution for desired separation. Direct optical resolutions of a- biphenyl dicarboxylate compounds on the phase of 20% (w/w) cellulose tris(3,5-dimethylphenylcarbamate) (CDMPC) coated zirconia/silica were obtained under normal mode by HPLC. Influence of solvent polarity and the second polar modifier in mobile phase on chromatographic behavior and chiral separation of the analytes was investigated. The chiral recognition mechanism of the chiral stationary phase was discussed. Better enantioseparation for a-biphenyl dicarboxylate compounds was achieved on CDMPC-ZrO_2/SiQ_2 phase than on CDMPC-ZrO2 phase.