几种手性醇在纤维素键合的SBA-15基手性固定相上的直接拆分

在强酸性条件下, 以三嵌段聚醚P123为模板, 合成了孔径大且粒径均匀的SBA-15介孔二氧化硅微球. 将含有少量三乙氧硅丙基氨基甲酸酯残基的纤维素-三(3,5-二甲基苯基氨基甲酸酯)通过分子间缩聚作用固载到氨丙基化的SBA-15微球上, 制得手性固定相; 采用常规和非常规的流动相模式, 对一些芳香醇的消旋体进行了手性拆分. 实验结果表明, 所制备的SBA-15微球不仅分散性良好, 具有规则的二维六方孔道结构, 而且消除了微孔; 所制备的键合手性固定相不仅固载手性选择剂的量大, 而且经六甲基二硅胺烷封端后可有效改善拖尾现象, 对实验选用的手性醇具有较高的拆分能力; 与大孔硅胶为基质的同类纤维素键合手性固定相相比, 该固定相对同种手性消旋体的分离因子明显提高.

Enantioseparation of Chiral Alcohols on Acellulose Derivative Immobilized onto Spherical Mesoporous SBA-15 by High Performance Liquid Chromatography

Ordered mesoporous SBA-15 silica spheres were synthesized using the triblock copolymer,Pluronic P123,as the template with the assistance of KCl and 1,3,5-trimethylbenzene in the acidic condition.The obtained SBA-15 silica spheres with the particle size of 4.5 μm,pore size of 22.8 nm,surface area of 546.99 m2/g,and pore volume of 1.747 m3/g were used as the support in high-performance liquid chromatography(HPLC).The 3,5-dimethylphenylcarbamates of cellulose bearing about 3% of 3-(triethoxysilyl)propyl residues was immobilized onto SBA-15 particles by intermolecular polycondensation of the triethoxysilyl groups as the chiral stationary phase(CSP).The CSP was evaluated by HPLC for ten chiral alcohols with the eluents containing chloroform and tetrahydrofuran,which cannot be used with the conventional coated-type CSPs.Using the eluents,this CSP showed higher chiral recognition abilities to compare with that CSP based the same cellulose derivative bonded onto silica gel.The results indicated that the mesoporous SBA-15 spheres could be used as a good candidate for HPLC packings.