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合成了均苯四甲酸酐修饰β-环糊精微球,通过红外光谱、X-射线光电子能谱、扫描电镜对其进行结构和形貌表征,获得了大小均匀、表面光滑、粒径为5~10μm的微球。以该微球为手性固定相,采用溶胶-凝胶法制备了颗粒固定化整体柱,并考察了柱制备过程中的影响因素,获得最佳的柱制备条件:聚乙二醇∶冰乙酸∶正硅酸甲酯为0.25 g∶2.5 m L∶1.5 m L,溶胶∶微球为2 m L∶1 g,水浴时间10 h,水浴温度40℃。利用该颗粒固定化整体柱对盐酸异丙肾上腺素和盐酸氯丙那林对映体进行手性拆分,达到了基线分离。
The pyromellitic dianhydride-modified β-cyclodextrin microspheres were synthesized and characterized by IR, XPS and SEM. The structure of the microspheres was characterized by uniform size, smooth surface and particle size of 5 ~ 10μm microspheres. With the microspheres as the chiral stationary phase, the immobilized monolithic columns were prepared by sol-gel method and the influencing factors in the preparation of the column were investigated. The optimum conditions for the preparation of the column were obtained: polyethylene glycol: glacial acetic acid : Methyl orthosilicate 0.25 g: 2.5 m L: 1.5 m L, sol: microspheres 2 m L: 1 g, water bath time 10 h, water bath temperature 40 ℃. The enantiomers of isoproterenol hydrochloride and promethazine hydrochloride were chirally resolved by the immobilized monolithic column and the baseline was separated.