环糊精聚合物键合手性固定相的合成及手性拆分应用

Synthesis of Cyclodextrin Polymer Bonded Chiral Stationary Phase and Its Application in High Performanc Liquid Chromatography for Enantioseparation

摘要:

手性固定相是液相色谱手性分离的基础与核心。本文用简单缩聚法合成环糊精聚合物(CDP)，并将这种CDP键合到自制二氧化硅微球上，合成了新型的环糊精聚合物键合型手性固定相（CSP）。在合成过程中考察了反应时间，原料比例及原料加入次序对所制CSP的影响。随后，用扫描电镜法检验了所制填料圆整度，用四氮唑蓝法检测环糊精的含量为42.4 μmol/g，其环糊精键合量明显高于CD单体键合硅胶。最后将最优条件下得到的手性填料用高压匀浆法装柱，并进行液相色谱法拆分手性药物。用二者与ODS在相同的色谱条件下进行对比，结果表明：环糊精聚合物键合硅胶手性固定相对所选手性药物拆分能力更强。

Abstract:

Chiral stationary phase was the foundation and core of liquid chromatography. In this paper, cyclodextrin polymer (CDP) was synthesized through a simple condensation, and then bonded onto homemade silica microspheres to develop a novel chiral stationary phase. The reaction time, material ratio and reaction pathways were investigated in the process of the synthesis. And then scanning electron microscopy (SEM) was utilized to characterize its ball roundness. Blue tetrazolium method was applied to detect the content of the cyclodextrin. The result was 42.4 μmol/g, which is markedly higher than CD bonded silica gel. Finally, the product was packed with high pressure slurry method, and the chiral column was tested by liquid chromatography to separate chiral drugs. Meanwhile, the above β-CD and β-CDP were compared with ODS to resolve chiral drugs under the same chromatographic conditions. The result demonstrated that better separation was obtained by β-CDP bonded silica gel.