发展了一种制备β-环糊精／硅基杂化手性固定相的简单方法。首先合成了β-环糊精硅基衍生物，然后在碱性条件下通过硅烷化试剂和β-环糊精硅基衍生物之间的聚合反应，制备了β-环糊精衍生物共价负载于孔道表面的球形β-环糊精／硅基杂化材料，去除模板剂，即可得到直接用于高效液相色谱填料的β-环糊精／硅基杂化手性固定相。制备的杂化固定相材料具有球形规则、单分散性好、比表面积高、机械性能好、化学稳定性高和制备过程简单等特点，结合了β-环糊精的手性识别功能与有机-无机杂化材料的优异性能。在反相色谱条件下的手性拆分结果表明杂化手性固定相具有较高的手性识别能力。本文所发展的方法为新型手性固定相的制备提供了一种新的思路。
A simple preparation method for β-cyclodextrin-silica hybrid chiral stationary phases was developed. Firstly,the β-cyclodextrin-silica derivative was synthesized by the reaction of 3-aminopropyltriethoxysilane and monochlorotriazinyl β-cyclodextrin under weak base condi-tion. Spherical β-cyclodextrin-silica hybrid materials with β-cyclodextrin in the surface of pores by covalent bonding were prepared using 1,2-bis( triethoxysilyl)ethane and the β-cyclodextrin-silica derivative under the alkaline condition by one-step polymerization reaction. The β-Cyclo-dextrin-silica hybrid chiral stationary phases could be directly used as high performance liquid chromatographic packings after the template removal. The hybrid materials prepared in this paper possessed regular spherical morphology,good monodispersion,high specific surface area,good mechanical property,high chemical stability and simple preparation process. It combined the chiral recognition performance of β-cyclodextrin and the outstanding performance of organic-inorganic hybrid material. The effect of the composition,ratio and pH of mobile phase on chiral separation was investigated,and the best chiral separation conditions had been optimized. The baseline chiral separations for five chiral compounds were obtained under the optimal conditions. The results of enantioseparation showed that the hybrid chiral stationary
phases had favorable chiral recognition ability. Compared with the traditional preparation process of chiral stationary phases,a new thought for new type of chiral stationary phase is provided by the present method in this paper.
参考文献
| [1] | Wang, Y.;Chen, H.;Xiao, Y.;Ng, C.H.;Oh, T.S.;Tan, T.T.Y.;Ng, S.C..Preparation of cyclodextrin chiral stationary phases by organic soluble catalytic 'click' chemistry[J].Nature protocols erecipes for researchers,20117(7):935-942. |
| [2] | Lin, C.;Liu, W.;Fan, J.;Wang, Y.;Zheng, S.;Lin, R.;Zhang, H.;Zhang, W..Synthesis of a novel cyclodextrin-derived chiral stationary phase with multiple urea linkages and enantioseparation toward chiral osmabenzene complex[J].Journal of chromatography, A: Including electrophoresis and other separation methods,2013:68-74. |
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