TpPa-NH2的(1s)-(+)-10-樟脑磺酰氯衍生物毛细管电色谱手性柱的研究

Capillary Electrochromatographic Chiral Column of TpPa-NH;(1s)-(+)-10-Camphorsulfonyl Chloride Derivative

本文采用溶剂热法,以2-硝基-1,4-苯二胺(Pa-NO_(2))和1,3,5-三甲基间苯三酚(Tp)合成一种非手性的共价有机骨架,将其还原后再用(1s)-(+)-10-樟脑磺酰氯修饰成具有手性的多孔有机材料。采用X射线衍射、红外光谱、圆二色谱、热重分析、氮吸附-脱附和扫描电镜对该材料进行表征。结果表明,经衍生后的手性材料有较好的空间结构和热稳定性。由该材料制成的手性毛细管电色谱柱成功拆分了乙酸仲丁酯及2-碘丁烷两种手性化合物。通过对分离电压、缓冲溶液的浓度和pH值等因素的考察,得到了乙酸仲丁酯及2-碘丁烷的最佳分离条件。以乙酸仲丁酯为分析物对该柱性能进行评价,表明该柱具有良好的稳定性和重现性,且对手性药物具有一定的拆分能力,可用作毛细管电色谱固定相。

A non-chiral covalent organic framework was synthesized by solvothermal method with 2-nitro-1,4-phenylenediamine(Pa-NO_(2)) and 1,3,5-trimethylphloroglucinol(Tp).The organic framework was reduced and then modified with(1 s)-(+)-10-camphorsulfonyl chloride to form a chiral porous organic material.The material was characterized by X-ray diffraction, infrared spectroscopy, circular dichroism, thermogravimetric analysis, nitrogen adsorption-desorption and scanning electron microscopy.The results showed that the derivatized chiral materials had good spatial structure and thermal stability.The chiral capillary electrochromatographic column made by this material successfully resolved two chiral compounds, sec-butyl acetate and 2-iodobutane.By investigating factors such as separation voltage, buffer solution concentration and pH value, the optimal separation conditions for sec-butyl acetate and 2-iodobutane were obtained.The column has good stability, reproducibility, and chiral resolution ability, and can be used as a capillary electrochromatographic stationary phase.