TpBD(NH_(2))_(2)的L-羟基脯氨酸衍生物制备及其用作固定相  

Preparation of L-hydroxyproline derivative of TpBD(NH_(2))_(2) and its use as stationary phase

作　　者：罗占丽 熊婉淇 段爱红[1] 袁黎明[1] LUO Zhanli;XIONG Wanqi;DUAN Aihong;YUAN Liming(School of Chemistry and Chemical Engineering,Yunnan Normal University,Kunming 650500,China)

机构地区：[1]云南师范大学化学化工学院,昆明650500

出　　处：《分析试验室》2022年第6期621-627,共7页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金项目(918526123)资助。

摘　　要：以3,5-三甲醛间苯三酚(Tp)和3,3′-二硝基联苯胺(DNB)为单体,L-羟基脯氨酸为手性源,采用溶剂热法合成了TpBD(NH_(2))_(2)的L-羟基脯氨酸衍生物,利用网包法制备了TpBD(NH_(2))_(2)的L-羟基脯氨酸衍生物手性柱并用于高效液相色谱固定相。在2种不同的流动相下,对多种外消旋化合物进行了分离实验。共分离11种外消旋体,在正己烷-异丙醇流动相下分离了2种外消旋化合物,分离效果最好的1-(9-蒽基)-2,2,2-三氟乙醇的分离度达到了7.16;在甲醇-水流动相下分离了9种外消旋化合物;色谱重现性良好。TpBD(NH_(2))_(2)的L-羟基脯氨酸衍生物材料在手性分离方面具有良好的分离效果。A chiral covalent organic framework material,L-hydroxyproline derivative of TpBD(NH_(2))_(2),was used as a stationary phase for high performance liquid chromatography,which was synthesized with 1,3,5-triformylphloroglucinol(Tp)and 3,3′-dinitrobenzidine(DNB)as monomers and L-hydroxyproline as the chiral source by solvothermal method.And the HPLC stationary phase was prepared by the net wrapping method.The separation experiments of a variety of racemic compounds on the chiral column of L-hydroxyproline derivative of TpBD(NH_(2))_(2) were carried out under two different mobile phases.The results showed that two racemic compounds were separated under n-hexane/isopropanol mobile phase,and nine racemates were separated with alcohol/water as mobile phase,in which the best separation example was 1-(9-anthracyl)-2,2,2-trifluoroethanol and the Rs value was up to 7.16.This chiral column has good chromatographic reproducibility.The L-hydroxyproline derivative material of TpBD(NH_(2))_(2) has a good enantio separation characteristic in the field of chiral separation.

关 键 词：手性共价有机骨架 L-羟基脯氨酸 高效液相色谱 手性分离 

分 类 号：O652.6[理学—分析化学] O657.7[理学—化学]