纤维素-三(4-甲基苯甲酸酯)手性固定相的制备及其在拆分叔丁基亚磺酰胺对映体中的应用  

Preparation of cellulose-tris-( 4-methylbenzoate) chiral stationary phase and its application in the resolution of enantiomers of 2-methylpropane-2-sulfinamide

作　　者：师香韵 高典楠[1] 苏宏久[1] 王树东[1] SHI Xiangyun;GAO Diannan;SU Hongjiu;WANG Shudong(Dalian National Laboratory for Clean Energy,Dalian Institute of Chemical Physics,Dalian 116023;University of Chinese Academy of Sciences,Beijing 100049)

机构地区：[1]中国科学院大连化学物理研究所洁净能源国家实验室,大连116023 [2]中国科学院大学,北京100049

出　　处：《分析试验室》2021年第5期547-551,共5页Chinese Journal of Analysis Laboratory

基　　金：中国科学院青年促进会项目(Y206060901)资助。

摘　　要：分别在自制的纤维素-三(3,5-二甲基苯基氨基甲酸酯)(CDMPC)和纤维素-三(4-甲基苯甲酸酯)(CTMB)涂覆型固定相上对叔丁基亚磺酰胺对映体进行手性拆分,并考察了流动相中异丙醇的含量对手性拆分的影响。结果表明,叔丁基亚磺酰胺在CTMB固定相上的分离效果更佳。随着异丙醇含量的减少,叔丁基亚磺酰胺对映体在两根色谱柱上的分离度和保留时间均随之增加。对CTMB固定相进一步探究柱温的影响,结果表明较低的温度有利于对映体保持稳定的手性构型,更易于与固定相反应。2-methylpropane-2-sulfinamide was used as a test compound to investigate the cellulose-tris( 3,5-dimethylphenylcarbamate)( CDMPC) and cellulose-tris( 4-methylbenzoate) coated stationary phase,respectively. The effect of the content of isopropanol in the mobile phase on the chiral resolution was also investigated. The results showed that the separation of 2-methylpropane-2-sulfinamide on CTMB stationary phase was better. With decrease of the isopropanol content in the mobile phase,the resolution and retention time of the2-methylpropane-2-sulfinamide enantiomer on the two columns both increased accordingly. The effect of column temperature was further investigated on the CTMB coated stationary phase. The results showed that a lower temperature was favorable for the enantiomer to maintain a stable chiral configuration and made it easier to react with the stationary phase.

关 键 词：手性分离 高效液相色谱(HPLC) 纤维素-三(4-甲基苯甲酸酯) 叔丁基亚磺酰胺 

分 类 号：O657.3[理学—分析化学] X832[理学—化学]