高速逆流色谱分离同分异构体 陈理.docxVIP

高速逆流色谱分离同分异构体 陈理 高速逆流色谱分离同分异构体lowbar;陈理 2021年11月November 2021 Chinese Journal of Chromatography Vo l. 24No. 6 570~573 高速逆流色谱分离同分异构体 陈 理1, 邓丽杰2, 陈 平2 (1. 杭州市药品检验所, 浙江杭州310014; 2. 浙江大学化学系, 浙江杭州310028) 摘要:应用高速逆流色谱法对同分异构体的分离纯化进行研究。实验结果表明, 以正己烷-乙酸乙酯-水(体积比为1 10 10) 为两相溶剂系统, 上相为固定相, 下相为流动相, 进行二次高速逆流色谱分离, 可从茶多酚中分离出g 级的儿茶素同分异构体 (-)-表没食子儿茶素没食子酸酯(EG CG) 和(-)-没食子儿茶素没食子酸酯(GCG) , 其高效液相色谱纯度均在98%以上。选择四氯化碳-氯仿-甲醇-水(体积比为7 3 7 3) 为溶剂系统, 下相为固定相, 上相为流动相, 经一次高速逆流色谱即可将药物中间体溴代苯胺同分异构体进行有效的分离。 关键词:高速逆流色谱法; 同分异构体; 儿茶素; 溴代苯胺; 分离中图分类号:O 658 文献标识码:A 文章编号:1000-8713(2021) 06-0570-04 栏目类别:研究论文 Separation of Isomeric Compounds by High Speed Countercurrent Chromatography CH EN Li , DENG Lijie , CH EN Ping (1. Institute for Drug Control of Hangzhou, Hangzhou 310014, China; 2. Department of Chemistr y, Zhejiang U niversity, Hang zhou 310028, China) Abstract :H ig h speed countercur rent chromatog raphy (H SCCC ) w as successfully used fo r the separation and preparatio n of isomeric co mpo unds. The influence of various tw o -phase solv ent system s o n the r esolutio n of the natural catechin isomers o f (-)-epigallocatechin gallate (EGCG) and (-)-g allocatechin g allate (GCG) fro m gr een tea polyphenols and the sy nthetic isomeric com -pounds of p ar a -, ortho -, meta -bro moanilline w as investig ated. The results indicated that the cat -echin isomers of (-)-EGCG and (-)-GCG can be isolated through tw o r uns o f preparative H SC -CC w ith tw o -phase so lvent system co mposed of n -hex ane -ethyl acetate -w ater (1 10 10in volume ratio) . T he upper org anic phase was used as stationar y phase and the low er aqueo us phase as mo -bile phase, w hile the m obile phase w as operated at a flow rate o f 3 5m L/min, and the apparatus rotated at 800r/min. H igh perform ance liquid chr omatogr aphic analysis of (-) -EGCG and (-)-GCG r evealed that the purity w as all over 98%. T he isomeric com pounds of p ara -, or tho -, meta -bro moaniline can