衍生化高效液相色谱法拆分1,1′-联萘-2,2′-二酚光学异构体  

Separation of 1,1'-Binaphthalene-2,2'-diol Optical Isomers by Derivatization High Performance Liquid Chromatography

作　　者：阮源萍[1] 敖小平 陈安齐[2] 黄培强[2] 

机构地区：[1]厦门大学现代分析科学教育部重点实验室,厦门361005 [2]厦门大学化学系,厦门361005

出　　处：《分析化学》2001年第12期1398-1401,共4页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金重点资助项目 (No .2 983 2 0 2 0 )

摘　　要：以基碳酸酰氯作衍生化试剂 ,采用高效液相色谱拆分 1,1′ 联萘 2 ,2′ 二酚光学异构体。当采用LichrosorbSi 6 0 (4mm× 30 0mm ,5 μm)柱 ,紫外 2 75nm检测 ,正己烷 乙醇 (98.5 1.5 ,V V)为流动相 ,1,1′ 联萘 2 ,2′ 二酚单基碳酸酯的分离因子和分离度分别为 1.36 8、3.0 5 1;用正己烷 乙醚 (98.5 1.5 ,V V)为流动相 ,1,1′ 联萘 2 ,2′ 二酚双基碳酸酯的分离因子和分离度分别为 1.0 5 5、1.347。这一方法可简便。Binaphthalene 2,2′ diol mono [( ) menthyl] carbonate (3) and 1,1′ binaphthalene 2,2′ diol bis [( ) menthyl] carbonate (4) are intermediates in the chemical resolution of racemic 1,1′ binaphthalene 2,2′ diols (1) utilizing ( ) (1R) menthyl chloroformate (2) as the derivating agent. In this paper, the optical separation of compound (3) and (4) has been investigated by high performance liquid chromatography on Lichrosorb Si 60(4 mm i.d.×300 mm, 5 μm)and YWG CN(4 mm i.d.×250 mm, 10 μm)column with hexane polar regulator mixture as an eluent. The results show that the optical isomers of compound (3) and (4) can be well separated. The optical isomers first eluted are (S, 1R′) 3 and (S, 1R′, 1R″) 4 respectively. The influence of polar solvents and their ratios in the mobile phase on the resolution is examined. This method has been applied to determine the optical purity of 1,1′ binaphthalene 2,2′ diol mono [( ) menthyl] carbonate obtained from a novel resolution process.

关 键 词：高效液相色谱 衍生化 1 1'-联萘-2 2’-二酚 联萘二酚单Mong基碳酸酯 联萘二酚双Mong基碳酸酯 光学异构体 拆分 

分 类 号：O657.7[理学—分析化学]