巴拉苏酰胺对映体的色谱分离研究  

The study of chiral recognition mechanism of balasubramide by HPLC

作　　者：方成乔 罗旭娜 苏金龙 饶雨 何冠涛 林汉森 FANG Chengqiao;LUO Xuna;SU Jinlong;RAO Yu;HE Guantao;LIN Hansen(College of Pharmacy,Guangdong Pharmaceutical University,Guangzhou 510006)

机构地区：[1]广东药科大学药学院

出　　处：《分析试验室》2020年第1期67-70,共4页Chinese Journal of Analysis Laboratory

基　　金：广东省科技厅项目(2015A020211031,2016A020217022)资助

摘　　要：利用手性HPLC法对天然产物(+)-巴拉苏酰胺(balasubramide)及其对映体进行分离和光学纯度测定。在手性分离过程中,考察了两种不同的手性固定相和不同比例的流动相(正己烷和异丙醇),以进行手性分离方法的优化。结果表明:正己烷和异丙醇(70/30,V/V)在手性柱Chiralpak AD-H上获得最佳分离。光学活性的巴拉苏酰胺的对映体过量值高于98%,其分离因子(α)和分离度为2.15和21.80。本研究为光学活性的巴拉苏酰胺及其后续衍生物光学纯度控制提供了方法学基础。Chiral HPLC was used to separate and determine the natural product balasubramide and its enantiomers.During chiral separation process,different chromatographic conditions were investigated to obtain the best separation method.Optimization of chiral separation was conducted in two different chiral stationary phases(CSPs)and different ratio of mobile phases(n-hexane and iso-propanol).Under different conditions,the best chiral recognition and resolution were obtained in the organic mode with n-hexane and iso-propanol(IPA)(70/30,V/V)on Chiralpak AD-H column.Moreover,the enantiomeric excess(ee)values of the optically active balasubramide were higher than 98%.Enantio selectivity and resolution(αand Rs,respectively)levels were with values 2.15 and 21.80,respectively.The present chiral HPLC method will provide a preliminary resolution for the optical purity control of optically active balasubramide and its derivatives.

关 键 词：手性柱 巴拉苏酰胺(balasubramide) 对映体分离 对映体过量 

分 类 号：R914[医药卫生—药物化学]