巴拉苏酰胺对映体的色谱分离研究

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。

The study of chiral recognition mechanism of balasubramide by HPLC

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.