三七素手性拆分方法的研究

使用气相色谱法和高效液相色谱法分离了三七素对映体，并探讨了影响液相色谱法分离效果的因素。结果表明，HPLC法利用手性固定相进行直接拆分，无法实现对映体的完全分离；GC法和HPLC的手性试剂衍生化法均可对三七素对映体进行较好的分离。但GC法由于衍生化过程中副产物的存在，干扰了对映体的准确定量。手性试剂衍生化HPLC法，以邻苯二甲醛、N-酰化-L-半胱氨酸为衍生化试剂，反应得到的三七素对映体的衍生物在ODS柱上分离良好，且方法简单、快速。

Enantiomeric Separation of Dencichine

Gas chromatography and high performance liquid chromatography(HPLC) were applied to separate dencichine enantiomers.When a direct HPLC with a chiral Crownpak CR(+) column was employed,the enantiomers of dencichine could not efficiently be resolved.The good resolution of enantiomers was achieved by chiral gas chromatography(GC) or indirect HPLC method using a pre-column chiral reagents derivatization.However,the GC assessment of enantiomeric purity was disturbed by the vice products resulting from the derivatization.For indirect HPLC method,some factors that influenced resolution incluing the kind of chiral(thiols),the pH of mobile phase,the column temperature were studied.The enantiomeric separation of dencichine was accomplished by pre-colunm derivatization with O-phthaldialdehyde(OPA) and chiral thiol-N-(acyl)-L-cysteine derivative to yield diastereoisomeric isoindole derivatives which are separable by common(reversed)-phase ODS column.The indirect HPLC method,which provides the simple,fast and(selective) detection of dencichine enatiomers,is suitable for the study of synthesis and pharmacokinetics of dencichie enantiomers.