新人参皂苷元HPD相关物质的分离鉴定研究

Study on isolation and identification of related substances of new sapogenin hydroxylation panoxadiol

目的分离纯化新人参皂苷元羟基人参二醇(hydroxylation panoxadiol,HPD)的主要相关物质,并进行结构确证。方法利用反复硅胶柱层析和重结晶方法对HPD合成过程中所产生的相关物质进行分离纯化,得到4个化合物,经理化性质及波谱学方法(LC-MS、~1H-NMR、^(13)C-NMR)鉴定其结构。结果新人参皂苷元HPD中4个相关物质分别是(20S,24R)-达玛-20,24-环氧-3β,6α,12β,25-四醇、(20S,24S)-达玛-20,24-环氧-3β,12β,25-三醇、(20S,25R)-达玛-20,25-环氧-3β,12β,26-三醇和达玛-24-烯-3β,12β,20S-三醇。结论新人参皂苷元HPD相关物质的定量和定性研究可以为HPD原料药的质量控制提供依据。

Objective To separate and purify the main related substances of new sapogenin hydroxylation panoxadiol(HPD), and to confirm their structures. Methods Four main impurities were isolated from new sapogenin HPD using repeated silica column chromatography and recrystallization. The structural characteristics of the impurities were determined by physical and chemical properties and spectral methods, such as LC-MS, 1H- NMR, and 13 C- NMR. Results The structrues of the four related substances for new sapogenin HPD were identified as (20S, 24R)-dammar-20, 24-epoxy-3 β, 6 α, 12 β, 25-tetraol,(20S, 24S)-dammar-20, 24-epoxy-3 β, 12 β, 25-triol,(20S, 25R)-dammar-20, 25-epoxy-3 β, 12 β, 26-triol and dammar-24-ene-3 β, 12 β, 20S-triol. Conclusion The quantitative and qualitative studies on the HPD related substances of new sapogenin HPD can provide a basis for the quality control of HPD active pharmaceutical ingredients.