大孔树脂纯化秦皮香豆素工艺研究

Purification process for coumarins in Fraxini Cortex by macroporous resin

目的考察大孔树脂纯化秦皮中秦皮甲素、秦皮苷、秦皮乙素、秦皮素工艺。方法静态吸附实验筛选树脂型号,单因素试验优化纯化工艺,UPLC-QTOF-MS/MS法鉴定主要成分,绘制热图。结果最佳树脂型号为ADS-5。最佳纯化工艺为上样量1.1 BV,上样液质量浓度0.75 g/mL,2 BV纯水清洗杂质,4 BV 25%乙醇洗脱有效成分,香豆素总转移率为84.42%,纯度为53.28%,得率为4.79%。共鉴定出37种成分,其中香豆素类、苯乙醇苷类主要富集在25%乙醇洗脱液中,有机酸类、环烯醚萜类、黄酮类主要富集在95%乙醇洗脱液中。结论该方法稳定、可行、准确,可表征大孔树脂不同洗脱液中秦皮香豆素分布规律,为后续相关药学研究提供指导。

AIM To investigate the purification process for esculin,fraxin,esculetin and fraxetin in Fraxini Cortex by macroporous resin.METHODS Static adsorption experiment was applied to screening resin model,single factor test was adopted in the optimization of purification process,UPLC-QTOF-MS/MS was used for identifying main components,after which heatmap was drawn.RESULTS The optimal resin model was ADS-5.The optimal purification process was determined to be 1.1 BV for loading amount,0.75 g/mL for loading concentration,2 BV pure water for washing impurity,and 4 BV 25%ethanol for eluting effective constituents,coumarins demonstrated the total transfer rate,purity and yield of 84.42%,53.28%and 4.79%,respectively.Total 37 constituents were identified,among which coumarins and phenylethanol glycosides were mainly concentrated in 25%ethanol eluent,organic acids,iridoids and flavonoids were mainly concentrated in 95%ethanol eluent.CONCLUSION This stable,feasible and accurate method can characterize the distribution patterns of coumarins in Fraxini Cortex in different eluents of macroporous resin,which provides guidance for further related pharmaceutical research.