目的 建立制备甘肃马先蒿中毛蕊花糖苷和异毛蕊花糖苷单体的方法。方法 以毛蕊花糖苷和异毛蕊花糖苷质量分数为考察指标,通过静态吸附和动态解吸附实验,从01A1、D101、HPD100、AB-8、XAD-6、DM130、DM-301、DM-201、YWD06B及YWD06C中筛选出最佳树脂,确定制备甘肃马先蒿总苯乙醇苷的最佳纯化工艺。并以中压柱色谱技术分离制备毛蕊花糖苷和异毛蕊花糖苷单体,根据波谱数据鉴定结构。结果 最佳纯化工艺为上样溶液含生药20 mg/mL,上样体积流量为3 BV/h,先用3 BV的水除杂,再用5 BV 50%乙醇以2 BV/h的体积流量洗脱,洗脱液减压浓缩,冷冻干燥,得甘肃马先蒿总苯乙醇苷纯化物,该纯化物中毛蕊花糖苷和异毛蕊花糖苷的质量分数为42.29%和28.51%。经中压柱色谱精制后分离制备的毛蕊花糖苷和异毛蕊花糖苷单体质量分数分别为98.33%和99.24%。结论 该方法高效快速、经济简单、易于实现,可用于毛蕊花糖苷和异毛蕊花糖苷单体的制备。

Objective To establish a preparation method for verbascoside and isoverbascoside with high purity from Pedicularis kansuensis. Methods With the contents of verbascoside and isoverbascoside as indexes, static and dynamic adsorption-desorption were used to select the best macroporous resin from 01A1, D101, HPD100, AB-8, XAD-6, DM130, DM-301, DM-201, YWD06B, and YWD06C. The purification technology parameters of total phenylethanoid glycosides (PhGs) from P. kansuensis were optimized by selected macroporous resin. Medium pressure column chromatography was further used to purify verbascoside and isoverbascoside. The chemical structures were identified on the basis of the spectral data. Results D101 type resin showed the best purifying profile, its optimum technology conditions were as follows:Sample injection concentration was 20 mg/mL, sample flow rate was 3 BV/h, then washing off the impurity with 3 BV deionized water, and being eluted by 5 BV 50% ethanol with the desorption rate at 2 BV/h. The 50% ethanol fraction was evaporated and dried with cry desiccation to obtain the total PhGs. The contents of verbascoside and isoverbascoside in total PhGs were 42.29% and 28.51%, respectively. After purified by medium pressure column chromatography, the contents of prepared verbascoside and isoverbascoside reached 98.3% and 99.2%, respectively. Conclusion This method can be used for the large-scale preparation of verbascoside and isoverbascoside with high purity, which is rapid, simple, and practicable with high efficiency.

国家自然科学基金面上项目(81374019);甘肃省中医药管理局科研立项课题(GZK-2015-59);全军医药卫生科研项目(CLZ15JA05)