[关键词]
[摘要]
目的 优化竹节参总皂苷大孔吸附树脂纯化和离子交换树脂脱色的工艺方法。方法 以竹节参皂苷IVa为对照品,采用香草醛-高氯酸显色后用分光光度法测定竹节参总皂苷的量;以动态吸附和静态解吸附实验方法筛选适宜型号的大孔吸附树脂并优化分离纯化工艺参数;以竹节参总皂苷保留率、脱色率为指标筛选合适类型的离子脱色树脂并优化其脱色效果。结果 X-5型大孔吸附树脂对竹节参总皂苷有较好的纯化效果,其最佳纯化条件为上样质量浓度为生药0.2 mg/mL,上样量为每克树脂10 g生药,洗脱剂为70%乙醇,洗脱剂用量为每克树脂5 mL;脱色工艺研究表明,732型阳离子交换树脂对大孔吸附树脂法得到的竹节参皂苷粗品具有良好的脱色效果,优化后的脱色工艺的操作方法是大孔吸附树脂醇洗脱液经回收溶剂至无醇味后,调整浓缩液pH值为10,上样于732型阳离子交换树脂,收集流出液脱色率大于50%的馏份,此时每克树脂脱色竹节参总皂苷量为290.5 mg。经减压干燥后,最终获得的精制竹节参总皂苷外观呈类白色至黄白色,其质量分数大于85.0%,总转移率超过70.0%。结论 建立的方法能较好地分离纯化竹节参总皂苷,适用于工业化生产。
[Key word]
[Abstract]
Objective To establish a simple and effective extraction method for the preparation of total saponins of Panax japonicas (TSPJ). Methods Combination of macroporous adsorption and ion exchange resin chromatography was adopted in the present study. For quality evaluation, chikusetsusaponin IVa was used as reference, and vanillin-perchloric acid was applied as chromogenic reagent to determine total saponin content at 545 nm. Results X-5 macrophous resin offered better adsorption and desorption capacities for TSPJ than other macrophous resins. The optimum purification process was confirmed as follows:The sample solution concentration was 0.2 mg/L; The sample volume was 10 g/g, and eluting with 5 mL of 70% aqueous ethanol solutions on 1 g wet macrophous resin column. Followed this step, decoloring of TSPJ was studied and the decoloring capacity of two different types of ion exchange resins was evaluated. The result showed that 732-type cation exchange resin was the better resin for decolorization of the TSPJ. The total saponin products with higher purity and quality were obtained, with the mass fraction more than 85.0%, and the transfer rate of TSPJ was more than 70.0%. Conclusion The results show that the total saponins can be separated and purified effectively from P. japonicus. The preparation method is simple, effective, and efficient for large-scale preparation of TSPJ.
[中图分类号]
[基金项目]
国家自然科学基金资助项目——基于分子谱系地理学与谱-效相关联方法研究竹节参资源品质差异形成机制(31570329)