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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/m L,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 m L;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p H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。
Objective To optimize the process of purification of macroporous absorbent resin and the decolorization of ion exchange resin. Methods Stemsaponin IVa was used as a reference substance. The total saponin content of Scutellaria barbata was determined by vanillin-perchloric acid colorimetric method after spectrophotometry. The suitable macroporous adsorption method was screened by dynamic adsorption and static desorption experiments Resin and optimize the separation and purification process parameters; the retention rate of bamboo ginseng saponins, decolorization rate as an indicator of screening the appropriate type of decolorization of ionic resins and optimize their decolorization. Results X-5 macroporous resin had good purification effect on total saponins of S. japonicus. The optimal purification conditions were as follows: the crude drug concentration was 0.2 mg / m L, the sample volume was 10 g crude drug per gram resin , The eluent was 70% ethanol and the eluent was 5 mL per gram of resin. The study of decolorization showed that the 732 cation exchange resin had good decolorization effect on the crude ginsenosides obtained by the macroporous adsorption resin method, Optimized decolorization process is the operation of the macroporous resin eluate by solvent recovery until no alcohol taste, adjust the concentrate p H value of 10, loaded on the 732 cation exchange resin, the collection effluent decolorization rate greater than 50% of the fraction, this time per gram of resin bleached bamboo ginseng total saponin amount of 290.5 mg. After drying under reduced pressure, the final purified rhodiola saponin showed a white to yellowish appearance with a mass fraction of more than 85.0% and a total transfer rate of more than 70.0%. Conclusion The established method can be better separation and purification of total Saponins of Panax japonicus, suitable for industrial production.