大孔吸附树脂富集金银花中环烯醚萜苷类成分的工艺优选

Optimization of Separation and Enrichment Process of Iridoid Glycosides from Lonicerae Japonicae Flos by Macroporous Resin

目的:优选大孔吸附树脂分离纯化金银花中环烯醚萜苷类成分的工艺条件,为该药材资源的充分利用与开发提供参考。方法:采用UPLC对马钱苷酸、獐芽菜苷、断氧化马钱子苷和7-表-马钱子苷进行定量分析,流动相0.1%甲酸水溶液-乙腈梯度洗脱,流速0.3 m L·min^(-1),柱温40℃,检测波长236.5 nm,进样量1μL。通过静态吸附-洗脱试验筛选大孔树脂型号,单因素试验优选金银花中环烯醚萜苷类成分的纯化工艺条件。结果:选择H-103型大孔树脂,上样液质量浓度100 g·L^(-1),吸附流速2.0 BV·h^(-1),上样量2.5 BV,吸附后加水2.5 BV和30%乙醇3 BV洗脱,洗脱流速2.0 BV·h^(-1)。总环烯醚萜苷的洗脱率达90.0%,浸膏中总环烯醚萜苷质量分数达25.6%。结论:H-103型大孔树脂对金银花中环烯醚萜苷类成分具有较好的分离和纯化效果,工艺操作简单、稳定可行,适用于工业化生产。

Objective： To optimize separation and purification technology of iridoid glycosides from Lonicerae Japonicae Flos by macroporous resin. Method： The content of loganic acid,7-epi-loganin,sweroside and secoxyloganin was determined by UPLC,static adsorption-elution test was adopted to screen type of macroporous resin,separation and purification process conditions of iridoid glycoside were optimized by single factor tests.Result： H-103 macroporous resin was selected,optimum technology was： sample solution concentration of 100 g·L^（-1）,adsorption flow rate of 2. 0 BV·h^（-1）,sample liquid volume of 2. 5 BV,eluted by 2. 5 BV of water and 3. 0 BV of 30% ethanol at elution flow rate of 2. 0 BV·h^（-1）. Under these conditions,elution rate and purity of iridoid glycosides were 90. 0% and 25. 6%,respectively. Conclusion： Iridoid glycosides from Lonicerae Japonicae Flos are purified effectively with H-103 macroporous resin,this optimized process is simple,stable and feasible.