管花肉苁蓉中苯乙醇苷的提取和大孔树脂纯化工艺研究

Extraction of phenylethanoid glycoside from Cistanche tubulosa and purification technology by macroporous resin

目的优选管花肉苁蓉Cistanche tubulosa中苯乙醇苷的提取纯化工艺。方法以松果菊苷和麦角甾苷质量分数为考察指标,采用L9(34)正交试验设计,对提取工艺进行优化;考察7种大孔树脂对2种苯乙醇苷的吸附和解吸附性能,确定最佳纯化工艺条件。结果最佳提取纯化工艺为管花肉苁蓉药材加12倍量50%乙醇,70℃温浸2次,温浸时间1 h,滤过,合并滤液,回收溶剂,加水调整为含生药0.2 g/mL的上样溶液,上样量为0.8倍柱体积(BV),大孔树脂柱的径高比为1∶9,先用3 BV的水除杂,再用4 BV的30%乙醇洗脱,洗脱液减压浓缩至干,即得肉苁蓉苯乙醇苷纯化物,该纯化物中2种苯乙醇苷质量分数>75%。结论优选得到的提取纯化工艺稳定可行,适合工业化生产。

Objective To optimize the extraction and purification technology of phenylethanoid glycoside from Cistanche tubulosa. Methods Orthogonal design L9（3a） was employed to optimize the extraction conditions by taking the extraction yield of echinacoside and acteoside as indexes. The absorption-desorption characteristics of seven macroporous resins were evaluated, then the best purification conditions were optimized. Results The optimal extraction conditions were as follows： The air-dried stems of C. tubulosa were powdered and extracted twice with 12-fold 50% ethanol for 1 h each time, temperature was 70 ~C; The supernatant was concentrated to 5-fold weight of the stems of C. tubulosa, The concentrated liquid was subjected to macroporous resin （HPD750） column and then eluted with deionezed water （3 BV） and 30% ethanol （4 BV）, respectively. The 30% ethanol fraction was evaporated under vacuum to give the phenylethanoid glycoside-rich C. tubulosa stem extract. The purity of phenylethanoid glycoside was above 75%. Conclusion The optimized extraction and purification process is stable, efficient, and suitable for industrial production.