泽泻对照品23-乙酰泽泻醇B克级制备工艺研究

Gram Size Preparation Process of 23-Acetyl Alisol B Reference Substance from Alisma orientalis

目的探索制备克级23-乙酰泽泻醇B化学对照品的工艺。方法通过高效液相色谱法比较提取溶剂、提取次数、提取时间和溶剂量等因素对23-乙酰泽泻醇B提取率的影响,选择最佳提取工艺放大到中试设备。结果采用95%乙醇,料液比10∶1回流提取药材2次,每次1 h,提取物经石油醚-醋酸乙酯混合液萃取后,经常规硅胶柱层析、精制,获得9.8 g对照品。结论该工艺高效、简便、廉价,适用于23-乙酰泽泻醇B对照品的克级制备。

Objective To reserach the process of preparing gram-size amount of 23-acetyl alisol B chemical reference substance. Methods The effects of solvent consentration,frequency,duration and solid-liquid ratio on extraction efficiency of 23-acetyl alisol B were evaluated by HPLC,the optimal extract process was scaled up to pilot device. Results Raw material was extracted with 95% ethanol at a 10∶1 solid-liquid ratio for twice and 1 h each time,the yielded extract was seperated by petroleum ether-acetyl acetate extraction and silica gel column chromatography to produce 9.8 g of reference substance. Conclusion The process is effective,simple and economic,and can meet the need of gram-size preparation.