[关键词]
[摘要]
目的从知母药材中快速分离制备知母皂苷BⅡ对照品。方法知母药材粗粉用80%乙醇提取,经大孔树脂D-101柱吸附,以30%乙醇洗脱,得到知母总皂苷。用制备RP-HPLC对总皂苷进行分离纯化,采用柱后分流,ELSD同时检测,收集含高质量分数知母皂苷BⅡ的组分。结果 制备产品经化学方法和13C-NMR鉴定;HPLC-ELSD检测,质量分数大于99%。结论 该制备方法简单,重复性好,效率较高,所得化合物质量分数高,可用于知母皂苷BⅡ对照品的制备。
[Key word]
[Abstract]
Objective To establish a method to isolate and prepare timosaponin BⅡ reference substance from Anemarrhenae Rhizoma.Methods Raw material of Anemarrhenae Rhizoma was extracted with 80% ethanol.The concentrated crude extract was separated on a D-101 macroporous resin column,by eluting the macroporous resin column with 30% ethanol, total saponins were collected.The timosaponin BⅡ was separated by preparative reversed-phase high performance liquid chromatography(RP-HPLC) coupled with ELSD and collected according to the chromatography.Results The prepared product was identified by nuclear magnetic resonance and chemical method.The purity of timosaponin BⅡ was 99% assayed by analytical HPLC-ELSD.Conclusion The preparation method is simple and rapid,and it can be used for preparation of timosaponin BⅡ reference substance.
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[基金项目]
国家药典委员会2010版一部标准研究项目(YZ-196~198);西北大学科研启动基金资助项目(OKYQDF159)