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目的建立毛鸡骨草中异夏佛塔苷对照品的制备分离方法。方法取毛鸡骨草药材醇提浸膏的正丁醇萃取部分用硅胶柱色谱分离,氯仿-甲醇(90∶10~70∶30)梯度洗脱,收集异夏佛塔苷富集流份,继续采用低压C18柱色谱及制备HPLC进行分离纯化,通过NMR、MS等波谱方法鉴定化合物结构,经TLC、HPLC-UV及MS联用等技术进行质量分数检测。结果从毛鸡骨草中制备分离的异夏佛塔苷对照品,质量分数>99%。结论本法得到的异夏佛塔苷对照品符合中药化学对照品的相关技术要求,为药材毛鸡骨草和含毛鸡骨草的成方制剂的质量控制及药效物质基础研究提供化学对照品。
OBJECTIVE To establish a method for the isolation and preparation of isofractafos reference substance from Abrus mollis. Methods The fraction of n-butanol extracted from the extract of alcohol extract of Grifola frondosa was separated by silica gel column chromatography and eluted with a gradient of chloroform-methanol (90:10 ~ 70:30) Continue to use low-pressure C18 column chromatography and preparative HPLC separation and purification, NMR, MS and other spectroscopic methods identified compounds by TLC, HPLC-UV and MS combined with other techniques for mass fraction detection. Results The isolated isoflavostigmine reference substance was prepared from Gracilaria graminis with the mass fraction> 99%. CONCLUSION The isoflavostigmine reference substance obtained by this method conforms to the relevant technical requirements of the Chinese traditional medicine reference substance and provides a chemical control for the quality control and effective substance basic research of Radix Aconiti Preparata and Radix Aconiti Preparatus Product