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目的采用高速逆流色谱技术分离纯化红景天苷、葛根素和淫羊藿苷3种标准样品。方法采用溶剂体系正丁醇:乙酸乙酯:水(2:3:5,V:V:V)分离红景天粗提物;采用溶剂体系正丁醇:乙酸乙酯:水(1:2:3,V:V:V)分离葛根粗提物;采用氯仿:甲醇:水(4:3.5:2,V:V:V)分离淫羊藿苷粗提物,并采用高效液相色谱法对所得单体进行纯度检测。结果所得红景天苷、葛根素、淫羊藿苷标准样品纯度分别为98.9%、99.8%和99.5%。将核磁共振(nuclear magnetic resonance,NMR)13C-NMR数据归属并与相关文献比对,进一步确认了该3种物质的结构。结论红景天苷、葛根素、淫羊藿苷3种样品满足GB/T 15000.3-2008标准样品工作导则的要求,可用于相关药品检测方法的校正和相关产品的质量控制。
Objective To separate and purify three standard samples of salidroside, puerarin and icariin by high-speed countercurrent chromatography. Methods Crude extracts of Rhodiola were separated by solvent system n-butanol: ethyl acetate: water (2: 3: 5, V: V: V) The crude extracts of Pueraria lobata were isolated by HPLC with chloroform: methanol: water (4: 3.5: 2, V: V: V) The purity of the obtained monomer was tested. Results The purity of standard samples of salidroside, puerarin and icariin were 98.9%, 99.8% and 99.5%, respectively. The 13C-NMR data of nuclear magnetic resonance (NMR) were attributed and compared with the related literatures, and the structures of these three substances were further confirmed. Conclusions The three samples of salidroside, puerarin and icariin can meet the requirements of GB / T 15000.3-2008 standard sample work guideline and can be used for the calibration of related drug testing methods and the quality control of related products.