摘要
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 establish a method for separation and purification of salidroside, puerarin and epimedium glycoside by high-speed counter current chromatography （HSCCC）. Methods The HSCCC solvent systems of N-butanol：ethyl acetate：water （2：3：5,V：V：V）, N-butanol：ethyl acetate：water （1：2：3, V：V：V） and chloroform：methyl alcohol：water （4：3.5：2, V：V：V） were used for isolation of salidroside, puerarin and epimedium glycoside, respectively. The purities of the end products were measured by high performance liquid chromatography （HPLC）. Result The purities of salidroside,puerarin and epimedium glycoside were 98.9%, 99.8%, and 99.5%, respectively. The structures of the target compounds were furtherly identified by data of 13C-nuclear magnetic resonance （13C-NMR） and comparison with the related literature. Conclusion The reference materials of salidroside, puerarin and epimedium glycoside can conform to directives of the reference materials of GB/T 15000.3-2008, which can be used for method validation and quality control of regarding drug products.
作者
徐双双
王尉
贺天雨
XU Shuang-Shuang WANG Wei HE Tian-Yu(Beijing Centre for Physical and Chemical Analysis, Beijing Key Laboratory of Organic Materials Testing Technology ＆ Quality Evaluation, Beijing 100089, China Beijing Academy of Science and Technology Key Laboratory of Analysis and Testing Technology, Beijing 100089, China)
出处
《食品安全质量检测学报》
CAS
2016年第11期4323-4328,共6页
Journal of Food Safety and Quality
关键词
高速逆流色谱法
分离纯化
红景天苷
葛根素
淫羊藿苷
high-speed counter current chromatography
isolation and purification
salidroside
puerarin
epimedium glycoside
