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高速逆流色谱分离纯化防风中升麻素苷和5-O-甲基维斯阿米醇苷
引用本文:韩忠明,王云贺,韩梅,赵淑杰,杨利民.高速逆流色谱分离纯化防风中升麻素苷和5-O-甲基维斯阿米醇苷[J].分析化学,2009,37(11).
作者姓名:韩忠明  王云贺  韩梅  赵淑杰  杨利民
作者单位:吉林农业大学中药材学院,长春,130118
基金项目:吉林省科技发展计划重大项目(No.20075022) 资助 
摘    要:建立了高速逆流色谱分离制备防风中有效成分升麻素苷和5-O-甲基维斯阿米醇苷的方法.防风根的粉末经甲醇浸泡提取和减压蒸馏,得粗提浸膏.以V(乙酸乙酯):V(正丁醇):V(水)=2:7:9为溶剂,上相为固定相,下相为流动相,流速2.0 mL/min.从316 mg防风粗提物中一步分离得到13.9 mg升麻素苷和25 mg 5-O-甲基维斯阿米醇苷,纯度分别为98.1%和99 2%.采用ESI-MS, 1H NMR 和13C NMR对目标化合物的结构进行了鉴定.

关 键 词:高速逆流色谱  防风  升麻素苷  5-O-甲基维斯阿米醇苷

Separation and Purification of Prim-O-glucosylcimifugin and 5-O-methylvisammioside from Saposhnikovia Divaricata by High-speed Counter-current Chromatography
HAN Zhong-Ming,WANG Yun-He,HAN Mei,ZHAO Shu-Jie,YANG Li-Min.Separation and Purification of Prim-O-glucosylcimifugin and 5-O-methylvisammioside from Saposhnikovia Divaricata by High-speed Counter-current Chromatography[J].Chinese Journal of Analytical Chemistry,2009,37(11).
Authors:HAN Zhong-Ming  WANG Yun-He  HAN Mei  ZHAO Shu-Jie  YANG Li-Min
Institution:HAN Zhong-Ming,WANG Yun-He,HAN Mei,ZHAO Shu-Jie,YANG Li-Min ( College of Chinese Medicinal Materials,Jilin Agricultural University,Changchun 130118)
Abstract:High-speed counter-current chromatographic ( HSCCC ) method was successfully used to separate and purify prim-O-glucosylcimifugin and 5-0-methylvisammioside from Saposhnikovia divaricata(Thicz. ) Schis-chk. ,a traditional Chinese herb,with a solvent system composed of ethyl acetate-n-butanol-water(2:7:9,V/V). The lower phase of the system was used as the mobile phase at the flow rate of 2.0 mL/min,and the upper phase was used as the stationary phase. The separation produced a total 13.9 mg prim-O-glucosylcimifugin and 25.0 mg 5-0-methylvisammioside with the purity of 98. 1% and 99.2% determined by high performance liquid chromatography (HPLC) from 316 mg of crude sample from S. divaricata. The structures of isolated compounds were identified by ESI-MS,~1H NMR and ~(13)C NMR.
Keywords:Counter-current chromatography  Saposhnikovia divaricata  Prim-O-glucosyl-cimifugin  5-O-methylvisammioside  
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