分析化学
分析化學
분석화학
CHINESE JOURNAL OF ANALYTICAL CHEMISTRY
2009年
11期
1679-1682
,共4页
韩忠明%王云贺%韩梅%赵淑杰%杨利民
韓忠明%王雲賀%韓梅%趙淑傑%楊利民
한충명%왕운하%한매%조숙걸%양이민
高速逆流色谱%防风%升麻素苷%5-O-甲基维斯阿米醇苷
高速逆流色譜%防風%升痳素苷%5-O-甲基維斯阿米醇苷
고속역류색보%방풍%승마소감%5-O-갑기유사아미순감
Counter-current chromatography%Saposhnikovia divaricata%Prim-O-glucosyl-cimifugin%5-0-methylvisammioside
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~(13)C NMR对目标化合物的结构进行了鉴定.
建立瞭高速逆流色譜分離製備防風中有效成分升痳素苷和5-O-甲基維斯阿米醇苷的方法.防風根的粉末經甲醇浸泡提取和減壓蒸餾,得粗提浸膏.以V(乙痠乙酯):V(正丁醇):V(水)=2:7:9為溶劑,上相為固定相,下相為流動相,流速2.0 mL/min.從316 mg防風粗提物中一步分離得到13.9 mg升痳素苷和25 mg 5-O-甲基維斯阿米醇苷,純度分彆為98.1%和99 2%.採用ESI-MS,~1H NMR 和~(13)C NMR對目標化閤物的結構進行瞭鑒定.
건립료고속역류색보분리제비방풍중유효성분승마소감화5-O-갑기유사아미순감적방법.방풍근적분말경갑순침포제취화감압증류,득조제침고.이V(을산을지):V(정정순):V(수)=2:7:9위용제,상상위고정상,하상위류동상,류속2.0 mL/min.종316 mg방풍조제물중일보분리득도13.9 mg승마소감화25 mg 5-O-갑기유사아미순감,순도분별위98.1%화99 2%.채용ESI-MS,~1H NMR 화~(13)C NMR대목표화합물적결구진행료감정.
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.