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pH区带精制逆流色谱法制备青风藤碱
引用本文:董红敬,张永清,庄会永,李佳,耿岩玲,王晓.pH区带精制逆流色谱法制备青风藤碱[J].山东科学,2011,24(6):36-38.
作者姓名:董红敬  张永清  庄会永  李佳  耿岩玲  王晓
作者单位:1.山东中医药大学药学院,山东 济南 250355; 2.山东省科学院中药过程控制研究中心,山东省分析测试中心,山东 济南 250014
基金项目:重大新药创制项目,山东省科技攻关项目,济南市高校院所自主创新计划,山东省中青年科学家科研奖励基金
摘    要:采用pH区带精制逆流色谱法从广西地不容中制备青风藤碱,溶剂系统为石油醚 乙酸乙酯 甲醇 水(3:7:1:9,V/V),上相加10 mmol/L三乙胺为固定相,下相加10 mmol/L盐酸为流动相。一次进样1.0 g,可得纯度为99.5%的青风藤碱600 mg,所得产物经ESI-MS,1H NMR和13C NMR进行结构鉴定。本方法效率高,制品纯度高,适合青风藤碱的大量制备。

关 键 词:广西地不容  青风藤碱  pH区带精制逆流色谱法  
收稿时间:2011-05-03

Preparation of sinoacutine from Stephania kwansiensis by pH-zone-refining counter-current chromatography
DONG Hong-jing,ZHANG Yong-qing,ZHUANG Hui-Yong,LI Jia,GENG Yan-ling,WANG Xiao.Preparation of sinoacutine from Stephania kwansiensis by pH-zone-refining counter-current chromatography[J].Shandong Science,2011,24(6):36-38.
Authors:DONG Hong-jing  ZHANG Yong-qing  ZHUANG Hui-Yong  LI Jia  GENG Yan-ling  WANG Xiao
Institution:1.School of Pharmacy, Shandong University of Traditional Chinese Medicine, Jinan 250035, China; 2.Process Control Center of Traditional Chinese Medicine, Shandong Analysis and Test Center, Shandong Academy of Sciences, Jinan 250014, China
Abstract:We employed pH-zone refining counter-current chromatography to prepare high-purity sinoacutine from Stephania kwangsiensis. Its solvent system was composed of petroleum ether-ethyl acetate-methanol-water (3 : 7: 1 : 9, V/V), in which triethylamine ( 10 mmol/L) was added to the upper organic stationary phase as a retainer and hydrochloric acid (10 mmol/L) was added to the aqueous mobile phase as an eluter. The structure of sinoautine was identified by ESI-MS,1H NMR and 13C NMR. The purity of sinoacutine determined by RP-HPLC was 99.5%. This approach has such advantages as high-efficiency and high-purity, suitable for the preparation of large amount of sinoacutine.
Keywords:Stephania kwangsiensis  Sinoacutine  pH-zone-refining counter-current chromatography
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