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离子交换-反相色谱纯化育亨宾
引用本文:陶蕾,赵明珠,赵凤生,徐伟,王芝祥.离子交换-反相色谱纯化育亨宾[J].中国生化药物杂志,2011,32(5).
作者姓名:陶蕾  赵明珠  赵凤生  徐伟  王芝祥
作者单位:1. 上海交通大学药学院,上海,200240
2. 上海医药工业研究院,上海,200040
基金项目:上海市科学技术委员会中药现代化项目(08DZ1973800)资助
摘    要:目的从育亨宾树皮中提取的育亨宾粗品,一般纯度较低(10%左右)。本文研究纯化育亨宾粗品的方法。方法结合离子交换与反相色谱两种方法,考察了洗脱条件对纯化效果的影响。结果采用1×2型阳离子交换树脂,以乙醇-水-氨水(40∶55∶5)为洗脱液,洗脱的育亨宾纯度最高;然后用C18反相色谱进一步纯化,流动相为甲醇-水(含0.01%三氟乙酸),甲醇浓度按3%,30%,40%,95%分阶段增加,洗脱液中的育亨宾纯度提高至71.2%。结论这项工艺具有成本低、收率高、纯度好、步骤少的特点,在天然产物的分离纯化方面具有潜在的应用价值。

关 键 词:育亨宾  纯化  离子交换  反相色谱

Purification of crude yohimbine by ion-exchange and reversed-phase chromatography
TAO Lei,ZHAO Ming-zhu,ZHAO Feng-sheng,XU Wei,WANG Zhi-xiang.Purification of crude yohimbine by ion-exchange and reversed-phase chromatography[J].Chinese Journal of Biochemical Pharmaceutics,2011,32(5).
Authors:TAO Lei  ZHAO Ming-zhu  ZHAO Feng-sheng  XU Wei  WANG Zhi-xiang
Institution:TAO Lei1,ZHAO Ming-zhu1,ZHAO Feng-sheng1,XU Wei2,WANG Zhi-xiang2(1.School of Pharmacy,Shanghai Jiao Tong University,Shanghai 200240,2.Shanghai Institute of Pharmaceutical Industry,Shanghai 200040,China)
Abstract:Purpose Crude yohimbine separated from Corynanthe yohimbe is only with low purity(about 10%).A method to purify crude yohimbine should be studied.Methods Ion-exchange and reversed-phase chromatography were combined in this study.The influence of elution conditions on purifying effects was investigated.Results By adsorption with 1×2 cation exchange resin and elution with mixture of ethanol,water and ammonia(40∶55∶5),highest purity of yohimbine was obtained.Next separation with C18 reversed-phase chromatography was eluted with the mixture of methanol and water(containing 0.01% trifluoroacetic acid).When the concentration of methanol increased progressively based on 3%-30%-40%-95%,the purity of yohimbine in eluent could increase to 71.2%.Conclusion This technique has advantages of low cost,high yield,good purity and fewer procedures and has potential application value in the separation and purification of natural products.
Keywords:yohimbine  purification  ion-exchange  reversed-phase chromatography  
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