离子交换-反相色谱纯化育亨宾

Purification of crude yohimbine by ion-exchange and reversed-phase chromatography

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。

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.