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高速逆流色谱分离纯化合成的和厚朴酚抗肿瘤衍生物
Separation and Purification of Anti-tumor Derivatives of Honokiol by High-speed Counter-current Chromatography
【摘要】 首次采用高速逆流色谱对合成的和厚朴酚生物进行分离纯化。本实验首先通过Reiman-Tie-mann反应将和厚朴酚甲酰化,再与盐酸羟胺生成3个和厚朴酚的衍生物,然后通过HSCCC将它们分离纯化。分离过程,我们对溶剂体系和样品浓度以及进样速度等参数条件进行了优化,获得了较好的分离。溶剂体系为正己烷-乙酸乙酯-甲醇-水(1:0.4:1:0.4,V/V),下相作为固定相,进样浓度为20mg/ml,进样体积为20ml,流速设定为2ml/min,转速为850rpm。分离产物经MS和NMR结构鉴定。
【Abstract】 High-speed counter-current chromatography was used first time to separate and purificate the derivatives of honokiol.In the experiment,we synthesis the derivatives of honokiol by Reiman-Tiemann reaction and hydroxylamine hydrochloride.We optimized the solvent system,sample concentration,and rotation speed.The solvent system:N-hexane:acetic ether:methanol:water(1∶0.4:1∶0.4,V/V),sample concentration is 20mg/ml,sample volume is 20ml,flow rate is 2ml/min rotation speed is 850rpm.The separation’s structure were identified by MS and NMR.
- 【文献出处】 四川化工 ,Sichuan Chemical Industry , 编辑部邮箱 ,2009年01期
- 【分类号】TQ461
- 【被引频次】2
- 【下载频次】320