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。
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.
出处
《四川化工》
CAS
2009年第1期33-36,共4页
Sichuan Chemical Industry
关键词
高速逆流色谱
和厚朴酚
合成
high-speed counter-current chromatography
honokiol
synthesis