气相色谱法测定2,3-二羟基-1,8-桉树脑的溶解度及油水两相体系分配比

Determination of Solubility and Distribution Ratio in Organic-Aqueous Biphasic System of 2,3-Dihydroxy-1,8-cineole by Gas Chromatography

采用气相色谱法测定2,3-二羟基-1,8-桉树脑在不同有机溶剂中的溶解度及在有机溶剂/水两相体系中的分配比,为设计该化合物的萃取分离工艺提供依据。结果表明:2,3-二羟基-1,8-桉树脑易溶于水、二氯甲烷和三氯甲烷,可溶于乙酸乙酯、1,2-二氯乙烷和α-蒎烯(25℃时的溶解度分别为26.1g·L-1、24.9g·L-1和14.9g·L-1),难溶于石油醚、环己烷等非极性有机溶剂;有机溶剂种类、温度、油水体积比对分配比有较大的影响;以二氯甲烷和三氯甲烷为有机溶剂,在温度为35℃、油水体积比为1.0的条件下,2,3-二羟基-1,8-桉树脑的分配比分别为16.3和10.3。

To provide a process for separating 2,3-dihydroxy-1,8-cineole from aqueous solution by solvent extraction method,the solubility of 2,3-dihydroxy-1,8-cineole in different organic solvents and its distribution ratio in organic-aqueous biphasic system were measured by gas chromatography.Results showed that 2,3-di-hydroxy-1 ,8-cineole was freely soluble in water,dichloromethane and chloroform;soluble in ethyl acetate,1 ,2-dichloroethane andα-pinene,the solubility at 25 ℃ were 26.1 g·L-1,24.9 g·L-1 and 14.9 g·L-1,respec-tively;hardly soluble in non-polar organic solvents such as petroleum ether and cyclohexane.The organic sol-vent type,temperature and volume ratio of organic solvent to water had obvious effect on distribution ratio of 2, 3-dihydroxy-1 ,8-cineole.Using dichloromethane or chloroform as organic solvent,when the temperature was 35 ℃,the volume ratio of organic solvent to water was 1.0,the distribution ratio of 2,3-dihydroxy-1,8-cineole were 16.3 and 10.3,respectively.