制备型高速逆流色谱分离纯化卷柏中的黄酮类化合物  

Separation and Purification of Flavones from Selaginella tamariscina by Preparative High-speed Counter-current Chromatography

作　　者：骆厚鼎[1] 袁媛[1] 彭爱华[1] 陈俐娟[1] 

机构地区：[1]四川大学生物治疗国家重点实验室,成都610041

出　　处：《四川化工》2008年第4期31-34,共4页Sichuan Chemical Industry

摘　　要：首次采用制备型高速逆流色谱仪TBE-300A对卷柏药材中的活性黄酮类化合物进行分离纯化。实验过程中对溶剂系统和参数条件进行系统的优化,获得较好的分离条件,溶剂系统:正庚烷-乙酸乙酯-甲醇-水(2∶3∶2∶3,V/V),上相(有机相)为固定相,下相(水相)为流动相,反相洗脱;进样浓度:20mg/mL;进样体积:20mL;流速:3.0 mL/min;转速:850 r/min。进一步分离获得三种高纯度黄酮类化合物,经HPLC、MS和NMR鉴定,分别为阿曼托双黄酮(246mg,95.6%)、罗伯茨双黄酮(11.4mg,91.3%)、扁柏双黄酮(8.7mg,88.2%)。另外还得到了一个化合物(27.3mg,94.2%),结构尚待确定。Preparative high-speed counter-current chromatography（TBE-300A） was employed first to separate and purify bioactivity flavones from the Selaginella tamariscina. In the experiment , we optimized the solvent system and the experiment parameters to be the following conditions： solvent system, n-heptaneethyl acetate-methanol-water（2 ： 3 ： 2 ： 3,V/V）, reverse phase ; sample concentration , 20mg/mL; sample volume , 20mL; flow rate, 3.0 mL/min; rotation speed , 850 r/min. Amentoflavone （246mg, 95.6%）, robustaflavone （11.4mg, 91.3%）, hinokiflavone （8.7mg, 88.2%） were obtained by only one step separation and their structure were identified by HPLC, MS, NMR. Another compound （27. 3mg, 94. 2%） was obtained. And its structure still needs to be further analyzed. n

关 键 词：高速逆流色谱 卷柏 黄酮 分离纯化 

分 类 号：TQ461[化学工程—制药化工]