制备型高速逆流色谱分离纯化木蝴蝶中的黄酮苷类化合物  

Separation of Flavonoid Glycosides from Oroxylum indicum by Preparative High-speed Counter-current Chromatography

作　　者：袁媛[1] 陈俐娟[2] 

机构地区：[1]四川大学化工学院,四川成都610065 [2]四川大学生物治疗国家重点实验室,四川成都610041

出　　处：《四川化工》2008年第2期37-42,共6页Sichuan Chemical Industry

摘　　要：采用制备型高速逆流色谱技术对木蝴蝶甲醇提取物中的活性黄酮苷类化合物进行分离纯化。实验过程中对二相溶剂体系、转速、流速、进样体积和进样浓度等参数进行了系统的优化,获得较优分离条件:溶剂体系,氯仿-甲醇-水(9.5:10:5),水相(上相)为固定相,有机相(下相)为流动相,正相洗脱;转速,800r/min;流速,3.0mL/min;进样体积,20mL;进样浓度,2.0×104mg/L;一步收集到五种高纯度黄酮苷类物质,经HPLC、MS和NMR鉴定分别为baicalein-7-O-glucoside(137.8mg,98.3%),baicalein-7-O-diglucoside(78.6mg,99.2%),chrysin-7-O-glucuronide(70.6mg,99.3%)和baicalin(57.2mg,99.6%),及一种新的chrysin-diglucoside(9.5mg,98.8%)。其中chrysin-7-O-glucuronide和baicalin是首次通过制备型高速逆流色谱从这种植物中分离得到。Preparative, high-speed counter-current chromatography was used to separate and purify flavonoid glycosides from the methanol extract of Oroxylum indicum. After the optimization of the two-phase sol- vent system, rotation speed, flow rate, sample volume and sample concentration, baicalein-7-O-glucoside （137.8 mg, 98.3%）, baicalein-7-O-diglucoside （78.6 mg, 99.2%）, chrysin-7-O-glucuronide （70.6 mg, 99.3%）, baicalin （57.2 mg, 99.6%） and a new chrysin-diglucoside （9.5 mg, 98. 8%） were obtained by only one step, with the amounts and purities in the parentheses, under the following conditions： chloro- form-methanol-water （9.5：10：5）, normal phase, 800 r/min, 3.0 mL/min, 20 mL, 2. 0×10^4 mg/L, fol- lowed separa by the HPI.C, MS and NMR analysis. Further more, chrysin-7-O-glucuronide and baicalin were ted for the first time from this plant by preparative high-speed counter-current chromatography.

关 键 词：黄酮苷 高速逆流色谱 木蝴蝶 分离纯化 

分 类 号：TQ461[化学工程—制药化工]