高速逆流色谱分离制备橘皮中多甲氧基黄酮  

Preparative Isolation and Purification of Polymethoxylated Flavones from Citrus Peel by High-speed Counter-counter Chromatography

作　　者：李成平[1,2] 饶桂维[1] 田红梅[2] 梅瑜[1] 严小平[1] 活泼 

机构地区：[1]浙江树人大学生物与环境工程学院,杭州310015 [2]浙江工业大学药学院,杭州310014

出　　处：《中国食品学报》2015年第6期117-122,共6页Journal of Chinese Institute Of Food Science and Technology

基　　金：浙江省科技厅公益性技术应用研究计划项目(2012C23028);浙江省科技厅分析测试科技计划项目(2015C37036);浙江省科技厅引进大院名校共建创新载体(2012E80002)

摘　　要：建立高速逆流色谱法分离制备橘皮中4种多甲氧基黄酮类化合物的方法。以石油醚-乙酸乙酯-甲醇-水(1∶0.8∶1∶1.2,V/V)为两相溶剂系统,上相为固定相,下相为流动相。在主机转速800 r/min、流动相流速2.0 m L/min、检测波长254 nm条件下分离,从200 mg橘皮粗提物中一步分离制备得到5,6,7,8,3’,4’-六甲氧基黄酮32.8 mg、3,5,6,7,8,3’,4’-七甲氧基黄酮10.9 mg、5,6,7,8,4’-五甲氧基黄酮43.5 mg和5-羟基-6,7,8,3’,4’-五甲氧基黄酮18.7 mg。产物纯度经HPLC检测分别为98.9%,97.8%,99.2%和99.8%。通过质谱和核磁共振氢谱、碳谱等波谱分析确定各化合物结构。Four polymethoxylated flavones （PMFs） were prepared, isolated and purified from citrus peel by highspeed counter-counter chromatography （HSCCC）. A two-phase solvent system composed of petroleumether ： ethyl acetate： methanol：water （1：0.8：1：1.2,V/V） was used, the top phase was stationary phase and the bottom phase was mobile phase. The 32.8 mg 5,6,7,8,3＇ ,4＇-hexamethoxyflavone, 10.9 nag 3,5,6,7,8,3＇,4＇-heptamethoxyflavone, 43.5 mg 5,6,7,8,4＇ -pentamethoxyflavone and 18.7 mg 5-hydroxy- 6,7,8,3＇ ,4＇- Pentamethoxyflavone were obtained from 200 mg of the crude extract of citrus peel in one-step elution under the conditions of a flow rate of 2.0 mL/min, the rotation speed was 800 r/min and the detection wave length of 254 nm. High performance liquid chromatographic analysis of nobiletin, 3,5, 6,7,8,3＇ ,4＇ -heptamethoxyflavone, 5,6,7,8,4＇ -pentamethoxyflavone and 5 -hydro xy-6,7,8,3＇ ,4＇ -pentamethoxyflavone revealed that their purity were individually 98.9%, 97.8%, 99.2% and 99.8%. And their structures were identified by MS, 1H-NMR and 13C-NMR. The results indicate that HSCCC is a powerful technique for the purification of polymethoxylated flavones from citrus peel.

关 键 词：高速逆流色谱 橘皮 多甲氧基黄酮 分离 

分 类 号：TS209[轻工技术与工程—食品科学]