高速逆流色谱技术分离纯化红葱中的萘醌类化合物  

Separation and Purification of Naphthoquinones from Eleutherine mericana by High-speed Counter-current Chromatography

作　　者：段文娟[1] 赵伟[1] 李月[1] 耿岩玲[1] 王晓[1] 

机构地区：[1]山东省中药质量控制技术重点实验室山东省分析测试中心,济南250014

出　　处：《天然产物研究与开发》2016年第12期1911-1914,共4页Natural Product Research and Development

基　　金：三院联合基金项目(ZR2016YL006);山东省自然科学基金(ZR2013HM075)

摘　　要：采用高速逆流色谱(HSCCC)技术从红葱中快速分离纯化得到红葱乙素和异红葱乙素,建立了快速分离制备红葱中萘酚类化合物的方法。首先采用95%乙醇加热回流提取得红葱提取物,再用乙酸乙酯萃取富集萘醌类成分,然后用高速逆流色谱分离纯化,以石油醚-乙酸乙酯-甲醇-水(6∶4∶5∶5,v/v)组成二元溶剂系统,上相为固定相,下相为流动相,仪器转速为850 rpm,流速为2.0 m L/min,检测波长为254 nm。从200 mg富集萘醌类成分的粗提物中,一次性分离制备得到60 mg异红葱乙素和49 mg红葱乙素,经高效液相色谱法(HPLC)分析,其纯度分别为97.3%和98.6%。通过核磁共振氢谱(~1H NMR)和核磁共振碳谱(^(13)C NMR)鉴定化合物为红葱乙素和异红葱乙素。研究结果表明,该方法快速、高效,适用于红葱中萘酚类化合物的分离纯化。An efficient method was established for the separation and purification of naphthoquinones from Eleutherine- mericana. The naphthols was extracted with 95% ethanol from E. mericana and then enriched by extracting with ethyl acetate. The crude naphthol extract were separated by High-speed Counter-current Chromatography （HSCCC） with petrole- um ether-ethyl acetate-methanol-water （6： 4： 5：5 ,v/v） as the solvent system. The revolution speed was 850 rpm with a flow rate of 2.0 mL/min. The eluent was continuously monitored by a UV monitor at 254 nm. Finally, 87 mg of eleutherin and 35 mg of isoeleutherin were obtained from 200 mg crude extract with purities of 97.3% and 98.6% by,HPLC analysis, respectively. Their structures were identified by mass spectrometry （MS） and nuclear magnetic resonance spectrum （NMR）. The result showed that this method was simple, efficient and suitable for the isolation and separation of naph- thols from E. mericana.

关 键 词：红葱 高速逆流色谱 红葱乙素 异红葱乙素 

分 类 号：R917[医药卫生—药物分析学]