用加速溶剂萃取及制备型高效液相色谱法从烟梗中制取多酚对照品

Preparation of Polyphenol Reference Substance from Peduncle of Tobacco by Accelerated Solvent Extraction and Pre-HPLC

提出用加速溶剂萃取及制备型高效液相色谱方法从烟梗中提取、制备多酚对照品的方法。样品粉碎后以乙醇(80+20)溶液为萃取溶剂经加速溶剂萃取仪在110℃静态萃取10min,提取液氮气吹扫60s后过MCI树脂和Sephadex LH 20凝胶净化,流出液用丙酮定容后,先通过制备型高效液相色谱初步分离,再通过半制备高效液相色谱进一步分离,得到5个多酚类化合物,经核磁共振波谱法鉴定分别为芸香苷、绿原酸、槲皮素、柚皮素和咖啡酸甲酯。5个多酚类化合物的纯度均大于99%,故可用作多酚对照品。

A method for the extraction and preparation of polyphenol reference substances from peduncle of tobacco by accelerated solvent extraction and pre-HPLC was proposed.The sample was crushed and extracted with ethanol（80＋20） solution under static condition at 110 ℃ for 10 min,and the extract was swept for 60 s by N2-blowing and purified by MCI resin and Sephadex LH 20 gel.The eluate collected was taken up with acetone and used for preliminary separation by pre-HPLC,and for further separation by semi-Pre-HPLC,and five polyphenols were obtained,which were identified by NMR to be rutin,chlorogenic acid,quercetin,naringenin and methyl caffeate.The purity of the 5 polyphenols were more than 99%,which could be used as reference materials.