色谱Issue(7):767-772,6.DOI:10.3724/SP.J.1123.2014.03027
亲水/反相二维色谱法制备桔梗中的三萜皂苷
Preparation of triterpene saponins from Platycodon grandiflorum by two-dimensional hydrophilic interaction liquid chromatography-reversed phase liquid chromatography
摘要
Abstract
A two-dimensional(2-D)preparative liquid chromatography method was developed for the preparation of triterpene saponins from Platycodon grandiflorum using hydrophilic interaction liquid chromatography( HILIC)coupled with reversed phase liquid chromatography ( RPLC). At first,the crude extract was obtained from Platycodon grandiflorum by boiled alco-hol precipitation. Then,the concentrated crude extracts were continuously pretreated using sol-id phase extraction( SPE)under reversed-phase and hydrophilic-phase modes to remove the impurities. Subsequently,XAmide column(150 mm×20 mm,5 μm)was selected to separate the triterpene saponin constituents under HILIC mode using water and acetonitrile as mobile phases. From 6 min to 25 min,each fraction was collected per minute under time-triggered mode and 20 fractions were collected. The 18th fraction( JG23)was selected for further purifi-cation. The column of Atlantis PrepT3(100 mm×30 mm,5 μm)was chosen and two monomer-ic compounds were obtained. The two compounds with over 90% purity were identified as dea-pi-platycoside E and platycoside E with mass spectrometry( MS)and nuclear magnetic reso-nance( NMR). This 2-D HILIC-RPLC method with high orthogonality can be used in the prepa-ration of triterpene saponins from natural products.关键词
反相色谱/亲水色谱/三萜皂苷/桔梗/制备Key words
reversed phase liquid chromatography ( RPLC )/hydrophilic interaction liquid chromatography( HILIC)/triterpene saponin/Platycodon grandiflorum/preparation分类
化学化工引用本文复制引用
邢倩倩,傅青,金郁,梁鑫淼..亲水/反相二维色谱法制备桔梗中的三萜皂苷[J].色谱,2014,(7):767-772,6.基金项目
上海市自然科学基金项目(13ZR1453200). ()