Sun Yinshi, Gu Shubo, Guo Linlin, Xia Xue, Zhang Hong, Wang Jianhua
State Key Laboratory of Crop Biology, Shandong Key Laboratory of Crop Biology, College of Agronomy, Shandong Agricultural University, Taian, China.
J Sep Sci. 2014 Jul;37(13):1703-9. doi: 10.1002/jssc.201400153. Epub 2014 May 19.
A preparative high-speed countercurrent chromatography method was successfully used for the isolation of five minor flavones from Polygonum cuspidatum flowers. Among them, three compounds were obtained from P. cuspidatum for the first time. A twin two-phase solvent system composed of n-hexane/ethyl acetate/ethanol/water (1:6:3:6, v/v/v/v) and petroleum ether/ethyl acetate/methanol/water (2:4:3:3, v/v/v/v) was developed. Compounds were obtained from the fraction B and fraction C prepurified by silica gel column chromatography. Five minor compositions, 6.8 mg of hesperidin, 11.2 mg of phloridzin, 4.9 mg of luteolin, 5.3 mg of hyperin, and 3.7 mg of luteoloside were obtained from 140 mg of the fraction B and 110 mg of fraction C with a purity of 95.3, 96.4, 98.0, 96.8, and 95.3%, respectively, as determined by high-performance liquid chromatography. The structures of these compounds were identified by (1) H and (13) C NMR spectroscopy.
一种制备型高速逆流色谱法成功用于从虎杖花中分离出5种次要黄酮。其中，有3种化合物首次从虎杖中获得。开发了由正己烷/乙酸乙酯/乙醇/水（1:6:3:6，v/v/v/v）和石油醚/乙酸乙酯/甲醇/水（2:4:3:3，v/v/v/v）组成的双两相溶剂体系。通过硅胶柱色谱预纯化从B馏分和C馏分中获得化合物。从140 mg的B馏分和110 mg的C馏分中分别获得了5种次要成分，即6.8 mg橙皮苷、11.2 mg根皮苷、4.9 mg木犀草素、5.3 mg金丝桃苷和3.7 mg木犀草苷，通过高效液相色谱测定其纯度分别为95.3%、96.4%、98.0%、96.8%和95.3%。这些化合物的结构通过（1）H和（13）C核磁共振光谱进行鉴定。
