The College of Chemistry, Changchun Normal University, China, Changchun.
J Sep Sci. 2013 Jun;36(11):1853-60. doi: 10.1002/jssc.201300029. Epub 2013 May 3.
Four flavonoids, isoastilbin, astilbin, isoengelitin, and engelitin were isolated and purified simultaneously from Smilacis Glabrae Roxb. for the first time by high performance counter-current chromatography using a system consisting of n-hexane-n-butanol-water (1:2:3, v/v/v). A total of 392.6 mg of astilbin, 71.4 mg of isoastilbin, 47.4 mg of engelitin, and 10.3 mg of isoengelitin were purified from 1.89 g of the ethyl acetate extract of Smilacis Glabrae Roxb. in six runs, each at over 94.51% purity as determined by HPLC. The structures of the four compounds were identified by their retention time, the LC-ESI-MS(n) in the negative ion mode, and confirmed by (1)H-NMR experiments. The characteristic LC-ESI-MS fragmentation patterns of the four compounds were discussed.
首次采用正相高效制备液相色谱，以正己烷-正丁醇-水（1:2:3，v/v/v）为两相溶剂系统，从菝葜药材乙酸乙酯提取物中分离并制备得到 4 种黄酮类化合物，分别为异牡荆素、荭草苷、异落新妇苷和新绿原酸，总收率为 0.33%，纯度均大于 94.51%。通过 HPLC 分析和 LC-ESI-MS(n)检测，结合一维和二维 NMR 谱解析，确定了这 4 个化合物的结构。探讨了这 4 个化合物的电喷雾质谱裂解规律。
