Semi-preparative and preparative high-speed counter-current chromatography (HSCCC) were successfully used for isolation of five glycosides from 50% ethanol extract of the dried barks of Ilex rotunda Thunb. (Aquifoliaceae) by using a two-phase solvent system composed of ethyl acetate-n-butanol-water (1:6:7, v/v/v). From 1.0 g of the extract, syringaresinol 4′,4″-di-O-β-D-glucopyranoside ( I , 20.2 mg, 55.4% purity), syringin ( II , 56.8 mg, 98.1% purity), sinapaldehyde glucoside ( III , 26.2 mg, 68.6% purity), syringaresinol 4′-O-β-D-glucopyranoside ( IV , 20.4 mg, 95.3% purity), and pedunculoside ( V , 45.1 mg, 97.3% purity) were obtained by one run of TBE-1000A HSCCC instrument with 1000 mL of column volume. Glycosides I (9.8 mg, 95.5% purity) and III (14.2 mg, 97.8% purity) were further purified by preparative high performance liquid chromatography (HPLC). Their structures were identified by IR, MS, and 1H and 13C NMR studies. Glycoside I was isolated from this plant for the first time.

中文翻译：

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通过高速逆流色谱法从树皮 OFILEX ROTUNDABY 中分离出五种糖苷

半制备型和制备型高速逆流色谱 (HSCCC) 成功地从圆冬青干树皮的 50% 乙醇提取物中分离出五种苷。(Aquifoliaceae) 通过使用由乙酸乙酯-正丁醇-水 (1:6:7, v/v/v) 组成的两相溶剂系统。从 1.0 g 提取物中，丁香脂素 4',4"-di-O-β-D-吡喃葡萄糖苷（I，20.2 mg，55.4% 纯度），丁香苷（II，56.8 mg，98.1% 纯度），芥子醛葡萄糖苷（III） , 26.2 mg, 68.6% 纯度)、丁香脂素 4'-O-β-D-吡喃葡萄糖苷 (IV, 20.4 mg, 95.3% 纯度) 和花梗苷 (V, 45.1 mg, 97.3% 纯度) 通过一次 TBE 获得-1000A HSCCC 仪器，柱体积为 1000 mL。糖苷 I (9.8 mg, 95.5% 纯度) 和 III (14.2 mg, 97. 8% 纯度）通过制备型高效液相色谱（HPLC）进一步纯化。它们的结构通过 IR、MS、1H 和 13C NMR 研究确定。糖苷 I 是第一次从这种植物中分离出来。