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Preparative Separation of Diterpene Lactones and Flavones from <i>Andrographis paniculate</i> Using Off-Line Two-Dimensional High-Speed Counter-Current Chromatography
oleh: Xiaowei Sun, Huijiao Yan, Yujie Zhang, Xiao Wang, Dawei Qin, Jinqian Yu
Format: | Article |
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Diterbitkan: | MDPI AG 2019-02-01 |
Deskripsi
Seven diterpene lactones, andrographolide (<b>1</b>), isoandrographolide (<b>2</b>), neo-andrographolide (<b>3</b>), 14-deoxy-11,12-didehydroandrographolide (<b>4</b>), 14-deoxyandrographiside (<b>5</b>), 14-deoxy-11,12-didehydroandrographiside (<b>6</b>), 3,14-dideoxyandrographolide (<b>10</b>), and three flavones, andrographidine C (<b>7</b>), andrographidine A (<b>8</b>), 5-hydroxy-7,8-dimethoxyflavanone (<b>9</b>) have been successfully and efficiently isolated from <i>A. paniculata</i> using an off-line two dimensional (2D) high-speed counter-current chromatography (HSCCC) method for the first time. For the first dimension HSCCC separation, petroleum ether-ethyl acetate-methanol-water 3:7:5:5 (<i>v</i>/<i>v</i>) was employed to isolate 14.4 mg of compound <b>1</b>, 3.1 mg of compound <b>2</b>, 7.8 mg of compound <b>3</b>, and 18.0 mg of compound <b>4</b> from 200 mg of the <i>A. paniculata</i> extract. For the second dimension HSCCC separation, petroleum ether-ethyl acetate-methanol-water 2:8:1:9 (<i>v</i>/<i>v</i>) and 5:5:6:4 (<i>v</i>/<i>v</i>) were employed to isolate the collected fractions ranged from 55 to 79 min and the flow out fraction, respectively, which led to 5.1 mg of compound <b>5</b>, 4.4 mg of compound <b>6</b>, 2.4 mg of compound <b>7</b>, 3.3 mg of compound <b>8</b>, 4.0 mg of compound <b>9</b>, 7.0 mg of compound <b>10</b>. The structures of these diterpene lactones and flavones were elucidated by extensive spectroscopic methods.