Optical rotations were measured on a JASCO P-1020 digital polarimeter (JASCO, Tokyo, Japan). The NMR spectra were recorded on a Bruker AVANCE 400 MHz spectrometer (Bruker, Ettlingen, Germany). HRESI-MS were obtained in the positive or negative ion mode with an AB SCIEX Trip TOFTM 5600+ (AB Sciex, Framingham, MA, USA). HPLC was carried out on a waters Breeze system (Waters, Milford, MA, USA) with an ODS column (Sunfire ODS, 4.6 × 250 mm, 5 μm,), Semipreparative HPLC was carried out on a waters Breeze system (Waters, Milford, MA, USA) with an ODS column (Sunfire ODS, 10 × 250 mm, 5 μm, 3 mL/min). MPLC was performed on a LC3000 series (Tong Heng Innovation Technology, Beijing, China) with a Flash C18 cartridge (50 μm, 40 g, YMC, Kyoto, Japan); all solvents were HPLC grade. Column chromatography was performed with silica (200–300 mesh, Qingdao Marine Chemical Inc, Qingdao, China) and Sephadex LH-20 (Amersham Biosciences Inc, Uppsala, Sweden), respectively. Thin layer chromatography (TLC) was carried out with glass precoated silica gel GF254 plates. The reagents for analysis were purchased from Xilong Scientific Co., Ltd. (Gongdong, China).
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