Varian 640 ir ft ir spectrophotometer

NMR spectra were performed on Bruker ascend 600 MHz and/or Bruker ascend 500 MHz NMR spectrometer (Bruker BioSpin AG Industriestrasse 26 CH-8117) with tetramethylsilane as an internal standard. Negative-ion mode ESI-Q-Orbitrap MS were determined on a Thermo ESI-Q-Orbitrap MS mass spectrometer connected to the UltiMate 3000 UHPLC instrument via ESI interface (Thermo Scientific). Optical rotations, UV, IR, and ECD spectra were run on a Rudolph Autopol^® IV automatic polarimeter (l = 50 mm) (Rudolph Research Analytical, Hackettstown), Varian Cary 50 UV-Vis (Varian, Inc.), Varian 640-IR FT-IR spectrophotometer (Varian Australia Pty Ltd.), and Circular dichroism spectrum (J-815, JASCO company), respectively.
Column chromatorgtaphies (CC) were accomplished on macroporous resin D101 (Haiguang Chemical Co., Ltd.), silica gel (48–75 μm, Qingdao Haiyang Chemical Co., Ltd.), ODS (50 μm, YMC Co., Ltd.), MCI gel CHP 20P (Mitsubishi Chemical Corporation, CHP20/P120), and Sephadex LH-20 (Ge Healthcare Bio-Sciences). HPLC column: Cosmosil 5C18-MS-II (4.6 mm i. d. × 250 and 20 mm i. d. × 250 mm) (5 μm, Nakalai Tesque, Inc.) were used to analysis and separate the constituents, respectively.
Dichloromethane (CH₂Cl₂), methanol (MeOH), acetonitrile (CH₃CN), acetic acid (HAc), and other reagents (chromatographically pure or analytical pure) were purchased from Tianjin Concord Technology Co., Ltd.

The following instruments were used to obtain physical data—NMR spectra were measured on Bruker ascend 600 MHz or a Bruker ascend 500 MHz NMR spectrometer (Bruker BioSpin AG Industriestrasse 26 CH-8117, Fällanden, Switzerland) with tetramethylsilane as an internal standard. The negative-ion mode ESI-Q-Orbitrap MS was obtained on a Thermo UltiMate 3000 UHPLC instrument (Thermo, Waltham, MA, USA). Optical rotations, UV, and IR spectra were run on a Rudolph Autopol^® IV automatic polarimeter (l = 50 mm) (Rudolph Research Analytical, Hackettstown NJ, USA), Varian Cary 50 UV–Vis (Varian, Inc., Hubbardsdon, MA, USA) and Varian 640-IR FT-IR spectrophotometer (Varian Australia Pty Ltd., Mulgrave, Australia), respectively.
CC were performed on macroporous resin D101 (Haiguang Chemical Co., Ltd., Tianjin, China), silica gel (48–75μm, Qingdao Haiyang Chemical Co., Ltd., Qingdao, China), ODS (50 μm, YMC Co., Ltd., Tokyo, Japan), MCI gel (Mitsubishi Chemical Corporation, Osaka, Japan), and Sephadex LH-20 (Ge Healthcare Bio-Sciences, Uppsala, Sweden). High performance liquid chromatography (HPLC) column—Cosmosil 5C₁₈-MS-II (4.6 mm i.d. × 250 mm, 5 µm) and Cosmosil 5C₁₈-MS-II (20 mmi.d. × 250 mm, 5 µm, NakalaiTesque, Inc., Tokyo, Japan) were used to analyze and separate the constituents.