Uv 260 spectrometer

The HR-ESI-MS analysis was performed on the Thermo Q-Exactive Orbitrap Mass spectrometer (Thermo Fisher Scientific Corporation, Waltham, MA, USA) equipped with electrospray ionization source (ESI). The preparative HPLC was performed with Varian binary gradient LC system (Varian Inc. Corporate, Santa Clara, CA, USA) containing two solvent deliver modules (PrepStar 218), a photodiode array detector (ProStar 335) and a fraction collector (ProStar 704), using an the preparative Cosmosil ODS column (250 mm × 20.0 mm i.d., 5 μm, Cosmosil, Nakalai Tesque Co. Ltd., Kyoto, Japan). UV spectra were recorded on a Shimadzu UV-260 spectrometer (Shimadzu Corporation, Tokyo, Japan). IR spectra were determined on a Perkin-Elmer 683 infrared spectrometer (PerkinElmer, Inc., Waltham, MA, USA) in KBr pellets. Optical rotations were measured using a JASCO P-200 polarimeter (JASCO Corporation, Tokyo, Japan) with a 5-cm cell. The NMR spectra were taken with TMS as the internal standard on a Brucker Avance III 600 FT NMR spectrometer (Bruker Corporation, Billerica, MA, USA). Column chromatography was performed on silica gel (Yantai Chemical Industry Research Institute, Yantai, China) and Cosmosil 75 C₁₈-OPN (75 μm, Nakalai Tesque Co. Ltd., Kyoto, Japan).

An electrospray ionization source (ESI)-equipped Q-Exactive Mass spectrometer (Thermo Fisher Scientific Corporation, Waltham, MA, USA) was used to analyze the HR-ESI-MS data. A Shimadzu UV-260 spectrometer (Shimadzu Corporation, Tokyo, Japan) and a Perkin-Elmer 683 infrared spectrometer (PerkinElmer, Inc., Waltham, MA, USA) were used to obtain the UV and IR spectra, respectively. A JASCO P-200 polarimeter (JASCO Corporation, Tokyo, Japan) with a 5 cm cell was applied to measure the optical rotation value. The NMR spectra with TMS as the internal standard were taken on a Brucker Avance III 600 FT NMR spectrometer (Bruker Corporation, Billerica, MA, USA).

An electrospray ionization source (ESI)-equipped Q-Exactive Mass spectrometer (Thermo Fisher Scientific Corporation, Waltham, MA, USA) was used to analyse the HR-ESI-MS data. A Shimadzu UV-260 spectrometer (Shimadzu Corporation, Tokyo, Japan) and a Perkin–Elmer 683 infrared spectrometer (PerkinElmer, Inc., Waltham, MA, USA) were used to obtain the UV and IR spectra, respectively. A JASCO P-200 polarimeter (JASCO Corporation, Tokyo, Japan) with a 5 cm cell was applied to measure the optical rotation value. The NMR spectra with TMS as the internal standard were taken on a Brucker Avance III 600 FT NMR spectrometer (Bruker Corporation, Billerica, MA, USA).
Column chromatography was performed with silica gel (Yantai Chemical Industry Research Institute, Shandong, China), Cosmosil 75 C18-MS-II (75 μm, Nacalai Tesqye corporation, Kyoto, Japan), and Spehadex LH-20 (GE Healthcare, Danderyd, Sweden). Semi-preparative HPLC was conducted on an Aglient HPLC (Agilent Technologies Inc., Santa Clara, CA, USA) system equipped with a diode array detector via a preparative Cosmosil ODS column. The HR-ESI-MS spectra were measured using a thermo Q-Exactive Mass spectrometer (Thermo Fisher Scientific Corporation).