Agilent 1100 series lc msd ion trap mass spectrometer

Data of optical rotations, UV, and ECD spectra were obtained using Jasco P2000, JASCO V-650, and Jasco J-815 spectrophotometers (Jasco Corporation, Tokyo, Japan), respectively. IR spectra were measured with a Nicolet 5700 spectrometer (Thermo Nicolet Corporation, Madison, SD, USA). GC was performed with an Agilent 7890A instrument (Agilent Technologies, Waldbronn, Germany). The 1D- and 2D-NMR spectra were obtained at 500 or 600 MHz for ¹H and at 125 or 150 MHz for ¹³C, using Bruker 600 and 500 MHz spectrometers (Bruker Corporation, Karlsruhe, Germany). HRESIMS data were acquired with an Agilent 1100 series LC/MSD ion trap mass spectrometer (Agilent Technologies, Waldbronn, Germany). Column chromatography was performed using macroporous resin (Diaion HP-20 and SP-700, from Mitsubishi Chemical Corp., Tokyo, Japan and Sephadex LH-20 columns Pharmacia Fine Chemicals, Uppsala, Sweden. Preparative HPLC was carried out with a Shimadzu LC-6AD instrument with an SPD-20A detector Shimadzu Corp., Tokyo, Japan, using a YMC-Pack ODS-A column (250 mm × 20 mm, 5 μm; YMC Corp., Kyoto, Japan). HPLC-DAD analysis was performed using an Agilent 1200 series system (Agilent Technologies, Waldbronn, Germany) with an Apollo C18 column (250 mm × 4.6 mm, 5 μm; Alltech Corp., Lexington, KY, USA).

ESIMS was performed using an Agilent 1100 series LC/MSD ion trap mass spectrometer (Agilent, Santa Clara, CA, USA). The 1D- and 2D-NMR spectra were obtained in CD₃OD and DMSO with TMS as the internal standard on Varian 500 MHz and Bruker AV500-III spetrometers (Bruker Corporation, Billerica, MA, USA). Column chromatography was performed over silica gel (160–200 mesh, Qingdao Marin Chemical, Inc., Qingdao, China), RP-18 reverse phase silica gel (43–60 μm), cyanopropyl silica gel (43–60 μm) and Sephadex LH-20 (Pharmacia Biotech AB, Uppsala, Sweden). LPLC experiments were performed with Combiflash with a UV-detector (ISCO Companion, Lincoln, NE, USA). HPLC experiments were performed using a Waters 2545 system with 2998 diode array detector (Waters Corporation, Milford, MA, USA), using the Waters Sunfire and X-Bridge (250 mm × 10 mm i.d.) preparative columns packed with C18 (5 μm) (Alltech Associates, Inc., Bannockburn, IL, USA). TLC was carried out with glass precoated silica gel GF254 glass plates. Spots were visualized under UV light and by spraying with 8% H₂SO₄ in 95% EtOH followed by heating.

Optical rotations were measured on a JASCO P-2000 polarimeter (JASCO Inc. Tokyo, Japan). UV spectra were measured on a JASCO V650 spectrophotometer (JASCO Inc.). The CD spectra were measured on a JASCO J-815 CD spectrometer (JASCO Inc.). IR spectra were recorded on a Nicolet 5700 FT-IR spectrometer (Thermo Nicolet, Waltham, MA, USA). NMR spectra were acquired with VNS-400 spectrometers and VNS-500 spectrometers (Varian Inc., Palo Alto, CA, USA). HRESI-MS spectra were collected on an Agilent 1100 series LC/MSD ion trap mass spectrometer (Agilent Technologies Ltd, Santa Clara, CA, USA). Preparative HPLC was performed on a Shimadzu LC-6AD (SHIMADZU Inc. Tokyo, Japan) instrument with an SPD-20A detector, using an YMC-Pack ODS-A column (2 × 25 cm, 5 µm). Column chromatography was performed with silica gel (200–300 mesh, Qingdao Marine Chemical Inc., Qingdao, China) and ODS (50 µm, YMC, Kyoto, Japan). Chiral AD-H column (4.6 mm × 250 mm, 5 µm, Daicel, Osaka, Japan); TLC was carried out on glass precoated silica gel GF254 plates. Spots were visualized under UV light or by spraying with 10% sulfuric acid in EtOH, followed by heating.