Agilent 6530 accurate mass q tof lc ms spectrometer

Optical rotations, CD, UV and FT-IR spectra were measured with a Rudolph Research analytical AutoPol automatic polarimeter (Rudolph Research Analytical, NJ, United States), JASCO J-815 CD (Jasco Corporation, Japan), Shimadzu UV spectrophotometer UV-1800 and Thermo Scientific Nicolet iS10 IR spectrometer (Thermo Fisher Scientific, WI, United States), respectively. The structure characterizations of all the compounds were based on 1D NMR (¹H, ¹³C) and 2D NMR (COSY, HSQC, HMBC, 1D-NOE and ROESY) data, recorded on a Bruker AM-400 spectrometer (Bruker BioSpin AG, Switzerland). An Agilent 6,530 Accurate-Mass Q-TOF LC-MS spectrometer (Agilent Technologies, Germany) was used to record high-resolution mass spectra. Preparative RP-HPLC was carried out on an Ultimate 3000 chromatographic system (Agilent Technologies, Germany) with a Phenomenex preparative column (Phenyl-hexyl, 5 μ, 100 × 21.2 mm) and semipreparative RP-HPLC on an Ultimate 3000 chromatographic system (Agilent Technologies, Germany) with a Phenomenex semipreparative column (C₁₈, 5 μ, 250 × 10 mm), connected to a Dionex Ultimate 3000 DAD detector (Agilent Technologies, Germany) (detected at 210, 254, 320, and 365 nm) and a Dionex Ultimate 3000 automated fraction collector. All solvents were HPLC grade. Diaion HP-20 (Alfa Aesar, Japan) was used to run the open-column chromatography.

Optical rotations, CD and IR spectra were measured with a Rudolph Research analytical AutoPol automatic polarimeter (Rudolph Research Analytical, Hackettstown, NJ, USA), JASCO J-815 CD (Jasco Corporation, Tokyo, Japan) and Thermo Scientific Nicolet iS10 IR spectrometer (Thermo Fisher Scientific, Madison, WI, USA), respectively. The structure characterizations of all the compounds were based on 1D NMR (¹H, ¹³C) and 2D NMR (COSY, HSQC, HMBC, 1D-NOE and ROESY) data, recorded on a Bruker AM-400 spectrometer (Bruker BioSpin AG, Faellanden, Switzerland). An Agilent 6530 Accurate-Mass Q-TOF LC-MS spectrometer (Agilent Technologies, Waldbronn, Germany) was used to record high-resolution mass spectra. Preparative RP-HPLC was carried out on an Ultimate 3000 chromatographic system (Agilent Technologies, Waldbronn, Germany) with a Phenomenex preparative column (Phenyl-hexyl, 5 μ, 100 × 21.2 mm) and semipreparative RP-HPLC on an Ultimate 3000 chromatographic system (Agilent Technologies, Waldbronn, Germany) with a Phenomenex semipreparative column (C₁₈, 5 μ, 250 × 10 mm), connected to a Dionex Ultimate 3000 DAD detector (Agilent Technologies, Waldbronn, Germany) (detected at 210, 254, 320 and 365 nm) and a Dionex Ultimate 3000 automated fraction collector. All solvents were HPLC grade. Diaion HP-20 (Alfa Aesar, Japan) was used to run the open-column chromatography.

Optical rotations were carried out on an MCP 200 (Anton Paar, Graz, Austria) polarimeter. UV spectra were measured at a Lambda 950 UV-Vis-NIR spectrophotometer (PerkinElmer, Akron, OH, USA). A Chirascan-plus Circular Dichroism Spectrometer (Applied Photophysics Ltd., Leatherhead, UK) was used to obtain experimental ECD data. A Fourier transformation infra-red spectrometer (FTIR) coupled with an infra-red microscope EQUINOX 55 (Bruker, Wissembourg, France) recorded the FTIR spectrum. NMR spectra were tested by a BRUKER AVANCE III HD (400 MHz) NMR spectrometer with tetramethylsilane (TMS) as the internal standard. HR-ESIMS data were determined using an Agilent 6530 accurate-Mass Q-TOF LC-MS spectrometer. Column chromatography (CC) was used using silica gel (200–300 mesh, Qingdao Marine Chemical Factory, Qingdao, China). The semi-preparative HPLC was performed on an Essentia LC-16 (Shimadzu, Jiangsu, China). Acetylcholine esterase (AChE) was from Electrophorus electricus (product number: C3389-2KU, Sigma-Aldrich, Saint Louis, MO, USA).