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4 protocols using cary 50

1

Structural Elucidation of Compounds

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Optical rotations were measured on a JASCO P-1010 polarimeter with a 1 cm cell and circular dichroism spectrum was recorded on a JASCO J-1500 CD spectrometer (Jasco Corporation, Tokyo, Japan). The UV and IR spectra were acquired on a Varian Cary 50 and JASCO FT/IR 4100 spectrometers, respectively. The NMR spectra were measured on a Varian VNMRS 500 MHz spectrometer (Varian, Palo Alto, CA, USA) with a 3 mm ID probe in MeOH-d4 solvent, which was referenced by residual solvent peaks at δH 3.30 and δC 49.0). The high-resolution ESI mass spectrum was acquired by using a SCIEX X500R (Sciex Co., Framingham, MA, USA). The HPLC was performed using an Agilent 1200 system (Santa Clara, CA, USA) using Phenomenex polar C18 and YMC ODS-A columns and an ELSD detector. Quantum calculations were conducted by Dell PowerEdge R740 server (Dell, Round Rocks, TX, USA) installed Gaussian 16 (Gaussian Inc., Wallingford, CT, USA) and Spartan 20 (Wavefunction Inc., Irvine, CA, USA) software.
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2

Analytical Techniques for Natural Product Characterization

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Optical rotations were determined with a Perkin-Elmer 341 polarimeter. UV, CD, and FT-IR spectra were measured using a Varian Cary 50, a JASCO-810 CD spectrometer, and a Bruker Vertex 70 instruments, respectively. NMR spectra were recorded on a Bruker AM-400 spectrometer, and the 1H and 13C NMR chemical shifts were referenced to the solvent or solvent impurity peaks for CD3OD (δH 3.31 and δC 49.0) and DMSO-d6 (δH 2.50 and δC 39.5). High-resolution electrospray ionization mass spectra (HRESIMS) were carried out in the positive ion mode on a Thermo Fisher LC-LTQ-Orbitrap XL spectrometer. Semipreparative HPLC was carried out on an Agilent 1200 quaternary system with a UV detector or a Dionex HPLC system equipped with an Ultimate 3000 pump, an Ultimate 3000 autosamper injector, and an Ultimate 3000 DAD detector controlled by Chromeleon software (version 6.80), using a reversed-phased C18 column (5 μm, 10 × 250 mm). Column chromatography was performed using silica gel (100–200 and 200–300 mesh), ODS (50 μm), and Sephadex LH-20. Thin-layer chromatography (TLC) was performed with silica gel 60 F254 and RP-C18 F254 plates.
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3

Characterization of Natural Products

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Optical rotations were determined with a Perkin-Elmer 41 polarimeter equipped with a sodium lamp (589 nm). UV, CD, and FT-IR spectra were performed on a Varian Cary 50, a JASCO-810 CD spectrometer, and a Bruker Vertex 70 instruments, respectively. 1D and 2D NMR spectra were recorded on a Bruker AM-400 spectrometer, and the 1H and 13C NMR chemical shifts were referenced with respect to the solvent or solvent impurity peaks. HRESIMS were carried out in the positive ion mode on a Thermo Fisher LC-LTQ-Orbitrap XL spectrometer. X-ray data were collected using a Bruker APEX DUO instrument. Column chromatography was conducted with silica gel (200–300 and 300–400 mesh; Qingdao Marine Chemical Inc., China), Sephadex LH-20 (GE Healthcare Bio-Sciences AB, Sweden), and MCI gel (75–150 μm, Mitsubishi Chemical Corporation, Tokyo, Japan). Semi-preparative HPLC was carried out on a Dionex quaternary system with a diode array detector at a flow rate of 2.5 mL/min using a reversed-phased C18 column (5 μm, 10 × 250 mm, YMC-pack ODS-A).Thin-layer chromatography (TLC) was performed with silica gel 60 F254 (Yantai Chemical Industry Research Institute) and RP-C18 F254 plates (Merck, Germany).
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4

Spectroscopic Characterization of Compounds

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Optical rotations were determined with a Perkin-Elmer 341 polarimeter. UV, ECD, and FT-IR spectra were measured using a Varian Cary 50, a JASCO-810 spectrometer, and a Bruker Vertex 70, respectively. NMR spectra were recorded on a Bruker AM-400 spectrometer, and the 1H and 13C NMR chemical shifts were referenced to the solvent or solvent impurity peaks for CDCl3 (δH 7.26 and δC 77.0) and pyridine-d5 (δH 7.19 and δC 123.5). High-resolution electrospray ionization mass spectra (HRESIMS) were obtained in the positive ion mode with a Thermo Fisher LC-LTQ-Orbitrap XL spectrometer. Semi-preparative HPLC was performed on an Agilent 1200 quaternary system with a UV detector or on a Dionex HPLC system equipped with an Ultimate 3000 pump, an Ultimate 3000 autosampler injector, and an Ultimate 3000 diode array detector (DAD) controlled by Chromeleon software (version 6.80) using a reverse-phase C18 column (5 μm, 10 × 250 mm, Welch Ultimate XB-C18). Column chromatography was performed using silica gel (100–200 and 200–300 mesh; Qingdao Marine Chemical Inc., China), ODS (50 μm, Merck, Germany), Sephadex LH-20 (Merck, Germany), or MCI gel (75–150 μm, Merck, Germany). Thin-layer chromatography (TLC) was performed with silica gel 60 F254 (Yantai Chemical Industry Research Institute) and RP-C18 F254 plates (Merck, Germany).
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