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3 protocols using g6230 tof ms

1

Comprehensive Characterization of Organic Compounds

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X-ray data were collected using a Bruker APEX DUO instrument. Optical rotations were measured with Horiba SEPA-300 and JASCO P-1020 polarimeters. UV spectra were recorded on a Shimadzu UV-2401A spectrophotometer. IR spectra were obtained on a Tenor 27 spectrophotometer with KBr pellets. One-dimensional (1D) and two-dimensional (2D) NMR spectra were recorded on Bruker DRX-600 spectrometers with TMS as the internal standard. Chemical shifts (δ) were expressed in parts per million with reference to the solvent signals. HRESIMS was performed on an Agilent G6230 TOF MS. Semi-preparative HPLC was performed on an Agilent 1260 liquid chromatograph with a Zorbax SB-C18 (9.4 mm × 25 cm) column. Column chromatography (CC) was performed on silica gel (100–200 mesh and 200–300 mesh; Qingdao Marine Chemical Inc., Qingdao, People's Republic of China), Lichroprep RP-18 gel (40–63 μm, Merck, Darmstadt, Germany), MCI gel (75–150 μm, Mitsubishi Chemical Corporation, Tokyo, Japan), and Sephadex LH-20 (Pharmacia). Fractions were monitored by TLC, and spots were visualized by UV light (254 nm) and sprayed with 8% H2SO4 in ethanol, followed by heating.
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2

Chromatography and Spectroscopy Techniques

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Column chromatography (CC) was run on silica gel (200–300 mesh, Qingdao Marine Chemical, Inc.) and Lichroprep RP-18 (40–63 μm, Merck). Semipreparative HPLC was carried out on an Agilent 1100 liquid chromatography system using a YMC-Pack 10 mm × 250 mm column (Pro C18 RS). Precoated TLC plates (200–250 μm thickness, silica gel 60 F254, Qingdao Marine Chemical, Inc.) were used for thin-layer chromatography. 1D and 2D NMR spectra were obtained using Bruker DRX-500 and Avance III-600 MHz spectrometers (Bruker, Zűrich, Switzerland) with solvent signal as internal reference. ESIMS and HRESIMS were run with a Shimadzu LCMS-IT-TOF mass spectrometer (Shimadzu, Kyoto, Japan) or an Agilent G6230 TOF MS (Agilent Technologies, Palo Alto, USA). Infrared spectra were obtained using a Shimadzu IR-450 instrument with KBr pellets. A JASCO P-1020 digital polarimeter was applied to record optical rotations, using MeOH as solvent. X-ray diffraction was realized with a Bruker SMART APEX CCD crystallography system. Flow cytometry analysis was conducted with a PARTEC brand flow cytometer (Germany). Quantitative PCR (q-PCR) was conducted with a ProFlex™ PCR system (Thermo Fisher, Shanghai, China). SDS-PAGE was carried out with a Mini-Protean Tetra Electrophoresis System (Bio-Rad, Shanghai, China).
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3

Analytical Techniques for Natural Product Characterization

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Optical rotations were carried out using a Horiba SEPA-300 polarimeter and JASCO DIP-370 digital polarimeter. UV spectra were recorded on Shimadzu 2401Aspectrophotometer. IR Spectra were obtained on Brucker Tensor 27 infrared spectrophotometer with KBr pellets. 1H, 13C and 2D NMR spectral data were measured on a Bruker Avance III-600, DRX-500, and AM-400 MHz spectrometers with SiMe4 as an internal standard. HRESIMS data were recorded on an Agilent G6230 TOF MS. Column chromatography (CC) was performed with silica gel (200–300 mesh, Qing-dao Haiyang Chemical Co., Ltd., Qingdao, China). RP-18 silica gel (20–45 μm, Fuji Silysia Chemical Ltd., Japan). Fractions were monitored by TLC on silica gel plates (GF254, Qingdao Haiyang Chemical Co., Ltd.) and spots visualized with Dragendorff’s reagent spray. MPLC was employed using a Buchi pump system coupled with RP-18 silica gel packed glass columns(15 × 230 and 26 × 460 mm, respectively). HPLC system was carried out on a Waters HPLC system (Waters 1525E pumps, Waters 2996 photodiode array detector, Waters fraction collector II) using a analytical semi-preparative or preparative Sunfire C18 column (4.6 × 150, 10 × 150, and 19 × 250 mm, respectively).
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