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8 protocols using agilent 6200 q tof ms system

1

Comprehensive Analytical Characterization Protocol

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Optical rotations were obtained on a JASCO P-1020 digital polarimeter (Horiba, Kyoto, Japan). UV spectra were recorded on a Shimadzu UV-2401PC UV–visible recording spectrophotometer (Shimadzu, Kyoto, Japan). 1D and 2D NMR spectra were obtained on a Bruker Avance III 600 MHz spectrometer (Bruker Corporation, Karlsruhe, Germany). HRESIMS were recorded on an Agilent 6200 Q-TOF MS system (Agilent Technologies, Santa Clara, CA, USA). HREIMS were obtained on a Waters Autospec Premier P776 mass spectrometer. Single crystal X-ray diffraction was performed on an APEX II DUO spectrophotometer (Bruker AXS GmbH, Karlsruhe, Germany). Sephadex LH-20 (Amersham Biosciences, Uppsala, Sweden) and silica gel (Qingdao Haiyang Chemical Co., Ltd) were used for column chromatography (CC). Medium pressure liquid chromatography (MPLC) was performed on a Büchi Sepacore System equipped with pump manager C-615, pump modules C-605 and fraction collector C−660 (Büchi Labortechnik AG, Flawil, Switzerland), and columns packed with Chromatorex C-18 (40–75 μm, Fuji Silysia Chemical Ltd., Kasugai, Japan). Preparative high performance liquid chromatography (prep-HPLC) were performed on an Agilent 1260 liquid chromatography system equipped with Zorbax SB−C18 column (particle size 5 μm, dimension 9.4 mm × 150 mm, flow rate 8 mL/min, respectively) and a DAD detector (Agilent Technologies, Santa Clara, CA, USA).
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2

Spectroscopic Characterization of Natural Products

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1D and 2D NMR spectra were obtained on a Bruker Avance III 600 MHz spectrometer (Bruker Biospin GmbH, Karlsruhe, Germany). HREIMS was measured on Waters Xevo TQ-S and Waters Autospec Premier P776 mass spectrometers (Waters, Milford, MA, USA). HRESIMS were recorded on an Agilent 6200 Q-TOF MS system (Agilent Technologies, Santa Clara, CA, USA). UV spectra were recorded on a Shimadzu UV-2401PC (Shimadzu, Kyoto, Japan). Optical rotations were obtained on a JASCO P-1020 digital polarimeter (Horiba, Kyoto, Japan). IR spectra were detected on Bruker Tensor 27 FTIR (KBr pellets) spectrometers. Sephadex LH-20 (Amersham Biosciences, Upssala, Sweden) and silica gel (Qingdao Haiyang Chemical Co., Ltd) were used for column chromatography (CC). Preparative high performance liquid chromatography (prep-HPLC) was performed on an Agilent 1100 liquid chromatography system equipped with Zorbax SB-C18 columns (9.4 mm × 250 mm) and a DAD detector (Agilent Technologies, Santa Clara, CA, USA). Thin-layer chromatography was performed on precoated TLC plates (200–250 μm thickness, silica gel 60 F254, Qingdao Marine Chemical, Inc.), and spots were visualized by heating after spraying.
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3

Analytical Techniques for Natural Products

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Optical rotations were obtained on a JASCO P-1020 digital polarimeter (Horiba, Kyoto, Japan). UV spectra were recorded on a Shimadzu UV-2401PC UV–visible recording spectrophotometer (Shimadzu, Kyoto, Japan). A Tenor 27 spectrophotometer (Bruker Optics GmbH, Ettlingen, Germany) was used for scanning IR spectroscopy using KBr pellets. 1D and 2D NMR spectra were obtained on Bruker DRX 500 MHz and Avance III 600 MHz spectrometers (Bruker Corporation, Karlsruhe, Germany). HRESIMS were recorded on an Agilent 6200 Q-TOF MS system (Agilent Technologies, Santa Clara, CA, USA). Sephadex LH-20 (Amersham Biosciences, Uppsala, Sweden) and silica gel (Qingdao Haiyang Chemical Co., Ltd, Qingdao, China) were used for column chromatography (CC). Medium pressure liquid chromatography (MPLC) was performed on a Büchi Sepacore System equipped with pump manager C-615, pump modules C-605 and fraction collector C-660 (Büchi Labortechnik AG, Flawil, Switzerland), and columns packed with Chromatorex C-18 (dimensions 450 mm × i.d. 14 mm, particle size: 40–75 μm, Fuji Silysia Chemical Ltd., Kasugai, Japan). Preparative high performance liquid chromatography (prep-HPLC) were performed on an Agilent 1260 liquid chromatography system equipped with a Zorbax SB-C18 column (particle size 5 μm, dimension 150 mm × i.d. 9.4 mm, flow rate 7 ml min−1, respectively) and a DAD detector (Agilent Technologies).
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4

Characterization of Natural Products

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Optical rotations were obtained on a JASCO P-1020 digital polarimeter (Horiba, Kyoto, Japan). UV spectra were recorded on a Shimadzu UV-2401PC UV–Visible recording spectrophotometer (Shimadzu, Kyoto, Japan). A Tenor 27 spectrophotometer (Bruker Optics GmbH, Ettlingen, Germany) was used for scanning IR spectroscopy using KBr pellets. 1D and 2D NMR spectra were obtained on a Bruker Avance III 600 MHz spectrometer (Bruker Corporation, Karlsruhe, Germany). HRESIMS were recorded on an Agilent 6200 Q-TOF MS system (Agilent Technologies, Santa Clara, CA, USA). Sephadex LH-20 (Amersham Biosciences, Uppsala, Sweden) and silica gel (Qingdao Haiyang Chemical Co., Ltd., Qingdao, China) were used for column chromatography (CC). Medium Pressure Liquid Chromatography (MPLC) was performed on a Büchi Sepacore System equipped with pump manager C-615, pump modules C-605 and fraction collector C-660 (Büchi Labortechnik AG, Flawil, Switzerland), and columns packed with Chromatorex C-18 (dimensions 450 mm × i.d. 14 mm, particle size: 40–75 μm, Fuji Silysia Chemical Ltd., Kasugai, Japan). Preparative high performance liquid chromatography (prep-HPLC) were performed on an Agilent 1260 liquid chromatography system equipped with a Zorbax SB-C18 column (particle size 5 μm, dimensions 150 mm × i.d. 9.4 mm, flow rate 7 ml min−1) and a DAD detector (Agilent Technologies, Santa Clara, CA, USA).
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5

Spectroscopic Analyses of Compound Structures

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Optical rotations were recorded on a JASCO P-1020 digital polari-meter (Horiba, Kyoto, Japan). UV/Vis spectra were obtained using a Shimadzu UV2401PC spectrometer (Shimadzu, Kyoto, Japan). 1D and 2D NMR spectra were measured on a Bruker Avance III 600 MHz spectrometers (Bruker Biospin GmbH, Karlsruhe, Germany). HRESIMS were recorded on an Agilent 6200 Q-TOF MS system (Agilent Technologies, Santa Clara, CA, USA). Silica gel (200–300 mesh, Qingdao Haiyang Chemical Co., Ltd., P. R. China) was used for chromatography column. Size exclusion chromatography was performed on Sephadex LH-20 (GE, Healthcare) columns. MPLC separation was conducted on a Biotage Isolera One using a Spherical C18 column. Semi-preparative HPLC was performed on an Agilent 1260 liquid chromatography system equipped with Zorbax SB-C18 columns (9.4 mm × 150 mm, particle size 5 μm).
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6

Analytical Characterization of Natural Products

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Optical rotations were obtained on a JASCO P-1020 digital polarimeter (Horiba, Kyoto, Japan). NMR spectra were obtained on Bruker 500 MHz and Bruker Avance III 600 MHz spectrometers (Bruker, Karlsruher, Germany). HRESIMS were recorded on an Agilent 6200 Q-TOF MS system (Agilent Technologies, Santa Clara, CA, USA). HREIMS were measured on a Waters Autospec Premier P776 mass spectrometer (Waters, Milford, MA, USA). Silica gel 200–300 mesh (Qingdao Marine Chemical Inc., Qingdao, China) and Sephadex LH-20 (Amersham Biosciences, Upssala, Sweden) were used for column chromatography. Preparative High Performance Liquid Chromatography (Pre-HPLC) was performed on an Agilent 1260 liquid chromatography system equipped with a Zorbax SB-C18 column (5 μm, 9.4 mm × 150 mm) (Agilent Technologies, Santa Clara, CA, USA).
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7

Analytical Techniques for Compound Characterization

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Optical rotations were obtained on a JASCO P-1020 digital polarimeter (Horiba, Kyoto, Japan). UV spectra were recorded on a Shimadzu UV-2401PC (Shimadzu, Kyoto, Japan). 1D and 2D NMR spectra were obtained on a Bruker Avance III 600 MHz spectrometer (Bruker Biospin GmbH, Karlsruhe, Germany). HREIMS was measured on Waters Xevo TQ-S and Waters Autospec Premier P776 mass spectrometers (Waters, Milford, MA, USA). HRESIMS were recorded on an Agilent 6200 Q-TOF MS system (Agilent Technologies, Santa Clara, CA, USA). Melting points were measured on an X-4 microscopic melting point meter (Yuhua Instrument Co., Ltd, Gongyi, China). Sephadex LH-20 (Amersham Biosciences, Upssala, Sweden) and silica gel (Qingdao Haiyang Chemical Co., Ltd) were used for column chromatography (CC). Medium Pressure Liquid Chromatography (MPLC) was performed on a Büchi Sepacore System equipping with pump manager C-615, pump modules C-605 and fraction collector C-660 (Büchi Labortechnik AG, Flawil, Switzerland), and columns packed with Chromatorex C-18 (40–75 μm, Fuji Silysia Chemical Ltd., Kasugai, Japan). Preparative High Performance Liquid Chromatography (prep-HPLC) was performed on an Agilent 1260 liquid chromatography system equipped with Zorbax SB-C18 columns (5 μm, 9.4 mm × 150 mm or 21.2 mm × 150 mm) and a DAD detector (Agilent Technologies, Santa Clara, CA, USA).
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8

Spectroscopic Analysis of Chemical Compounds

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UV spectra were recorded on a Thermo Fisher Scientific NanoDrop One micro-spectrophotometer (Thermo Fisher Scientific, Waltham, MA, United States). 1H NMR, 13C NMR, and 2D NMR spectra were recorded on a Bruker Avance 500 MHz spectrometer with tetramethylsilane (TMS; Alfa Chemistry, United States) as an internal standard. Mass spectra were recorded on an Agilent 6200 Q-TOF MS system. TLC was performed on plates precoated with silica gel GF254 (10–40 μm, Qingdao Marine Chemical Ltd., Qingdao, China). Column chromatography was performed on silica gel (100–200, 200–300, and 300–400 mesh; Qingdao Marine Chemical Ltd., Qingdao, China), RP-18 gel (20–45 μm), and Sephadex LH-20 (Amersham Biosciences, United Kingdom). Medium-pressure liquid chromatography (MPLC; CXTH-3000, China) was performed using columns packed with RP-18 gel and an LC3000 system equipped with P3000A pump modules. Semipreparative high performance liquid chromatography (HPLC; Waters 1525, United States) was performed using a column (YMC-pakODS-A, 10 × 250 mm, 5 μm, 4 mL/min).
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