All conventional reagents and solvents are purchased directly from commercial companies and no further purification is required. Organic solvents were purchased from Sinopharm chemical reagent Co., Ltd. and purified by distillation and moisture was excluded from the glass apparatus using CaCl2 drying tubes. Throughout this study, silica gel H (200–300 mesh; Qingdao Marine Chemical Factory, Qingdao, China) was used for the column chromatography. For thin layer chromatographic (TLC) plates, Silica gel (GF254) (Qingdao Marine Chemical Factory, Qingdao, China) were used for thin layer chromatographic (TLC) analysis, and all of the spots and bands were detected by UV irradiation (254, 365 nm). The intermediates and products were characterized by electrospray ionization mass spectrometry (TripleTOF5600þ; AB SCIEX Pte. Ltd., Boston, MA, USA), 1H NMR and 13C NMR (Bruker AM500 spectrometer; Bruker Corporation, Berne, Switzerland). The derivatives were dissolved in 100% dimethyl sulfoxide (DMSO; Beyotime Biotechnology, Haimen, China), stored at 4 °C prior to antiviral evaluation, and used within 6 months. For solubility, the stock solutions, at a concentration of 50 mg/mL, were sonicated for approximately 10 min to ensure that the derivatives were fully dissolved and mixed.
Silica gel h
Manufactured by Qingdao Marine Chemical
Sourced in China
Silica gel H is a fine white powder composed of amorphous silicon dioxide particles. It is a highly porous material with a large surface area, making it a versatile adsorbent for a variety of applications. The core function of Silica gel H is to act as a desiccant, absorbing moisture from its surrounding environment.
Automatically generated - may contain errors
Lab products found in correlation
Sephadex lh 20, by Cytiva (5 mentions)
Silica gel, by Qingdao Marine Chemical (4 mentions)
P 1020, by Jasco (3 mentions)
Lichroprep rp 18 gel, by Merck Group (2 mentions)
Waters 1525 pump, by Waters Corporation (2 mentions)
Avance 600 spectrometer, by Bruker (2 mentions)
J 815 spectrometer, by Jasco (2 mentions)
Perkin elmer 241 mc, by PerkinElmer (2 mentions)
Avance 800 spectrometer, by Bruker (2 mentions)
Silica gel gf254, by Qingdao Marine Chemical (1 mentions)
Dimethyl sulfoxide (dmso), by Beyotime (1 mentions)
2487 dual λ absorbance detector, by Waters Corporation (1 mentions)
Sq detector 2 mass spectrometer, by Waters Corporation (1 mentions)
400 mhz spectrometer, by Bruker (1 mentions)
Beckman du 640 spectrophotometer, by Beckman Coulter (1 mentions)
Micromass q tof ultima global gaa076 lc mass spectrometer, by Waters Corporation (1 mentions)
Gemini a ultra system, by Agilent Technologies (1 mentions)
Agilent eclipse xdb c18 column, by Agilent Technologies (1 mentions)
Agilent 500 mhz, by Agilent Technologies (1 mentions)
Micromass q tof ultima global gaa076lc mass spectrometers autospec ultima tof, by Waters Corporation (1 mentions)
16 protocols using silica gel h
1
Purification and Characterization of Organic Compounds
2
Spectroscopic Characterization of Compounds
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Ultraviolet
(UV) data were obtained using a Waters 2487 dual λ absorbance
detector. Infrared (IR) spectra were measured on a Nicolet Nexus 470
spectrophotometer using KBr disks. NMR spectra were recorded using
a Varian System 500. The corresponding residual solvent signals (δH/C 2.50/39.5 for DMSO-d6, 7.26/77.2
for CDCl3, or 3.31/49.2 for CD3OD) were used
to reference the chemical shifts in NMR spectra. Furthermore, HRESIMS
spectra were measured using a Q-TOF Ultima Global GAA076 LC mass spectrometer,
and LRESIMS spectra were obtained using a Waters SQ Detector 2 mass
spectrometer. Semipreparative HPLC was performed using a phenyl column
(YMC-pack Ph, 10 mm × 250 mm) or a π-NAP column (COSMOSIL,
10 mm × 250 mm). TLC was performed on plates precoated with silica
gel GF254 (10–40 μm). Column chromatography (CC) was
performed over silica gel (200–300 mesh, Qingdao Marine Chemical
Factory) and Sephadex LH-20 (Amersham Biosciences). Finally, vacuum
liquid chromatography (VLC) was performed using silica gel H (Qingdao
Marine Chemical Factory).
(UV) data were obtained using a Waters 2487 dual λ absorbance
detector. Infrared (IR) spectra were measured on a Nicolet Nexus 470
spectrophotometer using KBr disks. NMR spectra were recorded using
a Varian System 500. The corresponding residual solvent signals (δH/C 2.50/39.5 for DMSO-d6, 7.26/77.2
for CDCl3, or 3.31/49.2 for CD3OD) were used
to reference the chemical shifts in NMR spectra. Furthermore, HRESIMS
spectra were measured using a Q-TOF Ultima Global GAA076 LC mass spectrometer,
and LRESIMS spectra were obtained using a Waters SQ Detector 2 mass
spectrometer. Semipreparative HPLC was performed using a phenyl column
(YMC-pack Ph, 10 mm × 250 mm) or a π-NAP column (COSMOSIL,
10 mm × 250 mm). TLC was performed on plates precoated with silica
gel GF254 (10–40 μm). Column chromatography (CC) was
performed over silica gel (200–300 mesh, Qingdao Marine Chemical
Factory) and Sephadex LH-20 (Amersham Biosciences). Finally, vacuum
liquid chromatography (VLC) was performed using silica gel H (Qingdao
Marine Chemical Factory).
3
Comprehensive Analytical Techniques for Chemical Characterization
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Optical rotations were measured with a JASCO P-1020 digital polarimeter (JASCO Corporation, Tokyo, Japan). UV spectra were recorded on a Beckman DU 640 spectrophotometer (Beckman Coulter, Inc., Miami, USA). IR spectra were recorded on a Nicolet Nexus 470 spectrophotometer (Thermo Fisher Scientific Inc., Massachusetts, USA) in KBr discs. HR-ESI-MS spectra were measured on a Micromass Q-TOF Ultima Global GAA076 LC mass spectrometer (waters corporation, Milford, USA). NMR spectra were recorded on Bruker 400 MHz spectrometers (Bruker Daltonics Inc., Karlsruhe, Germany) using TMS (Tetramethyl silane) as an internal standard δ. X-ray diffraction data were collected on an Agilent Technologies Gemini A Ultra system (Agilent Technologies Inc., Palo Alto, USA). Semipreparative HPLC was performed on an Agilent 1260 LC series with a DAD detector using an Agilent Eclipse XDB-C18 column (250 × 10.0mm, 5 µm). Silica gel (300-400 mesh, Qingdao Marine Chemical Inc., China), Silica gel (200-300) mesh (Qingdao Marine Chemical Inc., China), Silica gel H (10-40 μm, Qingdao Marine Chemical Inc., China), Lichroprep RP-18 gel (40-63 μm, Merck, Darmstadt, Germany), and Sephadex LH-20 (40-70 μm, Amersham Biosciences, Sweden) were used for column chromatography (CC).
4
Spectroscopic Analysis of Chemical Compounds
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Optical rotations were measured using a Jasco P-1020 digital polarimeter (Jasco, Tokyo, Japan). The UV spectra were recorded using a Beckman DU640 spectrophotometer (Beckman Ltd., Shanghai, China). The CD spectra were obtained using a Jasco J-810 spectropolarimeter (Jasco, Tokyo, Japan). The NMR spectra were measured using Agilent 500 MHz (Agilent, Beijing, China) and JEOL JNMECP 600 spectrometers (JEOL, Beijing, China). The 7.26 ppm and 77.16 ppm resonances of CDCl3 were used as internal references for the 1H and 13C NMR spectra, respectively. The HRESIMS spectra were measured using Micromass Q-Tof Ultima GLOBAL GAA076LC mass spectrometers (Autospec-Ultima-TOF, Waters, Shanghai, China). Semi-preparative HPLC was performed using a Waters 1525 pump (Waters, Singapore) equipped with a 2998 photodiode array detector and a YMC C18 column (YMC, 10 × 250 mm, 5 μm). Silica gel (200–300 mesh, 300–400 mesh, and silica gel H, Qingdao Marine Chemical Factory, Qingdao, China) was used for column chromatography.
5
Structural Elucidation of Natural Compounds
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Optical rotations were measured with a JASCO P-1020 digital polarimeter. UV data were recorded with a Beckman DU 640 spectrophotometer, and CD data were collected using a JASCO J-815 spectropolarimeter. IR spectra were taken on a Nicolet NEXUS 470 spectrophotometer as KBr disks. 1H NMR, 13C NMR, DEPT, HMQC, HMBC, COSY, and NOESY spectra were recorded using Bruker Avance 500 spectrometer using TMS as an internal standard, and chemical shifts were recorded as δ values. Chemical shift values were referenced to residual solvent signals for DMSO (δH/δC, 2.50/ 39.5). HRESIMS data were recorded using a Q-TOF ULTIMA GLOBAL GAA076 LC mass spectrometer. HPLC and semi-preparative HPLC were performed using a Cholester column (COSMOSIL-pack, 4.6 × 250 mm, 5 μm, 1 mL/min) and an ODS column [YMC-pack ODS-A, 10 × 250 mm, 5 μm, 4 mL/min], respectively. TLC and column chromatography (CC) were performed on plates precoated with silica gel GF254 (10−40 μm) and over silica gel (200−300 mesh, Qingdao Marine Chemical Factory) and Sephadex LH-20 (Amersham Biosciences). Vacuum-liquid chromatography (VLC) used silica gel H (Qingdao Marine Chemical Factory).
6
Spectroscopic Analysis of Natural Compounds
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NMR spectra were recorded on a Bruker DRX-500 spectrometer (500 MHz for 1 H NMR and 125 MHz for 13 C-NMR) and a Varian UNITY INOVA 600 spectrometer (600 MHz for 1 H NMR and 150 MHz for 13 C-NMR) in pyridine-d 5 (Sigma-Aldrich), and the chemical shifts are given in δ (ppm). HRESIMS was performed on the Synapt MS (Waters Corporation). Optical rotations were measured with the Perkin-Elmer 343 polarimeter (PerkinElmer) and JASCO J-810 polarimeter (JASCO Corporation). UV data were recorded on a UV-2500 spectrophotometer (MAPADA Corporation). HPLC analyses were performed on an Agilent 1100 series (Agilent Technologies) equipped with an Alltech 2000 evaporative light scattering detector (temp: 110 °C, gas: 2.4 L/min, Alltech Corporation) and a Techmate C18 column (4.6 mm × 250 mm, ODS, 5 µm, Techmate Co. Ltd.). Semipreparative HPLC separations were carried out using a system consisting of an NP7000 module (Hanbon Co. Ltd.), a Shodex RID 102 detector (Showa Denko Group), and a Venusil XBP C18 column (8.0 mm × 250 mm, ODS, 5 µm, Bonna-Agela Technologies). silica gel H (Qingdao marine Chemical), MCI resin (50 µm, Mitsubishi Chemicals), and ODS (Octadecylsilyl) silica gel (120 Å, 50 µm, YMC) were used for column chromatography performance.
7
Extraction and Purification of Magnolol
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Magnolol (>99% purity) was purchased from Aladdin Biochemical Technology (Shanghai, China). Other chemicals were obtained from Sigma-Aldrich (St. Louis, MO, USA) and used without further purification. Anhydrous acetone, methanol, and dimethyl sulfate (DMS) were bought from Sinopharm Chemical Reagent Co., Ltd. (Beijing, China). Silica gel H (200–300 mesh, Qingdao Marine Chemical Factory, Qingdao, China) was applied for column chromatography. Silica gel (cat no. GF254, Qingdao Marine Chemical Factory, Qingdao, China) was used for thin-layer chromatography (TLC). Milli-Q water (Millipore, Burlington, MA, USA) was used to make aqueous solutions.
8
Spectroscopic Characterization of Organic Compounds
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Optical rotations were obtained on a JASCO P-1020 digital polarimeter. UV spectra were recorded on a Primaide 1430 DAD detector of Hitachi. Electron circular dichroism (ECD) spectra were measured on a JASCO J-815 spectrometer. Measurement of HRESIMS used a Q-TOF Ultima Global GAA076 LC mass spectrometer. The 1H, 13C, DEPT, and 2D NMR spectral data were recorded on a Bruker Avance 600 spectrometer (Bruker, Karlsruhe, Germany). Vacuum–liquid chromatography (VLC) used silica gel H (Qingdao Marine Chemical Factory, Qingdao, China). Sephadex LH-20 (Pharmacia Biotec AB, Uppsala, Sweden) and reversed-phase C18 silica gel (Merck, Darmstadt, Germany) were used for column chromatography (CC). Thin-layer chromatography (TLC) was performed on plates pre-coated with silica gel GF 254 (10–40 µm) and silica gel (200–300 mesh) (Qingdao Ocean Chemical Co., Ltd., Qingdao, China). MPLC was performed on a SepaBean machineT (Santai Technologies Co., Ltd., Changzhou, China). The semi-preparative HPLC method used was an ODS column (YMC-pack ODS-A, 10 × 250 mm, 5 µm, 4.0 mL/min). All solvents used were of analytical grade (Sinopharm Chemical Reagent Co., Ltd., Shanghai, China).
9
Spectroscopic and Chromatographic Techniques
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Optical rotations were measured on a JASCO P-2000 digital polarimeter (JASCO, Tokyo, Japan). UV spectra were performed on an Eppendorf BioSpectrometer Basic photometer. IR spectra were recorded on a JASCO FT/IR-4600 spectrometer in KBr discs. CD data were obtained on a JASCO J-810 spectropolarimeter. NMR spectra were collected using a JEOL JNM-ECP 600 spectrometer (JEOL, Tokyo, Japan). HRESIMS data were acquired on an Agilent 6210 ESI/TOF mass spectrometer (Agilent, Santa Clara, CA, USA). Analytical high performance liquid chromatography (HPLC) system (Waters, Milford, MA, USA) consisted of Waters e2695, UV Detector 2489, and software Empower using a C18 column (Diamonsil C18(2), 250 × 4.6 mm, 5 μM). Semipreparative HPLC was operated on the same system using a C18 column (Cosmosil 5C18-MS-II, 250 × 10 mm, 5 μM). Vacuum-liquid chromatography (VLC) used silica gel H (Qingdao Marine Chemical Factory, Qingdao, China). Thin layer chromatography (TLC) and column chromatography were performed on plates pre-coated with silica gel GF254 (10–40 μm) and Sephadex LH-20 (GE Healthcare Biosciences, Uppsala, Sweden), respectively.
10
Spectroscopic Characterization of Compounds
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Optical rotations were measured on a Perkin-Elmer 241 MC digital polarimeter (German PerkinElmer Corporation, Boelingen, Germany). 1D and 2D-NMR spectral experiments were measured in CD3OD on a Bruker AVANCE-800 spectrometer (Bruker Corporation, Karlsruhe, Germany) with TMS as an internal standard. The HR-ESI-MS spectra were carried out on AB SCIEX X500R high-resolution liquid chromatography-mass spectrometer (SCIEX, Framingham, MA, USA). GC-MS analysis was performed on an Agilent GC-MS 6890-5973 instrument equipped with an RXI-5 SIL MS column (30 m × 0.25 mm × 0.25 µm). Column chromatography (CC) was operated on a Sephadex LH-20 (GE-Healthcare, Uppsala, Sweden), Pure C-810 middle pressure liquid chromatography (BUCHI, Flawil, Switzerland), and silica gel H (10−40 µm, Qingdao Marine Chemical Inc., Qingdao, China). Standards for D-glucose (D-Glc), L-rhamnose (L-Rha), D-fructose (D-Fru), and L-arabinose (L-Ara) were purchased from Sigma Chemical Co. (St. Louis, MO, USA).
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