NMR spectra were measured on a Bruker Avance AV500 spectrometer (Bruker, Germany). LC-MS was conducted with an Agilent 1290-6120 LC-Quadrupole MSD mass spectrometer (Agilent Technologies, USA). HRESIMS spectra were obtained on a Q-Exactive Plus mass spectrometer (Thermo Scientific, USA). HPLC analyses were performed on an Agilent 1260 HPLC with PDA detector (Agilent Technologies, USA). Preparative HPLC was performed on a Waters 150 LC system by using a Ultimate®AQ-C18 column (250 × 21.2 mm, 5 µm, Welch Material, USA). MCI gel High porous polymer (75-150 µm) was purchased from Mitsubishi chemical corporation (Japan). Sephadex LH-20 (25-100 µm) was obtained from GE Healthcare (Sweden). XAD16N resin (20-60 mesh) was obtained from Yuanye (Nanjing, Jiangsu, China). TaKaRa Ex Taq DNA Polymerase (USA) and OMEGA gel extraction kit (200) were purchased from Kaimoer (Nanjing, China). TLC silica gel plates (HSGF254) were obtained from Juyou company (Shandong, China). Chemicals were purchased from Acros or Juyou and used without further purification unless otherwise noted.
Avance av 500 spectrometer
Manufactured by Bruker
Sourced in Germany
The Avance AV-500 is a high-performance nuclear magnetic resonance (NMR) spectrometer manufactured by Bruker. It is designed to provide accurate and reliable analysis of samples through the detection and measurement of nuclear magnetic resonances. The spectrometer operates at a frequency of 500 MHz and is capable of performing a variety of NMR experiments.
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Lab products found in correlation
Mci gel high porous polymer, by Mitsubishi (1 mentions)
Q exactive plus mass spectrometer, by Thermo Fisher Scientific (1 mentions)
Sephadex lh 20, by GE Healthcare (1 mentions)
Mci gel high porous polymer, by Mitsubishi Chemical Corporation (1 mentions)
Thin layer chromatography, by Merck Group (1 mentions)
Caco 2, by Thermo Fisher Scientific (1 mentions)
3 4 5 dimethylthiazol 2 yl 2 5 diphenyltetrazolium bromide, by Merck Group (1 mentions)
Cary 630 ftir spectrophotometer, by Agilent Technologies (1 mentions)
Ftir affinity 1s spectrometer, by Shimadzu (1 mentions)
Triple tof 4600 mass spectrometer, by AB Sciex (1 mentions)
Kieselgel 60 f254 aluminum sheets, by Merck Group (1 mentions)
6 protocols using avance av 500 spectrometer
1
Analytical Techniques for Natural Product Research
2
Characterization and Cytotoxicity Evaluation
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A StuartTM SMP3 melting point apparatus (Scientific Laboratory Supplies Ltd, Nottingham, England) was used to measure uncorrected melting points.
Thin layer chromatography (Merck, Darmstadt, Germany) monitored the reactions using a pre-coated silica gel plate (kieselgel 60G/F254, 0.25 mm).
A Fourier transform infrared spectrophotometer (FTIR-4200, PerkinElmer, Shimadzu, Japan) was used to record the FTIR spectra at 400-4000 cm-1.
A Bruker Avance AV-500 spectrometer (Bruker, Bremen, Germany) recorded the 1H and 13C nuclear magnetic resonance (NMR) spectra. A Shimadzu UV-1800 UV/Vis scan
spectrophotometer (Shimadzu, Kyoto, Japan) was used to record the ultraviolet, and visible light absorbed by the samples.
Combustion analysis was performed on a Carlo Erba automated elemental analyzer, model 1106 (Carlo Erba, Milan, Italy). 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium
bromide (MTT) was provided by Sigma-Aldrich, Baghdad, Iraq. The cell lines (CaCo-2 and Vero) were purchased from Thermo Fisher Scientific, Waltham, USA.
All the synthesis reagents were supplied by Sigma-Aldrich, Baghdad, Iraq.
Thin layer chromatography (Merck, Darmstadt, Germany) monitored the reactions using a pre-coated silica gel plate (kieselgel 60G/F254, 0.25 mm).
A Fourier transform infrared spectrophotometer (FTIR-4200, PerkinElmer, Shimadzu, Japan) was used to record the FTIR spectra at 400-4000 cm-1.
A Bruker Avance AV-500 spectrometer (Bruker, Bremen, Germany) recorded the 1H and 13C nuclear magnetic resonance (NMR) spectra. A Shimadzu UV-1800 UV/Vis scan
spectrophotometer (Shimadzu, Kyoto, Japan) was used to record the ultraviolet, and visible light absorbed by the samples.
Combustion analysis was performed on a Carlo Erba automated elemental analyzer, model 1106 (Carlo Erba, Milan, Italy). 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium
bromide (MTT) was provided by Sigma-Aldrich, Baghdad, Iraq. The cell lines (CaCo-2 and Vero) were purchased from Thermo Fisher Scientific, Waltham, USA.
All the synthesis reagents were supplied by Sigma-Aldrich, Baghdad, Iraq.
3
Comprehensive Melanin Characterization
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The GD melanin extract was characterized using electron ionization mass spectrometry (EI-MS), Fourier transform infrared (FTIR) spectroscopy and carbon-13 nuclear magnetic resonance (13C-NMR) imaging. The EI-MS was measured using a Jeol JMS-600 W mass spectrometer (Agilent Technologies Inc, Santa Clara, CA, USA). Attenuated total reflectance (ATR)-FTIR mounted with a diamond ATR crystal was used for spectral acquisition. The spectrum was recorded at 400-4,000 cm−1 using a cary 630 FTIR spectrophotometer (Agilent Technologies Inc.). The 13C-NMR was measured using a Bruker Avance AV-500 spectrometer (Bruker BioSpin GmbH, Rheinstetten, Germany) at a frequency of 115.91 MHz and 1,024 scans. The purified melanin was dissolved in dimethyl sulfoxide (DMSO), and the chemical shifts are expressed in parts per million (ppm).
4
Synthesis and Characterization of 6-Acetyl-5-hydroxy-4-methylcoumarin
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Melting points were determined by open capillary method on STUART SMP3 (BIBBY STERILIN, UK). The IR spectra were recorded on FT-IR Affinity-1S Spectrometer (Shimadzu, Japan) in KBr pellet. The 1H and 13C NMR spectra were recorded on Avance AV500 Spectrometer (Bruker, Germany) at 500 MHz and 125 MHz, respectively, using DMSO-d6 as solvent and TMS as an internal standard. ESI-mass spectra were recorded on LC-MS LTQ Orbitrap XL spectrometers (ThermoScientific, USA) in methanol using ESI method. The analytical thin-layer chromatography (TLC) was performed on silica gel 60 WF254S aluminum sheets (Merck, Germany) and was visualized with UV light or by iodine vapor. Chemical reagents in high purity were purchased from the Merck Chemical Company (in Viet Nam). All materials were of reagent grade for organic synthesis. 6-Acetyl-5-hydroxy-4-methylcoumarin 3 was synthesized according to literature procedures [37 (link)].
5
High-Resolution ESI Mass Spectrometry for Chemical Analysis
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High-resolution ESI− mass spectra were obtained on an LC-Q-TOF-MS/MS system, which was composed of an Agilent 1290 Infinity HPLC system coupled with a Sciex Triple TOF 4600 mass spectrometer. The chromatographic separation was accomplished on an Agilent Extent C18 (50 × 2.1 mm, 1.8 μm) column at 30 °C. A linear gradient program was used, starting at 0 min from 10% pump B and maintaining 10% pump B over 1 min (pump A, water containing 0.1% (v/v) formic acid; pump B, acetonitrile) at a flow rate of 0.3 mL/min, at 1 min from 10% pump B to 95% pump B over 5 min, maintaining 95% pump B over 3 min, at 9 min from 95% pump B to 10% pump B over 0.1 min, and stopped at 12 min. The injection volume was 1 μL. The tandem mass spectrometric analysis was performed under the ESI− mode with the settings as follows: ISV, −5000 V; TEM, 500 °C; CUR, 35 psi; GS1, 50 psi; GS2, 50 psi; declustering potential (DP) 100 V; collision energy (CE), 5 V.
NMR data were collected on a Bruker Instruments Avance AV500 spectrometer (500 MHz) (Bruker Corporation, Billerica, MA, USA).
NMR data were collected on a Bruker Instruments Avance AV500 spectrometer (500 MHz) (Bruker Corporation, Billerica, MA, USA).
6
Characterization of Organic Compounds
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Mass spectral data (TOF-ESI-MS + ) were obtained from a Q-TOF Ultima spectrometer (Waters). 1 H (500 MHz) and 13 C NMR (125 MHz) spectra were run on a Bruker Avance AV-500 spectrometer using TMS as internal standard, chemical shifts being quoted in parts per million (ppm) . The solvents used to dissolve compounds for the NMR experiment were DMSO-d6, CD3OD or CDCl3; For column chromatography separations, silica gel Merck 60 was used. Thin-layer chromatography was performed on pre-coated Kieselgel 60 F254 aluminum sheets (Merck) and spots were detected under ultraviolet uorescence and then sprayed with 10% H2O-H2SO4 reagent, followed by heating at 105°C for 10 mins.
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