Reagents and anhydrous solvents were purchased from Sigma-Aldrich (St. Louis, MO, USA) or Alfa Aesar (Tewksbury, MA, USA). All other chemicals were used without purification unless otherwise noted. NMR spectra were acquired on a JEOL 400 MHz NMR spectrometer (JEOL, Peabody, MA, USA) with chloroform-d1 (δH = 7.26 ppm δC = 77.23 ppm) or acetone-d6 (δH = 2.05 ppm δC = 206.26 ppm). All coupling constants were generated by the MestReNova (Version 11.0, Mestrelab, Santiago de Compostela, Spain) program and were uncorrected. Chromatography was performed with Biotage KP-SIL™ (Biotage USA, Charlotte, NC, USA) or KP-NH™ (Biotage USA, Charlotte, NC, USA) cartridges or Silicycle silica gel (porosity = 60 Å, particle size 40–63 μm). Microwave reactions were run on the Discover Microwave System by CEM Corporation (Matthews, NC, USA). HRMS was acquired with an Agilent 7200 GC/QTOF (Agilent Technologies, Santa Clara, CA, USA) or Bruker Bio TOF II (Bruker, Billerica, MA, USA) with Electrospray Ionization.
400 mhz nmr spectrometer
Manufactured by JEOL
Sourced in Japan
The 400 MHz NMR spectrometer is a high-performance analytical instrument designed for nuclear magnetic resonance spectroscopy. It operates at a frequency of 400 MHz, allowing for the analysis of chemical samples to identify and characterize their molecular structures.
Automatically generated - may contain errors
Lab products found in correlation
Deuterated solvent, by Merck Group (3 mentions)
Ftir spectrometer, by PerkinElmer (3 mentions)
Anhydrous solvents, by Merck Group (2 mentions)
Dichloromethane, by Merck Group (2 mentions)
Human serum, by Merck Group (2 mentions)
Agilent 7200 gc qtof, by Agilent Technologies (1 mentions)
Deuterium oxide, by Merck Group (1 mentions)
Toluene, by Merck Group (1 mentions)
Acetonitrile, by Merck Group (1 mentions)
Melting point m 560 apparatus, by Büchi (1 mentions)
V 630 uv vis spectrophotometer, by Jasco (1 mentions)
Nicolet is10 spectrometer, by Thermo Fisher Scientific (1 mentions)
Inosine, by Thermo Fisher Scientific (1 mentions)
Nicolet is10 ft ir spectrometer, by Thermo Fisher Scientific (1 mentions)
Agilent cary eclipse fluorescence spectrophotometer, by Agilent Technologies (1 mentions)
Erythro 9 2 hydroxy 3 nonyl adenine, by Merck Group (1 mentions)
Terbium 3 chloride hexahydrate, by Thermo Fisher Scientific (1 mentions)
Microtof q 2 mass spectrometer, by Bruker (1 mentions)
Acetone d6, by Merck Group (1 mentions)
Nh4pf6, by Merck Group (1 mentions)
20 protocols using 400 mhz nmr spectrometer
1
Detailed NMR and Chromatography Methods
2
Synthesis and Characterization of Novel Compounds
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At El-Gomhouria Company
for Drugs in Egypt, all the chemicals were readily available for purchase,
and they were all used without additional purification. The uncorrected
melting points were all determined in open-glass capillaries using
a Griffin melting point equipment. On a Perkin Elmer 1430 infrared
spectrophotometer, IR spectra were captured. At Sohag University in
Egypt, 1H NMR and 13C NMR spectra were recorded
using a Jeol-400 MHz NMR-spectrometer (DMSO-d6) and CDCl3 (see theSupporting Information ). Tetramethylsilane (TMS) is used as an internal
standard, and the chemical shifts are presented in ppm downfield.
The Vario El Fab-Nr elemental analyzer underwent micro studies. A
Hewlett Packard 5988 spectrometer was used to record the mass spectra
(Microanalysis Center, Cairo University, Egypt). It was done by using
TLC to monitor the reactions.
for Drugs in Egypt, all the chemicals were readily available for purchase,
and they were all used without additional purification. The uncorrected
melting points were all determined in open-glass capillaries using
a Griffin melting point equipment. On a Perkin Elmer 1430 infrared
spectrophotometer, IR spectra were captured. At Sohag University in
Egypt, 1H NMR and 13C NMR spectra were recorded
using a Jeol-400 MHz NMR-spectrometer (DMSO-d6) and CDCl3 (see the
standard, and the chemical shifts are presented in ppm downfield.
The Vario El Fab-Nr elemental analyzer underwent micro studies. A
Hewlett Packard 5988 spectrometer was used to record the mass spectra
(Microanalysis Center, Cairo University, Egypt). It was done by using
TLC to monitor the reactions.
3
Polysaccharide NMR Analysis Protocol
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The polysaccharides were dried for 72 h in a vacuum dryer filled with silica gel and then dissolved in 0.6 mL deuterium oxide (D2O). The 1H NMR spectra of eight samples were performed on a JEOL 400 MHz NMR spectrometer. All NMR data were analysed using MestReNova software.
4
Quantifying Methacrylation Degree in Gelatins
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To determine the degree of substitution, the alternation in the amounts of primary amino functional groups of gelatins before and after methacrylation was quantitatively measured as suggested by a previous report [32 (link)]. To this end, a ninhydrin test (Sigma-Aldrich, St. Louis, MO, USA) was used according to the manufacturer’s instructions. Both gelatin and GelMa were dissolved in deionized water, after which ninhydrin solution was dripped into the solutions and allowed to react for 10 min in an oven. An amount of 500 μL of pure ethanol was used to stop the reaction, and the absorbance was measured at a wavelength of 570 nm. Glycine, with its known wavelength among the various amino groups, was used as the comparison group. In addition, 1H NMR was used to determine for the degree of substitution. Both gelatin and GelMa were dissolved in deuterium oxide (Sigma-Aldrich) and analyzed using a 400 MHz NMR spectrometer (JEOL Co. Ltd., Tokyo, Japan). The degree of substitution was calculated using the following formula [33 (link)]:
5
Synthesis and Characterization of Iron-Naphthalene Complexes
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All the experiments were carried out under an inert atmosphere using Schlenk techniques unless otherwise specified. Complex [Fe 2 (CO) 6 (µ-naphthalene-2-thiolate) 2 ] 1 was prepared according to the reported procedure. 25 All the anhydrous solvents (dichloromethane, acetonitrile and toluene) and starting materials were obtained from Sigma-Aldrich and used without further purification. The deuterated solvents were also obtained from Sigma-Aldrich. The 1 H and 31 P NMR spectra were recorded at room temperature in CDCl 3 solution with a JEOL 400 MHz NMR Spectrometer. FTIR spectra were recorded from dichloromethane solutions of the samples over the range of 400-4000 cm -1 on a Perkin Elmer FTIR Spectrometer. The UV-Vis spectra for complex 1 were recorded on a PerkinElmer Lambda-25 spectrophotometer and for complex 2 on an Avantes The elemental analyses were carried out with a Vario Micro Cube elemental analyzer.
6
Synthesis and Characterization of Fe2(CO)6(μ-Mebdt) Complex
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All of the experiments were carried
out in an inert atmosphere using Schlenk techniques unless otherwise
specified. [Fe2(CO)6(μ-Mebdt)] was prepared
according to the procedure reported in literature.49 (link) All of the starting materials and anhydrous solvents were
obtained from Sigma-Aldrich and used without any further purification.
The deuterated solvents were also obtained from Sigma-Aldrich. The 1H and 31P NMR spectra were recorded at room temperature
in CDCl3 with a JEOL 400 MHz NMR spectrometer. The FTIR
spectra were recorded from dichloromethane and acetonitrile solutions
of the samples over the range of 400–4000 cm–1 on a PerkinElmer FTIR spectrometer. The UV–vis spectra for
the complexes1 and 2 were recorded on a
PerkinElmer Lambda-25 spectrophotometer. The elemental analyses were
carried out with a Vario Micro Cube elemental analyzer.
out in an inert atmosphere using Schlenk techniques unless otherwise
specified. [Fe2(CO)6(μ-Mebdt)] was prepared
according to the procedure reported in literature.49 (link) All of the starting materials and anhydrous solvents were
obtained from Sigma-Aldrich and used without any further purification.
The deuterated solvents were also obtained from Sigma-Aldrich. The 1H and 31P NMR spectra were recorded at room temperature
in CDCl3 with a JEOL 400 MHz NMR spectrometer. The FTIR
spectra were recorded from dichloromethane and acetonitrile solutions
of the samples over the range of 400–4000 cm–1 on a PerkinElmer FTIR spectrometer. The UV–vis spectra for
the complexes
PerkinElmer Lambda-25 spectrophotometer. The elemental analyses were
carried out with a Vario Micro Cube elemental analyzer.
7
Characterization of Organic Compounds
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Chemical reagents were purchased from commercial sources (Sigma-Aldrich, Tokyo Chemical Industry, and Duksan Pure Chemical, Korea) and used without further purification. Human serum was purchased from Sigma-Aldrich. 1H and 13C nuclear magnetic resonance (NMR) spectra were recorded using a JEOL 400 MHz NMR spectrometer. High-resolution mass spectra (HRMS) were recorded using a Bruker Impact II quadruple time-of-flight (QToF) mass spectrometer with an electrospray ionization (ESI) source. Melting point analysis was performed using a Büchi M-560 melting point apparatus. The fluorescence spectra were recorded using an Agilent Cary Eclipse fluorescence spectrophotometer, and absorbance spectra were recorded on a JASCO V-630 UV-Vis spectrophotometer. Fourier-transform infrared (FTIR) spectra were recorded on a Thermo Scientific NICOLET iS10 spectrometer using a KBr disc (Thermo Scientific, 25 × 4 mm).
8
Spectroscopic Enzyme Assays with Reagents
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Chemical reagents were purchased from commercial sources and, unless otherwise stated, were used without further purification. For enzyme assay, hexokinase (HK, EC 2.7.1.1) and creatine kinase (CK, EC 2.7.3.2) were purchased from Sigma Aldrich. Florescence spectra were recorded on an Agilent Cary Eclipse fluorescence spectrometer using a 1 cm path length quartz cell. 1H NMR spectrums were recorded on a JEOL 400 MHz NMR spectrometer.
9
Adenosine Deaminase Activity Assay
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For the enzyme assay, ADA (from calf intestine) and erythro-9-(2-hydroxy-3-nonyl)adenine (EHNA) were purchased from Sigma-Aldrich. Adenosine, inosine, and terbium(III) chloride hexahydrate (TbCl3·6H2O) were purchased from Alfa Aesar and all reagents were used without further purification.
Luminescence spectra were obtained via Agilent Cary Eclipse Fluorescence Spectrophotometer (Agilent, Santa Clara, CA, USA). FT-IR spectra were obtained using a Thermo Scientific Nicolet iS10 FT-IR spectrometer (Thermo Fisher Scientific, Waltham, MA, USA). NMR spectra were recorded using a JEOL (400 MHz) NMR spectrometer (JEOL Ltd., Tokyo, Japan).
Luminescence spectra were obtained via Agilent Cary Eclipse Fluorescence Spectrophotometer (Agilent, Santa Clara, CA, USA). FT-IR spectra were obtained using a Thermo Scientific Nicolet iS10 FT-IR spectrometer (Thermo Fisher Scientific, Waltham, MA, USA). NMR spectra were recorded using a JEOL (400 MHz) NMR spectrometer (JEOL Ltd., Tokyo, Japan).
10
Synthesis and Characterization of MGTP-HSA Complex
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All chemicals
were purchased from Spectrochem and Sigma-Aldrich and were used as
received.MGZ was synthesized by the reported procedure
given in Supporting InformationSection S2 . Thin-layer chromatography was performed on aluminum sheets coated
with silica gel 60F254 (Merk, Darmstadt). Deionized water was obtained
from an ULTRA UV/UF Rions Lab Water system Ultra 370 series. NMR spectra
were recorded on a JEOL 400 MHz NMR spectrometer with TMS as the internal
standard. Mass spectra were obtained from a mass Bruker micro TOF
QII mass spectrometer. Absorption spectra were recorded on a SHIMADZU-2450
spectrometer equipped with a Peltier system as the temperature controller.
Fluorescence spectra were recorded on a Fluorolog Horiba scientific
model: FL-1039A/40A. Quartz cuvettes of 1 cm path length were used
for the absorbance and fluorescence measurements. Dynamic light scattering
(DLS) measurements were performed at 25.0 + 0.1 °C using a Zetasizer
nano ZS instrument. The details of preparation of stock solutions,
recording of UV–visible and fluorescence spectra, DLS studies,
determination of the detection limit and binding constants, and stoichiometry
and drug binding studies ofMGTP –HSA with warfarin,
ibuprofen, and bilirubin are given in theSupporting Information
were purchased from Spectrochem and Sigma-Aldrich and were used as
received.
given in Supporting Information
with silica gel 60F254 (Merk, Darmstadt). Deionized water was obtained
from an ULTRA UV/UF Rions Lab Water system Ultra 370 series. NMR spectra
were recorded on a JEOL 400 MHz NMR spectrometer with TMS as the internal
standard. Mass spectra were obtained from a mass Bruker micro TOF
QII mass spectrometer. Absorption spectra were recorded on a SHIMADZU-2450
spectrometer equipped with a Peltier system as the temperature controller.
Fluorescence spectra were recorded on a Fluorolog Horiba scientific
model: FL-1039A/40A. Quartz cuvettes of 1 cm path length were used
for the absorbance and fluorescence measurements. Dynamic light scattering
(DLS) measurements were performed at 25.0 + 0.1 °C using a Zetasizer
nano ZS instrument. The details of preparation of stock solutions,
recording of UV–visible and fluorescence spectra, DLS studies,
determination of the detection limit and binding constants, and stoichiometry
and drug binding studies of
ibuprofen, and bilirubin are given in the
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