All the solvents and reagents were reagent grade and used as received. Nicotinohydrazide, isonicotinohydrazide, 2-pyridinecarboxaldehyde, and Mn(NO 3 ) 2 • 4H 2 O were purchased from Aladdin Industrial Corporation (China). Superoxide Dismutase Assay Kit was purchased from Nanjing Jiancheng Bioengineering Insitute (China). N'-(pyridin-2-ylmethylene)nicotinohydrazide (L 1 ) and N'-(pyridin-2-ylmethylene)isonicotinohydrazide (L 2 ) were synthesized according to the literature. 16 The IR spectra were taken on a Vector 22 Bruker spectrophotometer (400-4000 cm -1 ) with KBr pellets. Elemental analyses for C, H and N were performed on a Perkin-Elmer 240C analyzer. 1 (link) H NMR spectra were measured on a Bruker AM 500 spectrometer.
Vector 22 spectrophotometer
Manufactured by Bruker
Sourced in Germany
The Vector 22 is a compact and versatile spectrophotometer designed for accurate absorbance measurements across a wide range of applications. It offers a wavelength range of 200 to 1100 nanometers and supports a variety of sample types and cuvette sizes. The instrument provides reliable and reproducible data for research, quality control, and routine analysis tasks.
Automatically generated - may contain errors
Lab products found in correlation
Am 500 spectrometer, by Bruker (2 mentions)
240c analyzer, by PerkinElmer (2 mentions)
Sephadex lh 20, by Cytiva (2 mentions)
Avance 300, by Bruker (2 mentions)
Escalab 250xi, by Thermo Fisher Scientific (2 mentions)
F 4500 fluorescence spectrophotometer, by Hitachi (1 mentions)
Cox 2, by Cell Signaling Technology (1 mentions)
Uv spectra, by Shimadzu (1 mentions)
Gel ods a hg, by YMC (1 mentions)
Am 400, by Bruker (1 mentions)
Nitric oxide kit, by Nanjing Jiancheng (1 mentions)
Fetal bovine serum (fbs), by Thermo Fisher Scientific (1 mentions)
Lipopolysaccharides (lps), by Merck Group (1 mentions)
Reactive oxygen species assay kit, by Beyotime (1 mentions)
P 2000 polarimeter, by Jasco (1 mentions)
Gemini nmr spectrometer, by Agilent Technologies (1 mentions)
Gcms qp1000 ex mass spectrometer, by Shimadzu (1 mentions)
Mercury vxr 300 nmr spectrometer, by Agilent Technologies (1 mentions)
Uv 2401 pc double beam spectrophotometer, by Shimadzu (1 mentions)
Delsa nano c particle analyzer, by Beckman Coulter (1 mentions)
27 protocols using vector 22 spectrophotometer
1
Synthesis and Characterization of Nicotinohydrazide Complexes
2
Spectroscopic Characterization of Compounds
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All the reactions were carried out under air atmosphere. All chemicals and solvents used in the synthesis were reagent grade without further purification.
The IR spectra were taken on a Vector22 Bruker spectrophotometer (400-4000 cm -1) with KBr pellets. NMR spectra were measured on a Bruker AM 500 spectrometer. Elemental analyses for C, H and N were performed on a Perkin-Elmer 240C analyzer. Fluorescence spectra were recorded on a Hitachi F-4500 fluorescence spectrophotometer.
The IR spectra were taken on a Vector22 Bruker spectrophotometer (400-4000 cm -1) with KBr pellets. NMR spectra were measured on a Bruker AM 500 spectrometer. Elemental analyses for C, H and N were performed on a Perkin-Elmer 240C analyzer. Fluorescence spectra were recorded on a Hitachi F-4500 fluorescence spectrophotometer.
3
Spectroscopic and Chromatographic Techniques
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The following technologies and materials were used in this research: UV spectra (Shimadzu, Kyoto, Japan); IR spectra (Bruker Vector 22 spectrophotometer, Bruker Optics GmbH, Ettlingen, Germany); Mass spectra (API QSTAR time-of-flight spectrometer, MDS Sciqaszex, Concord, Ontario, Canada). NMR spectra (Bruker AM-400, Bremerhaven, Germany); silica gel (200–300 and 300–400 mesh, Qingdao Marine Chemical Inc., China); Rp-18 gel (40–63 μm, Merck, Darmstadt, Germany); Sephadex LH-20 (20–150 μm, Amersham Biosciences, Uppsala, Sweden); YMC*GEL ODS-A-HG (50 μm, YMC Co. Ltd., Kyoto, Japan) (34 (link)).
The following reagents were used in this research: FBS (Gibco, Grand Island, NE, USA); DMEM, neutral red (Solarbio, Beijing, China); Nitric oxide kit (Nanjing Jiancheng Bioengineering Institute); IL-6 and TNF-α ELISA kit (Beijing 4A Biotech Co., Ltd., Beijing, China); Primer iNOS, TNF-α, IL-6 and COX-2 (Thermo Fisher Scientific, Shanghai, China); Reactive Oxygen Species Assay Kit (Beyotime Biotechnology, Shanghai, China); PrimeScriptTMRT reagent kit with gDNA Eraser kit and TB Green TM Ex TaqTM II (Tli RNadeH Plus, Accurate Biology, Hunan, China), Bulk kit (TaKaRa, Accurate Biology, Hunan, China); Antibody NF-κB p65, phospho-NF-κB p65, iNOS, COX-2, IκBα, and phospho-IκBα (Cell Signaling, Beverly, MA, USA); LPS (Sigma-Aldrich, St. Louis, MO, USA) (35 (link)).
The following reagents were used in this research: FBS (Gibco, Grand Island, NE, USA); DMEM, neutral red (Solarbio, Beijing, China); Nitric oxide kit (Nanjing Jiancheng Bioengineering Institute); IL-6 and TNF-α ELISA kit (Beijing 4A Biotech Co., Ltd., Beijing, China); Primer iNOS, TNF-α, IL-6 and COX-2 (Thermo Fisher Scientific, Shanghai, China); Reactive Oxygen Species Assay Kit (Beyotime Biotechnology, Shanghai, China); PrimeScriptTMRT reagent kit with gDNA Eraser kit and TB Green TM Ex TaqTM II (Tli RNadeH Plus, Accurate Biology, Hunan, China), Bulk kit (TaKaRa, Accurate Biology, Hunan, China); Antibody NF-κB p65, phospho-NF-κB p65, iNOS, COX-2, IκBα, and phospho-IκBα (Cell Signaling, Beverly, MA, USA); LPS (Sigma-Aldrich, St. Louis, MO, USA) (35 (link)).
4
Isolation and Characterization of Metenolone Acetate
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Metenolone acetate (1 ), (m/z = 344.2, C22H32O3), was procured from the Shenzhen Simeiquan Biotechnology Company Limited, China. Media constituents were acquired from VWR Chemicals (UK), Oxoid Limited (UK), Sigma-Aldrich (Germany), Scharlau Chemicals & Reagents (Spain), and Dae-Jung Chemicals & Metals Company Limited (Korea). Number of compounds, along with their purity, were determined on silica-coated (PF254) TLCs. Silica gel (70–230 mesh) column chromatography was performed for the fractionation of gummy crude materials. Fractions were fully-purified via recycling reverse phase HPLC (LC–908, YMC L-80) using acetonitrile/water. 1D, and 2D NMR of compounds 1 –14 were performed in deuterated-chloroform on the Bruker Avance-NMR (Bruker, Switzerland). FAB-, and HRFAB-MS were done on the mass spectrometer, Joel JMS H × 110 (Joel, Japan). Absorbances for compounds 2 –14 in the UV spectrum were noted on spectrophotometer, Evolution 300 UV–visible (Hitachi, Japan). Optical rotations (JASCO P–2000 polarimeter, JASCO, Japan), and melting points (Buchi 560 device, Buchi, Switzerland) were performed for compounds 2 –14 . Bruker Vector 22 spectrophotometer (Bruker, France) was used for IR data of metabolites.
5
Spectroscopic Analysis of Organic Compounds
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Melting points were measured with a Stuart
melting point apparatus and were uncorrected. The IR spectra were
recorded using a FTIR Bruker-vector 22 spectrophotometer as KBr pellets.
The 1H NMR spectra were recorded in DMSO-d6 as a solvent on a Varian Gemini NMR spectrometer at
300 MHz using TMS as the internal standard. Chemical shifts were reported
as δ values in ppm. Mass spectra were recorded with a Shimadzu
GCMS-QP-1000 EX mass spectrometer in an EI (70 eV) model. The elemental
analyses were performed at the Microanalytical Center at Cairo University.
melting point apparatus and were uncorrected. The IR spectra were
recorded using a FTIR Bruker-vector 22 spectrophotometer as KBr pellets.
The 1H NMR spectra were recorded in DMSO-d6 as a solvent on a Varian Gemini NMR spectrometer at
300 MHz using TMS as the internal standard. Chemical shifts were reported
as δ values in ppm. Mass spectra were recorded with a Shimadzu
GCMS-QP-1000 EX mass spectrometer in an EI (70 eV) model. The elemental
analyses were performed at the Microanalytical Center at Cairo University.
6
Characterization of Novel Compounds
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Melting points were measured with using a Stuart melting point apparatus and were uncorrected. The IR spectra were recorded using an FTIR Bruker-vector 22 spectrophotometer as KBr pellets. The 1H and 13C NMR spectra were recorded in DMSO-d6 as a solvent with Varian Mercury VXR-300 NMR spectrometer operating at 300 MHz and 75 MHz, using TMS as an internal standard. Chemical shifts were reported as δ values in ppm. Mass spectra were recorded with a Shimadzu GCMS-QP-1000 EX mass spectrometer in EI (70 eV) model. The elemental analyses were performed at the Micro Analytical Centre, Cairo University.
7
Characterization of Functionalized Polystyrenes
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The poly(St-VBC), poly(St-VBC)-NH2, and
poly(St-VBC)-NH2-SO3H were characterized using
FT-IR spectroscopy (Bruker vector 22 spectrophotometer, Germany) by
preparing their KBr pellets from 400 to 4000 cm–1. The samples were dried before characterization with a vacuum oven
at 60 °C for 24 h.
poly(St-VBC)-NH2-SO3H were characterized using
FT-IR spectroscopy (Bruker vector 22 spectrophotometer, Germany) by
preparing their KBr pellets from 400 to 4000 cm–1. The samples were dried before characterization with a vacuum oven
at 60 °C for 24 h.
8
Structural Characterization of Polysaccharides
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EPSR3 FTIR spectra were obtained using KBr pellets (2.0 mg sample and 200 mg KBr, respectively, using the FTIR-UNIT Bruker Vector 22 Spectrophotometer), as described in the paper [51 ]. The m-hydroxybiphenyl colorimetric technique was used to identify uronic acids at 525 nm [52 (link)]. The turbidity technique determined sulfate [53 (link)]. The monosaccharide composition was defined (Agilate Pack, serics1, 200), using an Aminex carbohydrate HP-87C column (300 × 7.8 mm) and 0.5 mL/min deionized water as the mobile phase [54 (link)]. High-performance chromatography (HPLC, Agilent 1100 Series System, Hewlett-Packard, Germany) with refractive index (RI) detection was used to measure the average molecular weight (Mw). The Mw/Mn ratio was used to construct the polydispersity index (PI) [55 (link)].
9
Structural Elucidation of Bioactive Compound
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The elucidation of the chemical structures of the promising active compound had been done using several instruments as infrared (FTIR), mass, nuclear magnetic resonance (NMR) and UV spectroscopy. An IR spectrum of the pure compound was performed with KBr pellets, 2.0 mg sample and 200 mg KBr using the FTIR-UNIT Bruker Vector 22 Spectrophotometer. NMR (1H and 13C NMR) were obtained on JEOL-ECA 500 MHz spectrometer using TMS as internal standard, the chemical shifts were expressed in d (ppm) and coupling constants J in Hz. Mass spectra were recorded on thermo scientific-trace GC Ultra, USA. Coupled with single quadrupole MS, temperature (0–300 °C) and UV spectroscopy were recorded on a Shimadzu UV-2401 PC double beam spectrophotometer using 1.0 cm quartz cells according to Paterson and Kemmelmeier 31. These experiments were carried out in central services laboratory at National Research Centre, Egypt.
10
NMR, IR, and Optical Characterization
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1H and 13C NMR spectra were recorded on a Bruker Fourier transform 400 NMR spectrometer at 25oC using CDCl3 as solvent and were calibrated referencing residual undeuterated solvent as an internal reference (1H NMR = 7.26, 13C NMR = 77.16). All chemical shifts were given in ppm and coupling constants (J) in Hz. The following abbreviations or combinations thereof were used to explain the multiplicities: s = singlet, t = triplet, m = multiplet. IR spectra were recorded on a Bruker Vector 22 spectrophotometer as KBr pellets. High resolution mass spectra (HRMS) were recorded on an Agilent 6224 TOF LC/MS spectrometer using ESI-TOF (electrospray ionization-time of flight). Absorption spectra were acquired using a Hitachi U-3010 spectrophotometer. Fluorescence measurements were carried out on a Perkin-Elmer LS 45 fluorescence spectrometer. Dynamic light scattering (Beckman-Coulter DelsaTM Nano-C particle analyzer) was used to determine the size of the aggregated particle colloids in aqueous solution.
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