1D- and 2D-NMR spectra (1H, 13C, HSQC, HMBC, COSY, and NOESY) were performed using Bruker Avance-NMR (600 and 800 MHz) spectrometers. All compounds were recorded in the solvent deuterochloroform (CDCl3).
Avance nmr
Manufactured by Bruker
Sourced in Switzerland, Germany
The Avance-NMR is a nuclear magnetic resonance (NMR) spectrometer developed by Bruker. It is designed to analyze the molecular structure and dynamics of chemical compounds. The Avance-NMR provides high-resolution data and advanced analytical capabilities for researchers and scientists working in various fields, including chemistry, biochemistry, and materials science.
Automatically generated - may contain errors
Lab products found in correlation
Ultimate 3000, by Thermo Fisher Scientific (1 mentions)
Esi q tof, by Bruker (1 mentions)
Vector 22 spectrophotometer, by Bruker (1 mentions)
P 2000 polarimeter, by Jasco (1 mentions)
Zncl2, by Merck Group (1 mentions)
Anhydrous dichloromethane, by Merck Group (1 mentions)
Hexadecyl isocyanate, by Merck Group (1 mentions)
Methanol, by Avantor (1 mentions)
Palmitoyl chloride, by Merck Group (1 mentions)
Hplc grade acetonitrile, by Avantor (1 mentions)
Milli q reference system, by Merck Group (1 mentions)
Chloroform hplc grade, by Carlo Erba (1 mentions)
Dspe peg2000, by Avanti Polar Lipids (1 mentions)
Triethylamine, by Merck Group (1 mentions)
Dexamethasone (dex), by Merck Group (1 mentions)
7 protocols using avance nmr
1
Comprehensive NMR Characterization of Compounds
2
Spectroscopic Characterization of Purified Compounds
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The infrared (IR) spectra of purified compounds 1 –3 were recorded on an FT-IR machine (Shimadzu-8900, Japan) using the KBR disc method. 1H and 13C-NMR spectra were recorded on Bruker Avance-NMR instruments (1H-NMR 400 and 500MHz, 13C-NMR 150 and 75 MHz) using CD3OD as a solvent. Multiplicities of carbon-13 signals were defined by using DEPT-90° and 135° experiments. HR-ESI-MS spectra of compounds 1 –3 were recorded on a mass spectrometer (ESI-QTOF, Bruker maXis II™, Bremen, Germany) coupled with reverse phase UPLC (Thermo ultimate-3000). 1H and 13C-NMR values for compounds 1 –3 are mentioned in Table 5 .
3
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.
4
NMR Spectroscopy of Serum Samples
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Five hundred microliters of thawed serum were mixed with 50 μl of 1 mM trimethylsilylpropionic acid (TSP, Sigma-Aldrich). (TSP served as a lock signal and chemical shift references (δ = 0.0)]. Sample pH measured ~8 and was not further adjusted. The sample was transferred to a 5mm NMR tube [13 (link)].
One-dimensional 1H-NMR spectra were acquired on a 700-MHz Bruker Avance NMR spectrometer with a 5-mm TXI proton-enhanced cryoprobe. A Carr-Purcell-Meiboom-Gill presaturation (CPMG) pulse sequence with a spectral width of 10 kHz was used to acquire all spectra with 128 scans, which were subsequently phase and baseline corrected [13 (link)]. Chemical shifts were assigned relative to the internal standard signal at 0 ppm.
One-dimensional 1H-NMR spectra were acquired on a 700-MHz Bruker Avance NMR spectrometer with a 5-mm TXI proton-enhanced cryoprobe. A Carr-Purcell-Meiboom-Gill presaturation (CPMG) pulse sequence with a spectral width of 10 kHz was used to acquire all spectra with 128 scans, which were subsequently phase and baseline corrected [13 (link)]. Chemical shifts were assigned relative to the internal standard signal at 0 ppm.
5
NMR Analysis and Cytotoxicity in HEK293 and HepG2 Cells
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Nuclear magnetic resonance (NMR): 1 H-, 13 C-NMR and all 2D spectra were recorded on an Avance NMR instrument (Bruker Daltonics, Bremen, Germany) operating at 400 MHz. Chemical shifts are reported as δ values (ppm) relative to an internal standard of tetramethylsilane (TMS) or to the solvent line of CDCl 3 ( δ H = 7.26 ppm, δ C = 77.16 ppm). a citotoxicidade destes compostos em células renais embrionárias humanas (HEK293) e células humanas de carcinoma hepatocelular (HepG2).
6
Isolation and Characterization of Bioactive Compounds
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Analytical grade Sigma-Aldrich product solvents, such as petroleum ether, n-hexane, chloroform, acetone, methanol, and ethyl acetate, were used for sequential extraction and column elution. Zinc (II) chloride, ZnCl 2 (Analytical grade Sigma-Aldrich) and standard antibiotic drug (gentamycin) were used. Mueller Hinton agar and saline solution were also used as a culture medium during antibacterial test. Rotary vapor, column chromatography, round bottom flask, electrical balance, volumetric flask, measuring cylinder, pestle and mortar, filter papers, weighing balances, water bath, Uv-tech-254 and 365 nm chamber were used. And 1D ( 1 H-NMR 500 MHz, 13 C-NMR (150 MHz), DEPT-135) and 2D (COSY, HSQC and HMBC) spectra were recorded on Bruker Avance NMR in deuterated solvent.
7
Dexamethasone Palmitate Nanoparticle Synthesis
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Palmitoyl chloride, dexamethasone, hexadecyl isocyanate, anhydrous dichloromethane, and triethyl amine were purchased from Sigma Aldrich (France). Hexadecyl chloroformate was obtained from Tokyo Chemical Industry, Co. LT (Japan). LDC1, LDC2, and LDC3 were synthesized as described below. DSPE-PEG 2000 was obtained from Avanti Polar Lipids, Inc. (USA). MilliQ reference system from Millipore (France) was used to purify water. Chloroform HPLC-grade (Carlo Erba Reagents, France), methanol, and acetonitrile HPLC-grade (VWR Chemicals, France) were used. NMR spectra were recorded on Bruker Avance-NMR (300, and 400 MHz) spectrometers in CDCl 3 . ESI-MS of compounds were measured on Thermofisher Scientific (LTQ, ion trap, H-ESI II). All experiments were performed in amber vials due to the photosensitivity of dexamethasone palmitate [28] (link)
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