The largest database of trusted experimental protocols

9 protocols using 500 mhz nmr

1

Analytical Characterization of Bioactive Compounds

Check if the same lab product or an alternative is used in the 5 most similar protocols
RAW 264.7 murine macrophage cells (ATCC®TIB-71™) and Nrf2-luciferase reporter MCF7 stable cells (SL-0010) were purchased from American Type Culture Collection (ATCC, Mannasas, VA, USA) and Signosis, Inc. (Santa Clara, CA, USA), respectively. Solid-phase extraction (SPE) was carried out using pre-packed Strata® SPE-C18 (1 g/6 mL, 55 µm) cartridges (Phenomenex, Torrance, CA, USA). Reversed-phase high performance liquid chromatography (RP-HPLC) was performed using Shimadzu Prominence LC-20AT equipped with an SPD-M20A photo-diode array (PDA) detector and Phenomenex Synergi Hydro-RP column (4 µm, 80 Å, 250 × 10 mm). Low resolution mass analysis was carried out on a Shimadzu LCMS-8040 triple quadrupole mass spectrometer equipped with electrospray ionization (ESI) ion source detector using a linear gradient 5–100% aq. CH3CN with 0.1% (v/v) formic acid. High resolution mass analysis was carried out on Waters Xevo® G2-XS Quadrupole Time-of-Flight (QToF) mass spectrometer equipped with ESI ion source detector using a linear gradient 5–100% aq. CH3CN with 0.1% (v/v) formic acid. The 1D- and 2D-NMR spectra were recorded on a Varian 500 MHz NMR equipped with a 3 mm probe. Statistical analyses were carried using GraphPad Prism version 9.3.1 for Windows, GraphPad Prism Software (San Diego, CA, USA).
+ Open protocol
+ Expand
2

Quantifying Residual PEG in Fiber Mats

Check if the same lab product or an alternative is used in the 5 most similar protocols
1H-NMR spectra of the fiber mats were obtained using a 500 MHz NMR (Varian, Palo Alto, CA, USA) to quantify the percent of residual PEG after washing. To obtain the NMR spectra, PEG was dissolved in D2O and others were dissolved in DMSO-d6. DSC scans of the mats were obtained using a Mettler DSC 823e instrument (Mettler Toledo Inc., Columbus OH, USA). The heating rate was 10 °C min−1.30 (link) Heat of fusion was determined from the DSC scans as the area under the melting peak using a base line extending to ~10 °C on either side of the PEG melting peak at 60 °C.
+ Open protocol
+ Expand
3

NMR Analysis of Organophosphorus Compounds

Check if the same lab product or an alternative is used in the 5 most similar protocols
The NMR samples were
prepared under a purified N2 atmosphere with dried, oxygen-free
THF.90 For 31P NMR, nondeuterated
THF90 was used while disabling the lock
function. The 13C and 31P NMR measurements were
performed with routine pulse programs and proton decoupling. The samples
were measured on a Varian 500 MHz NMR with the external standard ClPPh2 (neat liquid, δ(31P) = +81.92 ppm) for 31P and the solvent signals for 13C. The 31P NMR spectra were typically obtained with satisfactory S/N ratio
with 128 or 256 scans. Line broadening factors of up to 10 Hz were
applied as needed.
+ Open protocol
+ Expand
4

Synthesis of Metal Salt Solutions

Check if the same lab product or an alternative is used in the 5 most similar protocols
Chemicals or metal salts were purchased from Sigma Aldrich, Acros organics, Alfa Aeser or LPS solution and used without further purification unless described. 1H-NMR spectra were collected with Varian 500 MHz NMR using CDCl3 or CD3OD solvents. All metal salts were prepared by dissolving metal chloride (MnCl2, CoCl2·6H2O, NiCl2·6H2O, CuCl2·2H2O, ZnCl2, NaCl, LiCl) in ddH2O. All aqueous solutions were prepared with ddH2O and filtered with 0.22 μm syringe-filters before usage.
+ Open protocol
+ Expand
5

Characterization of Conulothiazoles via NMR

Check if the same lab product or an alternative is used in the 5 most similar protocols
Optical rotations were measured using a Jasco P-200 polarimeter. UV spectra were measured using a Beckman Coulter DU-800 spectrophotometer. ECD spectra were recorded on a Jasco J-715 spectrophotometer using a 1-mm cell. NMR spectra were determined on Varian Unity Inova spectrometers at 700 MHz; chemical shifts were referenced to the residual solvent signal (CD3OD: δH 3.31, δC 49.00). Other NMR data were recorded using a Bruker 800 MHz NMR and a Varian 500 MHz NMR; chemical shifts were referenced to the residual solvent signal (DMSO-d6: δH 2.51, δC 39.5). For an accurate measurement of the coupling constants, the one-dimensional 1H NMR spectra were transformed at 64 K points (digital resolution: 0.09 Hz). Through-space 1H connectivities were evidenced using a ROESY or NOESY experiment with a mixing time of 450 ms. The HSQC spectra were optimized for 1JCH = 142 Hz, and the HMBC experiments for 2 (link),3 JCH = 8.3 Hz. HRESIMS analysis of the new conulothiazoles was performed using an AB SCIEX TripleTOF 4600 mass spectrometer with Analyst TF software. High performance liquid chromatography (HPLC) separations were achieved on an Agilent 1260 Infinity Quaternary LC apparatus equipped with a Diode-Array Detector (DAD). The new conulothiazoles were isolated using a Dionex UltiMate 3000 HPLC system each equipped with a micro vacuum degasser, an autosampler, and a DAD.
+ Open protocol
+ Expand
6

NMR Characterization of TNT-APTES Complexes

Check if the same lab product or an alternative is used in the 5 most similar protocols
Samples of 750 µL of 5 mM TNT, APTES, and TNT - APTES complex in d6 - Acetone were recorded with the Varian 500 MHz NMR. The TNT - APTES complex samples were in 1:1, 1:2, and 1:3 mole ratios.
+ Open protocol
+ Expand
7

Ammonium Bicarbonate Buffers for Reverse Phase Chromatography

Check if the same lab product or an alternative is used in the 5 most similar protocols
Ammonium bicarbonate buffers used for analytical and preparative reverse phase chromatography were prepared and adjusted to pH 7 upon addition of the appropriate amount of acetic acid. All compounds purified by reversed phase chromatography were lyophilized to remove buffer and acetonitrile. Compounds were lyophilized for no fewer than two days. Reactions were monitored with a Waters Acquity H Class UPLC equipped with PDA detector and SQ mass detector using a Waters UPLC BEH C18 1.7 μm, 2.1 X 50 mm column. Reverse phase preparative chromatography was performed on a Biotage Isolera One utilizing SNAP Ultra C18 columns. 1H NMR were obtained on an Agilent 500 MHz NMR. All experiments were conducted at 25°C.
+ Open protocol
+ Expand
8

Synthesis and Characterization of Ester-Protected Amino Acids

Check if the same lab product or an alternative is used in the 5 most similar protocols
Ester protected valine, alanine and phenylalanine in l- and d- configurations were purchased from Sigma Aldrich (Castle Hill, NSW, Australia). All other protected amino acids were purchased from Fluorochem (Derbyshire, United Kingdom). General reagents and anhydrous solvents were purchased from Sigma Aldrich and Astatech (Bristol, USA). Reactions were monitored by thin-layer chromatography (TLC) using silica gel 60 F254 plates. TLC plates were visualised with UV light and potassium permanganate TLC stain. Reaction products were purified by dry column vacuum chromatography on silica gel using gradient elutions. 1H and 13C NMR spectra were recorded on an Agilent 500 MHz NMR. Spectra were referenced internally to residual solvent (CDCl3; 1H δ 7.26, 13C δ 77.10. DMSO-d6; 1H δ 2.49, 13C δ 39.52). High resolution mass spectra (HRMS) were recorded on an Agilent Technologies 6510 Q-TOF LCMS. The purity of all test compounds was confirmed to be >95% by absolute quantitative NMR (see Supporting Information for further details).
+ Open protocol
+ Expand
9

Synthesis and Characterization of Monounsaturated Fatty Acids

Check if the same lab product or an alternative is used in the 5 most similar protocols
(Z)-hexadec-13-enoic acid and (Z)-octadec-15-enoic acid were prepared by our previously reported procedures 39, 40 . (E)-octadec-9-enoic acid was purchased from Chemsupply (Gillman, SA, Australia). (Z)-hexadec-9-enoic acid, (Z)-octadec-11-enoic acid, (E)-octadec-11-enoic acid, (Z)-octadec-6-enoic acid and all other reagents and anhydrous solvents were purchased from Sigma Aldrich (Castle Hill, NSW, Australia).
Non-commercially available MUFAs were synthesised as described in the supporting information. The purity of all test compounds (3 -20) was confirmed by elemental analysis carried out in the Campbell Microanalytical Laboratory at the Department of Chemistry, University of Otago. All values were within ±0.4% of the calculated values.
Dry Column Vacuum Chromatography (DCVC) was used to purify reaction products on silica gel with gradient elutions. TLC was performed on silica gel 60 F254 plates. 1 H and 13 C NMR spectra were recorded on an Agilent 500 MHz NMR. Spectra were referenced internally to residual solvent (CDCl3; 1 H  7.26, 13 C  77.10. d6-DMSO; 1 H  2.49, 13 C  39.52). High resolution mass spectra were recorded on Agilent 6510 Q-TOF LC/MS.
+ Open protocol
+ Expand

About PubCompare

Our mission is to provide scientists with the largest repository of trustworthy protocols and intelligent analytical tools, thereby offering them extensive information to design robust protocols aimed at minimizing the risk of failures.

We believe that the most crucial aspect is to grant scientists access to a wide range of reliable sources and new useful tools that surpass human capabilities.

However, we trust in allowing scientists to determine how to construct their own protocols based on this information, as they are the experts in their field.

Ready to get started?

Sign up for free.
Registration takes 20 seconds.
Available from any computer
No download required

Sign up now

Revolutionizing how scientists
search and build protocols!