Nuclear magnetic resonance monitoring of centrifugal partition chromatography in pH-zone-refining mode

1997 ◽  
Vol 766 (1-2) ◽  
pp. 255-260 ◽  
Author(s):  
Manfred Spraul ◽  
Ulrich Braumann ◽  
Jean-Hugues Renault ◽  
Philippe Thépenier ◽  
Jean-Marc Nuzillard
Molecules ◽  
2020 ◽  
Vol 25 (21) ◽  
pp. 5061
Author(s):  
Marine Canton ◽  
Jane Hubert ◽  
Stéphane Poigny ◽  
Richard Roe ◽  
Yves Brunel ◽  
...  

For scientific, regulatory, and safety reasons, the chemical profile knowledge of natural extracts incorporated in commercial cosmetic formulations is of primary importance. Many extracts are produced or stabilized in glycerin, a practice which hampers their characterization. This article proposes a new methodology for the quick identification of metabolites present in natural extracts when diluted in glycerin. As an extension of a 13C nuclear magnetic resonance (NMR) based dereplication process, two complementary approaches are presented for the chemical profiling of natural extracts diluted in glycerin: A physical suppression by centrifugal partition chromatography (CPC) with the appropriate biphasic solvent system EtOAc/CH3CN/water 3:3:4 (v/v/v) for the crude extract fractionation, and a spectroscopic suppression by presaturation of 13C-NMR signals of glycerin applied to glycerin containing fractions. This innovative workflow was applied to a model mixture containing 23 natural metabolites. Dereplication by 13C-NMR was applied either on the dry model mixture or after dilution at 5% in glycerin, for comparison, resulting in the detection of 20 out of 23 compounds in the two model mixtures. Subsequently, a natural extract of Cedrus atlantica diluted in glycerin was characterized and resulted in the identification of 12 metabolites. The first annotations by 13C-NMR were confirmed by two-dimensional NMR and completed by LC-MS analyses for the annotation of five additional minor compounds. These results demonstrate that the application of physical suppression by CPC and presaturation of 13C-NMR solvent signals highly facilitates the quick chemical profiling of natural extracts diluted in glycerin.


1962 ◽  
Vol 40 (12) ◽  
pp. 2394-2401 ◽  
Author(s):  
R. U. Lemieux ◽  
A. G. McInnes

The composition of the sucrose monomyristate which is obtained by reaction of sucrose with methyl myristate in dimethylformamide and in the presence of a basic catalyst was established by application of gas–liquid partition chromatography and nuclear magnetic resonance spectroscopy to appropriate derivatives. The substance is a mixture of 6′-myristoyl sucrose, 6-myristoyl sucrose, and unidentified isomeric esters in the relative proportions of 0.62:0.28:0.10, respectively.


Author(s):  
M.J. Hennessy ◽  
E. Kwok

Much progress in nuclear magnetic resonance microscope has been made in the last few years as a result of improved instrumentation and techniques being made available through basic research in magnetic resonance imaging (MRI) technologies for medicine. Nuclear magnetic resonance (NMR) was first observed in the hydrogen nucleus in water by Bloch, Purcell and Pound over 40 years ago. Today, in medicine, virtually all commercial MRI scans are made of water bound in tissue. This is also true for NMR microscopy, which has focussed mainly on biological applications. The reason water is the favored molecule for NMR is because water is,the most abundant molecule in biology. It is also the most NMR sensitive having the largest nuclear magnetic moment and having reasonable room temperature relaxation times (from 10 ms to 3 sec). The contrast seen in magnetic resonance images is due mostly to distribution of water relaxation times in sample which are extremely sensitive to the local environment.


Author(s):  
Paul C. Lauterbur

Nuclear magnetic resonance imaging can reach microscopic resolution, as was noted many years ago, but the first serious attempt to explore the limits of the possibilities was made by Hedges. Resolution is ultimately limited under most circumstances by the signal-to-noise ratio, which is greater for small radio receiver coils, high magnetic fields and long observation times. The strongest signals in biological applications are obtained from water protons; for the usual magnetic fields used in NMR experiments (2-14 tesla), receiver coils of one to several millimeters in diameter, and observation times of a number of minutes, the volume resolution will be limited to a few hundred or thousand cubic micrometers. The proportions of voxels may be freely chosen within wide limits by varying the details of the imaging procedure. For isotropic resolution, therefore, objects of the order of (10μm) may be distinguished.Because the spatial coordinates are encoded by magnetic field gradients, the NMR resonance frequency differences, which determine the potential spatial resolution, may be made very large. As noted above, however, the corresponding volumes may become too small to give useful signal-to-noise ratios. In the presence of magnetic field gradients there will also be a loss of signal strength and resolution because molecular diffusion causes the coherence of the NMR signal to decay more rapidly than it otherwise would. This phenomenon is especially important in microscopic imaging.


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