scholarly journals Dereplication of Natural Extracts Diluted in Glycerin: Physical Suppression of Glycerin by Centrifugal Partition Chromatography Combined with Presaturation of Solvent Signals in 13C-Nuclear Magnetic Resonance Spectroscopy

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.

1997 ◽  
Vol 766 (1-2) ◽  
pp. 255-260 ◽  
Author(s):  
Manfred Spraul ◽  
Ulrich Braumann ◽  
Jean-Hugues Renault ◽  
Philippe Thépenier ◽  
Jean-Marc Nuzillard

2019 ◽  
Vol 4 (1) ◽  
pp. 181
Author(s):  
Myrnille Joy B. Zabala ◽  
Lolita G. Lagurin ◽  
Fabian M. Dayrit

Vitex negundo has been known since ancient times as a medicinal plant. The objective of this study is to investigate the effect of methanol and ethanol extracts, and ethyl acetate, chloroform and aqueous fractions of Vitex negundo using an in vitro model to test glucose diffusion and to determine the phytochemical profile of the extracts and fractions using 13C nuclear magnetic resonance (NMR) spectroscopy. The chloroform fractions, ethyl acetate-EtOH and ethyl acetate-MeOH gave the highest inhibitory effect on both the diffusion activities in vitro. Retardation of glucose diffusion suggests that negundo has the potential to lower postprandial glucose. Correlation analysis of the 13C NMR profile with retardation activity suggests that compounds containing glycosidic residues may be responsible for the glucose retardation activity. This is the first example where activity has been correlated with specific structural features of compounds from a crude extract using 13C NMR chemical shifts to assist in the identification of active compounds.


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