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Tuesday 16 December 2014

Real-time separation of natural products by ultrafast 2D NMR coupled to on-line HPLC

 

Hyphenated HPLC-NMR is an extremely efficient analytical tool, which makes it possible to perform on-flow experiments where 1D NMR spectra are obtained in real time as the analytes are separated and eluted from the chromatographic column. However, it is incompatible with multidimensional NMR methods that form an indispensible tool for the study of complex mixtures. Recently, Frydman and co-workers have proposed an ultrafast 2D NMR approach, where a complete 2D NMR correlation can be recorded in a single scan, thus providing a solution to the irreversibility of hyphenated techniques. This paper presents the first implementation of on-line ultrafast HPLC-NMR. Ultrafast COSY spectra are acquired every 12 s in the course of a chromatographic run performed on a mixture of natural aromatic compounds. The results, obtained on a commercial HPLC-NMR setup, highlight the generality of the ultrafast HPLC-NMR methodology, thus opening the way to a number of applications in the numerous fields in which HPLC-NMR forms a routine analytical tool.


Graphical abstract: Real-time separation of natural products by ultrafast 2D NMR coupled to on-line HPLC 

Real-time separation of natural products by ultrafast 2D NMR coupled to on-line HPLC

*Corresponding authors
aLaboratório de Ressonância Magnética Nuclear—Departamento de Química, Universidade Federal de São Carlos (UFSCar), Rod. Washington Luís, Km 235, C.P. 676, São Carlos, Brazil
bLaboratory of Pharmacognosy and Pharmaceutical Analysis, Department of Pharmaceutical Sciences, University of Antwerp, Universiteitsplein 1, B-2610 Antwerp, Belgium
cUniversité de Nantes, CNRS, Chimie et Interdisciplinarité: Synthèse, Analyse, Modélisation (CEISAM) UMR 6230, Faculté des Sciences, B.P. 92208, 2 rue de la Houssinière, 44322 Nantes Cedex 03, France
E-mail: patrick.giraudeau@univ-nantes.fr;
Fax: +33(0)2 51 12 57 12 ;
Tel: +33(0)2 51 12 57 09
Analyst, 2012,137, 2357-2361

DOI: 10.1039/C2AN16208C 
 http://pubs.rsc.org/en/content/articlelanding/2012/an/c2an16208c#!divAbstract




 
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