Magn Reson Chem. 2016 Oct;54(10):815-820. doi: 10.1002/mrc.4459. Epub 2016 Jun 07.

Matrix-assisted diffusion-ordered spectroscopy: choosing a matrix.

Magnetic resonance in chemistry : MRC

Nilce V Gramosa, Nágila M S P Ricardo, Ralph W Adams, Gareth A Morris, Mathias Nilsson

PMID: 27272403 PMCID: PMC5031188 DOI: 10.1002/mrc.4459

Abstract

Diffusion-ordered spectroscopy (DOSY) is an important technique for separating the NMR signals of the components in a mixture, and relies on differences in diffusion coefficient. Standard DOSY experiments therefore struggle when the components of a mixture are of similar size, and hence diffuse at similar rates. Fortunately, the diffusion coefficients of solutes can be manipulated by changing the matrix in which they diffuse, using matrix components that interact differentially with them, a technique known as matrix-assisted DOSY. In the present investigation, we evaluate the performance of a number of new, previously used, and mixed matrices with an informative test mixture: the three positional isomers of dihydroxybenzene. The aim of this work is to present the matrix-assisted DOSY user with information about the potential utility of a set of matrices (and combinations of matrices), including ionic and non-ionic surfactants, complexing agents, polymers, and mixed solvents. A variety of matrices improved the diffusion resolution of the signals of the test system, with the best separation achieved by mixed micelles of sodium dodecyl sulfate and cetyl trimethylammonium bromide. The use of mixed matrices offers great potential for the analyst to tailor the matrix to a particular sample under study. © 2016 The Authors Magnetic Resonance in Chemistry Published by John Wiley & Sons, Ltd.

© 2016 The Authors Magnetic Resonance in Chemistry Published by John Wiley & Sons, Ltd.

Keywords: 1H; Brij; CTAB; DOSY; MAD; NMR; SDS; dihydroxybenzene isomers; matrix-assisted DOSY

References

1. J Nat Prod. 2012 Feb 24;75(2):131-4 - PubMed
2. Chem Commun (Camb). 2011 Jul 7;47(25):7063-4 - PubMed
3. J Magn Reson. 2011 Feb;208(2):270-8 - PubMed
4. J Magn Reson. 2009 May;198(1):121-31 - PubMed
5. Anal Chem. 2009 Jun 1;81(11):4548-50 - PubMed
6. Angew Chem Int Ed Engl. 2013 Mar 11;52(11):3199-202 - PubMed
7. Int J Pharm. 2012 Oct 15;436(1-2):631-5 - PubMed
8. J Magn Reson. 2009 Oct;200(2):296-302 - PubMed
9. J Phys Chem B. 2013 Mar 7;117(9):2734-41 - PubMed
10. Magn Reson Chem. 2010 Oct;48(10):777-81 - PubMed
11. Org Biomol Chem. 2011 Oct 21;9(20):7062-4 - PubMed
12. Angew Chem Int Ed Engl. 2013 Mar 11;52(11):3255-8 - PubMed
13. Magn Reson Chem. 2016 Oct;54(10):815-820 - PubMed
14. Org Lett. 2009 Mar 19;11(6):1349-52 - PubMed
15. Magn Reson Chem. 2007 Dec;45 Suppl 1:S48-55 - PubMed
16. Magn Reson Chem. 2010 Jul;48(7):550-3 - PubMed
17. J Am Chem Soc. 2011 May 25;133(20):7640-3 - PubMed
18. Magn Reson Chem. 2012 Jun;50(6):458-65 - PubMed

Publication Types

• Journal Article

Grant support

• 10240/12-8 (NVG)/Coordination for the Improvement of Higher Education Personnel (CAPES) for a Senior Research Fellowship,
• EP/H024336/1 and EP/I00789/1/EPSRC