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J Magn Reson. 2015 Sep;258:12-6. doi: 10.1016/j.jmr.2015.06.002. Epub 2015 Jun 23.

Accurate DOSY measure for out-of-equilibrium systems using permutated DOSY (p-DOSY).

Author information

1
Laboratory of BioNanoTechnology, Wageningen University, PO Box 8038, 6700 EK Wageningen, The Netherlands.
2
Institut de Génétique et de Biologie Moléculaire et Cellulaire, INSERM, U596, CNRS, UMR 7104, Université de Strasbourg, 67404 Illkirch-Graffenstaden, France; NMRTEC, bioparc, 1 Bd Brandt, Illkirch-Graffenstaden 67400, France.
3
Laboratory of BioNanoTechnology, Wageningen University, PO Box 8038, 6700 EK Wageningen, The Netherlands; Instituto Regional de Investigación Científica Aplicada (IRICA), Universidad de Castilla-La Mancha, Avda. Camilo José Cela, s/n, 13071 Ciudad Real, Spain.
4
Institut de Génétique et de Biologie Moléculaire et Cellulaire, INSERM, U596, CNRS, UMR 7104, Université de Strasbourg, 67404 Illkirch-Graffenstaden, France. Electronic address: madelsuc@unistra.fr.

Abstract

NMR spectroscopy is a excellent tool for monitoring in-situ chemical reactions. In particular, DOSY measurement is well suited to characterize transient species by the determination of their sizes. However, here we bring to light a difficulty in the DOSY experiments performed in out-of-equilibrium systems. On such a system, the evolution of the concentration of species interferes with the measurement process, and creates a bias on the diffusion coefficient determination that may lead to erroneous interpretations. We show that a random permutation of the series of gradient strengths used during the DOSY experiment allows to average out this bias. This approach, that we name p-DOSY does not require changes in the pulse sequences nor in the processing software, and restores completely the full accuracy of the measure. This technique is demonstrated on the monitoring of the anomerization reaction of α- to β-glucose.

KEYWORDS:

Complex mixtures; DOSY; Glucose; Out-of-equilibrium; Permutation

PMID:
26150378
DOI:
10.1016/j.jmr.2015.06.002
[Indexed for MEDLINE]

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