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Determination of glucan phosphorylation using heteronuclear 1 H, 13 C double and 1 H, 13 C, 31 P triple‐resonance NMR spectra
Author(s) -
Schmieder Peter,
Nitschke Felix,
Steup Martin,
Mallow Keven,
Specker Edgar
Publication year - 2013
Publication title -
magnetic resonance in chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.483
H-Index - 72
eISSN - 1097-458X
pISSN - 0749-1581
DOI - 10.1002/mrc.3996
Subject(s) - heteronuclear molecule , chemistry , nuclear magnetic resonance spectroscopy , phosphorus 31 nmr spectroscopy , nmr spectra database , mass spectrometry , dephosphorylation , molecule , glucan , phosphorylation , analytical chemistry (journal) , spectral line , crystallography , stereochemistry , chromatography , biochemistry , phosphatase , organic chemistry , physics , astronomy
Phosphorylation and dephosphorylation of starch and glycogen are important for their physicochemical properties and also their physiological functions. It is therefore desirable to reliably determine the phosphorylation sites. Heteronuclear multidimensional NMR‐spectroscopy is in principle a straightforward analytical approach even for complex carbohydrate molecules. With heterogeneous samples from natural sources, however, the task becomes more difficult because a full assignment of the resonances of the carbohydrates is impossible to obtain. Here, we show that the combination of heteronuclear 1 H, 13 C and 1 H, 13 C, 31 P techniques and information derived from spectra of a set of reference compounds can lead to an unambiguous determination of the phosphorylation sites even in heterogeneous samples. Copyright © 2013 John Wiley & Sons, Ltd.