Premium
Heteronuclear chemical shift correlation and J ‐resolved MAS NMR spectroscopy of lipid membranes
Author(s) -
Zorin Vadim,
Ciesielski Filip,
Griffin David C.,
Rittig Michael,
Bonev Boyan B.
Publication year - 2010
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.2690
Subject(s) - homonuclear molecule , chemistry , heteronuclear molecule , membrane , nuclear magnetic resonance spectroscopy , analytical chemistry (journal) , spectroscopy , spectral line , solid state nuclear magnetic resonance , chemical shift , nuclear magnetic resonance , stereochemistry , molecule , chromatography , physics , organic chemistry , biochemistry , quantum mechanics , astronomy
Direct observation of J ‐couplings remains a challenge in high‐resolution solid‐state NMR. In some cases, it is possible to use Lee–Goldburg (LG) homonuclear decoupling during rare spin observation in MAS NMR correlation spectroscopy of lipid membranes to obtain J ‐resolved spectra in the direct dimension. In one simple implementation, a wide line separation‐type 13 C‐ 1 H HETCOR can provide high‐resolution 1 H/ 13 C spectra, which are J ‐resolved in both dimensions. Coupling constants, 1 J HC , obtained from 1 H doublets, can be compared with scaled 1 J θ CH ‐values obtained from the 13 C multiplets to assess the LG efficiency and scaling factor. The use of homonuclear decoupling during proton evolution, LG‐HETCOR‐LG, can provide J ‐values, at least in the rare spin dimension, and allows measurements in less mobile membrane environments. The LG‐decoupled spectroscopic approach is demonstrated on pure dioleoylphosphatidylcholine (DOPC) membranes and used to investigate lipid mixtures of DOPC/cholesterol and DOPC/cholesterol/sphingomyelin. Copyright © 2010 John Wiley & Sons, Ltd.