Heteronuclear chemical shift correlation and J-resolved MAS NMR spectroscopy of lipid membranes

✍ Scribed by Vadim Zorin; Filip Ciesielski; David C. Griffin; Michael Rittig; Boyan B. Bonev

• Publisher: John Wiley and Sons
• Year: 2010
• Tongue: English
• Weight: 408 KB
• Volume: 48
• Category: Article
• ISSN: 0749-1581
• DOI: 10.1002/mrc.2690

✦ Synopsis

Abstract

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.