High-resolution J-coupled 13C MAS NMR spectroscopy of lipid membranes

Filip Ciesielski, David C. Griffin, Michael Rittig, Boyan B. Bonev

Research output: Journal PublicationArticlepeer-review

14 Citations (Scopus)

Abstract

We propose the use of Lee-Goldburg decoupling in high-resolution natural abundance 13C CP-MAS NMR spectroscopy to obtain J-resolved multiplets from membrane lipids, and the use of these in spectral assignment and to investigate changes in molecular and segmental dynamics within chemical shift-resolved lipid groups. Spectroscopic characteristics of hydrated DPPC bilayers are reported, including J1CH-couplings from the liquid crystalline and gel phases. The observed JCH values are scaled in the Lee-Goldburg experiment by a factor of approximately 3-1/2 and corrected J1CH values on the order of 150 Hz compare well with indirect measurements. The J-resolved multiplets show JCH-couplings from the chain region to be approximately 20% lower than couplings determined from the headgroup, with backbone values falling between the two. Sensitivity of Lee-Goldburg decoupling to molecular motions reveals changes in hydrocarbon chain and backbone segmental dynamics across the main phospholipid transition and reduction in headgroup mobility below the pre-transition.

Original languageEnglish
Pages (from-to)77-85
Number of pages9
JournalChemistry and Physics of Lipids
Volume161
Issue number2
DOIs
Publication statusPublished - Oct 2009
Externally publishedYes

Keywords

  • DPPC
  • FSLG decoupling
  • J-coupling
  • Lipid membrane
  • Lipid phase transition
  • Solid-state NMR

ASJC Scopus subject areas

  • Biochemistry
  • Molecular Biology
  • Organic Chemistry
  • Cell Biology

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