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 J1θCH 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 J1θCH-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 language | English |
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Pages (from-to) | 77-85 |
Number of pages | 9 |
Journal | Chemistry and Physics of Lipids |
Volume | 161 |
Issue number | 2 |
DOIs | |
Publication status | Published - Oct 2009 |
Externally published | Yes |
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