The truncated driven NOE and (13)C NMR sensitivity enhancement in magnetically-aligned bicelles.
The truncated driven nuclear Overhauser effect (NOE) sequence is examined as a means of sensitivity enhancement in (13)C NMR spectroscopy of magnetically-aligned bicelles consisting of 4.5:1 mixtures of DMPC (1,2-dimyristoyl-sn-glycero-3-phosphocholine) plus DHPC (1,2-dihexanoyl-sn-glycero-3-phosphocholine), with 1 mole% DMPE-PEG 2000 (1,2-dimyristoyl-sn-glycero-3-phosphoethanolamine-N-methoxy(polyethylene glycol)-2000). Steady-state NOE enhancements were observed at all carbon segments except the lipid carbonyls, but full NOE enhancements were obtained only for the most mobile carbon segments, specifically the choline quaternary methyls and terminal acyl chain methyls of both DMPC and DHPC, as well as the ethylene oxide segments of the PEG head group of DMPE-PEG 2000. Other carbon segments exhibited NOE enhancements that scaled with mobility as determined by transient NOE measurements combined with spin-lattice relaxation measurements. We conclude that the truncated driven NOE provides sensitivity enhancement complimentary to that yielded by cross-polarization techniques and for mobile membrane-associated species may be preferred for its robustness and ease of setup.
Macdonald
Peter M
PM
Department of Chemical and Physical Sciences, University of Toronto at Mississauga, 3359 Mississauga Road North, Mississauga, Ontario, Canada L5L 1C6. pmacdona@utm.utoronto.ca
Soong
Ronald
R
D000465:Algorithms; D002247:Carbon Isotopes; D002462:Cell Membrane / Q000737:chemistry; D004134:Dimyristoylphosphatidylcholine / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D015394:Molecular Structure; D010742:Phospholipid Ethers / Q000737:chemistry*; D011092:Polyethylene Glycols / Q000737:chemistry*
C052298:1,2-dihexadecyl-sn-glycero-3-phosphocholine; D002247:Carbon Isotopes; D010742:Phospholipid Ethers; D011092:Polyethylene Glycols; D004134:Dimyristoylphosphatidylcholine