Sensitivity and resolution enhancement in solid-state NMR spectroscopy of bicelles
2007 (English)In: Journal of magnetic resonance (San Diego, Calif. 1997: Print), ISSN 1090-7807, E-ISSN 1096-0856, Vol. 184, no 2, 228-235 p.Article in journal (Refereed) Published
Magnetically aligned bicelles are becoming attractive model membranes to investigate the structure, dynamics, geometry, and interaction of membrane-associated peptides and proteins using solution- and solid-state NMR experiments. Recent studies have shown that bicelles are more suitable than mechanically aligned bilayers for multidimensional solid-state NMR experiments. In this work, we describe experimental aspects of the natural abundance C-13 and N-14 NMR spectroscopy of DMPC/DHPC bicelles. In particular, approaches to enhance the sensitivity and resolution and to quantify radio-frequency heating effects are presented. Sensitivity of C-13 detection using single pulse excitation, conventional cross-polarization (CP), ramp-CP, and NOE techniques are compared. Our results suggest that the proton decoupling efficiency of the FLOPSY pulse sequence is better than that of continuous wave decoupling, TPPM, SPINAL, and WALTZ sequences. A simple method of monitoring the water proton chemical shift is demonstrated for the measurement of sample temperature and calibration of the radio-frequency-induced heating in the sample. The possibility of using N-14 experiments on bicelles is also discussed.
Place, publisher, year, edition, pages
2007. Vol. 184, no 2, 228-235 p.
bicelles, sensitivity, resolution, RF heating, proton decoupling, nitrogen-14 NMR, nuclear-magnetic-resonance, angle-spinning nmr, membrane-associated peptides, band decoupling sequence, local field spectra, magic-angle, phospholipid-bilayers, cross-polarization, lipid-membranes, liquid-crystals
IdentifiersURN: urn:nbn:se:kth:diva-16389DOI: 10.1016/j.jmr.2006.10.004ISI: 000244237000005OAI: oai:DiVA.org:kth-16389DiVA: diva2:334431
QC 201005252010-08-052010-08-05Bibliographically approved