Publication year: 2011 Source: Journal of Magnetic Resonance, Available online 9 November 2011
Morten*Bjerring, Berit*Paaske, Hartmut*Oschkinat, Umit*Akbey, Niels Chr.*Nielsen
We present a novel sampling strategy, interleaving acquisition of multiple NMR spectra by exploiting initial polarization subsequently fromH andH spins, taking advantage of their differentT1relaxation times. DifferentH- andH-polarization based spectra are in this way simultaneously recorded improving either information content or sensitivity by adding spectra. The so-called RAPID (Relaxation-optimized Acquisition of Proton Interleaved with Deuterium)H->C/H->C CP/MAS multiple-acquisition method is demonstrated by 1D and 2D experiments using a uniformlyH,N,C-labelled ?-spectrin SH3 domain sample with all or 30% back-exchanged labileH toH. It is demonstrated how 1DC CP/MAS or 2DC-C correlation spectra initialized with polarization from eitherH orH may be recorded simultaneously with flexibility to be added or used individually for spectral editing. It is also shown how 2DC-C correlation spectra may be recorded interleaved withH-C correlation spectra to obtainC-C correlations along with information about dynamics fromH sideband patterns. Graphical abstract
Highlights
? Simultaneous acquisition of multiple 1D or 2D solid-state NMR spectra on single-receiver instrumentation. ? Interleaved sampling exploiting polarization from different spin species. ? Polarization from fast-relaxingH spins while restoring slow-relaxingH polarization for deuterated proteins. ? Sensitivity enhancement or spectral editing in solid-state NMR of deuterated proteins.
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Repetitive cross-polarization contacts via equilibration-re-equilibration of the proton bath: sensitivity enhancement for NMR of membrane proteins reconstituted in magnetically aligned bicelles
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Source: Journal of Magnetic Resonance, In Press, Accepted Manuscript, Available online 2 July 2011</br>
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Abstract High resolution 13C-detected solid-state NMR spectra of the deuterated beta-1 immunoglobulin binding domain of the protein G (GB1) have been collected to show that all 15N, 13Cā?², 13CĪ± and 13CĪ² sites are resolved in 13Cā??13C and 15Nā??13C spectra, with significant improvement in T 2 relaxation times and resolution at high magnetic field (750 MHz). The comparison of echo T 2 values between deuterated and protonated GB1 at various spinning rates and under different decoupling schemes indicates...
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MAS solid-state NMR experiments applied to biological solids are still hampered by low sensitivity and resolution. In this work, we employ a deuteration scheme in which individual methyl groups are selectively protonated. This labeling scheme...
Rapid Solid-State NMR of Deuterated Proteins by Interleaved Cross-Polarization fromH andH Nuclei
Linear Mode
