Simultaneous cross polarization to (13)C and (15)N with (1)H detection at 60kHz MAS solid-state NMR.

 In
by Bibhuti B Das, Stanley J Opella
Abstract:
We describe high resolution MAS solid-state NMR experiments that utilize (1)H detection with 60kHz magic angle spinning; simultaneous cross-polarization from (1)H to (15)N and (13)C nuclei; bidirectional cross-polarization between (13)C and (15)N nuclei; detection of both amide nitrogen and aliphatic carbon (1)H; and measurement of both (13)C and (15)N chemical shifts through multi-dimensional correlation experiments. Three-dimensional experiments correlate amide (1)H and alpha (1)H selectively with (13)C or (15)N nuclei in a polypeptide chain. Two separate three-dimensional spectra correlating (1)H__MATH0__/(13)C__MATH0__/(1)H(N) and (1)H(N)/(15)N/(1)H__MATH0__ are recorded simultaneously in a single experiment, demonstrating that a twofold savings in experimental time is potentially achievable. Spectral editing using bidirectional coherence transfer pathways enables simultaneous magnetization transfers between (15)N, (13)C__MATH0__(()(i)()) and (13)C'(()(i)(-1)), facilitating intra- and inter-residue correlations for sequential resonance assignment. Non-uniform sampling is integrated into the experiments, further reducing the length of experimental time.
Reference:
Simultaneous cross polarization to (13)C and (15)N with (1)H detection at 60kHz MAS solid-state NMR. (Bibhuti B Das, Stanley J Opella), In Journal of magnetic resonance (San Diego, Calif. : 1997), volume 262, 2016.
Bibtex Entry:
@article{Das2016,
abstract = {We describe high resolution MAS solid-state NMR experiments that utilize (1)H detection with 60kHz magic angle spinning; simultaneous cross-polarization from (1)H to (15)N and (13)C nuclei; bidirectional cross-polarization between (13)C and (15)N nuclei; detection of both amide nitrogen and aliphatic carbon (1)H; and measurement of both (13)C and (15)N chemical shifts through multi-dimensional correlation experiments. Three-dimensional experiments correlate amide (1)H and alpha (1)H selectively with (13)C or (15)N nuclei in a polypeptide chain. Two separate three-dimensional spectra correlating (1)H$alpha$/(13)C$alpha$/(1)H(N) and (1)H(N)/(15)N/(1)H$alpha$ are recorded simultaneously in a single experiment, demonstrating that a twofold savings in experimental time is potentially achievable. Spectral editing using bidirectional coherence transfer pathways enables simultaneous magnetization transfers between (15)N, (13)C$alpha$(()(i)()) and (13)C'(()(i)(-1)), facilitating intra- and inter-residue correlations for sequential resonance assignment. Non-uniform sampling is integrated into the experiments, further reducing the length of experimental time.},
author = {Das, Bibhuti B and Opella, Stanley J},
doi = {10.1016/j.jmr.2015.12.004},
issn = {1096-0856},
journal = {Journal of magnetic resonance (San Diego, Calif. : 1997)},
keywords = {Dual observation,Magic angle spinning,Peptides,Proteins,Triple-resonance},
month = {jan},
pages = {20--6},
pmid = {26705905},
title = {{Simultaneous cross polarization to (13)C and (15)N with (1)H detection at 60kHz MAS solid-state NMR.}},
url = {http://linkinghub.elsevier.com/retrieve/pii/S1090780715002979 http://www.ncbi.nlm.nih.gov/pubmed/26705905 http://www.pubmedcentral.nih.gov/articlerender.fcgi?artid=PMC4716881},
volume = {262},
year = {2016}
}

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