Simultaneous Cross Polarization to 13C and 15N with 1H Detection at 60 kHz MAS Solid-state NMR

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Simultaneous Cross Polarization to 13C and 15N with 1H Detection at 60 kHz MAS Solid-state NMR

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12-12-2015, 05:40 PM

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Simultaneous Cross Polarization to 13C and 15N with 1H Detection at 60 kHz MAS Solid-state NMR

Simultaneous Cross Polarization to 13C and 15N with 1H Detection at 60 kHz MAS Solid-state NMR

Publication date: Available online 12 December 2015
Source:Journal of Magnetic Resonance

Author(s): Bibhuti B. Das, Stanley J. Opella

We describe high resolution MAS solid-state NMR experiments that utilize 1H detection with 60 kHz magic angle spinning; simultaneous cross-polarization from 1H to 15N and 13C nuclei; bidirectional cross-polarization between 13C and 15N nuclei; detection of both amide nitrogen and aliphatic carbon 1H; and measurement of both 13C and 15N chemical shifts through multi-dimensional correlation experiments. Three-dimensional experiments correlate amide 1H and alpha 1H selectively with 13C or 15N nuclei in a polypeptide chain. Two separate three-dimensional spectra correlating 1H?/13C?/1HN and 1HN/15N/1H? are recorded simultaneously in a single experiment, demonstrating that a two-fold savings in experimental time is potentially achievable. Spectral editing using bidirectional coherence transfer pathways enables simultaneous magnetization transfers between 15N, 13C?(i) and 13C’(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.
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Source: Journal of Magnetic Resonance

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