Title |
Detection of side-chain proton resonances of fully protonated biosolids in nano-litre volumes by magic angle spinning solid-state NMR
|
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Published in |
Journal of Biomolecular NMR, March 2018
|
DOI | 10.1007/s10858-018-0168-3 |
Pubmed ID | |
Authors |
James Tolchard, Manoj Kumar Pandey, Mélanie Berbon, Abdelmajid Noubhani, Sven J Saupe, Yusuke Nishiyama, Birgit Habenstein, Antoine Loquet |
Abstract |
We present a new solid-state NMR proton-detected three-dimensional experiment dedicated to the observation of protein proton side chain resonances in nano-liter volumes. The experiment takes advantage of very fast magic angle spinning and double quantum 13C-13C transfer to establish efficient (H)CCH correlations detected on side chain protons. Our approach is demonstrated on the HET-s prion domain in its functional amyloid fibrillar form, fully protonated, with a sample amount of less than 500 µg using a MAS frequency of 70 kHz. The majority of aliphatic and aromatic side chain protons (70%) are observable, in addition to Hα resonances, in a single experiment providing a complementary approach to the established proton-detected amide-based multidimensional solid-state NMR experiments for the study and resonance assignment of biosolid samples, in particular for aromatic side chain resonances. |
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