Sensitive 13C–13C correlation spectra of amyloid fibrils at very high spinning frequencies and magnetic fields
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Sensitive 2D solid-state 13C–13C correlation spectra of amyloid β fibrils have been recorded at very fast spinning frequencies and very high magnetic fields. It is demonstrated that PARIS-xy recoupling using moderate rf amplitudes can provide structural information by promoting efficient magnetization transfer even under such challenging experimental conditions. Furthermore, it has been shown both experimentally and by numerical simulations that the method is not very sensitive to dipolar truncation effects and can reveal direct transfer across distances of about 3.5–4Å.
KeywordsAmyloid β fibrils Solid-state NMR 13C–13C 2D correlation spectra Dipolar truncation PARIS-xy dipolar recoupling Ultra-high magnetic field
Financial support from the Agence Nationale de la Recherche (ANR-09-BLAN-0111-01) and from the Fédération de Recherche (FR 3050) Très Grands Equipements de Résonance Magnétique Nucléaire à Très Hauts Champs (TGE RMN THC) of the CNRS is gratefully acknowledged. We thank Prof. Kazuhiro Irie at the Division of Food Science and Biotechnology, Graduate School of Agriculture, Kyoto University, for the use of a peptide synthesizer. We are grateful to Dr. Ken-ichi Akagi, Ms. Youko Monobe, and Dr. Takayoshi Imazawa at Laboratory of Common Apparatus, Division of Biomedical Research, National Institute of Biomedical Innovation for obtaining electron micrographs.
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