title: Rapid proton-detected NMR assignment for proteins with fast magic angle spinning.
abstract: Using a set of six (1)H-detected triple-resonance NMR experiments, we establish a method for sequence-specific backbone resonance assignment of magic angle spinning (MAS) nuclear magnetic resonance (NMR) spectra of 5-30 kDa proteins. The approach relies on perdeuteration, amide (2)H/(1)H exchange, high magnetic fields, and high-spinning frequencies (ωr/2π ≥ 60 kHz) and yields high-quality NMR data, enabling the use of automated analysis. The method is validated with five examples of proteins in different condensed states, including two microcrystalline proteins, a sedimented virus capsid, and two membrane-embedded systems. In comparison to contemporary (13)C/(15)N-based methods, this approach facilitates and accelerates the MAS NMR assignment process, shortening the spectral acquisition times and enabling the use of unsupervised state-of-the-art computational data analysis protocols originally developed for solution NMR.
authors.affiliation: Centre de RMN à Très Hauts Champs, Institut des Sciences Analytiques (CNRS, ENS Lyon, UCB Lyon 1), Université de Lyon , 69100 Villeurbanne, France.
authors.forename: Emeline
authors.initials: E
authors.lastname: Barbet-Massin
authors.forename: Andrew J
authors.initials: AJ
authors.lastname: Pell
authors.forename: Joren S
authors.initials: JS
authors.lastname: Retel
authors.forename: Loren B
authors.initials: LB
authors.lastname: Andreas
authors.forename: Kristaps
authors.initials: K
authors.lastname: Jaudzems
authors.forename: W Trent
authors.initials: WT
authors.lastname: Franks
authors.forename: Andrew J
authors.initials: AJ
authors.lastname: Nieuwkoop
authors.forename: Matthias
authors.initials: M
authors.lastname: Hiller
authors.forename: Victoria
authors.initials: V
authors.lastname: Higman
authors.forename: Paul
authors.initials: P
authors.lastname: Guerry
authors.forename: Andrea
authors.initials: A
authors.lastname: Bertarello
authors.forename: Michael J
authors.initials: MJ
authors.lastname: Knight
authors.forename: Michele
authors.initials: M
authors.lastname: Felletti
authors.forename: Tanguy
authors.initials: T
authors.lastname: Le Marchand
authors.forename: Svetlana
authors.initials: S
authors.lastname: Kotelovica
authors.forename: Inara
authors.initials: I
authors.lastname: Akopjana
authors.forename: Kaspars
authors.initials: K
authors.lastname: Tars
authors.forename: Monica
authors.initials: M
authors.lastname: Stoppini
authors.forename: Vittorio
authors.initials: V
authors.lastname: Bellotti
authors.forename: Martino
authors.initials: M
authors.lastname: Bolognesi
authors.forename: Stefano
authors.initials: S
authors.lastname: Ricagno
authors.forename: James J
authors.initials: JJ
authors.lastname: Chou
authors.forename: Robert G
authors.initials: RG
authors.lastname: Griffin
authors.forename: Hartmut
authors.initials: H
authors.lastname: Oschkinat
authors.forename: Anne
authors.initials: A
authors.lastname: Lesage
authors.forename: Lyndon
authors.initials: L
authors.lastname: Emsley
authors.forename: Torsten
authors.initials: T
authors.lastname: Herrmann
authors.forename: Guido
authors.initials: G
authors.lastname: Pintacuda
mesh_terms: D002247:Carbon Isotopes / Q000032:analysis; D041961:Deuterium Exchange Measurement; D006859:Hydrogen / Q000032:analysis*; D008958:Models, Molecular; D009587:Nitrogen Isotopes / Q000032:analysis; D019906:Nuclear Magnetic Resonance, Biomolecular / Q000379:methods*; D011506:Proteins / Q000737:chemistry; D011522:Protons
chemical_list: D002247:Carbon Isotopes; D009587:Nitrogen Isotopes; D011506:Proteins; D011522:Protons; D006859:Hydrogen
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