title: 1H detection in MAS solid-state NMR spectroscopy of biomacromolecules employing pulsed field gradients for residual solvent suppression.
abstract: In this communication, we demonstrate the feasibility of 1H detection in MAS solid-state NMR for a microcrystalline, uniformly 2H,15N-labeled sample of a SH3 domain of chicken alpha-spectrin, using pulsed field gradients for suppression of water magnetization. Today, B0 gradients are employed routinely in solution-state NMR for coherence order selection and solvent suppression. We suggest to use gradients to purge water magnetization which cannot be suppressed using conventional water suppression schemes. The achievable gain in sensitivity for 1H detection is in the order of 5 compared to the 15N detected version of the experiment (at a MAS rotation frequency of 13.5 kHz). We expect that this labeling concept which achieves high sensitivity due to 1H detection, in combination with the possibility to measure long range 1H-1H distances as we have shown previously, to be a useful tool for the determination of protein structures in the solid state.
authors.affiliation: Institut für Organische Chemie und Biochemie II, Technische Universität München, Lichtenbergstrasse 4, 85747 Garching, Germany.
authors.forename: Veniamin
authors.initials: V
authors.lastname: Chevelkov
authors.forename: Barth J
authors.initials: BJ
authors.lastname: van Rossum
authors.forename: Federica
authors.initials: F
authors.lastname: Castellani
authors.forename: Kristina
authors.initials: K
authors.lastname: Rehbein
authors.forename: Anne
authors.initials: A
authors.lastname: Diehl
authors.forename: Morten
authors.initials: M
authors.lastname: Hohwy
authors.forename: Stefan
authors.initials: S
authors.lastname: Steuernagel
authors.forename: Frank
authors.initials: F
authors.lastname: Engelke
authors.forename: Hartmut
authors.initials: H
authors.lastname: Oschkinat
authors.forename: Bernd
authors.initials: B
authors.lastname: Reif
mesh_terms: D000818:Animals; D002645:Chickens; D009587:Nitrogen Isotopes; D019906:Nuclear Magnetic Resonance, Biomolecular / Q000379:methods*; D011522:Protons; D012996:Solutions; D013049:Spectrin / Q000737:chemistry*; D018909:src Homology Domains
chemical_list: D009587:Nitrogen Isotopes; D011522:Protons; D012996:Solutions; D013049:Spectrin