Is protein deuteration beneficial for proton detected solid-state NMR at and above 100 kHz magic-angle spinning?
| Autor: | Kristaps Jaudzems, Guido Pintacuda, Loren B. Andreas, Kaspars Tars, Diane Cala de Paepe, Jan Stanek |
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| Přispěvatelé: | Biological Solid-State NMR Methods - Méthodes de RMN à l'état solide en biologie, Institut des Sciences Analytiques (ISA), Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS)-Institut de Chimie du CNRS (INC)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Centre National de la Recherche Scientifique (CNRS), Biomed Res & Study Ctr, Max Planck Institute for Biophysical Chemistry (MPI-BPC), Max-Planck-Gesellschaft, The financial support from CNRS (IR-RMN FR3050 and Fondation pour la Chimie des Substances Naturelles) and European Research Council (ERC) under the European Union's Horizon 2020 research and innovation programme (ERC-2014-CoG 'P-MEM-NMR' GA n°648974) is gratefully acknowledged. J.S., K.J. and L.B.A. are supported by individual MSCA incoming fellowships (REA grant agreements n°661799 'COMPLEX-FAST-MAS', n°661175 'virus-DNP-NMR', n°624918 'MEM-MAS')., European Project: 648974,H2020,ERC-2014-CoG,P-MEM-NMR(2015), European Project: 661799,H2020,H2020-MSCA-IF-2014,COMPLEX-fastMAS-NMR(2016), European Project: 661175,H2020,H2020-MSCA-IF-2014,virus-DNP-NMR(2015), European Project: 624918,EC:FP7:PEOPLE,FP7-PEOPLE-2013-IIF,MEM-MAS(2014), Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS)-Université Claude Bernard Lyon 1 (UCBL), Université de Lyon-Université de Lyon-Institut de Chimie du CNRS (INC)-Centre National de la Recherche Scientifique (CNRS) |
| Jazyk: | angličtina |
| Předmět: |
Nuclear and High Energy Physics
Fast magic-angle spinning Analytical chemistry Protonation 010402 general chemistry 01 natural sciences Spectral line Nuclear magnetic resonance Sensitivity [CHIM.ANAL]Chemical Sciences/Analytical chemistry Magic angle spinning Side chain Protein assemblies [SDV.BBM.BC]Life Sciences [q-bio]/Biochemistry Molecular Biology/Biochemistry [q-bio.BM] Nuclear Magnetic Resonance Biomolecular Instrumentation Full protonation Proton detection Radiation Side-chains 010405 organic chemistry Chemistry Fractional deuteration Proteins General Chemistry Deuterium 0104 chemical sciences Dilution Microcrystalline Solid-state nuclear magnetic resonance Protons Resolution Ultrashort pulse |
| Zdroj: | Solid State Nuclear Magnetic Resonance Solid State Nuclear Magnetic Resonance, Elsevier, 2017, 87, pp.126-136. ⟨10.1016/j.ssnmr.2017.07.004⟩ Solid State Nuclear Magnetic Resonance, 2017, 87, pp.126-136. ⟨10.1016/j.ssnmr.2017.07.004⟩ |
| ISSN: | 0926-2040 |
| DOI: | 10.1016/j.ssnmr.2017.07.004 |
| Popis: | We thank the members of technical staff of ISA for assistance with NMR spectrometers.; International audience; 1H-detection in solid-state NMR of proteins has been traditionally combined with deuteration for both resolution and sensitivity reasons, with the optimal level of proton dilution being dependent on MAS rate. Here we present 1H-detected 15N and 13C CP-HSQC spectra on two microcrystalline samples acquired at 60 and 111 kHz MAS and at ultra-high field. We critically compare the benefits of three labeling schemes yielding different levels of proton content in terms of resolution, coherence lifetimes and feasibility of scalar-based 2D correlations under these experimental conditions. We observe unexpectedly high resolution and sensitivity of aromatic resonances in 2D 13C-1H correlation spectra of protonated samples. Ultrafast MAS reduces or even removes the necessity of 1H dilution for high-resolution 1H-detection in biomolecular solid-state NMR. It yields 15N,1H and 13C,1H fingerprint spectra of exceptional resolution for fully protonated samples, with notably superior 1H and 13C lineshapes for side-chain resonances. |
| Databáze: | OpenAIRE |
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