MAS dependent sensitivity of different isotopomers in selectively methyl protonated protein samples in solid state NMR
Jazyk angličtina Země Nizozemsko Médium print-electronic
Typ dokumentu časopisecké články
Grantová podpora
ERC-2014-CoG "P-MEM-NMR" GA n 648974
European Research Council - International
GA 653706
EU access project iNext
Project B07
Deutsche Forschungsgemeinschaft
SFB-1035
Deutsche Forschungsgemeinschaft
Grant Re1435
Deutsche Forschungsgemeinschaft
PubMed
31515660
DOI
10.1007/s10858-019-00274-0
PII: 10.1007/s10858-019-00274-0
Knihovny.cz E-zdroje
- Klíčová slova
- CH3 labelling, Magic angle spinning (MAS), Methyl isotopomers, Microcrystalline proteins, Selective deuteration, Solid state NMR,
- MeSH
- deuterium chemie MeSH
- metylace * MeSH
- nukleární magnetická rezonance biomolekulární metody MeSH
- protony * MeSH
- senzitivita a specificita MeSH
- spektrin chemie MeSH
- src homologní domény MeSH
- Publikační typ
- časopisecké články MeSH
- Názvy látek
- deuterium MeSH
- protony * MeSH
- spektrin MeSH
Sensitivity and resolution together determine the quality of NMR spectra in biological solids. For high-resolution structure determination with solid-state NMR, proton-detection emerged as an attractive strategy in the last few years. Recent progress in probe technology has extended the range of available MAS frequencies up to above 100 kHz, enabling the detection of resolved resonances from sidechain protons, which are important reporters of structure. Here we characterise the interplay between MAS frequency in the newly available range of 70-110 kHz and proton content on the spectral quality obtainable on a 1 GHz spectrometer for methyl resonances. Variable degrees of proton densities are tested on microcrystalline samples of the α-spectrin SH3 domain with selectively protonated methyl isotopomers (CH3, CH2D, CHD2) in a perdeuterated matrix. The experimental results are supported by simulations that allow the prediction of the sensitivity outside this experimental frequency window. Our results facilitate the selection of the appropriate labelling scheme at a given MAS rotation frequency.
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