Straightforward, effective calibration of SPINAL-64 decoupling results in the enhancement of sensitivity and resolution of biomolecular solid-state NMR

Gemma Comellas, Jakob J. Lopez, Andrew J. Nieuwkoop, Luisel R. Lemkau, Chad M. Rienstra

Research output: Contribution to journalArticle

29 Scopus citations

Abstract

We describe a simple yet highly effective optimization strategy for SPINAL-64 1H decoupling conditions for magic-angle spinning solid-state NMR. With adjustment of the phase angles in a coupled manner, the optimal conditions resulting from three parameter optimizations can be determined with adjustment of a single phase. Notably, echo T2 relaxation times for 13C and 15N show significant enhancement (up to 64%), relative to the previous described SPINAL-64 conditions, under the moderate 1H decoupling levels (60-100 kHz) and MAS rate (13.3 kHz) commonly employed for high-resolution SSNMR spectroscopy of proteins. Additionally, we also investigated the effect at higher spinning rate (33.3 kHz) and compared the results with other 1H decoupling schemes (TPPM, XiX), as well as SPINAL-64 with the originally reported optimal values.

Original languageEnglish (US)
Pages (from-to)131-135
Number of pages5
JournalJournal of Magnetic Resonance
Volume209
Issue number2
DOIs
StatePublished - Apr 1 2011
Externally publishedYes

All Science Journal Classification (ASJC) codes

  • Condensed Matter Physics
  • Nuclear and High Energy Physics
  • Biophysics
  • Biochemistry

Keywords

  • Magic-angle spinning
  • Proton decoupling
  • SPINAL-64
  • Solid-state MMR

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