Straightforward, effective calibration of SPINAL-64 decoupling results in the enhancement of sensitivity and resolution of biomolecular solid-state NMR |
| |
| Authors: | Comellas Gemma Lopez Jakob J Nieuwkoop Andrew J Lemkau Luisel R Rienstra Chad M |
| |
| Institution: | a Center for Biophysics and Computational Biology, University of Illinois at Urbana-Champaign, 600 South Mathews Avenue, Urbana, IL 61801, USA;b Department of Chemistry, University of Illinois at Urbana-Champaign, 600 South Mathews Avenue, Urbana, IL 61801, USA;c Department of Biochemistry, University of Illinois at Urbana-Champaign, 600 South Mathews Avenue, Urbana, IL 61801, USA |
| |
| 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 T? relaxation times for 13C and 1?N 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. |
| |
| Keywords: | Magic-angle spinning Solid-state MMR Proton decoupling SPINAL-64 |
| 本文献已被 ScienceDirect PubMed 等数据库收录！ |
|
