Straightforward, effective calibration of SPINAL-64 decoupling results in the enhancement of sensitivity and resolution of biomolecular solid-state NMR.
Straightforward, effective calibration of SPINAL-64 decoupling results in the enhancement of sensitivity and resolution of biomolecular solid-state NMR.
J Magn Reson. 2010 Dec 31;
Authors: Comellas G, Lopez JJ, Nieuwkoop AJ, Lemkau LR, Rienstra CM
We describe a simple yet highly effective optimization strategy for SPINAL-64 (1)H 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(2) relaxation times for (13)C and (15)N show significant enhancement (up to 64%), relative to the previous described SPINAL-64 conditions, under the moderate (1)H decoupling levels (60-100kHz) and MAS rate (13.3kHz) commonly employed for high-resolution SSNMR spectroscopy of proteins. Additionally, we also investigated the effect at higher spinning rate (33.3kHz) and compared the results with other (1)H decoupling schemes (TPPM, XiX), as well as SPINAL-64 with the originally reported optimal values.
PMID: 21296014 [PubMed - as supplied by publisher]
Source:
PubMed