Center for Biophysics and Computational Biology, University of Illinois at Urbana-Champaign, Urbana, IL 61801, USA.
J Magn Reson. 2011 Apr;209(2):131-5. doi: 10.1016/j.jmr.2010.12.011. Epub 2010 Dec 31.
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.
我们描述了一种简单而高效的优化策略，用于魔角旋转固态 NMR 的 SPINAL-64¹H 去耦条件。通过以耦合的方式调整相角，可以仅通过调整一个相角来确定来自三个参数优化的最佳条件。值得注意的是，与以前描述的 SPINAL-64 条件相比，在通常用于蛋白质高分辨率 SSNMR 光谱学的中等¹H 去耦水平（60-100 kHz）和 MAS 速率（13.3 kHz）下，¹³C 和 ¹⁵N 的回波 T₂弛豫时间显著增强（高达 64%）。此外，我们还研究了在更高的旋转速度（33.3 kHz）下的效果，并将结果与其他¹H 去耦方案（TPPM、XiX）以及具有原始报道的最佳值的 SPINAL-64 进行了比较。
