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
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DOI：
10.1016/j.jmr.2010.12.011
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发表时间：
2011-04-01
影响因子：
2.2
通讯作者：
Rienstra, Chad M.
中科院分区：
文献类型：
--
作者：
Comellas, Gemma;Lopez, Jakob J.;Rienstra, Chad M.
我们描述了一种简单而高效的优化策略，用于魔角旋转固体核磁共振的脊椎H-1去耦合条件。以耦合的方式调整相角，可以通过调整单相来确定三个参数优化所得到的最优条件。值得注意的是，C-13和N-15的回波T-2弛豫时间与前面描述的脊柱-条件相比有显著的提高(高达%)，在中等H-1去耦合水平(60-100 kHz)和MAS速率(13.3 kHz)下，通常用于高分辨率蛋白质的SSNMR谱。此外，我们还研究了在较高旋转速度(33.3 kHz)下的影响，并将结果与其他H-1去耦合方案(TPPM、XIX)以及脊柱的结果进行了比较。由爱思唯尔公司出版。
We describe a simple yet highly effective optimization strategy for SPINAL-64 H-1 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 C-13 and N-15 show significant enhancement (up to 64%), relative to the previous described SPINAL-64 conditions, under the moderate H-1 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 H-1 decoupling schemes (TPPM, XiX), as well as SPINAL-64 with the originally reported optimal values. Published by Elsevier Inc.