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魔角旋转核磁共振下的低功率WALTZ去耦

Low-power WALTZ decoupling under magic-angle spinning NMR.

作者信息

Thomas Luzian, Ernst Matthias

机构信息

Department of Chemistry and Applied Biosciences, ETH Zurich, Vladimir-Prelog-Weg 2, 8093 Zurich, Switzerland.

出版信息

Magn Reson (Gott). 2024 Nov 19;5(2):153-166. doi: 10.5194/mr-5-153-2024. eCollection 2024.

Abstract

Heteronuclear low-power decoupling using the solution-state wideband alternating-phase low-power technique for zero-residual splitting (WALTZ) sequences has become quite popular in solid-state protein NMR and seems to work well. However, there are no systematic studies that characterize these sequences under magic-angle spinning (MAS) and give recommendations on which parameter should be used. We have studied in detail the use of WALTZ-16 and WALTZ-64 as low-power decoupling sequences under 100 kHz MAS by characterizing the resonance conditions analytically using numerical simulations and experiments on model substances. The recoupling heteronuclear resonance conditions between the modulation frequency of the sequences and the MAS frequency is the most important feature. Pulse lengths corresponding to areas with vanishing first-order heteronuclear recoupling are good candidates for efficient decoupling. We have characterized two such conditions which can be defined using the nutation frequency of the radio frequency (RF) field ( ) and the spinning frequency ( ) by and , which both lead to narrow lines and are stable against RF-field variations and chemical-shift offsets. More such conditions might exist but were not investigated here.

摘要

使用溶液态宽带交替相位低功率技术实现零残留分裂(WALTZ)序列的异核低功率去耦在固态蛋白质核磁共振中已相当流行,且似乎效果良好。然而,尚无系统研究在魔角旋转(MAS)条件下对这些序列进行表征,也未就应使用哪些参数给出建议。我们通过对模型物质进行数值模拟和实验,从分析共振条件的角度详细研究了WALTZ - 16和WALTZ - 64作为100 kHz MAS下的低功率去耦序列的情况。序列调制频率与MAS频率之间的再耦合异核共振条件是最重要的特征。对应于一阶异核再耦合消失区域的脉冲长度是高效去耦的良好候选。我们已表征了两种这样的条件,它们可通过射频(RF)场的章动频率( )和自旋频率( )定义为 和 ,这两种条件都能产生窄线,并且对RF场变化和化学位移偏移具有稳定性。可能存在更多这样的条件,但本文未作研究。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/56ae/12178133/60e09658edc8/mr-5-153-2024-f01.jpg

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