Low power supercycled TPPM decoupling

IF 2 3区 化学 Q3 BIOCHEMICAL RESEARCH METHODS Journal of magnetic resonance Pub Date : 2024-07-02 DOI:10.1016/j.jmr.2024.107726
Rajat Garg , Barry DeZonia , Alexander L. Paterson , Chad M. Rienstra
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Abstract

Improving the spectral sensitivity and resolution of biological solids is one of the long-standing problems in nuclear magnetic resonance (NMR) spectroscopy. In this report, we introduce low-power supercycled variants of two-pulse phase-modulated (TPPM) sequence for heteronuclear decoupling. The utility of the sequence is shown by improvements in the transverse relaxation time of observed nuclei (with 1H decoupling) with its application to different samples (uniformly 13C, 15N, 2H-labeled GB1 back-exchanged with 25% H2O and 75% D2O, uniformly 13C, 15N, 2H-labeled human derived Asyn fibril back-exchanged with 100% H2O and uniformly 13C, 15N -labeled human derived Asyn fibril) at fast MAS using low radiofrequency (RF) fields. To understand the effect of spinning speed, the transverse relaxation time is monitored under different spinning frequencies. In comparison to existing heteronuclear decoupling sequences, the supercycled TPPM (sTPPM) sequence significantly improves the spectral sensitivity and resolution and is robust towards B1 inhomogeneity and decoupler offset.

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低功耗超循环 TPPM 去耦。
提高生物固体的光谱灵敏度和分辨率是核磁共振(NMR)光谱学的长期难题之一。在本报告中,我们介绍了用于异核去耦的双脉冲相位调制(TPPM)序列的低功率超循环变体。在使用低射频(RF)场的快速 MAS 条件下,该序列应用于不同样品(25% H2O 和 75% D2O 反向交换的均匀 13C、15N、2H 标记的 GB1,100% H2O 反向交换的均匀 13C、15N、2H 标记的人源性 Asyn 纤维,以及均匀 13C、15N 标记的人源性 Asyn 纤维)时,观察到的原子核横向弛豫时间(1H 去耦)的改善表明了该序列的实用性。为了解旋转速度的影响,在不同旋转频率下对横向弛豫时间进行了监测。与现有的异核去耦序列相比,超循环 TPPM(sTPPM)序列显著提高了光谱灵敏度和分辨率,并对 B1 不均匀性和去耦器偏移具有鲁棒性。
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来源期刊
CiteScore
3.80
自引率
13.60%
发文量
150
审稿时长
69 days
期刊介绍: The Journal of Magnetic Resonance presents original technical and scientific papers in all aspects of magnetic resonance, including nuclear magnetic resonance spectroscopy (NMR) of solids and liquids, electron spin/paramagnetic resonance (EPR), in vivo magnetic resonance imaging (MRI) and spectroscopy (MRS), nuclear quadrupole resonance (NQR) and magnetic resonance phenomena at nearly zero fields or in combination with optics. The Journal''s main aims include deepening the physical principles underlying all these spectroscopies, publishing significant theoretical and experimental results leading to spectral and spatial progress in these areas, and opening new MR-based applications in chemistry, biology and medicine. The Journal also seeks descriptions of novel apparatuses, new experimental protocols, and new procedures of data analysis and interpretation - including computational and quantum-mechanical methods - capable of advancing MR spectroscopy and imaging.
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