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Relaxation Editing in NMR Using a New Two-Dimensional Long-Lived Coherence Method for Mixture Analysis
Analytical Chemistry ( IF 7.4 ) Pub Date : 2024-05-10 , DOI: 10.1021/acs.analchem.3c05574
Upanshu Gangwar 1 , Narayanan D. Kurur 1
Affiliation  

The exploration of metabolomics and targeted segments of proteins stands as a pivotal facet of Nuclear Magnetic Resonance (NMR) analysis, furnishing valuable insights into molecular architectures and potential therapeutic applications. The issue of spectral congestion frequently presents challenges in ascribing distinct peaks within the confines of both one-dimensional (1D) and two-dimensional (2D) NMR spectra. Numerous strategies have been proposed to resolve specific resonances in NMR spectra differentially. Among these approaches, relaxation editing emerges as a viable solution. In the realm of relaxation phenomena within NMR, Long-Lived States (LLS) and Long-Lived Coherences (LLC) manifest as promising phenomena, offering enhanced relaxation lifetimes in comparison to the traditional longitudinal (T1) and transverse (T2) relaxation times for coupled nuclear spins. Notably, LLC presents a pathway to attenuate uncoupled high-intensity peaks, effectively diminishing their impact. The foundation of this technique rests upon the premise that the relaxation lifetime in the rotating frame (T) remains smaller than TLLC. In pursuit of refining spectral assignments within complex mixtures, we introduce a new pulse sequence tailored for LLC Total Correlation Spectroscopy (LLC-TOCSY). This demonstrates efficacy in extracting LLC signals within configurations involving multiple coupled spins, thereby decluttering the spectrum and enhancing the accuracy of peak assignments. To validate the effectiveness of this method, a collection of samples was subjected to scrutiny, yielding compelling results.

中文翻译:


使用新的二维长寿命相干方法进行混合物分析的 NMR 弛豫编辑



对代谢组学和蛋白质目标片段的探索是核磁共振 (NMR) 分析的关键方面,为分子结构和潜在治疗应用提供了宝贵的见解。光谱拥塞问题经常给在一维 (1D) 和二维 (2D) NMR 光谱范围内归属不同峰带来挑战。已经提出了许多策略来差异化地解决 NMR 谱中的特定共振。在这些方法中,松弛编辑成为一种可行的解决方案。在 NMR 的弛豫现象领域,长寿命态 (LLS) 和长寿命相干性 (LLC) 表现出有希望的现象,与传统的纵向 (T 1 ) 和耦合核自旋的横向 (T 2 ) 弛豫时间。值得注意的是,LLC 提供了一种减弱非耦合高强度峰值的途径,从而有效地减少其影响。该技术的基础基于旋转坐标系中的弛豫寿命 (T ) 保持小于 T LLC 的前提。为了在复杂混合物中精细化光谱分配,我们引入了专为 LLC 全相关光谱 (LLC-TOCSY) 量身定制的新脉冲序列。这证明了在涉及多个耦合自旋的配置中提取 LLC 信号的功效,从而整理光谱并提高峰值分配的准确性。为了验证该方法的有效性,对一组样本进行了仔细检查,得出了令人信服的结果。
更新日期:2024-05-10
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