Low-field, not low quality: 1D simplification, selective detection, and heteronuclear 2D experiments for improving low-field NMR spectroscopy of environmental and biological samples

IF 1.9 3区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY
Katelyn Downey, Wolfgang Bermel, Ronald Soong, Daniel H. Lysak, Kiera Ronda, Katrina Steiner, Peter M. Costa, William W. Wolff, Venita Decker, Falko Busse, Benjamin Goerling, Agnes Haber, Myrna J. Simpson, Andre J. Simpson
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引用次数: 0

Abstract

Understanding environmental change is challenging and requires molecular-level tools to explain the physicochemical phenomena behind complex processes. Nuclear magnetic resonance (NMR) spectroscopy is a key tool that provides information on both molecular structures and interactions but is underutilized in environmental research because standard “high-field” NMR is financially and physically inaccessible for many and can be overwhelming to those outside of disciplines that routinely use NMR. “Low-field” NMR is an accessible alternative but has reduced sensitivity and increased spectral overlap, which is especially problematic for natural, heterogeneous samples. Therefore, the goal of this study is to investigate and apply innovative experiments that could minimize these challenges and improve low-field NMR analysis of environmental and biological samples. Spectral simplification (JRES, PSYCHE, singlet-only, multiple quantum filters), selective detection (GEMSTONE, DREAMTIME), and heteronuclear (reverse and CH3/CH2/CH-only HSQCs) NMR experiments are tested on samples of increasing complexity (amino acids, spruce resin, and intact water fleas) at-high field (500 MHz) and at low-field (80 MHz). A novel experiment called Doubly Selective HSQC is also introduced, wherein 1H signals are selectively detected based on the 1H and 13C chemical shifts of 1H–13C J-coupled pairs. The most promising approaches identified are the selective techniques (namely for monitoring), and the reverse and CH3-only HSQCs. Findings ultimately demonstrate that low-field NMR holds great potential for biological and environmental research. The multitude of NMR experiments available makes NMR tailorable to nearly any research need, and low-field NMR is therefore anticipated to become a valuable and widely used analytical tool moving forward.

Abstract Image

Abstract Image

低场,而不是低质量:1D简化、选择性检测和异核2D实验,用于改进环境和生物样品的低场NMR光谱。
理解环境变化具有挑战性,需要分子水平的工具来解释复杂过程背后的物理化学现象。核磁共振(NMR)光谱是一种提供分子结构和相互作用信息的关键工具,但在环境研究中没有得到充分利用,因为标准的“高场”NMR在经济和物理上对许多人来说都是不可获得的,并且对那些常规使用NMR的学科之外的人来说可能是压倒性的。“低场”NMR是一种可供选择的方法,但灵敏度降低,光谱重叠增加,这对天然、异质样品来说尤其有问题。因此,本研究的目标是研究和应用创新实验,以最大限度地减少这些挑战,并改进环境和生物样品的低场NMR分析。在高场(500 MHz)和低场(80 MHz)。还介绍了一种称为双选择性HSQC的新实验,其中基于1H-13C J耦合对的1H和13C化学位移选择性地检测1H信号。确定的最有前景的方法是选择性技术(即监测),以及反向和仅CH3的HSQC。研究结果最终表明,低场核磁共振在生物和环境研究中具有巨大的潜力。大量的核磁共振实验使核磁共振几乎可以满足任何研究需求,因此低场核磁共振有望成为一种有价值且广泛使用的分析工具。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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来源期刊
CiteScore
4.70
自引率
10.00%
发文量
99
审稿时长
1 months
期刊介绍: MRC is devoted to the rapid publication of papers which are concerned with the development of magnetic resonance techniques, or in which the application of such techniques plays a pivotal part. Contributions from scientists working in all areas of NMR, ESR and NQR are invited, and papers describing applications in all branches of chemistry, structural biology and materials chemistry are published. The journal is of particular interest not only to scientists working in academic research, but also those working in commercial organisations who need to keep up-to-date with the latest practical applications of magnetic resonance techniques.
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