Indirect Zero-Field Nuclear Magnetic Resonance Spectroscopy.

IF 6.7 1区化学 Q1 CHEMISTRY, ANALYTICAL

Analytical Chemistry Pub Date : 2025-07-25 DOI:10.1021/acs.analchem.5c00874

Kai Buckenmaier,Richard Neumann,Friedemann Bullinger,Nicolas Kempf,Pavel Povolni,Jörn Engelmann,Judith Samlow,Jan-Bernd Hövener,Klaus Scheffler,Adam Ortmeier,Markus Plaumann,Rainer Körber,Thomas Theis,Andrey N Pravdivtsev

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Abstract

This study develops the two-field correlation spectroscopy (COSY) in zero to ultralow field (ZULF) liquid state nuclear magnetic resonance (NMR). We demonstrated the successful integration of signal amplification by reversible exchange (SABRE) hyperpolarization with two-dimensional (2D) NMR spectroscopy, enabling the detection of ZULF COSY spectra with increased sensitivity. Field cycling allowed the acquisition of two-field COSY spectra at varying magnetic field strengths, including zero-field conditions. This enabled insight into both J-coupling and Zeeman-dominated regimes, benefiting from ultralow field observation sensitivity and mitigating the low-frequency noise by conducting readout at higher fields (>5 μT). Our study explores the effects of polarization transfer, apodization techniques, and the potential for further application of ZULF NMR in chemical analysis exemplified for three X-nuclei and three corresponding molecules: [1-13C]pyruvate, [15N]acetonitrile, and [3-19F]pyridine. These findings pave the way for more sensitive and cost-effective NMR spectroscopy in low-field regimes.

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间接零场核磁共振波谱。

本文研究了零至超低场（ZULF）液态核磁共振（NMR）中的双场相关光谱（COSY）。我们成功地将可逆交换（SABRE）超极化的信号放大与二维（2D）核磁共振光谱相结合，从而提高了ZULF COSY光谱的检测灵敏度。磁场循环允许在不同磁场强度下（包括零场条件下）获取双场COSY光谱。这使得j -耦合和zeeman主导的机制都能得到深入的了解，受益于超低场观测灵敏度，并通过在高场（bbb50 μT）下进行读出来减轻低频噪声。我们的研究探讨了极化转移、离体技术的影响，以及ZULF NMR在化学分析中的进一步应用潜力，以三个x核和三个相应的分子为例：[1-13C]丙酮酸酯、[15N]乙腈和[3-19F]吡啶。这些发现为在低场环境中实现更灵敏、更经济的核磁共振波谱技术铺平了道路。

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

Analytical Chemistry 化学-分析化学

CiteScore

12.10

自引率

12.20%

发文量

1949

审稿时长

1.4 months

期刊介绍： Analytical Chemistry, a peer-reviewed research journal, focuses on disseminating new and original knowledge across all branches of analytical chemistry. Fundamental articles may explore general principles of chemical measurement science and need not directly address existing or potential analytical methodology. They can be entirely theoretical or report experimental results. Contributions may cover various phases of analytical operations, including sampling, bioanalysis, electrochemistry, mass spectrometry, microscale and nanoscale systems, environmental analysis, separations, spectroscopy, chemical reactions and selectivity, instrumentation, imaging, surface analysis, and data processing. Papers discussing known analytical methods should present a significant, original application of the method, a notable improvement, or results on an important analyte.