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采用高场和低场 NMR 的稳态自由进动(SSFP)NMR 光谱法提高复杂环境和生物样本的灵敏度。

Steady-State Free Precession (SSFP) NMR Spectroscopy for Sensitivity Enhancement in Complex Environmental and Biological Samples Using Both High-Field and Low-Field NMR.

机构信息

Environmental NMR Centre, University of Toronto Scarborough, Toronto, Ontario M1C 1A4, Canada.

Bruker Biospin GmbH, Ettlingen 76275, Germany.

出版信息

Anal Chem. 2024 Oct 15;96(41):16260-16268. doi: 10.1021/acs.analchem.4c03200. Epub 2024 Oct 1.

Abstract

Nuclear magnetic resonance (NMR) spectroscopy is a valuable and complementary tool in environmental research, but it is underutilized due to the cost, size, and maintenance requirements of standard "high-field" NMR spectrometers. "Low-field" NMR spectrometers are a financially and physically accessible alternative, but their lower sensitivity and increased spectral overlap limit the analysis of heterogeneous environmental/biological media, especially with fast-relaxing samples that produce broad, low-intensity spectra. This study therefore investigates the potential of the steady-state free precession (SSFP) experiment to enhance signal-to-noise ratios (SNRs) of fast-relaxing, complex samples at both high- and low-field. SSFP works by obtaining steady-state transverse signal using a train of equally spaced radiofrequency pulses with the same flip angle and a time between pulses less than the transverse relaxation time, allowing for thousands of scans to be summed in a short time period. Here, C-SSFP is applied to samples of varying complexity (egg white, dissolved organic matter, and crude oil) at low-field and at high-field for testing and comparison. The potential of SSFP NMR is additionally investigated by applying P-SSFP to live at high-field. In some samples, SSFP increased C SNR by over 2000% at both high-field and low-field compared to standard C NMR and enabled detection of peaks that were not observable by standard C NMR. Ultimately, SSFP holds great potential for improving analysis of fast-relaxing, complex samples, which could in turn make low-field NMR spectroscopy a more effective tool not only in environmental/biological research but also in numerous other disciplines.

摘要

核磁共振(NMR)光谱学是环境研究中一种有价值且互补的工具,但由于标准“高场”NMR 光谱仪的成本、体积和维护要求,其应用受到限制。“低场”NMR 光谱仪是一种经济实惠且易于获取的替代方案,但它们的灵敏度较低,谱线重叠增加,限制了对异质环境/生物介质的分析,特别是对快速弛豫的样品,这些样品会产生宽而强度低的谱线。因此,本研究调查了稳态自由进动(SSFP)实验在高低场增强快速弛豫、复杂样品的信噪比(SNR)的潜力。SSFP 通过使用相同翻转角的等间隔射频脉冲序列获得稳态横向信号,并使脉冲之间的时间小于横向弛豫时间,从而在短时间内可以累加数千次扫描。在这里,C-SSFP 应用于不同复杂度的样品(蛋清、溶解有机物和原油),在低场和高场进行测试和比较。通过在高场应用 P-SSFP,进一步研究了 SSFP NMR 的潜力。在一些样品中,与标准 C NMR 相比,SSFP 在高低场均可将 C SNR 提高 2000%以上,并能够检测到标准 C NMR 无法检测到的峰。总之,SSFP 具有很大的潜力,可以改善快速弛豫、复杂样品的分析,这反过来又可以使低场 NMR 光谱学不仅在环境/生物研究中,而且在许多其他领域成为一种更有效的工具。

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