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

Authors :
Downey, Katelyn
Costa, Peter M.
Ronda, Kiera
Kock, Flavio V. C.
Lysak, Daniel H.
Wolff, William W.
Steiner, Katrina
Pellizzari, Jacob
Haber, Agnes
Elliott, Colin
Busse, Venita
Busse, Falko
Goerling, Benjamin
Moraes, Tiago B.
Colnago, Luiz A.
Simpson, Andre J.
Source :
Analytical Chemistry; October 2024, Vol. 96 Issue: 41 p16260-16268, 9p
Publication Year :
2024

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, 13C-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 in vivoSSFP NMR is additionally investigated by applying 31P-SSFP to live Eisenia fetidaat high-field. In some samples, SSFP increased 13C SNR by over 2000% at both high-field and low-field compared to standard 13C NMR and enabled detection of peaks that were not observable by standard 13C 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.

Details

Language :
English
ISSN :
00032700 and 15206882
Volume :
96
Issue :
41
Database :
Supplemental Index
Journal :
Analytical Chemistry
Publication Type :
Periodical
Accession number :
ejs67564010
Full Text :
https://doi.org/10.1021/acs.analchem.4c03200