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

Author

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., and Simpson, Andre J.

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.

Published
2024
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3. Exploration of Materials for Three-Dimensional NMR Microcoil Production via CNC Micromilling and Laser Etching.

Author

Moxley-Paquette, Vincent, Pellizzari, Jacob, Lane, Daniel, Steiner, Katrina, Costa, Peter M., Wolff, William W., Lysak, Daniel H., Ghosh Biswas, Rajshree, Downey, Katelyn, Ronda, Kiera, Soong, Ronald, Zverev, Dmitri, De Castro, Peter, Frei, Thomas, Al Adwan-Stojilkovic, Danijela, Graf, Stephan, Gloor, Simon, Schmidig, Daniel, Kuemmerle, Rainer, and Kuehn, Till

Published
2024
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5. Low‐field, not low quality: 1D simplification, selective detection, and heteronuclear 2D experiments for improving low‐field NMR spectroscopy of environmental and biological samples.

Author

Downey, Katelyn, Bermel, Wolfgang, Soong, Ronald, Lysak, Daniel H., Ronda, Kiera, Steiner, Katrina, Costa, Peter M., Wolff, William W., Decker, Venita, Busse, Falko, Goerling, Benjamin, Haber, Agnes, Simpson, Myrna J., and Simpson, Andre J.

Subjects
NUCLEAR magnetic resonance spectroscopy, ENVIRONMENTAL sampling, ENVIRONMENTAL research, SPECTRAL sensitivity, NUCLEAR magnetic resonance, CLADOCERA
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 FROM AUTHOR]

Published
2024
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6. 13C‐depleted algae as food: Permitting background free in‐vivo nuclear magnetic resonance of Daphnia magna at natural abundance

Author

Wolff, William W., primary, Pellizzari, Jacob, additional, Soong, Ronald, additional, Lysak, Daniel H., additional, Steiner, Katrina, additional, Ronda, Kiera, additional, Costa, Peter, additional, Downey, Katelyn, additional, Moxley‐Paquette, Vincent, additional, Suszczynski, Chris, additional, Boehmer, Steven, additional, Prat, Jacob R., additional, and Simpson, Andre J., additional

Published
2023
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7. Low‐field, not low quality: 1D simplification, selective detection, and heteronuclear 2D experiments for improving low‐field NMR spectroscopy of environmental and biological samples

Author

Downey, Katelyn, primary, Bermel, Wolfgang, additional, Soong, Ronald, additional, Lysak, Daniel H., additional, Ronda, Kiera, additional, Steiner, Katrina, additional, Costa, Peter M., additional, Wolff, William W., additional, Decker, Venita, additional, Busse, Falko, additional, Goerling, Benjamin, additional, Haber, Agnes, additional, Simpson, Myrna J., additional, and Simpson, Andre J., additional

Published
2023
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8. Development of Low-Magnetic Susceptibility Microcoils via 5-Axis Machining for Analysis of Biological and Environmental Samples

Author

Moxley-Paquette, Vincent, primary, Lane, Daniel, additional, Steiner, Katrina, additional, Downey, Katelyn, additional, Costa, Peter M., additional, Lysak, Daniel H., additional, Ronda, Kiera, additional, Soong, Ronald, additional, Zverev, Dimitri, additional, De Castro, Peter, additional, Frei, Thomas, additional, Stuessi, Juerg, additional, Al Adwan-Stojilkovic, Danijela, additional, Graf, Stephan, additional, Gloor, Simon, additional, Schmidig, Daniel, additional, Kuemmerle, Rainer, additional, Kuehn, Till, additional, Busse, Falko, additional, Utz, Marcel, additional, Lacerda, Andressa, additional, Nashman, Ben, additional, Albert, Larry, additional, Anders, Jens, additional, and Simpson, André J., additional

Published
2023
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9. Exploring the Potential of Broadband Complementary Metal Oxide Semiconductor Micro-Coil Nuclear Magnetic Resonance for Environmental Research

Author

Lysak, Daniel H., primary, Grisi, Marco, additional, Marable, Kathryn, additional, Conley, Gaurasundar M., additional, Michal, Carl A., additional, Moxley-Paquette, Vincent, additional, Wolff, William W., additional, Downey, Katelyn, additional, Kock, Flavio V. C., additional, Costa, Peter M., additional, Ronda, Kiera, additional, Moraes, Tiago B., additional, Steiner, Katrina, additional, Colnago, Luiz A., additional, and Simpson, Andre J., additional

Published
2023
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11. 13C‐depleted algae as food: Permitting background free in‐vivo nuclear magnetic resonance of Daphnia magna at natural abundance.

Author

Wolff, William W., Pellizzari, Jacob, Soong, Ronald, Lysak, Daniel H., Steiner, Katrina, Ronda, Kiera, Costa, Peter, Downey, Katelyn, Moxley‐Paquette, Vincent, Suszczynski, Chris, Boehmer, Steven, Prat, Jacob R., and Simpson, Andre J.

Subjects
NUCLEAR magnetic resonance, DAPHNIA magna, ALGAE, RESEARCH personnel, GLUTEN-free foods
Abstract

This article explores the use of 13C-depleted algae as a food source for in-vivo NMR experiments on organisms like Daphnia magna. By feeding the organisms with this algae, researchers were able to eliminate interference from the food source in NMR spectra, allowing for more accurate analysis of the organisms' responses to stressors. The study provides details on the experimental methods used and presents qualitative and quantitative analyses of the 13C-depleted algae. The authors suggest that this approach could also be applied to study xenobiotic transformations in organisms and expand the scope of environmental NMR studies. The research was funded by various organizations. [Extracted from the article]

Published
2024
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