Challenges and Advances in the Application of Dynamic Nuclear Polarization to Liquid-State NMR Spectroscopy

Abhyankar, Nandita; Szalai, Veronika A.

doi:10.1021/acs.jpcb.0c10937

Cited by 20 publications

(11 citation statements)

References 178 publications

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“…The instrumentation required for OE-DNP depends on the magnetic field used for the microwave excitation and NMR detection. 170 If the OE-DNP experiment is performed at low magnetic fields (0.3 T) to achieve optimal coupling factors, standard X-band EPR equipment can be used for the irradiation of the electron spin of the free radical. With NMR detection at the same field the challenge is to obtain enough spectral resolution, especially for proton spins.…”

Section: Practical Aspectsmentioning

confidence: 99%

Spin Hyperpolarization in Modern Magnetic Resonance

et al. 2023

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Magnetic resonance techniques are successfully utilized in a broad range of scientific disciplines and in various practical applications, with medical magnetic resonance imaging being the most widely known example. Currently, both fundamental and applied magnetic resonance are enjoying a major boost owing to the rapidly developing field of spin hyperpolarization. Hyperpolarization techniques are able to enhance signal intensities in magnetic resonance by several orders of magnitude, and thus to largely overcome its major disadvantage of relatively low sensitivity. This provides new impetus for existing applications of magnetic resonance and opens the gates to exciting new possibilities. In this review, we provide a unified picture of the many methods and techniques that fall under the umbrella term "hyperpolarization" but are currently seldom perceived as integral parts of the same field. Specifically, before delving into the individual techniques, we provide a detailed analysis of the underlying principles of spin hyperpolarization. We attempt to uncover and classify the origins of hyperpolarization, to establish its sources and the specific mechanisms that enable the flow of polarization from a source to the target spins. We then give a more detailed analysis of individual hyperpolarization techniques: the mechanisms by which they work, fundamental and technical requirements, characteristic applications, unresolved issues, and possible future directions. We are seeing a continuous growth of activity in the field of spin hyperpolarization, and we expect the field to flourish as new and improved hyperpolarization techniques are implemented. Some key areas for development are in prolonging polarization lifetimes, making hyperpolarization techniques more generally applicable to chemical/biological systems, reducing the technical and equipment requirements, and creating more efficient excitation and detection schemes. We hope this review will facilitate the sharing of knowledge between subfields within the broad topic of hyperpolarization, to help overcome existing challenges in magnetic resonance and enable novel applications.

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Section: Practical Aspectsmentioning

confidence: 99%

Spin Hyperpolarization in Modern Magnetic Resonance

et al. 2023

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“…Implementing nuclear hyperpolarization in a microfluidic context is currently a lively area of research. 14,15…”

Section: Discussionmentioning

confidence: 99%

Hyphenated structural identification of additives in transmission fluids

Zelst¹,

Romanuka

Kentgens³

2022

Analyst

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“…Dynamic nuclear polarization (DNP) − relies on the fact that microwave irradiation of an electron paramagnetic agent (EPA, which is in the form of an organic free radical) together with the target substance, both of which are dispersed in a glassy state at low temperature of ∼ 1 K, leads to a close to unit polarization transfer from the electrons to the nuclei of interest; as a result, an increase of the nuclear polarization occurs, improving the sensitivity of the resonances when detected by NMR spectroscopy. The polarization transfer in the dissolution DNP (dDNP) technique , is often carried out in a separate system, e.g., with a relatively low magnetic field of 3.35 T and an irradiation frequency of 94 GHz, although higher magnetic fields (6.7 T) and irradiation frequencies (188 GHz) have also been used .…”

Section: Technological Developmentsmentioning

confidence: 99%

Primary Structure of Glycans by NMR Spectroscopy

Fontana

Widmalm

2023

Chem. Rev.

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Glycans, carbohydrate molecules in the realm of biology, are present as biomedically important glycoconjugates and a characteristic aspect is that their structures in many instances are branched. In determining the primary structure of a glycan, the sugar components including the absolute configuration and ring form, anomeric configuration, linkage(s), sequence, and substituents should be elucidated. Solution state NMR spectroscopy offers a unique opportunity to resolve all these aspects at atomic resolution. During the last two decades, advancement of both NMR experiments and spectrometer hardware have made it possible to unravel carbohydrate structure more efficiently. These developments applicable to glycans include, inter alia, NMR experiments that reduce spectral overlap, use selective excitations, record tilted projections of multidimensional spectra, acquire spectra by multiple receivers, utilize polarization by fast-pulsing techniques, concatenate pulse-sequence modules to acquire several spectra in a single measurement, acquire pure shift correlated spectra devoid of scalar couplings, employ stable isotope labeling to efficiently obtain homo-and/or heteronuclear correlations, as well as those that rely on dipolar cross-correlated interactions for sequential information. Refined computer programs for NMR spin simulation and chemical shift prediction aid the structural elucidation of glycans, which are notorious for their limited spectral dispersion. Hardware developments include cryogenically cold probes and dynamic nuclear polarization techniques, both resulting in enhanced sensitivity as well as ultrahigh field NMR spectrometers with a 1 H NMR resonance frequency higher than 1 GHz, thus improving resolution of resonances. Taken together, the developments have made and will in the future make it possible to elucidate carbohydrate structure in great detail, thereby forming the basis for understanding of how glycans interact with other molecules.

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Challenges and Advances in the Application of Dynamic Nuclear Polarization to Liquid-State NMR Spectroscopy

Cited by 20 publications

References 178 publications

Spin Hyperpolarization in Modern Magnetic Resonance

Spin Hyperpolarization in Modern Magnetic Resonance

Hyphenated structural identification of additives in transmission fluids

Primary Structure of Glycans by NMR Spectroscopy

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