Fast magic angle spinning for the characterization of milligram quantities of organic and biological solids at natural isotopic abundance by 13C–13C correlation DNP-enhanced NMR

Adam N. Smith; Rania Harrabi; Thomas Halbritter; Daniel Lee; Fabien Aussenac; Patrick C.A. van der Wel; Sabine Hediger; Snorri Þór Sigurðsson; Gaël De Paëpe

doi:10.1016/j.ssnmr.2022.101850

Fast magic angle spinning for the characterization of milligram quantities of organic and biological solids at natural isotopic abundance by ¹³C–¹³C correlation DNP-enhanced NMR

Adam N. Smith, Rania Harrabi, Thomas Halbritter, Daniel Lee, Fabien Aussenac, Patrick C.A. van der Wel, Sabine Hediger, Snorri Þór Sigurðsson, Gaël De Paëpe

University of Iceland

Research output: Contribution to journal › Article › peer-review

Abstract

We show that multidimensional solid-state NMR ¹³C–¹³C correlation spectra of biomolecular assemblies and microcrystalline organic molecules can be acquired at natural isotopic abundance with only milligram quantities of sample. These experiments combine fast Magic Angle Spinning of the sample, low-power dipolar recoupling, and dynamic nuclear polarization performed with AsymPol biradicals, a recently introduced family of polarizing agents. Such experiments are essential for structural characterization as they provide short- and long-range distance information. This approach is demonstrated on diverse sample types, including polyglutamine fibrils implicated in Huntington's disease and microcrystalline ampicillin, a small antibiotic molecule.

Original language	English
Article number	101850
Journal	Solid State Nuclear Magnetic Resonance
Volume	123
DOIs	https://doi.org/10.1016/j.ssnmr.2022.101850
Publication status	Published - Feb 2023

Bibliographical note

Other keywords

Dynamic nuclear polarization
Fast MAS
MAS-DNP
Magnetic Resonance Imaging
Magnetic Resonance Spectroscopy/methods
Nuclear magnetic resonance
Pharmaceuticals

Access to Document

10.1016/j.ssnmr.2022.101850

Cite this

Smith, A. N., Harrabi, R., Halbritter, T., Lee, D., Aussenac, F., van der Wel, P. C. A., Hediger, S., Sigurðsson, S. Þ., & De Paëpe, G. (2023). Fast magic angle spinning for the characterization of milligram quantities of organic and biological solids at natural isotopic abundance by ¹³C–¹³C correlation DNP-enhanced NMR. Solid State Nuclear Magnetic Resonance, 123, Article 101850. https://doi.org/10.1016/j.ssnmr.2022.101850

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title = "Fast magic angle spinning for the characterization of milligram quantities of organic and biological solids at natural isotopic abundance by 13C–13C correlation DNP-enhanced NMR",

abstract = "We show that multidimensional solid-state NMR 13C–13C correlation spectra of biomolecular assemblies and microcrystalline organic molecules can be acquired at natural isotopic abundance with only milligram quantities of sample. These experiments combine fast Magic Angle Spinning of the sample, low-power dipolar recoupling, and dynamic nuclear polarization performed with AsymPol biradicals, a recently introduced family of polarizing agents. Such experiments are essential for structural characterization as they provide short- and long-range distance information. This approach is demonstrated on diverse sample types, including polyglutamine fibrils implicated in Huntington's disease and microcrystalline ampicillin, a small antibiotic molecule.",

keywords = "Dynamic nuclear polarization, Fast MAS, MAS-DNP, Magnetic Resonance Imaging, Magnetic Resonance Spectroscopy/methods, Nuclear magnetic resonance, Pharmaceuticals",

author = "Smith, \{Adam N.\} and Rania Harrabi and Thomas Halbritter and Daniel Lee and Fabien Aussenac and \{van der Wel\}, \{Patrick C.A.\} and Sabine Hediger and Sigur{\dh}sson, \{Snorri {\TH}{\'o}r\} and \{De Pa{\"e}pe\}, Ga{\"e}l",

year = "2023",

month = feb,

doi = "10.1016/j.ssnmr.2022.101850",

language = "English",

volume = "123",

journal = "Solid State Nuclear Magnetic Resonance",

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Smith, AN, Harrabi, R, Halbritter, T, Lee, D, Aussenac, F, van der Wel, PCA, Hediger, S, Sigurðsson, SÞ & De Paëpe, G 2023, 'Fast magic angle spinning for the characterization of milligram quantities of organic and biological solids at natural isotopic abundance by ¹³C–¹³C correlation DNP-enhanced NMR', Solid State Nuclear Magnetic Resonance, vol. 123, 101850. https://doi.org/10.1016/j.ssnmr.2022.101850

Fast magic angle spinning for the characterization of milligram quantities of organic and biological solids at natural isotopic abundance by ¹³C–¹³C correlation DNP-enhanced NMR. / Smith, Adam N.; Harrabi, Rania; Halbritter, Thomas et al.
In: Solid State Nuclear Magnetic Resonance, Vol. 123, 101850, 02.2023.

Research output: Contribution to journal › Article › peer-review

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AU - Smith, Adam N.

AU - Harrabi, Rania

AU - Halbritter, Thomas

AU - Lee, Daniel

AU - Aussenac, Fabien

AU - van der Wel, Patrick C.A.

AU - Hediger, Sabine

AU - Sigurðsson, Snorri Þór

AU - De Paëpe, Gaël

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KW - Fast MAS

KW - MAS-DNP

KW - Magnetic Resonance Imaging

KW - Magnetic Resonance Spectroscopy/methods

KW - Nuclear magnetic resonance

KW - Pharmaceuticals

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