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Updated: Jan 31, 2026

Preparation of Fungal and Plant Materials for Structural Elucidation Using Dynamic Nuclear Polarization Solid-State NMR

Preparation of Fungal and Plant Materials for Structural Elucidation Using Dynamic Nuclear Polarization Solid-State NMR

Published on: February 12, 2019

EXchangeにおける13Cセンターバンドオンリー検出（Dynamic Nuclear Polarizationを利用）

Abel Cherian Varkey¹, Kai Xue^2,3, Evgeny Nimerovsky¹

¹Department of NMR Based Structural Biology, Max Planck Institute for Multidisciplinary Sciences, Am Fassberg 11, 37077, Göttingen, Germany.

Chemphyschem : a European journal of chemical physics and physical chemistry

|January 30, 2026

Abstract:

The magic-angle spinning NMR technique, Centerband-Only Detection of EXchange (CODEX), can be used to determine the oligomerization state of molecules when combined with site-specific labeling. Calibrated with amino acid crystals, the method is successfully applied to proteins, primarily combined with ¹⁹F labeling. The use of ¹³C spins for CODEX-based oligomer determination in proteins is hampered by limited sensitivity of ¹³C spins due to the low gyromagnetic ratio of ¹³C and the presence of natural abundance background spins which contribute to the observed CODEX decay. The use of CODEX is proposed in conjunction with dynamic nuclear polarization (DNP) at low temperature to increase sensitivity. It is necessary to correct for effects of ¹³C present at natural abundance. A (PDSD) proton driven spin diffusion-based correction is demonstrated to be effective when the isotropic chemical shifts of the natural abundance background are distinct from the labeled site. Using a ¹³C-ζ-phenylalanine-labeled GB1 sample, it is demonstrated that the autocorrelation peak decay observed in a series of PDSD spectra can be utilized to correct for the additional dephasing and recover the expected CODEX decay curve. With ¹³C-γ-phenylalanine labeling and ¹³C-depleted background, mixing times up to 1500 s are demonstrated.

キーワード:

センターバンドオンリー検出（EXchange）動的核分極マジックアングルスピニングオリゴマーフェニルアラニン

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Dissolution Dynamic Nuclear Polarization Instrumentation for Real-time Enzymatic Reaction Rate Measurements by NMR

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Real-Time Metabolic Detection in Living Cells Using Hyperpolarized 13C NMR

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