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Hyperpolarized 13C Metabolic Magnetic Resonance Spectroscopy and Imaging
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Trityl-Nitroxide Triradicals for Efficient High-Field Dynamic Nuclear Polarization.

Jiaxin Zhou1, Andrei Gurinov2, Mang Huang1

  • 1The Province and Ministry Co-Sponsored Collaborative Innovation Center for Medical Epigenetics, Tianjin Key Laboratory on Technologies Enabling Development of Clinical Therapeutics and Diagnostics, School of Pharmacy, Tianjin Medical University, Tianjin 300070, P. R. China.

Analytical Chemistry
|May 25, 2026
PubMed
Summary
This summary is machine-generated.

New multiradical polarizing agents (PAs) significantly enhance solid-state NMR sensitivity by reducing polarization buildup times. The triradical cMRPol-2 shows superior DNP efficiency, demonstrating potential for biological applications.

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Area of Science:

  • Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy
  • Dynamic Nuclear Polarization (DNP) enhancement techniques
  • Materials science of polarizing agents

Background:

  • Dynamic Nuclear Polarization (DNP) is crucial for overcoming low sensitivity in solid-state NMR.
  • Advancement of DNP relies on rational design of polarizing agents (PAs).
  • Conflicting reports on multiradical PAs necessitate further investigation.

Purpose of the Study:

  • To develop and evaluate novel multiradical-based PAs (MRPols and cMRPols) for enhanced DNP performance.
  • To investigate the relationship between PA structure, physicochemical properties, and DNP efficiency.
  • To assess the biological application potential of the optimized PAs.

Main Methods:

  • Synthesis of two series of multiradical PAs: MRPols and cMRPols, featuring trityl OX063 tethered to TEMPO or spirocyclohexanoyl nitroxides (SCHN).
  • Solid-state DNP experiments on [13C-15N] proline at 18.8 T to measure polarization buildup times (TB) and efficiency (εon/off/√TB).
  • Correlation analysis of DNP performance with radical moiety properties and inter-radical interactions; evaluation in cell membrane fractions.

Main Results:

  • Linked nitroxides in PAs (MRPol-2, cMRPol-2) significantly reduced polarization buildup times compared to single-nitroxide PAs.
  • The SCHN-based triradical cMRPol-2 exhibited a short TB (3.24 s) and high εon/off (160), yielding superior DNP efficiency.
  • cMRPol-2 demonstrated 65% and 35% DNP efficiency improvements over biradical cMRPol-1 and benchmark SNAPol-1, respectively.
  • cMRPol-2 showed high DNP efficiency in cell membrane fractions, good bioreduction resistance, and minimal protein binding.

Conclusions:

  • The hetero triradical design, balancing TB and εon/off, is an effective strategy for optimizing DNP efficiency at high magnetic fields.
  • cMRPol-2 represents a highly efficient PA with significant potential for biological applications in solid-state NMR.
  • This work provides a pathway for the rational design of advanced PAs for DNP.