4.8 Article

Hyperpolarized Solution-State NMR Spectroscopy with Optically Polarized Crystals

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JOURNAL OF THE AMERICAN CHEMICAL SOCIETY
卷 144, 期 6, 页码 2511-2519

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AMER CHEMICAL SOC
DOI: 10.1021/jacs.1c09119

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Nuclear spin hyperpolarization can be transferred to target molecules through dissolution of spin-polarized pentacene-doped naphthalene crystals at room temperature and moderate magnetic fields. This method allows for enhanced NMR signals for small molecules within a time scale of 1 minute.
Nuclear spin hyperpolarization provides a promising route to overcome the challenges imposed by the limited sensitivity of nuclear magnetic resonance. Here we demonstrate that dissolution of spin-polarized pentacene-doped naphthalene crystals enables transfer of polarization to target molecules via intermolecular cross-relaxation at room temperature and moderate magnetic fields (1.45 T). This makes it possible to exploit the high spin polarization of optically polarized crystals, while mitigating the challenges of its transfer to external nuclei. With this method, we inject the highly polarized mixture into a benchtop NMR spectrometer and observe the polarization dynamics for target H-1 nuclei. Although the spectra are radiation damped due to the high naphthalene magnetization, we describe a procedure to process the data to obtain more conventional NMR spectra and extract the target nuclei polarization. With the entire process occurring on a time scale of 1 min, we observe NMR signals enhanced by factors between -200 and -1730 at 1.45 T for a range of small molecules.

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