Hyperpolarized 13C NMR Spectroscopy of Urine Samples at Natural Abundance by Quantitative Dissolution Dynamic Nuclear Polarization

Hyperpolarized nuclear magnetic resonance (NMR) offers an ensemble of methods that remarkably address the sensitivity issues of conventional NMR. Dissolution Dynamic Nuclear Polarization (d‐DNP) provides a unique and general way to detect 13C NMR signals with a sensitivity enhanced by several orders of magnitude. The expanding application scope of d‐DNP now encompasses the analysis of complex mixtures at natural 13C abundance. However, the application of d‐DNP in this area has been limited to metabolite extracts. Here, we report the first d‐DNP‐enhanced 13C NMR analysis of a biofluid ‐urine‐ at natural abundance, offering unprecedented resolution and sensitivity for this challenging type of sample. We also show that accurate quantitative information on multiple targeted metabolites can be retrieved through a standard addition procedure. Hyperpolarized 13C NMR spectroscopy by dissolution dynamic nuclear polarization provides a rich and resolved 13C metabolic profile on urine samples at natural abundance while retaining precious quantitative information using a standard addition workflow.