Ultrafast 2D ¹H–¹H NMR spectroscopy of DNP-hyperpolarised substrates for the analysis of mixtures

Abstract

We show that TOCSY and multiple-quantum (MQ) 2D NMR spectra can be obtained for mixtures of substrates hyperpolarised by dissolution dynamic nuclear polarisation (D-DNP). This is achieved by combining optimised...

Absolute Metabolite Quantification Using Pure Shift NMR: Toward Quantitative Metabolic Profiling of Aqueous Biological Samples

“…This might, for instance, be the case in the foreseeable future with hyperpolarization methods, or more generally, any technique providing sensitivity enhancement. We note that the formalism used in this work to calibrate pure shift data will allow accounting for the implementation of new preparation steps, such as hyperpolarization, which paves the way to sensitivity improvements that should allow for the quantitative analysis of challenging biological samples. − …”

NMR Metabolomics Methods for Investigating Disease

“…And the combination of ultrafast experiments with hyperpolarization promises important applications in metabolomics. Recently, such experiments were demonstrated for mixtures of substrates . Here, TOCSY (total correlation spectroscopy) and multiple quantum 2D NMR spectra of hyperpolarized specimens were obtained based on dissolution DNP (dDNP) in which the sample is dissolved in a radical containing matrix that is hyperpolarized using microwave irradiation.…”

NMR methods for the analysis of mixtures

“…164 The combination of UF 2D NMR and single-shot hyperpolarisation methods is particularly promising for mixture analysis. 102,[165][166][167][168][169] This is notably the case for dissolution DNP, which provides high polarisation levels for a broad range of molecules, but which is also not generally compatible with multi-scan pulse sequences. For example, the mixing step of a COSY pulse sequence would completely deplete the enhanced polarisation.…”

“…102,165,171 Provided that the delay between dissolution and detection can be made sufficiently short, homonuclear 2D spectra can also be recorded in a single scan with 1 H hyperpolarisation. 169,172 This combination is not limited to 2D spectroscopy, and Guduff et al have shown that reliable 2D DOSY spectra can also be recorded in a singlescan from DNP-hyperpolarised substrates. 167…”