Quantitative reaction monitoring using <i>para</i>hydrogen-enhanced benchtop NMR spectroscopy

Robinson, Alastair D.; Hill-Casey, Fraser; Duckett, Simon B.; Halse, Meghan E.

doi:10.1039/d3cp06221j

Phys. Chem. Chem. Phys.

2024

DOI: 10.1039/d3cp06221j

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Quantitative reaction monitoring using parahydrogen-enhanced benchtop NMR spectroscopy

Alastair D. Robinson,

Fraser Hill-Casey,

Simon B. Duckett

et al.

Abstract: The parahydrogen-induced polarisation (PHIP) NMR signal enhancement technique is used to study H2 addition to Vaska’s complex (trans-[IrCl(CO)(PPh3)2]) with both standard high-field (9.4 T) NMR and benchtop (1 T) NMR...

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Cited by 2 publications

References 74 publications

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Homogeneous Catalysts for Hydrogenative PHIP Used in Biomedical Applications

Huynh,

Kovacs

2024

Analysis & Sensing

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At present, two competing hyperpolarization (HP) techniques, dissolution dynamic nuclear polarization (DNP) and parahydrogen (para‐H2) induced polarization (PHIP), can generate sufficiently high liquid state 13C signal enhancement for in vivo studies. PHIP utilizes the singlet spin state of para‐H2 to create non‐equilibrium spin populations. In hydrogenative PHIP, para‐H2 is irreversibly added to unsaturated precursors, typically in the presence of a homogeneous catalyst. The hydrogenation catalyst plays a crucial role in converting the singlet spin order of para‐H2 into detectable nuclear polarization. Currently, rhodium(I) bisphosphine complexes are the most widely employed catalysts for PHIP, capable of catalyzing the addition of para‐H2 to unsaturated precursors in organic solvents or aqueous media, depending on the ligand. Chiral catalysts enable the stereoselective production of hyperpolarized substrates. Ruthenium(II) piano stool complexes are capable of trans addition and are used to generate hyperpolarized fumarate. However, these catalysts systems are not optimal, and the greatest source of nuclear spin polarization loss is attributed to the mixing of singlet and triplet states of the protons derived from the para‐H2 during the hydrogenation process. Hence, future efforts should focus on enhancing the efficiency and kinetics of these catalysts.

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Homogeneous Catalysts for Hydrogenative PHIP Used in Biomedical Applications

Huynh,

Kovacs

2024

Analysis & Sensing

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Hyperpolarised benchtop NMR spectroscopy for analytical applications

Silva Terra,

Taylor,

Halse

2024

Progress in Nuclear Magnetic Resonance Spectroscopy

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Quantitative reaction monitoring using parahydrogen-enhanced benchtop NMR spectroscopy

Abstract: The parahydrogen-induced polarisation (PHIP) NMR signal enhancement technique is used to study H2 addition to Vaska’s complex (trans-[IrCl(CO)(PPh3)2]) with both standard high-field (9.4 T) NMR and benchtop (1 T) NMR...

Cited by 2 publications

References 74 publications

Homogeneous Catalysts for Hydrogenative PHIP Used in Biomedical Applications

Homogeneous Catalysts for Hydrogenative PHIP Used in Biomedical Applications

Hyperpolarised benchtop NMR spectroscopy for analytical applications

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