Rapid13C NMR hyperpolarization delivered frompara-hydrogen enables the low concentration detection and quantification of sugars

Richardson, Peter M.; Iali, Wissam; Roy, Soumya Singha; Rayner, Peter J.; Halse, Meghan E.; Duckett, Simon B.

doi:10.1039/c9sc03450a

Cited by 31 publications

(34 citation statements)

References 81 publications

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“…Recently, these restrictions are being lifted through the use of relayed polarization transfer (SABRE‐Relay) [37–42] which allows polarization of molecules such as alcohols, [38] sugars, [39] silanols [40] and others [41] without their direct ligation to iridium. Similarly, the hyperpolarization of weakly donating O‐donor molecules such as pyruvate [43] and acetate [44] has been demonstrated.…”

Section: Methodsmentioning

confidence: 99%

Reversible Hyperpolarization of Ketoisocaproate Using Sulfoxide‐containing Polarization Transfer Catalysts

et al. 2020

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The substrate scope of sulfoxide‐containing magnetisation transfer catalysts is extended to hyperpolarize α‐ketoisocaproate and α‐ketoisocaproate‐1‐[13C]. This is achieved by forming [Ir(H)2(κ2‐ketoisocaproate)(N‐heterocyclic carbene)(sulfoxide)] which transfers latent magnetism from p‐H2 via the signal amplification by reversible exchange (SABRE) process. The effect of polarization transfer field on the formation of enhanced 13C magnetization is evaluated. Consequently, performing SABRE in a 0.5 μT field enabled most efficient magnetisation transfer. 13C NMR signals for α‐ketoisocaproate‐1‐[13C] in methanol‐d4 are up to 985‐fold more intense than their traditional Boltzmann derived signal intensity (0.8 % 13C polarisation). Single crystal X‐ray diffraction reveals the formation of the novel catalyst decomposition products [Ir(μ‐H)(H)2(IMes)(SO(Ph)(Me)2)]2 and [(Ir(H)2(IMes)(SO(Me)2))2(μ‐S)] when the sulfoxides methylphenylsulfoxide and dimethylsulfoxide are used respectively.

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Section: Methodsmentioning

confidence: 99%

Reversible Hyperpolarization of Ketoisocaproate Using Sulfoxide‐containing Polarization Transfer Catalysts

et al. 2020

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“…The ability to observe glucose and distinguish its isomeric forms in solution by ZULF NMR using an inexpensive and portable setup is promising, especially given recent demonstration of hyperpolarization of sugars using SABRE-Relay technique. 24 The collected spectra match the simulation for the spin systems obtained by numerical diagonalization of the density matrix performed in the SpinDynamica package (Wolfram Mathematica). 22 In general, for small biomolecules containing 13 C, 15 N, and 1 H nuclei, the whole J-spectrum is expected to be visible within the detection bandwidth of optical magnetometer since typical J-coupling values are less than 300 Hz.…”

Section: Magnetization Precession At Ultralow Fieldsmentioning

confidence: 70%

Zero- to Ultralow-Field NMR Spectroscopy of Small Biomolecules

Put¹,

Pustelny²,

Budker³

et al. 2020

Preprint

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Nuclear magnetic resonance (NMR) spectroscopy is a well-established analytical technique used to study chemicals and their transformations. However, high-eld NMR spectroscopy necessitates advanced infrastructure and even cryogen-free benchtop NMR spectrometers cannot be readily assembled from commercially available components. We demonstrate construction of a portable zero-field NMR spectrometer employing a commercially available magnetometer and investigate its applications in analytical chemistry. In particular, J-spectra of small representative biomolecules [13C]-formic acid, [1-13C]-glycine, [2,3-13C]-fumarate, and [1-13C]-D-glucose were acquired and an approach relying on the presence of a transverse magnetic eld during the detection was investigated for relaxometry purposes. We found that water relaxation time strongly depends on the concentration of dissolved D-glucose in the range of 1-10 mM suggesting opportunities for indirect assessment of glucose concentration in aqueous solutions. Extending analytical capabilities of zero-field NMR to aqueous solutions of simple biomolecules (aminoacids, sugars and metabolites) and relaxation studies of aqueous solutions of glucose highlight the analytical potential of non-invasive and portable ZULF NMR sensors for applications outside of research laboratories.

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“…Recently, the development of co-ligand strategy have expanded the scopes of SABRE where suitable ligand design route facilitated hyperpolarising highly important molecules, for example, pyruvate, acetate and glucose. [14,20,42] Earlier, Shchepin et al, has described a similar approach called 'pyridine aided activation' that improves the efficacy of SABRE process to nicotinamide. [43] This stems from the fact that a suitable coligand can provide the desired stabilisation to the active species when a substrate binds to the iridium metal centre very weakly.…”

Section: Co-ligand Strategymentioning

confidence: 99%

¹⁵N hyperpolarisation of the antiprotozoal drug ornidazole by Signal Amplification By Reversible Exchange in aqueous medium

Iali

Moustafa

Dagys

et al. 2021

Magnetic Reson in Chemistry

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Signal amplification by reversible exchange (SABRE) offers a cost-effective route to boost nuclear magnetic resonance (NMR) signal by several orders of magnitude by employing readily available para-hydrogen as a source of hyperpolarisation. Although 1 H spins have been the natural choice of SABRE hyperpolarisation since its inception due to its simplicity and accessibility, limited spin lifetimes of 1 H makes it harder to employ them in a range of timedependent NMR experiments. Heteronuclear spins, for example, 13 C and 15 N, in general have much longer T 1 lifetimes and thereby are found to be more suitable for hyperpolarised biological applications as demonstrated previously by para-hydrogen induced polarisation (PHIP) and dynamic nuclear

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Rapid¹³C NMR hyperpolarization delivered frompara-hydrogen enables the low concentration detection and quantification of sugars

Abstract: The monosaccharides glucose and fructose are rapidly detected and quantified by13C NMR in conjunction with the hyperpolarisation method signal amplification by reversible exchange-relay.

Cited by 31 publications

References 81 publications

Reversible Hyperpolarization of Ketoisocaproate Using Sulfoxide‐containing Polarization Transfer Catalysts

Reversible Hyperpolarization of Ketoisocaproate Using Sulfoxide‐containing Polarization Transfer Catalysts

Zero- to Ultralow-Field NMR Spectroscopy of Small Biomolecules

¹⁵N hyperpolarisation of the antiprotozoal drug ornidazole by Signal Amplification By Reversible Exchange in aqueous medium

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Rapid13C NMR hyperpolarization delivered frompara-hydrogen enables the low concentration detection and quantification of sugars

Abstract: The monosaccharides glucose and fructose are rapidly detected and quantified by13C NMR in conjunction with the hyperpolarisation method signal amplification by reversible exchange-relay.

Cited by 31 publications

References 81 publications

Reversible Hyperpolarization of Ketoisocaproate Using Sulfoxide‐containing Polarization Transfer Catalysts

Reversible Hyperpolarization of Ketoisocaproate Using Sulfoxide‐containing Polarization Transfer Catalysts

Zero- to Ultralow-Field NMR Spectroscopy of Small Biomolecules

15N hyperpolarisation of the antiprotozoal drug ornidazole by Signal Amplification By Reversible Exchange in aqueous medium

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Rapid¹³C NMR hyperpolarization delivered frompara-hydrogen enables the low concentration detection and quantification of sugars

¹⁵N hyperpolarisation of the antiprotozoal drug ornidazole by Signal Amplification By Reversible Exchange in aqueous medium