An inexpensive apparatus for up to 97% continuous-flow parahydrogen enrichment using liquid helium

Du, Yong; Zhou, Ronghui; Ferrer, Maria-Jose; Chen, Minda; Graham, John T.; Malphurs, Bill; Labbe, Greg; Huang, Wenyu; Bowers, Clifford R.

doi:10.1016/j.jmr.2020.106869

Cited by 14 publications

(22 citation statements)

References 14 publications

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“…Such labeling was exemplified with ab ioactive derivative of the sunflower trypsin inhibitor-1 (SFTI-1). [13] SFTI-1, adisulfide-bridged cyclic tetradecapeptide (Figures 5 and 6) found in nature, [36][37][38][69][70][71] is av ery potent inhibitor of serine protease trypsin [71,72] and is applied for tumor diagnostics and treatment. [73,74] Manual ALTADENA [37] experiments with ap ropargylfunctionalized tyrosine mutant of SFTI-1 [68] revealed a70-fold signal enhancement of the protons in the O-allyl-l-tyrosyl unit, with the inhibitory activity of the peptide also preserved.…”

Section: Phip Of Peptides By Side-chain Hydrogenation (Phip-label)mentioning

confidence: 99%

Parahydrogen‐Induced Polarization of Amino Acids

et al. 2021

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Nuclear magnetic resonance (NMR) has become a universal method for biochemical and biomedical studies, including metabolomics, proteomics, and magnetic resonance imaging (MRI). By increasing the signal of selected molecules, the hyperpolarization of nuclear spin has expanded the reach of NMR and MRI even further (e.g. hyperpolarized solid‐state NMR and metabolic imaging in vivo). Parahydrogen (pH2) offers a fast and cost‐efficient way to achieve hyperpolarization, and the last decade has seen extensive advances, including the synthesis of new tracers, catalysts, and transfer methods. The portfolio of hyperpolarized molecules now includes amino acids, which are of great interest for many applications. Here, we provide an overview of the current literature and developments in the hyperpolarization of amino acids and peptides.

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Section: Phip Of Peptides By Side-chain Hydrogenation (Phip-label)mentioning

confidence: 99%

Parahydrogen‐Induced Polarization of Amino Acids

et al. 2021

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“…pH 2 fraction, f pH 2 , of 90 % and above is produced by PHGs with single-or dual-stage cryostats run by helium compres- (Hövener et al, 2013), (3) (Feng et al, 2012), (4) HyperSpin-PHG (Meier et al, 2019), (5) automated PHG (Birchall et al, 2020), (6) He-dewar PHG (Du et al, 2020), (7) U-shaped PHG (Kiryutin et al, 2017), (8) economical PHG (Jeong et al, 2018), ( 9) glass-trap PHG (Gamliel et al, 2010) (Haynes, 2011). All these PHGs were specifically designed with PHIP (parahydrogeninduced polarization) in mind, meaning for a relatively low scale of production and in-lab use (not for industry).…”

Section: Technology Reviewmentioning

confidence: 99%

“…The compressed wool insets have a length of 20 mm. Wool as a particulate filter was used before in another PHG (Du et al, 2020). During the 6 months of weekly use of our generator, there was no sign of a moving catalyst.…”

Section: D Design Of Phgmentioning

confidence: 99%

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Open-source, partially 3D-printed, high-pressure (50-bar) liquid-nitrogen-cooled parahydrogen generator

2021

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Abstract. The signal of magnetic resonance imaging (MRI) can be enhanced by several orders of magnitude using hyperpolarization. In comparison to a broadly used dynamic nuclear polarization (DNP) technique that is already used in clinical trials, the parahydrogen (pH2)-based hyperpolarization approaches are less cost-intensive, are scalable, and offer high throughput. However, a pH2 generator is necessary. Available commercial pH2 generators are relatively expensive (EUR 10 000–150 000). To facilitate the spread of pH2-based hyperpolarization studies, here we provide the blueprints and 3D models as open-source for a low-cost (EUR <3000) 50-bar liquid-nitrogen-cooled pH2 generator.

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“…Note that had the experiments been performed using 100 % para-enrichment, all of the signal enhancements would have been approximately three times greater. [28] A limited optimisation of the CF ALTADENA experimental conditions was performed by conducting the hydrogenation at several different flow rates and temperatures. The effect of temperature was studied at two different temperatures, 50°C and 80°C, while keeping the liquid flow rate constant at 1.5 mL/ min, and the results are shown in Figure 4.…”

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confidence: 99%

Toward Continuous‐Flow Hyperpolarisation of Metabolites via Heterogenous Catalysis, Side‐Arm‐Hydrogenation, and Membrane Dissolution of Parahydrogen

et al. 2021

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Side‐arm hydrogenation (SAH) by homogeneous catalysis has extended the reach of the parahydrogen enhanced NMR technique to key metabolites such as pyruvate. However, homogeneous hydrogenation requires rapid separation of the dissolved catalyst and purification of the hyperpolarised species with a purity sufficient for safe in‐vivo use. An alternate approach is to employ heterogeneous hydrogenation in a continuous‐flow reactor, where separation from the solid catalysts is straightforward. Using a TiO2‐nanorod supported Rh catalyst, we demonstrate continuous‐flow parahydrogen enhanced NMR by heterogeneous hydrogenation of a model SAH precursor, propargyl acetate, at a flow rate of 1.5 mL/min. Parahydrogen gas was introduced into the flowing solution phase using a novel tube‐in‐tube membrane dissolution device. Without much optimization, proton NMR signal enhancements of up to 297 (relative to the thermal equilibrium signals) at 9.4 Tesla were shown to be feasible on allyl‐acetate at a continuous total yield of 33 %. The results are compared to those obtained with the standard batch‐mode technique of parahydrogen bubbling through a suspension of the same catalyst.

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An inexpensive apparatus for up to 97% continuous-flow parahydrogen enrichment using liquid helium

Cited by 14 publications

References 14 publications

Parahydrogen‐Induced Polarization of Amino Acids

Parahydrogen‐Induced Polarization of Amino Acids

Open-source, partially 3D-printed, high-pressure (50-bar) liquid-nitrogen-cooled parahydrogen generator

Toward Continuous‐Flow Hyperpolarisation of Metabolites via Heterogenous Catalysis, Side‐Arm‐Hydrogenation, and Membrane Dissolution of Parahydrogen

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