A multi-sample 94GHz dissolution dynamic-nuclear-polarization system

Batel, Michael; Krajewski, Marcin; Weiss, Kilian; Däpp, Alexander; Hunkeler, Andreas; Gimersky, M.; Pruessmann, Klaas P.; Boesiger, Peter; Meier, Beat H.; Kozerke, Sebastian; Ernst, Matthias

doi:10.1016/j.jmr.2011.11.002

Cited by 69 publications

(89 citation statements)

References 25 publications

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“…The throughput of polarized samples can be increased with a multiple-sample approach. The samples can be polarized simultaneously and subsequently dissolved at wish one after the other [9,10].…”

Section: Dnp Polarizermentioning

confidence: 99%

“…D-DNP has rapidly found a 'killer' application in in vivo MRI. The high signal-to-noise ratio provided by d-DNP for 13 C labeled molecules has enabled the observation of hyperpolarized [1][2][3][4][5][6][7][8][9][10][11][12][13] C pyruvate in humans shortly after infusion, and its enzymatic in-cello conversion into 1-…”

Section: Dissolution and Liquid State Mri And Nmr Applicationsmentioning

confidence: 99%

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Optimizing dissolution dynamic nuclear polarization

Bornet

2016

Journal of Magnetic Resonance

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Section: Dnp Polarizermentioning

confidence: 99%

Section: Dissolution and Liquid State Mri And Nmr Applicationsmentioning

confidence: 99%

Optimizing dissolution dynamic nuclear polarization

Bornet

2016

Journal of Magnetic Resonance

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“…22,23 Nitroxide free radicals have relatively wide EPR linewidths, which are better suited for DNP of high-γ nuclei such as 1 H spins and also provide decent polarization levels for low-γ nuclei such as 13 C. 24 This class of free radicals maintain their popularity by being comparatively inexpensive, highly water soluble, easily scavenged, and effective for cross polarization DNP. [25][26][27][28][29][30] Additionally, the DNP efficiency of these radicals may be increased through other means such as deuteration of the glassing matrix. [31][32][33] Meanwhile, the trityls, particularly OX063, which have some of the narrowest EPR linewidths among free radicals, were found to be excellent polarizing agents for low-γ nuclei like 13 C. 16,34 When using these radicals, DNP enhancements may be improved further by the addition of trace amounts of gadolinium.…”

Section: Introductionmentioning

confidence: 99%

Influence of Dy3+ and Tb3+ doping on 13C dynamic nuclear polarization

Niedbalski

Parish

Kiswandhi

et al. 2017

The Journal of Chemical Physics

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Dynamic nuclear polarization (DNP) is a technique that uses a microwave-driven transfer of high spin alignment from electrons to nuclear spins. This is most effective at low temperature and high magnetic field, and with the invention of the dissolution method, the amplified nuclear magnetic resonance (NMR) signals in the frozen state in DNP can be harnessed in the liquid-state at physiologically acceptable temperature for in vitro and in vivo metabolic studies. A current optimization practice in dissolution DNP is to dope the sample with trace amounts of lanthanides such as Gd 3+ or Ho 3+ , which further improves the polarization. While Gd 3+ and Ho 3+ have been optimized for use in dissolution DNP, other lanthanides have not been exhaustively studied for use in 13 C DNP applications. In this work, two additional lanthanides with relatively high magnetic moments, Dy 3+ and Tb 3+ , were extensively optimized and tested as doping additives for 13 C DNP at 3.35 T and 1.2 K. We have found that both of these lanthanides are also beneficial additives, to a varying degree, for 13 C DNP. The optimal concentrations of Dy 3+ (1.5 mM) and Tb 3+ (0.25 mM) for 13 C DNP were found to be less than that of Gd 3+ (2 mM). W-band electron paramagnetic resonance shows that these enhancements due to Dy 3+ and Tb 3+ doping are accompanied by shortening of electron T 1 of trityl OX063 free radical. Furthermore, when dissolution was employed, Tb 3+ -doped samples were found to have similar liquid-state 13 C NMR signal enhancements compared to samples doped with Gd 3+ , and both Tb 3+ and Dy 3+ had a negligible liquid-state nuclear T 1 shortening effect which contrasts with the significant reduction in T 1 when using Gd 3+ . Our results show that Dy 3+ doping and Tb 3+ doping have a beneficial impact on 13 C DNP both in the solid and liquid states, and that Tb 3+ in particular could be used as a potential alternative to Gd 3+ in 13 C dissolution DNP experiments. Published by AIP Publishing.

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“…P b ) = 35 % with a build-up time constant s DNP ( 13 C) = 2300 s at T = 1 K. Although such high polarization levels can provide intense NMR signals after dissolution, the long DNP build-up times s DNP ( 13 C) do not allow one to perform several dissolution processes in rapid succession, as required for many in vivo experiments with high throughput. Two approaches have been described recently to enable multiple in vivo experiments at higher repetition rates: the design of a multiple-sample DNP polarizer [11] and the use of cross polarization [12][13][14].…”

Section: Introductionmentioning

confidence: 99%

Cross Polarization for Dissolution Dynamic Nuclear Polarization Experiments at Readily Accessible Temperatures 1.2 < T < 4.2 K

Bornet

Melzi²,

Jannin

et al. 2012

Appl Magn Reson

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Cross polarization can provide significant enhancements with respect to direct polarization of low-c nuclei such as 13 C. Substantial gains in sample throughput (shorter polarization times) can be achieved by exploiting shorter buildup times s DNP ( 1 H) \ s DNP ( 13 C). To polarize protons rather than low-c nuclei, nitroxide radicals with broad ESR resonances such as TEMPO are more appropriate than Trityl and similar carbon-based radicals that have narrow lines. With TEMPO as polarizing agent, the main Dynamic Nuclear Polarization (DNP) mechanism is thermal mixing (TM). Cross polarization makes it possible to attain higher polarization levels at 2.2 K than one can obtain with direct DNP of low-c nuclei with TEMPO at 1.2 K, thus avoiding complex cryogenic technology.

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A multi-sample 94GHz dissolution dynamic-nuclear-polarization system

Cited by 69 publications

References 25 publications

Optimizing dissolution dynamic nuclear polarization

Optimizing dissolution dynamic nuclear polarization

Influence of Dy3+ and Tb3+ doping on 13C dynamic nuclear polarization

Cross Polarization for Dissolution Dynamic Nuclear Polarization Experiments at Readily Accessible Temperatures 1.2 < T < 4.2 K

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