Boosting dissolution-dynamic nuclear polarization by multiple-step dipolar order mediated 1H→13C cross-polarization

被引:6
|
作者
Elliott, Stuart J. [1 ,2 ]
Cala, Olivier [1 ]
Stern, Quentin [1 ]
Cousin, Samuel F. [1 ,3 ]
Ceillier, Morgan [1 ]
Decker, Venita [4 ]
Jannin, Sami [1 ]
机构
[1] Univ Claude Bernard Lyon 1, Univ Lyon, Ctr Resonance Magnet Nucl Tres Hauts Champs, ENS Lyon,CNRS,FRE 2034, 5 Rue Doua, F-69100 Villeurbanne, France
[2] Univ Liverpool, Dept Chem, Liverpool L69 7ZD, England
[3] Aix Marseille Univ, Inst Chim Radicalaire, CNRS, UMR 7273, St Jerome Campus,Ave Esc Normandie Niemen, F-13397 Marseille 20, France
[4] Bruker Biospin GMBH, Silberstreifen 4, D-76289 Rheinstetten, Germany
来源
基金
欧洲研究理事会;
关键词
NMR; Hyperpolarization; DNP; dDNP; CP; dCP; Dissolution; MAGNETIC-RESONANCE; ZEEMAN; NMR; DNP; SPECTROSCOPY; TEMPERATURES; SOLIDS; SIGNAL; WATER;
D O I
10.1016/j.jmro.2021.100018
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Dissolution-dynamic nuclear polarization can be boosted by employing multiple-contact cross-polarization techniques to transfer polarization from 1H to 13C spins. The method is efficient and significantly reduces po-larization build-up times, however, it involves high-power radiofrequency pulses in a superfluid helium envi-ronment which limit its implementation and applicability and prevent a significant scaling-up of the sample size. We propose to overcome this limitation by a stepwise transfer of polarization using a low-energy and low-peak power radiofrequency pulse sequence where the 1H -> 13C polarization transfer is mediated by a dipolar spin order reservoir. An experimental demonstration is presented for [1-13C]sodium acetate. A solid-state 13C polarization of-43.5% was achieved using this method with a build-up time constant of-5.1 minutes, leading to a-27.5% 13C polarization in the liquid-state after sample dissolution. The low-power multiple-step polarization transfer efficiency achieved with respect to the most advanced and highest-power multiple-contact cross-polarization approach was found to be-0.69.
引用
收藏
页数:6
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