Boosting 1H and 13C NMR signals by orders of magnitude on a bench

被引:4
作者
Bocquelet, Charlotte [1 ]
Rougier, Nathan [1 ]
Le, Huu-Nghia [2 ]
Veyre, Laurent [2 ]
Thieuleux, Chloe [2 ]
Melzi, Roberto [3 ]
Purea, Armin [4 ]
Banks, Daniel [5 ]
Kempf, James G. [5 ]
Stern, Quentin [1 ]
Vaneeckhaute, Ewoud [1 ]
Jannin, Sami [1 ]
机构
[1] Univ Claude Bernard Lyon 1, CRMN, CNRS, ENS Lyon,UMR 5082, F-69100 Villeurbanne, France
[2] Univ Claude Bernard Lyon 1, Inst Chim Lyon, CP2M, CNRS,UCBL,CPE Lyon,UMR 5128, F-69616 Villeurbanne, France
[3] Bruker Italia Srl, Viale V Lancetti 43, I-20158 Milan, Italy
[4] Bruker BioSpin, D-76287 Rheinstetten, Germany
[5] Bruker BioSpin, Billerica, MA 01821 USA
基金
欧洲研究理事会;
关键词
DYNAMIC NUCLEAR-POLARIZATION; PARA-HYDROGEN; HYPERPOLARIZED WATER; SPIN-EXCHANGE; STATE; DNP; SPECTROSCOPY; SENSITIVITY;
D O I
10.1126/sciadv.adq3780
中图分类号
O [数理科学和化学]; P [天文学、地球科学]; Q [生物科学]; N [自然科学总论];
学科分类号
07 ; 0710 ; 09 ;
摘要
Sensitivity is often the Achilles' heel of liquid-state nuclear magnetic resonance (NMR) experiments. This problem is perhaps most pressing at the lowest fields (e.g., 80-MHz 1H frequency), with rapidly increasing access to NMR through benchtop systems, but also sometimes for higher-field NMR systems from 300 MHz to 1.2 GHz. Hyperpolarization by dissolution dynamic nuclear polarization (dDNP) can address this sensitivity limitation. However, dDNP implies massive and complex cryogenic and high-field instrumentation, which cannot be installed on the bench. We introduce here a compact helium-free 1-T tabletop polarizer as a simple and low-cost alternative. After freezing and polarizing the frozen analyte solutions at 77 K, we demonstrate 1H signal enhancement factors of 100, with rapid 1-s buildup times. The high polarization is subsequently transferred by 1H -> 13C cross polarization (CP) to 13C spins. Such a simple benchtop polarizer, in combination with hyperpolarizing solid matrices (HYPSOs), may open the way to replenishable hyperpolarization throughout multiple liquid-state NMR experiments.
引用
收藏
页数:11
相关论文
共 62 条
[1]   Reversible Interactions with para-Hydrogen Enhance NMR Sensitivity by Polarization Transfer [J].
Adams, Ralph W. ;
Aguilar, Juan A. ;
Atkinson, Kevin D. ;
Cowley, Michael J. ;
Elliott, Paul I. P. ;
Duckett, Simon B. ;
Green, Gary G. R. ;
Khazal, Iman G. ;
Lopez-Serrano, Joaqun ;
Williamson, David C. .
SCIENCE, 2009, 323 (5922) :1708-1711
[2]   Benchtop NMR-Based Metabolomics: First Steps for Biomedical Application [J].
Alonso-Moreno, Pilar ;
Rodriguez, Ignacio ;
Izquierdo-Garcia, Jose Luis .
METABOLITES, 2023, 13 (05)
[3]   Increase in signal-to-noise ratio of >10,000 times in liquid-state NMR [J].
Ardenkjaer-Larsen, JH ;
Fridlund, B ;
Gram, A ;
Hansson, G ;
Hansson, L ;
Lerche, MH ;
Servin, R ;
Thaning, M ;
Golman, K .
PROCEEDINGS OF THE NATIONAL ACADEMY OF SCIENCES OF THE UNITED STATES OF AMERICA, 2003, 100 (18) :10158-10163
[4]   Cubic three-dimensional hybrid silica solids for nuclear hyperpolarization [J].
Baudouin, D. ;
van Kalkeren, H. A. ;
Bornet, A. ;
Vuichoud, B. ;
Veyre, L. ;
Cavailles, M. ;
Schwarzwaelder, M. ;
Liao, W. -C. ;
Gajan, D. ;
Bodenhausen, G. ;
Emsley, L. ;
Lesage, A. ;
Jannin, S. ;
Coperet, C. ;
Thieuleux, C. .
CHEMICAL SCIENCE, 2016, 7 (11) :6846-6850
[5]   Highly Repeatable Dissolution Dynamic Nuclear Polarization for Heteronuclear NMR Metabolomics [J].
Bornet, Aurelien ;
Maucourt, Mickael ;
Deborde, Catherine ;
Jacob, Daniel ;
Milani, Jonas ;
Vuichaud, Basile ;
Ji, Xiao ;
Dumez, Jean-Nicolas ;
Moing, Annick ;
Bodenhausen, Geoffrey ;
Jannin, Sami ;
Giraudeau, Patrick .
ANALYTICAL CHEMISTRY, 2016, 88 (12) :6179-6183
[6]   Boosting Dissolution Dynamic Nuclear Polarization by Cross Polarization [J].
Bornet, Aurelien ;
Melzi, Roberto ;
Linde, Angel J. Perez ;
Hautle, Patrick ;
van den Brandt, Ben ;
Jannin, Sami ;
Bodenhausen, Geoffrey .
JOURNAL OF PHYSICAL CHEMISTRY LETTERS, 2013, 4 (01) :111-114
[7]   NUCLEAR POLARIZATION IN HE-3 GAS INDUCED BY OPTICAL PUMPING AND DIPOLAR EXCHANGE [J].
BOUCHIAT, MA ;
CARVER, TR ;
VARNUM, CM .
PHYSICAL REVIEW LETTERS, 1960, 5 (08) :373-375
[8]   TRANSFORMATION OF SYMMETRIZATION ORDER TO NUCLEAR-SPIN MAGNETIZATION BY CHEMICAL-REACTION AND NUCLEAR-MAGNETIC-RESONANCE [J].
BOWERS, CR ;
WEITEKAMP, DP .
PHYSICAL REVIEW LETTERS, 1986, 57 (21) :2645-2648
[9]   PARA-HYDROGEN AND SYNTHESIS ALLOW DRAMATICALLY ENHANCED NUCLEAR ALIGNMENT [J].
BOWERS, CR ;
WEITEKAMP, DP .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1987, 109 (18) :5541-5542
[10]   Tailored Microstructured Hyperpolarizing Matrices for Optimal Magnetic Resonance Imaging [J].
Cavailles, Matthieu ;
Bornet, Aurelien ;
Jaurand, Xavier ;
Vuichoud, Basile ;
Baudouin, David ;
Baudin, Mathieu ;
Veyre, Laurent ;
Bodenhausen, Geoffrey ;
Dumez, Jean-Nicolas ;
Jannin, Sami ;
Coperet, Christophe ;
Thieuleux, Chloe .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2018, 57 (25) :7453-7457