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用于研究生物固体的高分辨率14N编辑的1H-13C相关核磁共振实验。

High-resolution 14N-edited 1H-13C correlation NMR experiment to study biological solids.

作者信息

Amoureux Jean-Paul, Trébosc Julien, Hu Bingwen, Halpern-Manners Nicholas, Antonijevic Sasa

机构信息

Unité de Catalyse et Chimie du Solide, UMR-CNRS 8181, Université de Lille 1, 59652 Villeneuve d'Ascq cedex, France.

出版信息

J Magn Reson. 2008 Oct;194(2):317-20. doi: 10.1016/j.jmr.2008.07.021. Epub 2008 Jul 29.


DOI:10.1016/j.jmr.2008.07.021
PMID:18707905
Abstract

It was recently shown that nuclear magnetic resonance (NMR) spectra of nitrogen-14 (spin I=1) can be obtained by indirect detection via spin S=1/2 nuclei in powders spinning at the magic angle. An increased number of solid-state NMR methods are now available to tailor sequences for specific purposes, e.g., hetero-nuclear dipolar recoupling or homo-nuclear dipolar decoupling schemes. Here, we combine the latest recoupling and decoupling techniques to obtain high-resolution (1)H-(13)C through-space correlation spectra, where only the correlation peaks of those carbons close to nitrogen nuclei are observed. The experiment is demonstrated on a (13)C enriched l-histidine. HCl x H(2)O powder sample.

摘要

最近研究表明,通过在魔角旋转的粉末中利用自旋S = 1/2原子核进行间接检测,可以获得氮-14(自旋I = 1)的核磁共振(NMR)谱。现在有越来越多的固态NMR方法可用于为特定目的定制序列,例如异核偶极重耦合或同核偶极去耦方案。在此,我们结合最新的重耦合和去耦技术来获得高分辨率的(1)H-(13)C空间相关谱,其中仅观察到那些靠近氮原子核的碳的相关峰。该实验在富含(13)C的l-组氨酸·HCl·H₂O粉末样品上进行了演示。

相似文献

[1]
High-resolution 14N-edited 1H-13C correlation NMR experiment to study biological solids.

J Magn Reson. 2008-10

[2]
3D 1H-13C-14N correlation solid-state NMR spectrum.

J Magn Reson. 2008-8

[3]
Indirect detection of nitrogen-14 in solids via protons by nuclear magnetic resonance spectroscopy.

J Magn Reson. 2006-9

[4]
Indirect detection via spin-1/2 nuclei in solid state NMR spectroscopy: application to the observation of proximities between protons and quadrupolar nuclei.

J Phys Chem A. 2009-11-19

[5]
Nitrogen-14 NMR spectroscopy using residual dipolar splittings in solids.

J Am Chem Soc. 2006-6-21

[6]
Probing amide bond nitrogens in solids using 14N NMR spectroscopy.

Solid State Nucl Magn Reson. 2008-5

[7]
Symmetry-based recoupling of proton chemical shift anisotropies in ultrahigh-field solid-state NMR.

J Magn Reson. 2007-3

[8]
Band-selective 1H-13C cross-polarization in fast magic angle spinning solid-state NMR spectroscopy.

J Am Chem Soc. 2008-12-24

[9]
A new approach in 1D and 2D 13C high-resolution solid-state NMR spectroscopy of paramagnetic organometallic complexes by very fast magic-angle spinning.

J Am Chem Soc. 2003-3-26

[10]
Comparison of several hetero-nuclear dipolar recoupling NMR methods to be used in MAS HMQC/HSQC.

J Magn Reson. 2008-5

引用本文的文献

[1]
(14)N overtone NMR under MAS: signal enhancement using symmetry-based sequences and novel simulation strategies.

Phys Chem Chem Phys. 2015-3-7

[2]
An efficient NMR method for the characterisation of 14N sites through indirect 13C detection.

Phys Chem Chem Phys. 2013-4-15

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