Simplifying proton NMR spectra by instant homonuclear broadband decoupling.

Simplifying proton NMR spectra by instant homonuclear broadband decoupling.
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DOI:
10.1002/anie.201300129
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发表时间:
2013-07-08
影响因子:
16.6
通讯作者:
Zangger, Klaus
Zangger, Klaus
中科院分区:
化学1区
文献类型:
--
作者:
Meyer, N. Helge;Zangger, Klaus

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NMR光谱是一种多功能的工具,用于确定分子的结构,化学和物理性质。一维1H NMR谱可能代表最常获得的NMR数据类型。然而,与其他NMR可检测的核相比,1H谱通常遭受低分辨率和严重的信号重叠,主要由质子之间的广泛标量耦合引起。homonucleotide宽带去耦,这导致1H信号的崩溃成单线态,已被建议是一个解决方案,以克服在1H NMR光谱的信号分散差的问题。事实上,它最近表明,在1H光谱中获得的宽带质子去耦的分辨率的增益是可比的理论信号分散在几GHz的常规光谱测量。[1]在过去的30年里,已经开发了几种方法来实现homemandro宽带去耦。[2-14]然而,这些技术尚未被广泛使用,因为它们不敏感,并且通常必须应用复杂的处理方案来实现期望的同态解耦。最近,在弱梯度场期间的切片选择性宽带去耦(也称为Zangger-Sterk或ZS方法)[14]已被重新发现和改进,成为记录纯位移谱的更通用的方法。[1,7,15] NMR方法采用弱磁梯度场切片选择性激发的概念来解耦所有自旋:当施加线性梯度时,NMR样品的不同部分经历不同的磁场强度。因此,通过观察到的原子核的旋磁比g和梯度强度G,建立了样品体积在s长度上的位置相关频移Δw= g* G* s。当梯度是有效的时,选择性脉冲因此激发整个光谱。但不同
NMR spectroscopy is a versatile tool to determine structural, chemical, and physical properties of molecules. One-dimensional 1H NMR spectra probably represent the most often acquired type of NMR data. However, compared to other NMR detectable nuclei, 1H spectra typically suffer from low resolution and severe signal overlap, mainly arising from extensive scalar coupling between protons. Homonuclear broadband decoupling, which leads to a collapse of 1H signals into singlets, has been suggested to be a solution to overcome the problem of poor signal dispersion in 1H NMR spectroscopy. Indeed, it was recently shown that the gain in resolution obtained in 1H spectra by broadband proton decoupling is comparable with the theoretical signal dispersion of regular spectra measured at several GHz.[1] Over the last 30years several methods have been developed which achieve homonuclear broadband decoupling.[2–14] However, these techniques have not been widely used, since they are insensitive and usually complicated processing schemes have to be applied to achieve the desired homonuclear decoupling. Recently, the slice-selective broadband-decoupling during a weak gradient field (also called Zangger–Sterk or ZS method)[14] has been rediscovered and improved to become a more general way to record pure shift spectra.[1, 7, 15]The ZS-method employs the concept of slice-selective excitation by a weak magnetic gradient field to decouple all spins: Different parts of the NMR sample experience different magnetic field strengths when a linear gradient is applied. Therefore, a location-dependent frequency shift Δw= g* G* s across the sample volume over a length of s is established, with the gyromagnetic ratio of the observed nucleus g and the gradient strength G. While the gradient is active, a selective pulse thus excites the whole spectrum. However, different
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