Ultrahigh-Resolution Total Correlation NMR Spectroscopy

Ultrahigh-Resolution Total Correlation NMR Spectroscopy
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DOI:
10.1021/ja507201t
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发表时间:
2014-08-27
影响因子:
15
通讯作者:
Morris, Gareth A.
Morris, Gareth A.
中科院分区:
化学1区
文献类型:
--
作者:
Foroozandeh, Mohammadali;Adams, Ralph W.;Morris, Gareth A.

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分辨率和灵敏度是使用核磁共振波谱提取详细结构信息的关键。最近发展起来的“纯移位”技术极大地提高了一维和二维核磁共振的分辨率,但在灵敏度方面付出了相当大的代价。一种新引入的方法,赛克,极大地减少了这种损失。与以前的方法相比,它产生的纯移位光谱具有显著提高的灵敏度、光谱纯度和对强耦合的耐受性。在这里,普赛克被应用于TOCSY实验。结合协方差处理,结果是一个高质量、高分辨率的TOCSY光谱,在两个维度上都有单线态:一个纯粹的化学位移相关图。这种光谱应该会极大地简化手动光谱分析和自动结构解析。
Resolution and sensitivity are paramount for extracting detailed structural information using NMR spectroscopy. Recently developed "pure shift" techniques have greatly improved the resolution attainable in one- and two-dimensional NMR, but at a considerable cost in sensitivity. A newly introduced method, PSYCHE, greatly reduces this loss. It produces pure shift spectra with significantly improved sensitivity, spectral purity, and tolerance of strong coupling compared to previous methods. Here PSYCHE is applied to the TOCSY experiment. In combination with covariance processing, the result is a high-quality, high-resolution TOCSY spectrum with singlets in both dimensions: a pure chemical shift correlation map. Such spectra should greatly simplify both manual spectral analysis and automated structure elucidation.