Toward single-shot pure-shift solution 1H NMR by trains of BIRD-based homonuclear decoupling
Toward single-shot pure-shift solution 1H NMR by trains of BIRD-based homonuclear decoupling
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DOI：
10.1016/j.jmr.2012.02.018
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发表时间：
2012-05-01
影响因子：
2.2
通讯作者：
Frydman, Lucio
中科院分区：
文献类型：
--
作者：
Lupulescu, Adonis;Olsen, Gregory L.;Frydman, Lucio
实现同核1H解耦仍然是液态核磁共振的关键挑战之一。这样的光谱将使各种有机和分析应用具有更高的分辨率，即使在一维格式下也能理想地做到这一点。已经提出了一些旨在利用二维采集实现这一目标的平行努力；近年来展示的方法包括实现纯吸收积分光谱的新模式，使用空间选择性操作，以及利用异核提供的自然自旋稀释。目前的研究依赖于后一种方法，并探索使用BIRD脉冲区分与C-13键合的质子和与C-12键合的质子，在连续的一维扫描中实现同核去耦。对几种代表性化合物的研究表明，只要适当注意抑制不需要的相干性，使所有操作足够宽，并提供目标质子的充分异核解耦，就可以以稳健的形式实现这一目标。然后可以实现可靠的同核解耦性能，以最小的线宽，微调和灵敏度损失。(C) 2012爱思唯尔公司版权所有。
Achieving homonuclear 1H decoupling remains one of the key challenges in liquid-state NMR. Such spectra would endow a variety of organic and analytical applications with an increased resolution, and would ideally do so even in a one-dimensional format. A number of parallel efforts aimed at achieving this goal using two-dimensional acquisitions have been proposed; approaches demonstrated over recent years include, among others, new modes for achieving purely-absorptive integral spectroscopy, the use of spatially-selective manipulations, and exploiting the natural spin dilution afforded by heteronuclei. The present study relies on the latter approach, and explores the use of BIRD pulses distinguishing between protons bonded to C-13 from those bonded to C-12, to achieve homonuclear decoupling in a continuous 1D scan. Studies on several representative compounds demonstrate that this goal can be implemented in a robust format, provided that suitable care is also taken to suppress unwanted coherences, of making all manipulations sufficiently broad-banded, and to provide adequate heteronuclear decoupling of the targeted protons. Dependable homonuclear decoupling performance can then be achieved, with minimal line width, fine-tuning, and sensitivity penalties. (C) 2012 Elsevier Inc. All rights reserved.