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通过在各向异性介质中单扫描二维 NMR 快速获取残差偶极耦合。

Fast access to residual dipolar couplings by single-scan 2D NMR in oriented media.

机构信息

CNRS, CEISAM UMR 6230, BP 92208, Université de Nantes, 2 rue de la Houssinière, 44322 Nantes Cedex 03, France.

出版信息

Magn Reson Chem. 2012 Dec;50 Suppl 1:S53-7. doi: 10.1002/mrc.3856. Epub 2012 Aug 5.

DOI:10.1002/mrc.3856
PMID:22865710
Abstract

Residual dipolar couplings (RDCs) have revolutionized the structure determination of biomolecular and organic compounds. So far, their measurement has been rather time-consuming, but one might imagine that RDCs can one day also be useful in the investigation of compounds with limited stability or short lifetimes. For such applications, it is indispensable to shorten the experiment time. In this communication, we show the first measurement of RDCs from single-scan two-dimensional NMR. An ultrafast HSQC NMR pulse sequence is presented, which includes several of the recent improvements brought to ultrafast NMR in terms of sensitivity, resolution, and spectral width. Ultrafast spectra are obtained in as little time as 60 s on an organic compound at natural abundance, namely (+)-isopinocampheol. When extracting the RDCs from these ultrafast data, a good agreement with those extracted from conventional spectra (obtained in a much longer time) is observed. These results point out the efficiency of the ultrafast approach, particularly when considering the total experiment duration.

摘要

残剩偶极耦合(RDC)彻底改变了生物分子和有机化合物的结构测定。到目前为止,它们的测量相当耗时,但人们可能会想象,RDC 有朝一日也可能对稳定性有限或寿命短的化合物的研究有用。对于此类应用,缩短实验时间是必不可少的。在本通讯中,我们展示了从单扫描二维 NMR 首次测量 RDC。提出了一种超快 HSQC NMR 脉冲序列,其中包括超快 NMR 在灵敏度、分辨率和光谱带宽方面的最新改进。在天然丰度的有机化合物(即(+)-异胡薄荷醇)上,仅需 60 秒即可获得超快光谱。从这些超快数据中提取 RDC 时,观察到与从常规光谱(在更长时间内获得)中提取的 RDC 非常吻合。这些结果表明了超快方法的效率,特别是在考虑总实验持续时间时。

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