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通过13C核磁共振光谱法对各种样品进行更快定量分析的逆门控去耦序列的改进。

Improvement of the inverse-gated-decoupling sequence for a faster quantitative analysis of various samples by 13C NMR spectroscopy.

作者信息

Giraudeau Patrick, Baguet Evelyne

机构信息

Laboratoire d'Analyse Isotopique et Electrochimique de Métabolismes, UMR CNRS 6006, Université de Nantes, B.P. 92208, 2 rue de la Houssinière, F-44322 Nantes Cedex 03, France.

出版信息

J Magn Reson. 2006 May;180(1):110-7. doi: 10.1016/j.jmr.2006.01.015. Epub 2006 Feb 20.

Abstract

The inverse-gated-decoupling sequence enables quantitative (1)H decoupled (13)C spectra to be obtained. We modified this sequence so as to obtain the same result in less time for molecules containing carbons with various relaxation properties. For that, we determined the optimal (13)C longitudinal-magnetization initial value for a faster relaxation while (1)H decoupler is stopped. This value can be calculated precisely via the nuclear Overhauser effects, the longitudinal relaxation times, together with the determination of the relaxation rate constants of carbons while (1)H are out of equilibrium. A supplementary delay of (1)H decoupling and/or a series of selective pulses applied at the beginning of the recovery delay allow an acceleration of (13)C longitudinal relaxation. We applied this method to the molecule of vanillin. The simultaneous quantification of all carbons was carried out with a recovery delay divided by two compared to the usual sequence.

摘要

逆门控去耦序列能够获取定量的(1)H 去耦(13)C 谱。我们对该序列进行了修改,以便在更短的时间内对含有具有各种弛豫特性的碳的分子获得相同的结果。为此,我们确定了在(1)H 去耦器停止时更快弛豫的最佳(13)C 纵向磁化初始值。该值可以通过核 Overhauser 效应、纵向弛豫时间精确计算,同时在(1)H 失衡时确定碳的弛豫速率常数。(1)H 去耦的补充延迟和/或在恢复延迟开始时施加的一系列选择性脉冲可加速(13)C 纵向弛豫。我们将此方法应用于香草醛分子。与常规序列相比,通过将恢复延迟除以二,实现了所有碳的同时定量。

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