Improvement of the inverse-gated-decoupling sequence for a faster quantitative analysis of various samples by 13C NMR spectroscopy
Improvement of the inverse-gated-decoupling sequence for a faster quantitative analysis of various samples by 13C NMR spectroscopy
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DOI：
10.1016/j.jmr.2006.01.015
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发表时间：
2006-05-01
影响因子：
2.2
通讯作者：
Baguet, E
中科院分区：
文献类型：
--
作者：
Giraudeau, P;Baguet, E
反向门控去耦序列使得能够获得定量H-1去耦C-13光谱。我们修改了这个序列，以便在更短的时间内获得相同的结果，含碳分子具有不同的弛豫特性。为此，我们确定了最佳的C-13的磁化强度的初始值为一个更快的弛豫，而H-1倍频器停止。这个值可以通过核Overhauser效应，纵向弛豫时间，以及确定H-1处于不平衡状态时碳的弛豫速率常数来精确计算。H-1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允许C-13纵向弛豫的加速。我们将此方法应用于香草醛分子。与通常的顺序相比，所有碳的同时定量以回收延迟除以2进行。(c)2006年爱思唯尔公司All rights reserved.
The inverse-gated-decoupling sequence enables quantitative H-1 decoupled C-13 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 C-13 longitudinal-magnetization initial value for a faster relaxation while H-1 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 H-1 are out of equilibrium. A supplementary delay of H-1 decoupling and/or a series of selective pulses applied at the beginning of the recovery delay allow an acceleration of C-13 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. (c) 2006 Elsevier Inc. All rights reserved.