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Nuclear magnetic resonance multi-dimensional spectrum method for measuring hydrogen-hydrogen coupling constant of specific hydrogen nucleus

A technology of nuclear magnetic resonance and coupling constant, which is applied in the direction of using nuclear magnetic resonance for analysis, etc. It can solve the problems of low spectral resolution, affecting the measurement of J coupling constant, and signal strength bandwidth, etc., and achieve the effect of strong spectral signal.

Inactive Publication Date: 2019-01-11
XIAMEN UNIV
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Problems solved by technology

However, this method is based on the ZS decoupling module, so the strength of the signal is affected by the bandwidth of the selective pulse
The resulting spectrograms often have extremely weak signal strength, resulting in low resolution of the spectrograms and affecting the measurement of the J coupling constant.

Method used

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  • Nuclear magnetic resonance multi-dimensional spectrum method for measuring hydrogen-hydrogen coupling constant of specific hydrogen nucleus
  • Nuclear magnetic resonance multi-dimensional spectrum method for measuring hydrogen-hydrogen coupling constant of specific hydrogen nucleus
  • Nuclear magnetic resonance multi-dimensional spectrum method for measuring hydrogen-hydrogen coupling constant of specific hydrogen nucleus

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Embodiment Construction

[0028] Below in conjunction with accompanying drawing and embodiment, the present invention will be further described:

[0029] refer to Figure 1a , Figure 1b and figure 2 , a nuclear magnetic resonance multidimensional spectrum method for measuring specific proton-nuclear hydrogen-hydrogen coupling constants, comprising the steps of:

[0030] 1) collecting the NMR one-dimensional spectrum of the sample;

[0031] 2) Measure the pulse width of the 90-degree hard pulse of the sample;

[0032] 3) Determine the proton nuclei that need to be measured, and record them as S nuclei;

[0033] 4) The frequency of the S nucleus to be measured in the hydrogen spectrum is used as the excitation center of the 180-degree soft pulse of the S nucleus, and the pulse width of the 180-degree soft pulse of the S nucleus is determined according to the interval between the hydrogen nucleus to be analyzed and the adjacent signal, Measure the power and time of the 180-degree soft pulse of the S...

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Abstract

The invention provides a nuclear magnetic resonance multi-dimensional spectrum method for measuring the hydrogen-hydrogen coupling constant of a specific hydrogen nucleus. The nuclear magnetic resonance multi-dimensional spectrum method comprises: applying a selective 90 DEG soft pulse while applying a Z-direction magnetic field gradient; applying a perfect echo module, and applying Z-direction magnetic field gradients with the same strength and the same direction on both sides of the selective 180 DEG soft pulse of the perfect echo; adding the 180 DEG soft pulse of an S nucleus after the first t1 / 2 evolution time in the second echo of the perfect echo so as to retain the J-coupling information of the S nucleus; adding the 180 DEG soft pulse of the S nucleus after the second t1 / 2 to compensate phase distortion; respectively applying the 180 DEG soft pulse of the selective S nucleus before the two t1 / 2 evolution times in the second echo so as to obtain a R type sequence corresponding toa N type sequence; and finally carrying out addition on a N type spectrum and a R type spectrum inverted along indirect dimension to obtain a phase-sensitive two-dimensional spectrum, and obtaining the corresponding J-coupling constant by measuring from the splitting of the peak in the indirect dimension.

Description

technical field [0001] The invention relates to a nuclear magnetic resonance multidimensional spectrum method, in particular to a nuclear magnetic resonance multidimensional spectrum method capable of accurately measuring the hydrogen-hydrogen J coupling constant of a specific hydrogen nucleus in a molecule. Background technique [0002] The interaction between spin nuclei and spin nuclei is a main information in the NMR spectrum, which reflects the information of organic structure, especially the information of three-dimensional structure chemistry. Among them, the triple bond J coupling between hydrogen and hydrogen is widely used in the study of molecular conformation because its coupling constant is related to the dihedral angle formed by the triple bond. However, the coupling constant between hydrogen and hydrogen is often difficult to measure from a simple one-dimensional hydrogen spectrum, because the narrow chemical shift distribution, complex split peak mode and lar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08
Inventor 林雁勤詹超群曾庆陈金永陈忠
Owner XIAMEN UNIV
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