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A phase-sensitive selective j-spectroscopy method for suppressing axial peaks

A selective, spectral method technology, applied in the direction of using nuclear magnetic resonance spectrum for measurement, using magnetic variable measurement, instrument, etc., can solve the problems of narrow chemical shift distribution, complex split peak pattern, high axial peak intensity, etc. High resolution and the effect of improving spectral resolution

Inactive Publication Date: 2021-02-26
XIAMEN UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Morris then proposed the PSYCHEDELIC method based on the PSYCHE module (A general method for extracting individual coupling constants from crowded 1H NMR spectrum, Angew.Chem.Int.Ed.55(2016) 1090-1093). However, in these conventional selective J spectrum methods Among them, the narrow chemical shift distribution, complex split peak mode and large spectral peak line width make the axial peak intensity of the two-dimensional spectrum too large to cover the response coupling signal, so that the J coupling cannot be identified

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  • A phase-sensitive selective j-spectroscopy method for suppressing axial peaks
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  • A phase-sensitive selective j-spectroscopy method for suppressing axial peaks

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Embodiment Construction

[0023] The following embodiments will further illustrate the present invention in conjunction with the accompanying drawings:

[0024] A phase-sensitive and selective J spectrum method for suppressing axial peaks described in the embodiment of the present invention, the main steps are:

[0025] 1) collecting the NMR one-dimensional spectrum of the sample;

[0026] 2) Measure the pulse width of the 90-degree hard pulse of the sample;

[0027] 3) Determine the range of hydrogen spectrum that needs to be analyzed;

[0028] 4) Take the frequency of the S nucleus to be measured in the hydrogen spectrum as the excitation center of the selectively excited 180-degree soft pulse, set the power and time of the selectively excited 180-degree soft pulse, and set the dephase gradient G 1 ;

[0029] 5) Take the central frequency of the hydrogen spectrum to be analyzed as the excitation center of the hard pulse, and set the power and time of the 90-degree and 180-degree hard pulse;

[00...

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Abstract

The invention discloses a phase-sensitive selective J spectrum method for suppressing an axial peak, and relates to a nuclear magnetic resonance multidimensional spectrum method. The method comprises:applying a 90-degree hard pulse, rotating a magnetization vector to an XY plane from a Z direction, selecting an S core by using a 180-degree selective pulse and a pair of phase dispersion gradients,other transverse magnetization vectors being subjected to phase dispersion, and applying a perfect echo module; setting parameters, an excitation angle and a corresponding gradient of the PSYCHE module; determining the number ni of indirect dimensional sampling points and the spectral width SW1, and ensuring that the J coupling constant measured by the SW1 is large; setting the cycle index Nt ofthe sampling window; performing direct dimensional Fourier transform on the sampled N-type signal and R-type signal, adding real parts of the N-type signal and R-type signal after Fourier transform toserve as a real part of a composite signal, subtracting the real parts to serve as an imaginary part of the composite signal, and performing indirect dimensional Fourier transform on the composite signal to obtain a phase-sensitive selective J spectrum. The method is more accurate, has high spectrogram resolution, and can be widely used in complex compound structure analysis.

Description

technical field [0001] The invention relates to a nuclear magnetic resonance multidimensional spectrum method, in particular to a phase-sensitive selective J spectrum method for suppressing axial peaks. 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, which is widely used in the study of molecular conformation. Selective J spectroscopy is a well-established NMR method for measuring J coupling constants. Denis Merlet from the UK proposed a G-SERF method based on the ZS module (Nicolas G, Laetitia B, Jacques C, Denis M. Nuclear Magnetic Resonance Using a Spatial Frequency Encoding: Application to J-Edited Spectroscopy along the Sample.Angew Chem Int Ed Engl.2009 ,55:1090-1093), this method can be used to analyze the J-coupling network of a certain hydrogen atom of interest, and mea...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01R33/46
CPCG01R33/4625
Inventor 林雁勤詹超群曾庆陈金永陈忠
Owner XIAMEN UNIV
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