Gadolinium complex used for solution paramagnetic relaxation enhancement probe and synthetic method thereof

A technology of paramagnetic relaxation enhancement and synthesis method, which can be applied to compounds containing Group 3/13 elements of the periodic table, Group 3/13 organic compounds without C-metal bonds, chemical instruments and methods, etc. , the research on the impact structure, etc., to achieve the effect of simple operation, reduced impact, and simple response

Inactive Publication Date: 2016-08-10
WUHAN INST OF PHYSICS & MATHEMATICS CHINESE ACADEMY OF SCI
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The existing sPRE probes mainly include Gd-DTPABMA and Gd-TTHATMA. The former makes some PRE values ​​abnormally high due to hydrogen exchange, while the latter, due to the introduction of too many hydrophobic groups, makes it different from Proteins interact, affecting the study of their structure

Method used

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  • Gadolinium complex used for solution paramagnetic relaxation enhancement probe and synthetic method thereof
  • Gadolinium complex used for solution paramagnetic relaxation enhancement probe and synthetic method thereof
  • Gadolinium complex used for solution paramagnetic relaxation enhancement probe and synthetic method thereof

Examples

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Effect test

Embodiment 1

[0025] Add 1 equivalent of DTPAA to 50 equivalents of dry DMF, add 10 equivalents of ethanolamine, the white solid dissolves rapidly, react at room temperature under argon protection for 12 hours, remove the solvent by rotary evaporation, dissolve the obtained solid in deionized water, and adjust the pH value to 4, add 0.5 equivalent of gadolinium oxide, reflux for 24 hours. After concentration, 40 equivalents of ethanol was added to precipitate a white solid. Filter and wash the white solid 5 times with ethanol or acetone. Then it was dissolved in deionized water, passed through a sodium ion exchange resin, the effluent was collected, and the solvent was removed by rotary evaporation to obtain a white powder, that is, Gd-DTPA-BEA. ESI-MS detection, C18H29GdN5010 [M+Na] + calculated value = 657.10 experimental value = 657.13.

Embodiment 2

[0027] Add 1 equivalent of DTPAA to 50 equivalents of dry DMF, add 5 equivalents of ethanolamine, the white solid dissolves rapidly, and react at room temperature under argon protection for 12 hours, remove the solvent by rotary evaporation, dissolve the obtained solid in deionized water, and adjust the pH value to 1, add 0.5 equivalent of gadolinium oxide, reflux for 24 hours. After concentration, 20 equivalents of ethanol was added to precipitate a white solid. Filter and wash the white solid 5 times with ethanol or acetone. Then it was dissolved in deionized water, passed through a sodium ion exchange resin, the effluent was collected, and the solvent was removed by rotary evaporation to obtain a white powder, namely Gd-DTPABEA. ESI-MS detection, C18H29GdN5010 [M+Na] + calculated value = 657.10 experimental value = 657.13.

Embodiment 3

[0029] Add 1 equivalent of DTPAA to 50 equivalents of dry DMF, add 6 equivalents of ethanolamine, the white solid dissolves rapidly, react at room temperature under argon protection for 12 hours, remove the solvent by rotary evaporation, dissolve the obtained solid in deionized water, and adjust the pH value to 2, add 0.5 equivalents of gadolinium oxide, and reflux for 24 hours. After concentration, 25 equivalents of ethanol was added to precipitate a white solid. Filter and wash the white solid 5 times with ethanol or acetone. Then it was dissolved in deionized water, passed through a sodium ion exchange resin, the effluent was collected, and the solvent was removed by rotary evaporation to obtain a white powder, namely Gd-DTPABEA. ESI-MS detection, C18H29GdN5010 [M+Na] + calculated value = 657.10 experimental value = 657.13.

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Abstract

The invention provides a kind of gadolinium complex Gd-DTPA-BEA used as a solution paramagnetic relaxation enhancement probe, the structural formula is The gadolinium complex has the advantages that it is not easy to interact with the hydrophobic region of the protein, and does not undergo hydrogen exchange, which is beneficial to the accurate analysis of protein dynamics. In addition, the synthesis method of the gadolinium complex is simple in operation and convenient in reaction.

Description

technical field [0001] The invention belongs to the field of gadolinium complexes, in particular to a gadolinium complex used as a solution paramagnetic relaxation enhancement probe and a synthesis method thereof. Background technique [0002] Paramagnetic relaxation enhancement (PRE) technology is one of the important means to study the structure of protein in solution, which can be used to analyze the dynamic characteristics of protein. The paramagnetic relaxation enhancement technology is to introduce a paramagnetic probe on the surface of the protein, and the relaxation rate of the nucleus is accelerated by the dipole-dipole interaction between the unpaired single electron on the probe and the nucleus on the protein. , namely the PRE effect. [0003] The solution paramagnetic relaxation enhancement (sPRE) technology is a new method developed in recent years. It is different from the traditional PRE technology. It distributes the paramagnetic probe evenly in the solution...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/00
CPCC07F5/003
Inventor 顾新华唐淳
Owner WUHAN INST OF PHYSICS & MATHEMATICS CHINESE ACADEMY OF SCI
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