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Covalent organic framework-modified graphene material and synthetic method and application thereof

A covalent organic framework and synthesis method technology, applied in the field of covalent organic framework modified graphene materials and their synthesis, can solve the problems of low abundance and weak ionization ability, and achieve high-efficiency release, strong selectivity, and excellent sensitivity Effect

Inactive Publication Date: 2017-06-23
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Separation, purification and identification are important steps in the research of glycoproteins. In recent years, biological mass spectrometry analysis technology has been widely used in the research of glycosylated proteins / peptides, but due to its weak ionization ability and low abundance, and the The mass spectrometry signals of glycosylated peptides are often masked by non-glycosylated peptides, salts, and impurity molecules, which will lead to great challenges for direct analysis and detection using mass spectrometry

Method used

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  • Covalent organic framework-modified graphene material and synthetic method and application thereof
  • Covalent organic framework-modified graphene material and synthetic method and application thereof
  • Covalent organic framework-modified graphene material and synthetic method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Embodiment 1: A kind of synthetic method of the graphene material of covalent organic framework modification.

[0028] (1) Disperse 450mg sheet-layer graphene in 70mL concentrated nitric acid, and reflux in a water bath at 60°C for 8 hours;

[0029] (2) Centrifuging and separating the product obtained in step (1), washing with deionized water until the solution is neutral;

[0030] (3) The product obtained in step (2) is vacuum-dried at 50° C., placed and preserved to obtain acidified graphene;

[0031] (4) 405mg FeCl 3 ·6H 2 O was dissolved in 40mL of ethylene glycol, and stirred to obtain a yellow transparent solution;

[0032] (5) Dispersing the product obtained in step (3) in the solution obtained in step (4), and ultrasonicating for 1.0 hour, the ratio of the product obtained in step (3) to the solution obtained in step (4) is: 150mg: 40mL;

[0033] (6) In the case of ultrasonic stirring, add trisodium citrate, sodium acetate, polyethylene glycol (Mr=20000) int...

Embodiment 2

[0042] Example 2: Applying the above-mentioned graphene material modified by a covalent organic framework to the separation, enrichment and MALDI-TOF-MS detection of glycosylated peptides in standard HRP enzymolysis solution:

[0043] (1) Preparation of standard HRP protein enzymatic solution: Accurately weigh 1mg of standard protein HRP and dissolve in 25mM ammonium bicarbonate buffer, boil for 10 minutes, dilute to 1mg / mL with 25mM ammonium bicarbonate buffer, and then Add an appropriate amount of trypsin at a ratio of 1:50, and digest overnight at 37°C for 16 hours;

[0044] (2) 2 mg of the graphene material modified by the covalent organic framework was washed 3 times with 95% acetonitrile / 1.0% trifluoroacetic acid buffer, and then dispersed in 200 μL of 95% acetonitrile / 1.0% trifluoroacetic acid buffer, Ultrasonic disperse until uniform, and prepare a 10μg / μL solution;

[0045] (3) Enrichment of glycosylated peptides: take 20 μL of the solution obtained in step (2), add ...

Embodiment 3

[0048] Example 3: The graphene material modified by the covalent organic framework obtained in Example 1 is applied to the enrichment and MALDI-TOF-MS detection of ultra-low concentration HRP hydrolyzate:

[0049] (1) Enrichment of glycosylated peptides: 200 μg of covalent organic framework-modified graphene materials were added to 80 μL of 95% acetonitrile / 1.0% trifluoroacetic acid buffer; standard proteolysis was diluted with 25 mM ammonium bicarbonate buffer , so that the final concentration of the proteolysis solution was 0.5 fmol / μL; incubate and vortex at 37°C for 10 minutes; magnetically separate, wash three times with 200 μL 95% acetonitrile / 1.0% trifluoroacetic acid buffer solution, and wash with 10 μL 30% acetonitrile / 0.1% Elution with trifluoroacetic acid buffer for 10 minutes, magnetic separation;

[0050] (2) Spotting the target: take 1 μL of the eluate described in step (1) and spot it on the MALDI-TOF-MS target plate, and then place it in the air at room tempera...

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Abstract

The invention belongs to the technical field of novel nanometer materials, in particular to a covalent organic framework-modified graphene material, and a synthetic method and application thereof. The synthetic method comprises the following steps of firstly, a magnetic graphene material is synthesized by a one-pot method; then magnetic graphene is dispersed in a solution of 1,3,5-trimethylbenzene and 1,4-dioxane; two monomers, i.e., 1,4-phenylenebisboronic acid and 2,3,6,7,10,11-hexahydroxy triphenyl are added into the solution; and ultrasonic reaction is performed at room temperature to manufacture the covalent organic framework-modified graphene material. Experiments show that the material has a loose and porous structure, a large specific surface area and stable biocompatibility; in a concentration study of biomolecules, the composite material has the advantages of high reaction efficiency, strong specificity, high stability and the like and can be used to efficiently identify a plurality of complex mixed samples. The covalent organic framework-modified graphene material has the advantages that the cost is low, the operation is simple, and the covalent organic framework-modified graphene material is practical, efficient, high in stability and good in repeatability, and has a great application prospect.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and in particular relates to a graphene material modified by a covalent organic framework and a synthesis method and application thereof. Background technique [0002] Proteins are the direct embodiment of life phenomena, and the study of protein functions will help to understand many physiological processes of life activities. Glycosylation is one of the most important ways of protein post-translational modification, and it is an essential physiological process that plays a vital role in the correct function of protein biology. Separation, purification and identification are important steps in the research of glycoproteins. In recent years, biological mass spectrometry analysis technology has been widely used in the research of glycosylated proteins / peptides, but due to its weak ionization ability and low abundance, and the The mass spectrometry signals of glycosylated peptides are ...

Claims

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Application Information

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IPC IPC(8): C01B32/194C07K1/14G01N30/02A61K47/04A61K31/704A61P35/00
CPCA61K31/704A61K47/02C01P2004/04C07K1/14G01N30/02
Inventor 高明霞王嘉希张祥民李杰
Owner FUDAN UNIV
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