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Synthesis method of magnetic metal organic framework composite material and application of material

An organic framework and composite material technology, applied in advanced nanomaterials and nanometer fields, can solve the problems of poor specific surface area, limited enrichment of phosphorylated peptides, etc., and achieve the effects of high magnetic responsiveness, strong adsorption, and strong adsorption.

Inactive Publication Date: 2014-07-02
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To date, many functionalized magnetic nanomaterials have been successfully synthesized and used for the enrichment of phosphopeptides, but their ability to enrich phosphopeptides is often limited by limited specific surface area and poor hydrophilicity.

Method used

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  • Synthesis method of magnetic metal organic framework composite material and application of material
  • Synthesis method of magnetic metal organic framework composite material and application of material
  • Synthesis method of magnetic metal organic framework composite material and application of material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: Synthesis of a metal-organic framework composite material with magnetic microsphere ferric oxide coated polydopamine and zirconium ion as the central metal ion

[0029] (1) 1.35 g ferric chloride hexahydrate (FeCl 3 ·6H 2 O) Dissolve in 75 mL of ethylene glycol, stir magnetically until clarified, add 3.6 g of sodium acetate, stir until dissolved, continue to stir for 0.5 h, ultrasonicate for 5 minutes, transfer to a hydrothermal reaction kettle, and heat at 200°C for 16 hours . The reactor was taken out and cooled for 10 hours; the magnetic balls obtained by the reaction were poured out from the reactor, and washed 5 times with deionized water. Dry under vacuum at 50°C.

[0030] (2) Prepare tris-hydrochloric acid (Tris-HCl) buffer (solvent is deionized water, pH=8.5), and disperse 0.1 g of magnetic balls obtained in step (1) in 80 mL of Tris-HCl buffer , ultrasonicated for several minutes, added 0.4 g of dopamine hydrochloride, and mechanically stirred at...

Embodiment 2

[0036] Example 2: The magnetic microsphere ferric oxide obtained in Example 1 is coated with polydopamine and a metal-organic framework composite material with zirconium ion as the central metal ion as a solid phase microextraction adsorbent for low concentration β-casein Enrichment of enzymatic hydrolyzate and detection by MALDI-TOF MS.

[0037] (1) Preparation of standard protein enzymatic hydrolysis solution: Accurately weigh 2 mg of standard protein β-casein and dissolve in 25mM ammonium bicarbonate buffer, boil for 10 minutes, dilute to 0.2 mg / mL with 25mM ammonium bicarbonate buffer, and then follow Add an appropriate amount of trypsin (trypsin) at a ratio of 1:40 to the protein, and digest at 37°C for 16 hours.

[0038] (2) Enrichment of samples: Dilute the standard protein hydrolysis solution with 25mM ammonium bicarbonate buffer to a concentration of 100 nM or 10 nM, take 1 μL of the dilution of the enzyme hydrolysis solution and add it to 200 μL of 50% acetonitrile / 0...

Embodiment 3

[0042] Example 3: Synthesis of a metal-organic framework composite material with magnetic microsphere ferric oxide coated with polydopamine and zirconium ion as the central metal ion

[0043] (1) 1.0 g ferric chloride hexahydrate (FeCl 3 ·6H 2 O) Dissolve in 55 mL of ethylene glycol, stir magnetically until clarified, add 3.0 g of sodium acetate, stir until dissolved, continue stirring for 0.5 h, ultrasonically transfer to a hydrothermal reaction kettle for 5 minutes, and heat at 190°C for 18 hours . The reactor was taken out and cooled for 12 hours; the magnetic balls obtained by the reaction were poured out from the reactor, and washed 9 times with deionized water. Dry under vacuum at 60°C.

[0044] (2) Prepare tris-hydrochloric acid (Tris-HCl) buffer (solvent is deionized water, pH=8.5), and disperse 0.05 g of magnetic balls obtained in step (1) in 40 mL of Tris-HCl buffer , ultrasonicated for several minutes, added 0.2 g of dopamine hydrochloride, and mechanically stir...

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Abstract

The invention discloses a synthesis method of a metal organic framework composite material which has a sandwich structure, comprises magnetic microsphere ferroferric oxide surface coating polydopamine and takes zirconium ion as central metal ion and application of the material. The synthesis method comprises the following steps: firstly synthesizing ferroferric oxide magnetic microspheres by using a hydrothermal synthesis method; dispersing the magnetic microspheres in an aqueous solution of polydopamine hydrochloride to coat the surfaces of the magnetic microspheres with polydopamine layers; dispersing the magnetic microspheres coated with the polydopamine in an N,N-dimethylformamide mixed solution of zirconium chloride and terephthalic acid to prepare the magnetic metal organic framework composite material with a sandwich structure. The synthesis method is simple and quick; the magnetic metal organic framework composite material obtained by synthesizing is high in specific surface area, good in biocompatibility and applicable to selective enrichment of phosphorylated peptide and MALDI-TOFMS detection in biological samples.

Description

technical field [0001] The invention belongs to the field of advanced nanomaterials and nanotechnology, and specifically relates to a magnetic microsphere iron ferric oxide surface coated with polydopamine and zirconium ion as the central metal for phosphorylated peptide enrichment and MALDI-TOF MS detection Synthesis methods and applications of ionic metal-organic framework composites. Background technique [0002] Phosphorylation is one of the most prevalent post-translational modifications in biological cells and plays an important role in signal transduction, gene expression, metabolism, cell growth, division and differentiation. It is estimated that 30-50% of proteins in a cell will be phosphorylated at any time, so the exploration of protein phosphorylation is a major topic in proteomics research. Mass spectrometry is the primary means of phosphorylation analysis. However, the abundance of phosphorylated proteins / phosphorylated peptides is very low, and the phospho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/10G01N1/40G01N27/62
Inventor 邓春晖赵曼
Owner FUDAN UNIV
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