Synthetic method for magnetic metal organic framework composite material coated by [Cu3(btc)2] on surfaces of ferroferric oxide microspheres and application of composite material

A technology of metal-organic framework and ferroferric oxide, which is applied in advanced nanomaterials and nanometer fields, can solve problems such as laboriousness, loss of target molecules, troublesome separation process, etc., and achieve good magnetic response, strong adsorption, and strong adsorption. Effect

Inactive Publication Date: 2013-06-12
FUDAN UNIV
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  • Abstract
  • Description
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Problems solved by technology

However, when MOF materials are used to enrich proteins/peptides or other organic molecules, it is inevitable to use centrifugation or filtration to separate...

Method used

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  • Synthetic method for magnetic metal organic framework composite material coated by [Cu3(btc)2] on surfaces of ferroferric oxide microspheres and application of composite material
  • Synthetic method for magnetic metal organic framework composite material coated by [Cu3(btc)2] on surfaces of ferroferric oxide microspheres and application of composite material
  • Synthetic method for magnetic metal organic framework composite material coated by [Cu3(btc)2] on surfaces of ferroferric oxide microspheres and application of composite material

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Embodiment 1

[0040] Embodiment 1: A kind of magnetic microsphere ferric oxide surface coating Cu 3 (btc) 2 Synthesis of metal-organic framework composites

[0041] (1) 1.35g ferric chloride hexahydrate (FeCl 3 ·6H 2 O) Dissolve in 75mL of ethylene glycol, stir magnetically until clarified, add 3.6g sodium acetate, stir until dissolved, continue stirring for 0.5h, sonicate 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.

[0042] (2) Disperse the product obtained in step (1) in 10 mL of ethanol solution of thioglycolic acid (0.29 mM), stir mechanically at room temperature for 24 hours; wash with distilled water and absolute ethanol several times. Dry under vacuum at 50°C.

[0043] (3) Disperse 0.05g of the product obtained in step (2) in 4mL, 10mM cop...

Embodiment 2

[0048] Embodiment 2: the surface of the magnetic microsphere ferric oxide obtained in embodiment 1 is coated with Cu 3 (btc) 2 Metal-organic framework composite material as solid-phase microextraction adsorbent for the enrichment and MALDI-TOF MS detection of low concentration standard peptide angiotensin II.

[0049] (1) Sample preparation: prepare a metal-organic framework composite suspension with a concentration of 10 mg / mL, the solvent ratio is water:ethanol=1:1 (v / v), and sonicate. The standard peptide Angiotensin II to be detected is accurately weighed and prepared into aqueous solutions with concentrations ranging from 10nM, 5nM, 2nM, 1nM and 0.5nM.

[0050] (2) Enrichment of samples: Add 10 μL metal-organic framework composite dispersion into 200 μL standard peptide Angiotensin II aqueous solution, and vortex at 25°C for 30 minutes; separate magnetic microspheres by applying an external magnetic field, and use 0.4M Elute with 10 μL of ammonia water for 10 minutes an...

Embodiment 3

[0054] Embodiment 3: A kind of magnetic microsphere ferric oxide surface coating Cu 3 (btc) 2 Synthesis of metal-organic framework composites

[0055] (1) 1.0g ferric chloride hexahydrate (FeCl 3 ·6H 2 O) Dissolve in 55mL of ethylene glycol, stir magnetically until clarified, add 3.0g sodium acetate, stir until dissolved, continue stirring for 0.5h, sonicate for 5 minutes, transfer to a hydrothermal reaction kettle, 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 40°C.

[0056] (2) Disperse the product obtained in step (1) in 10 mL of ethanol solution of thioglycolic acid (0.29 mM), stir mechanically at room temperature for 24 hours; wash with distilled water and absolute ethanol several times. Dry under vacuum at 30°C.

[0057] (3) Disperse 0.10 g of the product obtained in step (2) in 4 mL, 20 mM c...

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Abstract

The invention relates to a synthetic method for a magnetic metal organic framework composite material coated by [Cu2(btc)2] on surfaces of ferroferric oxide microspheres and application of the composite material. The method comprises the following steps of: firstly synthesizing ferroferric oxide microspheres by a hydrothermal synthesis method; dispersing magnetic spheres in an ethanol liquid of mercaptoacetic acid, wherein hydroxyls are formed on the surface of the spheres; dispersing mercaptoacetic acid modified magnetic spheres to an ethanol liquid of copper acetate, reacting for 15 minutes at 70 DEG C, and then dispersing the product in an ethanol liquid of trimesic acid and reacting for 30 minutes at 70 DEG C; and performing alternate reaction of magnetic spheres with copper acetate and the ethanol liquid of trimesic acid to finally, obtain the magnetic metal organic framework composite material with a core-shell structure. The material has a metal organic framework shell layer and can be coordinated with peptide fragments with amino groups and carboxylic group so as to enrich low concentration peptide. Meanwhile, the enriching and separating process is fast, simple and convenient due to high paramagnetism of ferroferric oxide. The synthetic method is simple and low in cost, and can be used for enrichment and separation of low abundance peptide fragments less than 1nM and MALDI-TOFMS (Matrix-Assisted Laser Desorption Ionization-Time Of Flight Mass Spectrometer) detection.

Description

technical field [0001] The invention belongs to the field of advanced nanomaterials and nanotechnology, and specifically relates to a magnetic microsphere ferric oxide surface-coated Cu for low-abundance peptide segment enrichment and MALDI-TOF MS detection 3 (btc) 2 Synthesis methods and applications of metal-organic framework composites. Background technique [0002] In complex tissues or cell fluids and body fluids, the abundance of peptides related to diseases and signal transduction is low, and these important peptides are easily adsorbed by high-abundance proteins, making it difficult to effectively identify them. Therefore, pre-enrichment and separation of low-abundance peptide samples is a prerequisite for accurate analysis and identification. Although MALDI-TOF MS and LC-ESI MS are very sensitive in identifying trace proteins / peptides, they are still insufficient in identifying low-abundance peptides in actual biological samples. This is because on the one hand, ...

Claims

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Application Information

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IPC IPC(8): B01J20/281B01J20/28B01J20/30G01N30/02C07K1/14
Inventor 邓春晖赵曼
Owner FUDAN UNIV
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