Preparation method and application of core-shell magnetic composite microsphere rich in boron ester

A magnetic composite microsphere, core-shell technology, applied in the preparation method of peptides, the magnetism of organic materials/organic magnetic materials, chemical instruments and methods, etc., can solve the problems of adsorption and inability to enrich glycoprotein markers, etc., and achieve Uniform particle size distribution, excellent effect, and good separation ability

Inactive Publication Date: 2013-12-11
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this enrichment will bring a certain amount of non-specific adsorption, because boric acid itself is hydrophobic, and when it is connected to the material, it will make the material have a certain degree of hydrophobicity, so that hydrophobic non-glycoproteins may be adsorbed during enrichment
In addition, the enrichment is carried out under alkaline conditions, and the environment in the human body is neutral. To enrich the most original glycoproteins in the human body, alkaline enrichment will often make some Stable glycoproteins decompose or denature, and cannot be enriched to obtain the most original glycoprotein markers in the human body

Method used

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  • Preparation method and application of core-shell magnetic composite microsphere rich in boron ester
  • Preparation method and application of core-shell magnetic composite microsphere rich in boron ester
  • Preparation method and application of core-shell magnetic composite microsphere rich in boron ester

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Experimental program
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Embodiment 1

[0034] Embodiment 1: shell layer thickness is about 10nm, and crosslinking degree is the core-shell type Fe of 20% 3 o 4 The preparation of / PAA-AOPB microspheres, concrete steps are as follows:

[0035] (1), preparation of magnetic clusters stabilized by sodium citrate

[0036] 1.3g ferric chloride hexahydrate (FeCl 3 ·6H 2 O), 3.8g ammonium acetate (NH 4 Ac), after dissolving 0.4g sodium citrate in 70mL ethylene glycol, put it into a 150mL three-necked flask, then raise the temperature to 170°C, stir and react for 1 hour, then transfer the liquid in the flask into a 100mL polytetrafluoroethylene-containing Lined autoclave, then put the autoclave into an oven at 200°C for 16 hours, take it out, and cool it to room temperature with tap water. The product is separated by magnetic separation, washed with absolute ethanol to remove unreacted reactants, and finally the product is dispersed in absolute ethanol for later use.

[0037] (2) Active vinyl modification on the surfa...

Embodiment 2

[0043] Example 2: Core-shell Fe with a shell thickness of about 30 nm and a crosslinking degree of 20% 3 o 4 Preparation of / PAA-AOPB microspheres (transmission electron microscope photos see figure 1 )

[0044] 1. The preparation of sodium citrate-stabilized magnetic clusters is the same as that described in step (1) of Example 1.

[0045] 2. Carrying out active vinyl modification on the surface of the magnetic cluster is the same as described in the step (20) of Example 1.

[0046] 3. Core-shell Fe 3 o 4 The preparation of / PAA is the same as described in Example 1 step (3). The difference is that acrylic, N, N' The dosages of -methylenebisacrylamide and 2,2-azobisisobutyronitrile are 400 μL, 100 mg, and 10 mg, respectively.

[0047] 4. The reaction of modifying aminophenyl borate is the same as that described in step (4) of Example 1.

Embodiment 3

[0048] Example 3: The shell thickness is about 50nm, and the cross-linking degree is 20% core-shell Fe 3 o 4 / Preparation of PAA-AOPB microspheres

[0049] 1. The preparation of sodium citrate-stabilized magnetic clusters is the same as that described in step (1) of Example 1.

[0050] 2. Carrying out active vinyl modification on the surface of magnetic clusters is the same as that described in step (2) of Example 1.

[0051] 3. Core-shell Fe 3 o 4 The preparation of / PAA is the same as described in Example 1 step (3). The difference is that acrylic, N, N' The dosages of -methylenebisacrylamide and 2,2-azobisisobutyronitrile are 600 μL, 150 mg, and 15 mg, respectively.

[0052] 4. The reaction of modifying aminophenyl borate is the same as described in the embodiment step (4).

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Abstract

The invention provides a preparation method and an application of a core-shell magnetic composite microsphere capable of separating glycoprotein. The preparation method is characterized in that a core of the core-shell magnetic composite microsphere is a magnetic iron oxide black nanoparticle cluster and a shell is a crosslinked polymer network rich in carboxyl, then carboxyl and aminobenzene boron ester carry out amidation to carry out surface modification, and glycoprotein can be quickly separated and enriched under the physiological conditions via plenty of surface immobilized boron esters. The preparation method comprises the following steps of: firstly preparing a magnetic nanoparticle cluster with stable sodium citrate, secondly adopting a sol-gel method to modify the surface of the magnetic cluster with active vinyl functional groups, thirdly preparing high-magnetic-responsiveness monodispersed core-shell magnetic polymer composite microsphere rich in carboxyl on the surface via reflux precipitation polymerization, fourthly carrying out amidation on aminobenzene boron ester and carboxyl to modify the surface of the core-shell magnetic composite microsphere with plenty of boron ester groups and finally carrying out separation and enrichment on glycoprotein. The method provided by the invention is simple, is controllable in process, has higher glycoprotein separation and purification efficiency and can carry out separation and enrichment under the physiological conditions.

Description

technical field [0001] The invention belongs to the technical field of nanometer functional materials, and in particular relates to a preparation method and application of core-shell magnetic composite microspheres rich in boron esters. Background technique [0002] In recent years, organic-inorganic hybrid composite microspheres, especially magnetic composite microspheres, are receiving widespread attention. Since magnetic polymer microspheres have both the magnetic responsiveness of inorganic magnetic materials and the surface modifyability of organic polymers, they can separate target biomolecules conveniently, quickly and efficiently under an external magnetic field. Therefore, it has broad application prospects in biomedical fields such as protein separation and purification, cell separation, magnetic resonance detection, and magnetically targeted drug loading. [0003] At present, magnetic polymer composite microspheres with different structures can be prepared by emu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F292/00C08F8/42H01F1/42C07K1/14
Inventor 汪长春章雨婷
Owner FUDAN UNIV
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