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Preparation method of molecularly-imprinted magnetic silica microsphere with hydrophilic external surface

A technology of silica gel microspheres and molecular imprinting, applied in chemical instruments and methods, ion exchange, ion exchange regeneration, etc., can solve problems such as low separation efficiency, high impurity content, and large detection interference, and achieve uniform particle size and selectivity Strong, enriched strong effect

Inactive Publication Date: 2014-07-30
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing molecularly imprinted magnetic silica gel microspheres with a hydrophilic outer surface, so as to solve the problem of separation efficiency caused by the silica gel microspheres prepared by the existing method when separating samples because the outer surface is easy to adsorb biological macromolecules. Low, high impurity content, and large interference to detection

Method used

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  • Preparation method of molecularly-imprinted magnetic silica microsphere with hydrophilic external surface
  • Preparation method of molecularly-imprinted magnetic silica microsphere with hydrophilic external surface
  • Preparation method of molecularly-imprinted magnetic silica microsphere with hydrophilic external surface

Examples

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Effect test

Embodiment 1

[0028] (1) Preparation of magnetic silica gel microspheres: weigh 0.5 g Fe 3 o 4 , add 80 ml ethanol and 20 ml distilled water mixed solvent, then adjust the pH value of the solution with 2.5 ml ammonia water (25-28%, w / w) to keep the pH value of the solution between 8-9, ultrasonically disperse After 5 min, 2 ml of tetraethoxysilane was added dropwise, and mechanically stirred at room temperature for 12 h. The product was collected, washed 3-4 times with distilled water, and dried at 60°C for 12 h to obtain magnetic silica gel microspheres. figure 2 (c) shown. From figure 2 It can be seen from the comparison that figure 2(c) The synthesized magnetic silica gel microspheres have good dispersibility, uniform particle size and beautiful appearance.

[0029] (2) Preparation of aminated magnetic silica gel microspheres: Disperse 0.5 g of magnetic silica gel microspheres into 50 ml of anhydrous toluene, then add 2 ml of silane KH-550, and reflux for 8 h under the protection...

Embodiment 2

[0034] When preparing magnetic silica gel microspheres, 90 ml of ethanol and 10 ml of distilled water were used as the reaction solvent, and the rest of the steps were the same as in Example 1. The scanning electron microscope images of the prepared magnetic silica gel microspheres are as follows: figure 2 (a) shown.

Embodiment 3

[0036] When preparing magnetic silica gel microspheres, 50 ml of ethanol and 50 ml of distilled water were used as the reaction solvent, and the rest of the steps were the same as in Example 1. The scanning electron microscope images of the prepared magnetic silica gel microspheres are as follows: figure 2 (b) shown.

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Abstract

The invention relates to a preparation method of a molecularly-imprinted magnetic silica microsphere with a hydrophilic external surface. The preparation method comprises the following steps: A, preparing a magnetic silica microsphere by taking Fe3O4 as magnetic particles, ethyl alcohol and distilled water as reaction solvents and TEOS (Tetraethyl Orthosilicate) as a molecular precursor; B, with anhydrous methylbenzene as a solvent, and reacting the magnetic silica microsphere with KH-550 to obtain an amination magnetic silica microsphere; C, with bisphenol A as a template molecule, TEOS and PTMS (Phenyltrimethoxysilane) as cross-linking agents and HCl as a catalyst, reacting with the amination magnetic silica microsphere, and eluting the template molecule to obtain a bisphenol A imprinted magnetic silica microsphere; and D, reacting the bisphenol A imprinted magnetic silica microsphere with KH-560, and performing hydrolysis to obtain the molecularly-imprinted magnetic silica microsphere with the hydrophilic external surface. The method has the advantages of simplicity in preparation, strong selectivity, excellent enrichment and high separation efficiency, is capable of effectively excluding biomacromolecules and reducing impurities of treated samples and can be widely used in separation and extraction of pretreatment of the samples.

Description

technical field [0001] The invention relates to a preparation method of extraction and separation materials, in particular to a preparation method of molecularly imprinted magnetic silica gel microspheres capable of repelling the hydrophilic outer surface of biological macromolecules. Background technique [0002] Bisphenol A (BPA) is an important chemical raw material, mainly used in the production of polycarbonate, epoxy resin, polyphenol oxide, etc. products. During use, bisphenol A may migrate into food, and after being ingested, it can bind to estrogen receptors in the human body, thereby affecting the normal endocrine and metabolic activities of the human body, and may cause diseases such as diabetes, heart disease, obesity and diseases such as breast cancer. In view of its potential safety hazards, countries around the world have strict restrictions on the dissolution of bisphenol A and its derivatives in food packaging materials. For example, the EU stipulates that...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/283B01J20/28B01J20/30B01D15/08
Inventor 吕运开何艳冬熊雪秦新英孙汉文
Owner HEBEI UNIVERSITY
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