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Magnetic silicon dioxide microspheres modified with diethylaminoethyl and preparation method and application thereof

A technology of diethylaminoethyl and silicon dioxide, which is used in the preparation of microspheres, chemical instruments and methods, microcapsule preparations, etc., can solve the problem of low ability of magnetic spheres to bind nucleic acid, etc.

Active Publication Date: 2010-01-20
XIAN GOLDMAG NANOBIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The above two magnetic microspheres with surface-modified DEAE, because DEAE is directly modified on the carbon hydroxyl of the matrix, the distance between the functional group DEAE and the matrix is ​​relatively close, and the combination of nucleic acid and DEAE is greatly affected by steric hindrance, so the magnetic Ball-binding nucleic acid is not high

Method used

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  • Magnetic silicon dioxide microspheres modified with diethylaminoethyl and preparation method and application thereof
  • Magnetic silicon dioxide microspheres modified with diethylaminoethyl and preparation method and application thereof
  • Magnetic silicon dioxide microspheres modified with diethylaminoethyl and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0081] 1. Preparation of magnetic silica microspheres

[0082] Take 7.2892g cetyltrimethylammonium bromide and 109.3g toluene into the four-necked flask, stir evenly with a mixer at 1000 rpm, add 0.329g FeCl 2 ·4H 2 O and 0.987g FeCl 3 ·6H 2 O was dissolved in 9.4397g secondary water to prepare an aqueous solution with a concentration of 140g / L, and was added dropwise to the above mixture at 4 to 5 mL / h under the protection of 2 to 3 mL / min nitrogen, and stirring was continued for 4 to 6 hours at 800 rpm , Then add 2 mL of 25% ammonia water with a mass concentration of 25%, and continue stirring at 800 rpm for 2 hours. In the mixture, Fe3O4 nanoparticles are formed. Slowly add 9.79 mL of ethyl orthosilicate and stir at 800 rpm for reaction. Adjust the pH to 8, add 2~3mL / h of ethyl orthosilicate for 1 hour, stop the nitrogen protection, stir at 800 rpm, and age for 5 days at room temperature and pressure. Add 16.4g of ethanol to the product to Centrifuge at 2000 rpm for 40 minutes...

Embodiment 2

[0088] 1. Preparation of magnetic silica microspheres

[0089] Take 7.2892g cetyltrimethylammonium bromide and 87.47g toluene into a four-necked flask, stir evenly with a mixer at 1000 rpm, and add 0.305g FeCl 2 ·4H 2 O and 0.916g FeCl 3 ·6H 2 O was dissolved in 9.4397g of secondary water to prepare an aqueous solution with a concentration of 130g / L, and added dropwise to the above mixture at 4 to 5 mL / h under the protection of 2 to 3 mL / min of nitrogen, and continued stirring at 800 rpm for 4 to 6 hours , Then add 1.15mL of 25% ammonia water with a mass concentration of 800 rpm and continue stirring for 2 hours. In the mixture, Fe3O4 nanoparticles are formed. Slowly add 6.78mL of ethyl orthosilicate and stir at 800 rpm. For the reaction, adjust the pH to 8, and add 2 to 3 mL / h of ethyl orthosilicate for 1 hour, stop the nitrogen protection, stir at 800 rpm, and age at room temperature and pressure for 5 days. Add ethanol 14.58g to the product Centrifuge at 2000 rpm for 40 minute...

Embodiment 3

[0095] 1. Preparation of magnetic silica microspheres

[0096] Take 7.2892g cetyltrimethylammonium bromide and 145.784g toluene into the four-necked flask, stir evenly with a mixer at 1000 rpm, add 0.354g FeCl 2 ·4H 2 O and 1.060g FeCl 3 ·6H 2 O was dissolved in 9.4397g of secondary water to prepare an aqueous solution with a concentration of 150g / L, and added dropwise to the above mixture at 4 to 5 mL / h under the protection of 2 to 3 mL / min of nitrogen, and continued stirring at 800 rpm for 4 to 6 hours , Then add 2.28 mL of 25% ammonia water with a mass concentration of 800 rpm and continue to stir for 2 hours. In the mixture, Fe3O4 nanoparticles are formed. Slowly add 11.76 mL of ethyl orthosilicate and stir at 800 rpm. After the reaction, adjust the pH to 8, add 2-3 mL / h of ethyl orthosilicate for 1 hour, stop the nitrogen protection, stir at 800 rpm, and age at room temperature and pressure for 5 days. Add ethanol 18.223 to the product. Centrifuge at 2000 rpm for 40 minutes ...

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Abstract

The invention relates to magnetic silicon dioxide microspheres modified with diethylaminoethyl on the surface and a preparation method and an application thereof; the sol-gel method is adopted to prepare magnetic silicon dioxide microspheres which have ferroferric oxide nanoparticles as cores and silicon source, namely tetraethoxysilane as shells; by adopting the microspheres as template, alkylene oxide coupling agent 3-glycidoxypropyltrimethoxysilane (GPTMS) as activator and diethylaminoethyl hydrochloride as functional group, the magnetic silicon dioxide microspheres modified with diethylaminoethyl (DEAE) on the surface are prepared. The method comprises the preparation of magnetic silicon dioxide microspheres, the epoxidation of magnetic silicon dioxide microspheres and the DEAE surface modification. The method solves the problems that the bindingability between the existing magnetic microspheres and nucleic acid is not high, the preparation processes are complicated and the like. The bindingability between the magnetic microspheres prepared by the method and nucleic acid is high so as to be used to separate nucleic acid from the biological sample.

Description

Technical field [0001] The invention belongs to the field of material synthesis and application, and relates to a material for separating nucleic acid from biological samples, and in particular to a surface-modified diethylaminoethyl (DEAE) magnetic silica microsphere, and a preparation method and application thereof . Background technique [0002] Biomagnetic separation technology is an efficient separation technology developed on the basis of traditional magnetic separation technology, using organisms such as cells, bacteria, nucleic acids and proteins as the application objects. It uses the characteristics of magnetic or magnetically labeled organisms to perform directional movement under the action of an external magnetic field to extract, enrich, separate and purify target organisms. Early work mainly focused on the development of the preparation technology of magnetic markers, including the adsorption of magnetic nanoparticles into polymer microspheres such as agarose, pol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/28B01J20/30B01J13/02H01F1/11C07H1/06C07H21/04
Inventor 冯国栋杨磊胡道道崔亚丽陈超
Owner XIAN GOLDMAG NANOBIOTECH
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