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 the low ability of magnetic spheres to bind nucleic acids, etc.

Active Publication Date: 2012-03-07
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
Comparison scheme
Effect test

Embodiment 1

[0081] 1. Preparation of Magnetic Silica Microspheres

[0082] Take 7.2892g of cetyltrimethylammonium bromide and 109.3g of toluene into the four-necked flask, stir evenly with a stirrer at 1000 rpm, mix 0.329g of FeCl 2 4H 2 O with 0.987g FeCl 3 ·6H 2 Dissolve O in 9.4397g of secondary water to prepare an aqueous solution with a concentration of 140g / L, add dropwise to the above mixture at 4-5mL / h under nitrogen protection at 2-3mL / min, and continue stirring at 800 rpm for 4-6 hours , then add 2 mL of ammonia water with a mass concentration of 25%, and continue to stir at 800 rpm for 2 hours. In the mixture, iron ferric oxide nanoparticles are formed, slowly add 9.79 mL of tetraethyl orthosilicate, and stir at 800 rpm. Adjust the pH to 8, 1 hour after adding tetraethyl orthosilicate dropwise at 2-3mL / h, stop the nitrogen protection, stir at 800 rpm, age for 5 days at normal temperature and pressure, add 16.4g of ethanol to the product to Centrifuge at 2000 rpm for 40 minu...

Embodiment 2

[0088] 1. Preparation of Magnetic Silica Microspheres

[0089] Take 7.2892g of cetyltrimethylammonium bromide and 87.47g of toluene into the four-necked flask, stir evenly with a stirrer at 1000 rpm, mix 0.305g of FeCl 2 4H 2 O with 0.916g FeCl 3 ·6H 2 Dissolve O in 9.4397g of secondary water to prepare an aqueous solution with a concentration of 130g / L, add it dropwise to the above mixture at 4-5mL / h under the protection of nitrogen at 2-3mL / min, and continue stirring at 800 rpm for 4-6 hours , then add 1.15 mL of ammonia water with a mass concentration of 25%, and continue stirring at 800 rpm for 2 hours. In the mixture, ferric oxide nanoparticles are formed, slowly add 6.78 mL of tetraethyl orthosilicate, and stir at 800 rpm Reaction, adjust the pH to 8, add orthosilicate ethyl ester dropwise at 2~3mL / h for 1 hour, stop the nitrogen protection, stir at 800 rpm, age at normal temperature and pressure for 5 days, add 14.58g of ethanol to the product , centrifuge at 2000 r...

Embodiment 3

[0095] 1. Preparation of Magnetic Silica Microspheres

[0096] Take 7.2892g of cetyltrimethylammonium bromide and 145.784g of toluene into the four-necked flask, stir evenly with a stirrer at 1000 rpm, mix 0.354g of FeCl 2 4H 2 O with 1.060g FeCl 3 ·6H 2 Dissolve O in 9.4397g of secondary water to prepare an aqueous solution with a concentration of 150g / L, add it dropwise to the above mixture at 4-5mL / h under the protection of nitrogen at 2-3mL / min, and continue stirring at 800 rpm for 4-6 hours , then add 2.28mL of ammonia water with a mass concentration of 25%, and continue to stir at 800 rpm for 2 hours. In the mixture, iron ferric oxide nanoparticles are formed, slowly add 11.76mL of tetraethyl orthosilicate, and stir at 800 rpm Reaction, adjust the pH to 8, add orthosilicate ethyl ester dropwise at 2-3mL / h for 1 hour, stop the nitrogen protection, stir at 800 rpm, age at normal temperature and pressure for 5 days, add ethanol 18.223 to the product, Centrifuge at 2000 ...

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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 acids from biological samples, in particular to a magnetic silica microsphere with surface-modified diethylaminoethyl (DEAE) and its preparation method and application . Background technique [0002] Biomagnetic separation technology is a high-efficiency separation technology developed on the basis of traditional magnetic separation technology, which is applied to organisms such as cells, bacteria, nucleic acids and proteins. It uses the characteristics of magnetic or magnetically labeled organisms to move directionally under the action of an external magnetic field to extract, enrich, separate and purify target organisms. Early work mainly focused on the development of preparation techniques for magnetic markers, including the adsorption of magnetic nanoparticles to polymer microspheres such as agarose, polyacrylamide, polyglutar...

Claims

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Application Information

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Patent Type & Authority Patents(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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