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High-density carboxyl modified magnetic microspheres and preparation method thereof

A technology of magnetic microspheres and carboxyl modification, which is applied in the field of high-density carboxyl-modified magnetic microspheres and its preparation, which can solve the problems of less bioligand coating, low carboxyl activity, and fewer active sites, and achieve coating The effect of large amount, high carboxyl density, and simple raw materials

Active Publication Date: 2016-12-21
SHANGHAI MAJORBIO BIO PHARM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the surface of carboxyl-modified magnetic microspheres has low carboxyl density, fewer active sites, low carboxyl activity, low coupling efficiency, and less coating of bioligands.

Method used

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  • High-density carboxyl modified magnetic microspheres and preparation method thereof
  • High-density carboxyl modified magnetic microspheres and preparation method thereof
  • High-density carboxyl modified magnetic microspheres and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) In the air, 7g FeCl 2 4H 2 O was added to 50 mL of deionized water to obtain a concentration of 0.14 g / mL of FeCl 2 aqueous solution. to 50mL FeCl 2 Add 30 mL of ammonia water to the aqueous solution, and after stirring for 45 minutes, the color gradually turns light green, then dark green, and finally black;

[0041] (2) Add 1.1 g of oleic acid to step (1), mix evenly, place the mixed solution in a closed reaction kettle, heat and react at 110° C. for 4 hours, then alternately wash each time with deionized water and ethanol once, Disperse in n-hexane after magnetic separation to obtain the black paramagnetic nano-Fe coated with oleic acid3 o 4 1;

[0042] (3) to the paramagnetic nano-Fe containing 10mg oleic acid 3 o 4 1 solution, add 125 mg ammonia water, 30 mg tetraethyl orthosilicate and 30 mg (3-aminopropyl) triethoxysilane, react for 1 day, perform magnetic separation, and alternately wash twice with ethanol and water to obtain amino Modified silica-...

Embodiment 2

[0045] (1) In the air, 10g FeCl 2 ·H 2 O was added to 100 mL of deionized water to obtain a concentration of 0.10 g / mL of FeCl 2 aqueous solution. to 100mLFeCl 2 ·H 2 Add 20 mL of ammonia water to the O aqueous solution, and after stirring for 60 minutes, the color gradually turns light green, then dark green, and finally black;

[0046] (2) Add 1 g of oleic acid to step (1), mix evenly, place the mixed solution in a closed reaction kettle, heat and react at 60° C. for 5 hours, then alternately wash twice with deionized water and ethanol, Disperse in octane after magnetic separation to obtain the black paramagnetic nano Fe coated with oleic acid 3 o 4 2;

[0047] (3) to the paramagnetic nano-Fe containing 10mg oleic acid 3 o 4 Add 250 mg of ammonia water, 20 mg of tetraethyl orthosilicate and 10 mg of (3-aminopropyl) triethoxysilane to the solution of 2, conduct magnetic separation after 2 days of reaction, and alternately wash twice with ethanol and water to obtain...

Embodiment 3

[0050] (1) In the air, 50gFeCl 2 ·H 2 O was added to 100 mL of deionized water to obtain a concentration of 0.50 g / mL of FeCl 2 aqueous solution. to 100mLFeCl 2 ·H 2 Add 50 mL of ammonia water to the O aqueous solution, and after stirring for 90 minutes, the color gradually turns light green, then dark green, and finally black;

[0051] (2) Add 5g of oleic acid to step (1), mix evenly, place the mixed solution in a closed reaction kettle, heat and react at 130°C for 3 hours, then alternately wash twice with deionized water and ethanol, Disperse in n-octane after magnetic separation to obtain the black paramagnetic nano-Fe coated with oleic acid 3 o 4 3.

[0052] (3) to the paramagnetic nano-Fe containing 10mg oleic acid 3 o 4 Add 125 mg of ammonia water, 40 mg of tetraethyl orthosilicate and 5 mg of (3-aminopropyl) triethoxysilane to the solution of 3, conduct magnetic separation after 3 days of reaction, and alternately wash twice with ethanol and water to obtain a...

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Abstract

The invention provides high-density carboxyl modified magnetic microspheres and a preparation method thereof. The preparation method comprises the following steps: preparing amino modified magnetic microspheres; and mixing the amino modified magnetic microspheres with organic carboxylic acid, and then adding EDC and NHS to react for 1-3 hours so as to obtain the high-density carboxyl modified magnetic microspheres. The carboxyl groups on surfaces of the magnetic microspheres provided by the invention have a characteristic of high density, and meanwhile, the carboxyl groups on the surfaces of the carboxyl modified magnetic microspheres provided by the invention are coupled with the magnetic microspheres through amino groups, and the spatial arm length of the carboxyl modified magnetic microspheres is longer than that of general carboxyl modified magnetic microspheres, therefore, the density of the carboxyl groups that can be arranged on the surfaces of the magnetic microspheres is higher. The raw materials of the high-density carboxyl modified magnetic microspheres provided by the invention is simple and easy to obtain, the cost is low, the process steps are simple, and the high-density carboxyl modified magnetic microspheres have very strong practicability.

Description

technical field [0001] The invention relates to the field of preparation of magnetic microspheres, in particular to a high-density carboxyl-modified magnetic microsphere and a preparation method thereof. Background technique [0002] Biomagnetic microspheres are a new type of functionalized solid carrier, the surface of which is modified with active groups, which can be coupled with a variety of biologically active substances, and has the characteristics of liquid fluidity and solid magnetic materials. Under the action, it can move and concentrate in a certain direction. When the external magnetic field is removed, it can be evenly dispersed in the liquid with a little vibration or suction, so that the separation of solid and liquid phases becomes very fast and convenient. Through simple elution, it can get very pure High target substance. The method of extracting nucleic acid using nano-micron superparamagnetic magnetic microspheres is simpler and more convenient than trad...

Claims

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Application Information

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IPC IPC(8): B01J13/02C12N15/10H01F1/42
CPCB01J13/02C12N15/1013H01F1/42C12Q2563/143C12Q2563/149
Inventor 刘关蔡红东陈昌岳张祥林
Owner SHANGHAI MAJORBIO BIO PHARM TECH
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