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Nano magnetic microsphere with hollow core-shell structure as well as preparation method and application of nano magnetic microsphere

A nano-magnetic, core-shell structure technology, applied in chemical instruments and methods, other chemical processes, alkali metal oxides/hydroxides, etc., can solve problems such as unsuitable for large-scale promotion, reduction of surface energy, loss of dispersion, etc.

Pending Publication Date: 2021-07-02
INST OF ANIMAL SCI OF CHINESE ACAD OF AGRI SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, there are three problems in the process of functionalizing magnetic nanospheres, (1) the loss of dispersion, that is, small nanoparticles are easy to aggregate to form large particles to reduce the surface energy; (2) the loss of magnetism, that is, Bare magnetic nanospheres, especially Fe 3 o 4 and γ-Fe 2 o 3 It is easy to oxidize in the air, and the acid environment during the enrichment of phosphorylated peptides will also destroy the integrity of the magnetic nanospheres; (3) The surface functionalization of the magnetic nanospheres takes a long time, and the synthesis conditions are harsh, so it is not suitable for large Scale promotion

Method used

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  • Nano magnetic microsphere with hollow core-shell structure as well as preparation method and application of nano magnetic microsphere
  • Nano magnetic microsphere with hollow core-shell structure as well as preparation method and application of nano magnetic microsphere
  • Nano magnetic microsphere with hollow core-shell structure as well as preparation method and application of nano magnetic microsphere

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preparation example Construction

[0038] Such as figure 1 As shown, the embodiment of the present disclosure provides a method for preparing nano-magnetic microspheres with a hollow core-shell structure, including:

[0039] S100, providing Fe 3 o 4 Nano magnetic microspheres;

[0040] S200, the Fe 3 o 4 Nano-magnetic microspheres are ultrasonically dispersed in ethanol, and hexadecyltrimethylammonium bromide, tetraethyl silicate and ammonia water are added in sequence to react to obtain Fe with a hollow core-shell structure. 3 o 4 @mSiO 2 ;

[0041] S300, the Fe 3 o 4 @mSiO 2 Ultrasonic dispersion in ethanol, followed by adding ammonia and glycidyloxypropyltrimethoxysilane to react to obtain Fe 3 o 4 @mSiO 2 @GPS;

[0042] S400, the Fe 3 o 4 @mSiO 2 @GPS ultrasonic dispersion in THF, adding NH 2 -PEG n -NH 2 reaction to obtain amine-modified Fe 3 o 4 @mSiO 2 @NH 2 Nano magnetic microspheres;

[0043] S500, the Fe 3 o 4 @mSiO 2 @NH 2 Nanomagnetic microspheres are ultrasonically disp...

Embodiment 1

[0073] Embodiment 1 Preparation of hollow core-shell structure nano-magnetic microspheres

[0074] 1. Ultrasonic disperse 0.2M ferric chloride in 40ml of mixed solution of sodium citrate, anhydrous sodium acetate and ethylene glycol. The mass ratio of the three substances in the mixed solution is 1:80:400. The mixed solution After heating and dissolving in an oil bath, put the reaction solution in an autoclave and react at 200°C for 10 hours. After the reaction, wash the product with 20ml of water and ethanol three times in sequence to obtain Fe with uniform particles. 3 o 4 Nano magnetic microspheres. The resulting Fe 3 o 4 Electron microscope image of nanomagnetic microspheres image 3 as shown in a.

[0075] 2, the Fe obtained in step 1 3 o 4 Ultrasonic dispersion in 60ml of aqueous solution containing 60% ethanol, sequentially add cetyltrimethylammonium bromide, tetraethyl silicate and ammonia water under the condition of mechanical stirring, wherein cetyltrimethyla...

Embodiment 2

[0087] Example 2 Purification of phosphorylated polypeptides in β-casein using hollow-core-shell nano-magnetic microspheres

[0088] 1. Dissolve 1mg β-casein in 1ml 50mM ammonium bicarbonate buffer to obtain a 1mg / ml β-casein solution;

[0089] 2. Take 10ugβ-casein, add trypsin according to the ratio of 1:50, carry out enzyme digestion for 12 hours under the condition of 37°C water bath, add trifluoroacetic acid with a final concentration of 1% after enzyme digestion to terminate the enzyme digestion reaction, and vacuum dry Afterwards, the β-casein digestion peptide was obtained;

[0090] 3. Use 100ul binding buffer (1% trifluoroacetic acid, 80% acetonitrile) to combine the Fe prepared in Example 1 3 o 4 @mSiO 2 @NTA@Fe 3+ Wash three times and set aside;

[0091] 4. Dissolve the peptide obtained in step 2 in 100ul binding buffer, and transfer to a well-balanced Fe 3 o 4 @mSiO 2 @NTA@Fe 3+ Magnetic microspheres in a centrifuge tube, and evenly disperse the magnetic mi...

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Abstract

The invention provides a nano magnetic microsphere with a hollow core-shell structure as well as a preparation method and application of the nano magnetic microsphere. The method comprises the following steps: providing Fe3O4 nano magnetic microspheres; enabling the Fe3O4 nano magnetic microspheres to react with hexadecyl trimethyl ammonium bromide and tetraethyl silicate in ethanol to obtain Fe3O4@mSiO2 with a hollow core-shell structure; ultrasonically dispersing in ethanol, and adding glycidyl oxypropyl trimethoxy silane to obtain Fe3O4@mSiO2@GPS; ultrasonically dispersing in tetrahydrofuran, and adding NH2-PEGn-NH2 to obtain amino-modified Fe3O4@mSiO2@NH2 nano magnetic microspheres; ultrasonically dispersing in 2, 4-epoxyhexane or tetrahydrofuran, adding N, N-carbonyl diimidazole to react, dispersing in an alkaline buffer solution, and adding N alpha, N alpha-bis (carboxymethyl)-L-lysine to obtain carboxylic acid modified Fe3O4@mSiO2@NTA; and ultrasonically dispersing in a ferric trichloride solution to obtain a finished product.

Description

technical field [0001] The present disclosure relates to the field of organic materials and analysis technology, in particular to a hollow core-shell structure nano magnetic microsphere, its preparation method and application. Background technique [0002] Nanomagnetic material is a new material developed in recent years, which is widely used in the fields of nuclear magnetic imaging, catalysis, sensing and enrichment materials. [0003] However, there are three problems in the process of functionalizing magnetic nanospheres, (1) the loss of dispersion, that is, small nanoparticles are easy to aggregate to form large particles to reduce the surface energy; (2) the loss of magnetism, that is, Bare magnetic nanospheres, especially Fe 3 o 4 and γ-Fe 2 o 3 It is easy to oxidize in the air, and the acid environment during the enrichment of phosphorylated peptides will also destroy the integrity of the magnetic nanospheres; (3) The surface functionalization of the magnetic nan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/28B01J20/22B01J20/30
CPCB01J20/28009B01J20/28007B01J20/28021B01J20/06B01J20/28054B01J20/103B01J20/22B01J2220/46Y02A50/30
Inventor 孟庆石冯潇慧张军民饶正华
Owner INST OF ANIMAL SCI OF CHINESE ACAD OF AGRI SCI
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