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Preparation method and application of a core-shell magnetic composite microsphere rich in nickel ions on the surface

A technology of magnetic composite microspheres and nickel ions, applied in peptide preparation methods, chemical instruments and methods, alkali metal compounds, etc., can solve problems such as poor ability and high price, and achieve good separation ability, simple process, and short preparation time short effect

Inactive Publication Date: 2016-04-13
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, the metal ions commonly used to enrich histidine proteins are nickel ions or copper ions, and the ligands used to fix these ions are usually nitrilotriacetic acid or iminodiacetic acid, but the former is more expensive as a ligand, while the latter Compared with the former, the ability to complex nickel ions is poor. It is necessary to develop a new type of ligand with better effect and low cost for immobilizing metal ions.

Method used

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  • Preparation method and application of a core-shell magnetic composite microsphere rich in nickel ions on the surface
  • Preparation method and application of a core-shell magnetic composite microsphere rich in nickel ions on the surface
  • Preparation method and application of a core-shell magnetic composite microsphere rich in nickel ions on the surface

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Example 1: Core-shell Fe with a shell thickness of about 10 nm and a crosslinking degree of 10% 3 o 4 / PVIM-Ni 2+ Preparation of microspheres

[0034] 1. Preparation of magnetic clusters stabilized by sodium citrate

[0035] 1.3g ferric chloride hexahydrate (FeCl 3 ·6H 2 O), 3.8g ammonium acetate (NH 4 Ac), after dissolving 0.4g sodium citrate in 70mL ethylene glycol, put it into a 150mL three-necked flask, then raise the temperature to 170°C, stir and react for 1 hour, then transfer the liquid in the flask into a 100mL polytetrafluoroethylene-containing Lined autoclave, then put the autoclave into an oven at 200°C for 16 hours, take it out, and cool it to room temperature with tap water. The product is separated by magnetic separation, washed with absolute ethanol to remove unreacted reactants, and finally the product is dispersed in absolute ethanol for later use;

[0036] 2. Active vinyl modification on the surface of magnetic clusters

[0037] Add 300mg of m...

Embodiment 2

[0042] Example 2: The core-shell Fe with a shell thickness of about 80 nm and a cross-linking degree of 20% 3 o 4 / PVIM-Ni 2+ Preparation of microspheres (transmission electron microscope photos see figure 1 );

[0043] 1. The preparation of sodium citrate-stabilized magnetic clusters is as described in Example 1-1;

[0044] 2. Carrying out active vinyl modification on the surface of magnetic clusters is the same as that described in Example 1-2;

[0045] 3. Core-shell Fe 3 o 4 / PVIM was prepared as described in Examples 1-3. The difference is vinylimidazole, N,N' - The dosages of methylene bisacrylamide and 2,2-azobisisobutyronitrile are 400 μL, 100 mg, and 10 mg, respectively;

[0046] 4. The reaction of complexed nickel ions is the same as that described in Examples 1-4.

Embodiment 3

[0047] Example 3: The shell thickness is about 80nm, and the cross-linking degree is 40% core-shell Fe 3 o 4 / PVIM-Ni 2+ Preparation of microspheres

[0048] 1. The preparation of sodium citrate-stabilized magnetic clusters is as described in Example 1-1;

[0049] 2. Carrying out active vinyl modification on the surface of magnetic clusters is the same as that described in Example 1-2;

[0050] 3. Core-shell Fe 3 o 4 / PVIM was prepared as described in Examples 1-3. The difference is vinylimidazole, N,N' - The dosages of methylenebisacrylamide and 2,2-azobisisobutyronitrile are 300 μL, 200 mg, and 10 mg, respectively;

[0051] 4. The reaction of complexed nickel ions is the same as that described in Examples 1-4.

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Abstract

The invention discloses a preparation method of a nuclear-shell type magnetic composite microsphere which can be used for separating histidine protein, and an application of the nuclear-shell type magnetic composite microsphere. The core of the nuclear-shell type magnetic composite microsphere is a magnetic ferriferrous oxide nano particle cluster, the shell of the nuclear-shell type magnetic composite microsphere is a crosslinked polymer network rich in imidazole groups, the imidazole groups are chelated with the nickel ions to ensure that a great number of the nickel ions are fixed on the surface of the microsphere, natural histidine protein or recombinant protein which contains six histidine tags is rapidly separated through the interaction of the fixed nickel ions and the imidazole groups in histidine under neutral conditions. The preparation method comprises the steps of firstly preparing a sodium citrate stabilized magnetic nano particle cluster; modifying active vinyl functional groups on the surface of the magnetic cluster by adopting a sol-gel method; then preparing a nuclear-shell type magnetic polymer composite microsphere with the surface rich in imidazole groups, which has high magnetic responsibility and monodispersity, through backflow, precipitation and polymerization; then performing complexing on the nickel ions lack in electrons by using imidazole rich in the electrons; finally enriching or removing histidine protein. The preparation method disclosed by the invention is simple, controllable in process and high in efficiency of separating and purifying histidine protein, can be recycled for many times, and has good application prospects.

Description

technical field [0001] The invention belongs to the technical field of nanometer functional materials, and in particular relates to a preparation method and application of a core-shell magnetic composite microsphere whose surface is rich in nickel ions. Background technique [0002] In recent years, organic-inorganic hybrid composite microspheres, especially magnetic composite microspheres, are receiving widespread attention. Since magnetic polymer microspheres have both the surface modification of organic polymers and the magnetic responsiveness of inorganic magnetic materials, they can separate target biomolecules conveniently, quickly and efficiently under an external magnetic field. Therefore, it has broad application prospects in biomedical fields such as protein separation and purification, cell separation, magnetic resonance imaging, and magnetically targeted drug loading. [0003] At present, magnetic polymer composite microspheres with different structures can be p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F292/00C08F226/06C08F222/38C08F8/42B01J20/26B01J20/28C07K1/14
Inventor 汪长春章雨婷
Owner FUDAN UNIV
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