Surface modification method of magnetic iron oxide nano-particles

A technology of magnetic iron oxide and nanoparticles, which is applied in the direction of pharmaceutical formulations, preparations for in vivo tests, emulsion delivery, etc., can solve the problems of inability to maintain blood concentration and circulation time, and achieve inhibition of plasma protein adsorption and good stability and biocompatibility, the effect of improving biocompatibility

Inactive Publication Date: 2012-07-11
QINGDAO UNIV OF SCI & TECH
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Problems solved by technology

[0004] The invention aims at the technical problem that the magnetic nanoparticles enter the blood circulation system and are cleared by the reticuloendothelial system, and cannot maintain effective blood concentration and circulation time to reach the target site for imaging diagnosis, and provide a magnetic iron oxide nanoparticle surface contact Surface modification method of branched 2-(meth)acryloyloxyethyl phosphorylcholine polymer

Method used

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  • Surface modification method of magnetic iron oxide nano-particles
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  • Surface modification method of magnetic iron oxide nano-particles

Examples

Experimental program
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Effect test

Embodiment 1

[0031] (1) Add 2mmol iron acetylacetonate and 25mL triethylene glycol into a three-necked flask and mix thoroughly, heat and stir with nitrogen gas for 2 minutes, raise the temperature to 190°C at a constant speed (0.5°C / min), keep it warm for 10 minutes, and then rapidly increase the temperature (10°C / min) min) to boiling, keep boiling for 30min to stop the reaction, cool, and the resulting reaction solution is flocculated and precipitated with ethyl acetate, separated with a magnet, and then washed 3 times with ethyl acetate to obtain a magnetic Fe 3 o 4 Nanoparticles.

[0032] Magnetic Fe 3 o 4 The morphology of the nanoparticles see figure 1 Transmission electron microscope (TEM) photo. Depend on figure 1 It can be seen that the nanoparticles obtained through the step (1) have a particle size of less than 10 nm, uniform size, and good dispersibility in aqueous solution.

[0033] (2) Take 50mg of the above-mentioned magnetic Fe 3 o 4 After cleaning the nanoparticles...

Embodiment 2

[0038] (1) Add 4mmol iron acetylacetonate and 25mL triethylene glycol into a three-necked flask and mix thoroughly, heat and stir after passing through nitrogen for 4 minutes, raise the temperature to 180°C at a uniform speed (1°C / min), keep it warm for 10 minutes, and then rapidly raise the temperature (8°C / min) min) to boiling, keep boiling for 40min to stop the reaction, cool, and the resulting reaction solution is flocculated and precipitated with ethyl acetate, separated with a magnet, and then washed 3 times with ethyl acetate to obtain a magnetic Fe 3 o 4 Nanoparticles;

[0039] (2) Take 100mg of the above-mentioned magnetic Fe 3 o 4 After cleaning the nanoparticles with dry toluene for 3 times, disperse them in 50ml of dry toluene, ventilate nitrogen, ultrasonically, add 1mlCTCS after 15 minutes, continue the ultrasonic reaction at room temperature for 3 hours, stop the reaction, and use tetrahydrofuran and a mixed solvent (ethanol: water The volume ratio is 1:2) to...

Embodiment 3

[0043] (1) Add 8mmol iron acetylacetonate and 25mL triethylene glycol into a three-necked flask and mix thoroughly, heat and stir after passing nitrogen gas for 2 minutes, raise the temperature to 170°C at a uniform speed (2°C / min), keep it warm for 13min, and then rapidly raise the temperature (6°C / min) min) to boiling, keep boiling for 30min to stop the reaction, cool, and the resulting reaction solution is flocculated and precipitated with acetone, separated with a magnet, and then washed 3 times with ethyl acetate to obtain a magnetic Fe 3 o 4 Nanoparticles;

[0044] (2) Take 100mg of the above-mentioned magnetic Fe 3 o 4 After cleaning the nanoparticles with dry toluene for 3 times, disperse them in 40ml of dry toluene, ventilate nitrogen, ultrasonically, add 0.7mlCTCS after 15 minutes, continue the ultrasonic reaction at room temperature for 3 hours, stop the reaction, use tetrahydrofuran and a mixed solvent (ethanol: The volume ratio of water is 1: 3) to wash the rea...

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Abstract

The invention relates to a surface modification method of magnetic iron oxide nano-particles. The method comprises the following steps: leading mixed solution consisting of iron acetylacetonate and triethylene glycol to react for a period at low and constant temperature, quickly heating to boil, and cooling to room temperature after the mixed solution reacts for a period to obtain a reaction solution; precipitating, magnetically separating and cleaning the reaction solution to obtain magnetic Fe3O4 nano-particles carrying hydroxyl on the surface; dispersing to dried toluene by ultrasonic, adding 2-(4-benzene sulfonyl chloride) trichlorosilane to obtain Fe3O4 nano-particles carrying a specific initiation group; and dispersing to mixed solution of water and ethanol by ultrasonic, and adding2,2'-bipyridyl, copper chloride, cuprous chloride and 2-(meth)acryloyloxyethyl phosphorylcholine to obtain phosphorylcholine polymer modified magnetic Fe3O4 nano-particles. The method is mild in reaction conditions, simple and feasible and strong in controllability; and the prepared magnetic Fe3O4-phosphorylcholine polymer nano-composite material has excellent stability and biocompatibility in aqueous solution.

Description

technical field [0001] The invention relates to a method for surface modification of magnetic iron oxide nanoparticles, in particular to a method for grafting 2-(meth)acryloyloxyethyl phosphoric acid on the surface of magnetic ferric iron tetroxide nanoparticles prepared by a polyol method Choline polymer approach. Background technique [0002] Magnetic iron oxide nanoparticles have excellent magnetic properties and good biocompatibility, not only can be used for the rapid separation of biomolecules and cells in vitro, but also can be used for high-sensitivity nuclear magnetic resonance imaging in vivo, targeted drug delivery, tumor hyperthermia, Frontier fields such as gene delivery have broad application prospects in the early diagnosis and treatment of cancer and other major diseases. However, magnetic nanoparticles without surface modification are not compatible with blood components. After entering the blood circulation system, a large amount of plasma proteins will be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K49/18A61K49/12
Inventor 陈克正万家齐于寿山孙晓燕
Owner QINGDAO UNIV OF SCI & TECH
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