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Preparation method of superparamagnetic carboxylated chitosan/Fe3O4 nanoparticle aggregate

A carboxylated chitosan, superparamagnetic technology, applied in the preparations for in vivo experiments, medical preparations with inactive ingredients, and medical preparations containing active ingredients, etc., can solve the problem of single superparamagnetic nanoparticles. Low magnetic responsiveness, difficult magnetic responsiveness and lateral relaxation rate of a single magnetic particle, etc., to achieve the effect of simple and efficient preparation process

Active Publication Date: 2018-11-27
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, even if the saturation magnetic moment of the material itself is very high, the magnetic responsiveness of a single superparamagnetic nanoparticle is not high.
In addition, due to the limitation of particle size by superparamagnetism, it is difficult to increase the magnetic responsivity and transverse relaxation rate of a single magnetic particle by increasing the particle size.

Method used

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  • Preparation method of superparamagnetic carboxylated chitosan/Fe3O4 nanoparticle aggregate
  • Preparation method of superparamagnetic carboxylated chitosan/Fe3O4 nanoparticle aggregate
  • Preparation method of superparamagnetic carboxylated chitosan/Fe3O4 nanoparticle aggregate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 6.33g FeCl 3 ·6H 2 O and 2.33 g FeCl 2 4H 2 O is dissolved in 100g deionized water, add 0.67g carboxylated chitosan (carboxyl substitution degree 0.8, viscosity average molecular weight about 200,000), heat up to 60°C, after the carboxylated chitosan is completely dissolved, under the speed of 100rpm , adding 10g of concentrated ammonia water, the system immediately formed a black precipitate, after 30 minutes of heat preservation, the reaction temperature was raised to 90°C, and the heat preservation was continued for 45 minutes to obtain Fe 3 o 4 Aqueous dispersion of nanoparticles. The whole reaction was carried out under nitrogen atmosphere. After the reaction, the precipitate was washed with deionized water until the conductivity of the dispersion reached 10 μS cm -1 the following. After concentration, Fe 3 o 4 Fe in the aqueous dispersion of nanoparticles 3 o 4The mass fraction of nanoparticles was increased to 5%.

[0037] Weigh 2.5 g of emulsifier Sp...

Embodiment 2

[0043] 8.1g Fe 2 (SO 4 ) 3 and 5.6g FeSO 4 Dissolve in 130g deionized water, add 6.5g carboxylated chitosan (the degree of carboxyl substitution is 0.65, the viscosity average molecular weight is about 300,000), heat up to 65°C, after carboxylated chitosan is completely dissolved, under the rotating speed of 600rpm, Add 21.6g of ammonia water, the system immediately forms a black precipitate, after 100 minutes of heat preservation, the reaction temperature is raised to 95°C, and the heat preservation is continued for 30 minutes to obtain Fe 3 o 4 Aqueous dispersion of nanoparticles. The whole reaction was carried out under nitrogen atmosphere. After the reaction, the precipitate was washed with deionized water until the conductivity of the dispersion reached 10 μS cm -1 the following. After concentration, Fe 3 o 4 Fe in the aqueous dispersion of nanoparticles 3 o 4 The mass fraction of nanoparticles was increased to 10%.

[0044] Weigh 1.5g Tween-80 and 1.5g Span-8...

Embodiment 3

[0050] 18.4g FeCl 3 ·6H 2 O and 11.5g Fe(BF 4 ) 2 ·6H 2 O is dissolved in 80g deionized water, add 4.6g carboxylated chitosan (carboxyl substitution degree 0.95, viscosity average molecular weight is about 80,000), heat up to 70°C, after carboxylated chitosan dissolves completely, under the rotating speed of 500rpm , add 22.9g of ammonia water, the system immediately forms a black precipitate, after 60min of heat preservation, the reaction temperature is raised to 85°C, and the heat preservation is continued for 60min to obtain Fe 3 o 4 Aqueous dispersion of nanoparticles. The whole reaction was carried out under nitrogen atmosphere. After the reaction, the precipitate was washed with deionized water until the conductivity of the dispersion reached 10 μS cm -1 the following. After concentration, Fe 3 o 4 Fe in the aqueous dispersion of nanoparticles 3 o 4 The mass fraction of nanoparticles was increased to 15%.

[0051] Weigh 0.255g of emulsifier P(E / B)-PEO, the p...

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Abstract

The invention provides a preparation method of superparamagnetic carboxylated chitosan / Fe3O4 nanoparticle aggregate. The method comprises the following steps: (1) preparing a stable superparamagneticFe3O4 nanoparticle water dispersion solution of carboxylated chitosan; (2) dissolving an emulsifier into a non-polar solvent to obtain an emulsifier solution; (3) dissolving hydrophilic metal salt orthe hydrophilic metal salt and the carboxylated chitosan into the superparamagnetic Fe3O4 nanoparticle water dispersion solution, so as to obtain a dispersion solution A; then adding the dispersion solution A into the emulsifier solution and stirring and pre-emulsifying to obtain crude emulsion; then putting a container filled with the crude emulsion into an ice water bath; carrying out ultrasonictreatment to obtain reverse-phase fine emulsion; and (4) directly dropwise adding a crosslinking agent into the reverse-phase fine emulsion, and enabling the crosslinking agent and the carboxylated chitosan to react to obtain the superparamagnetic carboxylated chitosan / Fe3O4 nanoparticle aggregate. The method provided by the invention is simple and efficient; and the prepared superparamagnetic nanoparticle aggregate has the advantages of good dispersity, high magnetic component content, strong magnetic responsibility, excellent biocompatibility and the like.

Description

1. Technical field [0001] The present invention relates to a kind of superparamagnetic carboxylated chitosan / Fe 3 o 4 Process for the preparation of particle nanoaggregates. 2. Background technology [0002] Superparamagnetic nanoparticles have important application value in biomedical fields such as magnetic resonance imaging, cancer hyperthermia, targeted drug delivery, and cell separation [Nanoscale 2014, 6, 11553–11573.]. The above applications generally require Fe 3 o 4 Nanoparticles have superparamagnetic, transverse relaxation rate (r 2 ), high magnetic response, and controllable size and distribution [Chemical Review 2008, 108, 2064-2110.]. The size of a single superparamagnetic nanoparticle is generally small, because when the particle size is larger than 30nm, the superparamagnetic nanoparticle will transform into a ferromagnetic particle. Therefore, even if the saturation magnetic moment of the material itself is very high, the magnetic responsiveness of a s...

Claims

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Application Information

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IPC IPC(8): A61K49/12A61K47/36A61K47/02A61K41/00A61K47/61
CPCA61K41/00A61K47/02A61K47/36A61K49/126A61K47/61
Inventor 曹志海尚怡肖立圣李永祥胡亚新戚栋明
Owner ZHEJIANG SCI-TECH UNIV
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