CN103405789B - Preparation method of biomembrane modified ferriferrous oxide nanoparticle - Google Patents
Preparation method of biomembrane modified ferriferrous oxide nanoparticle Download PDFInfo
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Abstract
The invention discloses a preparation method of a biomembrane modified ferriferrous oxide nanoparticle. The preparation method comprises the following steps: (1) preparing Fe3O4 water-soluble nanoparticles; (2) preparing Fe3O4 oil-soluble nanoparticles, and reacting a Fe3O4 nanoparticle dry powder with a hexane solution containing silane; and (3) ) preparing Fe3O4 water-soluble nanoparticles by reacting the obtained oil-soluble nanoparticles with a phosphatide vesicle solution. The oil-soluble magnetic nanoparticles can dissolve in an organic carrier to form magnetofluid and can be widely applied. The modified water-soluble nanoparticles have significantly improved stability, and good biocompatibility. The modified oil-soluble magnetic nanoparticles react with the phosphatide vesicle solution to convert into water-soluble nanoparticles; and the reaction has mild conditions and is simple and practicable. The modified phosphatide can solve the problem of biocompatibility, and due to the protection of double molecular films on the surface, the stability of the nanoparticles is substantially enhanced.
Description
Technical field
The present invention relates to the preparation method of the ferriferrous oxide nano-particle that a kind of biomembrane is modified.
Background technology:
Ferriferrous oxide nanometer material obtains very large attention in today of nanotechnology high speed development, mainly because its magnetic changes with the change of particle diameter, so the nanoparticle of different size has different application.Current four oxidation three nanoparticle Application comparison are extensive, are mainly used in information storage, stealth material and biologic medical field.Verified its of U.S. FDA can be used for the contrast agent of magnetic resonance.
The synthetic method of ferroso-ferric oxide is a lot, as hydro-thermal method, and coprecipitation, microemulsion method, solvent-thermal method etc.Although the preparation of ferroso-ferric oxide is very ripe, causing it easily to reunite because it has magnetic, just affecting its application in each field once reunite.
The finishing of nano material can improve its stability and reduce reunion, and ferriferrous oxide nano-particle is by the Coulomb force between particle, and Van der Waals force and magnetic force three force balance realize its stability.Ferriferrous oxide nano-particle finishing carries out finishing by two kinds of methods usually: 1. modify Polyethylene Glycol, polyacrylic acid, the macromolecules such as polyvinylpyrrolidone; 2. one deck inorganic compound shell is wrapped on surface, as silicon dioxide etc.Above two kinds of methods or need pyroreaction, or the response time is longer.
The present invention utilizes phase transfer method, uses silylating reagent to make water-soluble ferroferric oxide become oil molten, avoids like this using expensive organic precursor, also avoids hot conditions when preparing oily molten nanoparticle simultaneously.Oily molten nanoparticle and phospholipid vesicle solution reaction are converted into water solublity, realize nanoparticle biomembranous coated.All at room temperature, the response time is a few minutes in whole reaction.
Summary of the invention
The preparation method of the ferriferrous oxide nano-particle that the present invention is modified by a kind of biomembrane, realizes ferriferrous oxide nano-particle surface modification, thus makes water soluble nanometer particles be converted into oil-soluble, then is converted into water solublity from oil-soluble.
The present invention adopts following technology: the preparation method of the ferriferrous oxide nano-particle that a kind of biomembrane is modified, as follows:
(1) be first, the FeCl of 2g: 1g: 70mL according to solid-liquid ratio
36H
2o and FeCl
24H
2o is dissolved in distilled water, to keep while 10 minutes adding and FeCl during this period after being heated to 80 DEG C
36H
2o solid-to-liquid ratio be 2g: 5mL mass concentration be the ammonia of 25% ~ 28%; Add and FeCl after 30 minutes
36H
2o solid-to-liquid ratio be 2g: 5mL volumetric concentration be 0.2g/mL sodium citrate solution, reflux cooled after 2 hours, then used ethanol, distilled water wash for subsequent use respectively;
(2), Fe
3o
4prepared by oil-soluble nano particles: get nanoparticle dry powder solid-to-liquid ratio 0.1g: 1mL of step (1) reaction preparation in hexane solution, then adding with above-mentioned nanoparticle dry powder solid-to-liquid ratio is the octadecyl trimethoxysilane supersound process of 0.1g: 1 ~ 10 μ L, final water soluble nanometer particles inversion of phases is oil-soluble, and reaction temperature is room temperature, ultrasonic time is 10 minutes;
(3), biomembrane modifies Fe
3o
4the preparation of water soluble nanometer particles: get dried oil-soluble ferroso-ferric oxide that step (2) prepares and phospholipid vesicle solution carries out ultrasonic according to solid-to-liquid ratio 0.1g: 2mL mixing, ultrasonic time 2 minutes, phospholipid vesicle uses ultrasonic method or squeezing and pressing method preparation, and concentration is 0.1mg/mL.
Because coprecipitation prepares ferroso-ferric oxide preparation method simply, reaction condition is gentle, is the method for the easiest suitability for industrialized production.And the water-soluble ferroferric oxide prepared by coprecipitation is converted into oil-soluble after ODTS room temperature lower surface is modified, oil-soluble magnetic nano-particle is dissolved in organic carrier and forms magnetic fluid, and be widely used, modified be finally the stability significance raising of water soluble nanometer particles, and has good biocompatibility.After modifying, oily molten magnetic nano-particle and phospholipid vesicle solution reaction are converted into water solublity, and reaction condition is gentle, simple.Can biocompatibility be solved after phospholipid modified, and because surface has Bilayer to protect, also substantially increase the stability of nanoparticle.
Detailed description of the invention
Embodiment 1
A preparation method for the ferriferrous oxide nano-particle that biomembrane is modified is as follows:
(1), first by 2.0g FeCl
36H
2o and 1.0g FeCl
24H
2o is dissolved in 70mL distilled water, to keep while 10 minutes adding the ammonia that 5mL mass concentration is 25% at this moment after being heated to 80 DEG C; Adding 5mL concentration after 30 minutes is 0.2g/mL sodium citrate solution, and reflux cooled after 2 hours, then uses ethanol, distilled water wash for subsequent use respectively;
(2), Fe
3o
4prepared by oil-soluble nano particles: get the 0.1g nanoparticle dry powder of step (1) reaction preparation in 1mL hexane solution, then add 1 μ L octadecyl trimethoxysilane supersound process, final water soluble nanometer particles inversion of phases is oil-soluble, and reaction temperature is room temperature, ultrasonic time is 10 minutes;
(3), biomembrane modifies Fe
3o
4the preparation of water soluble nanometer particles: get dried 0.1g oil-soluble ferroso-ferric oxide that step (2) prepares and the mixing of 2mL phospholipid vesicle is carried out ultrasonic, ultrasonic time 2 minutes, phospholipid vesicle uses ultrasonic method or squeezing and pressing method preparation, and concentration is 0.1mg/mL.
Embodiment 2
A preparation method for the ferriferrous oxide nano-particle that biomembrane is modified is as follows:
(1), first by 2.0g FeCl
36H
2o and 1.0g FeCl
24H
2o is dissolved in 70mL distilled water, to keep while 10 minutes adding the ammonia that 5mL mass concentration is 28% at this moment after being heated to 80 DEG C; Adding 5mL concentration after 30 minutes is 0.2g/mL sodium citrate solution, and reflux cooled after 2 hours, then uses ethanol, distilled water wash for subsequent use respectively;
(2), Fe
3o
4prepared by oil-soluble nano particles: get the 0.1g nanoparticle dry powder of step (1) reaction preparation in 1mL hexane solution, then add 10 μ L octadecyl trimethoxysilane supersound process, final water soluble nanometer particles inversion of phases is oil-soluble, and reaction temperature is room temperature, ultrasonic time is 10 minutes;
(3), biomembrane modifies Fe
3o
4the preparation of water soluble nanometer particles: get dried 0.1g oil-soluble ferroso-ferric oxide that step (2) prepares and the mixing of 2mL phospholipid vesicle is carried out ultrasonic, ultrasonic time 2 minutes, phospholipid vesicle uses ultrasonic method or squeezing and pressing method preparation, and concentration is 0.1mg/mL.
The present invention realizes the quick phase transfer of magnetic nano-particle, both water soluble nanometer particles can be converted into oil-soluble, oil-soluble nano particles can be converted into water solublity again.The molten ferriferrous oxide nano-particle of oil after conversion and phospholipid vesicle solution reaction superscribe monolayer phospholipid molecule, are converted into water-soluble ferroferric oxide nano particle, improve stability.Due to the composition that phospholipid molecule itself is cell membrane, so the ferriferrous oxide nano-particle that biomembrane is modified has very high biocompatibility, can break through blood brain barrier becomes brain tumor medical magnetic resonance contrast agent.This kind of method of modifying is applicable to oxide nano-particles as TiO
2, Fe
2o
3, SiO
2deng.
Claims (1)
1. a preparation method for the ferriferrous oxide nano-particle of biomembrane modification, it is characterized in that, method is as follows:
(1) be first, the FeCl of 2g: 1g: 70mL according to solid-liquid ratio
36H
2o and FeCl
24H
2o is dissolved in distilled water, to keep while 10 minutes adding and FeCl during this period after being heated to 80 DEG C
36H
2o solid-to-liquid ratio be 2g: 5mL mass concentration be the ammonia of 25% ~ 28%; Add and FeCl after 30 minutes
36H
2o solid-to-liquid ratio be 2g: 5mL volumetric concentration be 0.2g/mL sodium citrate solution, reflux cooled after 2 hours, then used ethanol, distilled water wash for subsequent use respectively;
(2), Fe
3o
4prepared by oil-soluble nano particles: get nanoparticle dry powder solid-to-liquid ratio 0.1g: 1mL of step (1) reaction preparation in hexane solution, then adding with above-mentioned nanoparticle dry powder solid-to-liquid ratio is the octadecyl trimethoxysilane supersound process of 0.1g: 1 ~ 10 μ L, final water soluble nanometer particles inversion of phases is oil-soluble, and reaction temperature is room temperature, ultrasonic time is 10 minutes;
(3), biomembrane modifies Fe
3o
4the preparation of water soluble nanometer particles: get dried oil-soluble ferroso-ferric oxide that step (2) prepares and phospholipid vesicle solution carries out ultrasonic according to solid-to-liquid ratio 0.1g: 2mL mixing, ultrasonic time 2 minutes, phospholipid vesicle uses ultrasonic method or squeezing and pressing method preparation, and concentration is 0.1mg/mL.
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| CN110157000B (en) * | 2018-02-12 | 2022-05-31 | 巨生生医股份有限公司 | Biocompatible magnetic material |
| CN108878940B (en) * | 2018-06-28 | 2021-06-01 | 广东工业大学 | Film forming method of electroactive biomembrane and application thereof |
| CN109879326B (en) * | 2019-03-22 | 2021-07-06 | 信阳师范学院 | Method for preparing iron oxide nanoparticles by using tea leaves |
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