CN102861921B - A kind of preparation method of core-shell magnetic/gold nanocomposite particles - Google Patents
A kind of preparation method of core-shell magnetic/gold nanocomposite particles Download PDFInfo
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- CN102861921B CN102861921B CN201110190350.5A CN201110190350A CN102861921B CN 102861921 B CN102861921 B CN 102861921B CN 201110190350 A CN201110190350 A CN 201110190350A CN 102861921 B CN102861921 B CN 102861921B
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Abstract
The invention discloses a kind of preparation method of golden magnetic composite nanoparticle, first this preparation method adopts coprecipitation to prepare magnetic Fe
3o
4nano particle, dopamine obtains the Fe of poly-dopamine modification at magnetic particle surface in-situ polymerization subsequently
3o
4nano particle, at Fe
3o
4nanoparticle surface introduces polyphenol and amino group, then by electrostatic interaction, nm of gold seed is adsorbed in the magnetic particle surface of modification, to be adsorbed in the nm of gold of magnetic particle surface for seed, the polyphenol of magnetic particle surface is reducing agent, successively drip chlorauric acid solution, progressively generate layer gold at magnetic particle surface, prepare gold magnetic core-shell nano-particle.This nano particle water dispersible is good, and magnetic responsiveness is strong.This diameter of nano particles is 30 ~ 100nm, and saturation magnetization is 30.1 ~ 38.7emu/g, presents superparamagnetism.This nano particle has broad application prospects in the field such as to be separated of targeted drug controlled release, thermotherapy, protein and enzyme.
Description
Technical field
The invention belongs to field of nanocomposite materials, particularly a kind of preparation (i.e. the outer golden core/shell nanoparticles of tri-iron tetroxide magnetic nuclear membrane) of gold-magnetic nanoparticle.
Background technology
The characteristics such as the peculiar magnetic field responsiveness of magnetic nano-particle, nanometer size effect, hypotoxicity and biocompatibility, make it be widely used in various fields.Magnetic nano-particle is that life science and biotechnology provide multiple possibility, is all widely used in bio-separation, target administration, thermotherapy and magnetic resonance radiography technology etc.In addition, in catalytic field, make catalyst carrier with it, not only greatly can improve catalyst activity, and be convenient to recovery and the recycling of catalyst.But nanomagnetic particle is easily oxidized and reduce magnetic, and surface is not easily modified.At its Surface coating one deck gold shell, form the magnetic/golden nanometer particle of nucleocapsid structure, the shortcoming of nanomagnetic particle can be overcome.Nucleocapsid magnetic/golden nanometer particle has magnetic field responsiveness, has the characteristic of nano Au particle concurrently, as: excellent optical property, catalytic performance, surface are easy to the characteristic such as modification and good biocompatibility.Significant application value is had in the photo-thermal therapy etc. of immunology detection, target drug-carrying, cancer cell.Also can be used for the mark of protein, nucleic acid, antibody, antigen etc., and the separation of protein, cell, DNA etc. detects.
The main method of current employing is exactly at Fe
3o
4existence under, add reducing agent reduction gold chloride, prepare the nano particle of nucleocapsid structure, reducing agent used is generally azanol, natrium citricum, sodium borohydride etc.Core-shell particles dispersiveness prepared by this method is bad, and is difficult to obtain coated uniform particle, and added reducing agent is most of poisonous in addition.Patent CN1736881 reports and prepares the coated nanometer Fe of natrium citricum by coprecipitation
3o
4particle, then make crystal seed with it, under boiling condition, use reduction of sodium citrate gold chloride, obtained nucleocapsid magnetic/golden nanometer particle, the nanometer Fe that this method obtains
3o
4particle easy oxidized magnetic under boiling condition reduces, and obtained nanoparticle dispersion is bad.Have employed seed mediator method afterwards, namely first to magnetic nano-particle modifying surface, make this particle surface can be positively charged, then electronegative nm of gold seed is passed through electrostatic attraction used load on magnetic nano-particle, with this seed for organic centre, core-shell particles is obtained by the method successively dripping gold chloride and the reducing agent aqueous solution, although the particle that this method obtains is coated comparatively regular, preparation process more complicated.
Recently, scientist find mussel can free adsorbing at wet body surface.By finding the research of its foot structure, containing a large amount of dopamines in the protein composition of mussel foot.Research finds that dopamine on the surface home position polymerization reaction can occur at a lot of inorganic or organic polymers in the basic conditions, and the poly-dopamine of formation has certain adhesiveness.In addition contain ortho position phenolic hydroxyl group, amino, Kun Deng functional group in poly-dopamine, the poly-dopamine film of material surface can be used as the platform of secondary response, carries out further modification to material surface.There are some researches show that poly-dopamine can help the metallization on surface as a kind of active principle.
Summary of the invention
Below in conjunction with embodiment, the invention will be further described, and subject area involved in the present invention is not limited only to this two examples.
(1) Fe
3o
4the preparation of nano particle: by title 3.90 ~ 4.20gFeCl
35H
2o and 2.10 ~ 2.35gFeCl
26H
2o is dissolved in 80 ~ 120ml water, logical N
2deoxygenation, then fast drop ammoniacal liquor, logical N at 70 ~ 90 DEG C
2stirring reaction 40 ~ 60min, generates Fe
3o
4nano particle black precipitate, after reaction terminates, is cooled to room temperature, Magneto separate, is washed to clear liquid in neutral, vacuum drying.
(2) poly-dopamine MODIFIED Fe
3o
4the preparation of nano particle: be dissolved in by dopamine in the Tris-HCl cushioning liquid of pH=8.5, the concentration of dopamine controls to be 1 ~ 2mg/ml, gets the Fe obtained in (1)
3o
4nano particle 100 ~ 200mg is scattered in the above-mentioned dopamine cushioning liquid of 50 ~ 100ml, ultrasonic under room temperature, stirring 2 ~ 4h, and Magneto separate, after distilled water washing is neutrality to clear liquid, is made into 10ml/mg dispersion liquid with distilled water, obtains the Fe of poly-dopamine modification
3o
4nanoparticle dispersion liquid;
(3) preparation of nm of gold seed: get 2%HAuCl
44H
2o aqueous solution 0.25ml joins in 50ml water, and the sodium citrate solution adding 0.5ml1% under stirring adds, and then adds 0.5mlNaBH
4the aqueous solution (37.5mgNaBH
4, be settled to 50ml with the sodium citrate solution of 1%), continue to stir 5min, after reaction terminates, put into refrigerator and preserve; Wherein, NaBH
4the aqueous solution is for being taken from 37.5mgNaBH
4sodium citrate solution with 1% is settled to the solution that 50ml is formed.
(4) Fe of loaded with nano gold seeds
3o
4the preparation of nano particle: the Fe getting in 1ml (2) the poly-dopamine modification obtained
3o
4nanoparticle dispersion liquid, add wherein by nm of gold seed solution obtained in 10ml (3), ultrasonic disperse was placed 15 minutes after 2 ~ 4 minutes, Magneto separate, and washing, adds 20ml distilled water and be configured to solution;
(5) preparation of core-shell magnetic/gold nanocomposite particles: get 2%HAuCl
44H
2o aqueous solution 0.1ml joins in the particle dispersion of (4) gained, ultrasonic under room temperature, stirring 20 ~ 30min, Magneto separate, washing, add 20ml distilled water and be configured to solution, repeat this experiment four times, obtain the dispersion liquid 20ml of core-shell magnetic/gold nanocomposite particles, Magneto separate, vacuum drying.
Core-shell magnetic/gold nanocomposite particles obtained by the inventive method good dispersion in water, magnetic responsiveness is strong, and this particle diameter is 30 ~ 100nm, and saturation magnetization is 30.1 ~ 38.7emu/g, presents superparamagnetism.
One of advantage of the present invention is that the preparation condition green of nucleocapsid magnetic/golden nanometer particle is easy, overcomes literature method severe reaction conditions, shortcoming that reaction reagent toxicity is high.
Two of advantage of the present invention is that the poly-dopamine of the magnetic nano particle sub-surface of poly-dopamine modification not only can adsorb nm of gold seed, and the effect of reducing agent can be played by central adjacent phenolic group group, it is a kind of very safe, green synthetic method, in addition preparation condition is gentle, ferriferrous oxide nano-particle is not easily oxidized, and magnetic can not reduce.
Three of advantage of the present invention is that nucleocapsid magnetic/gold compound nano-particle that this method obtains can stably be dispersed in water.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of the core-shell magnetic/gold nanocomposite particles obtained by the present invention.
Fig. 2 is the poly-dopamine MODIFIED Fe obtained by the present invention
3o
4the X-ray diffractogram of (a) and core-shell magnetic/gold nanocomposite particles (b).
Fig. 3 is the poly-dopamine MODIFIED Fe obtained by the present invention
3o
4the hysteresis curve figure of (a) and core-shell magnetic/gold nanocomposite particles (b).
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, and subject area involved in the present invention is not limited only to this two examples.
Embodiment 1
This example is intended to illustrate exploitativeness prepared by nucleocapsid of the present invention magnetic/gold nanocomposite particle.
1. magnetic nano-particle preparation:
Claim 4.1gFeCl
35H
2o and 2.35gFeCl
26H
2o, in flask, adds the water-soluble solution of 100ml, and after 0.5 hour, fast drop 10ml30 ℅ ammoniacal liquor, is warming up to 80 DEG C, slaking 1 hour under vigorous stirring, is cooled to Magneto separate after room temperature, is washed to clear liquid in neutral, products therefrom vacuum drying.
2. poly-dopamine MODIFIED Fe
3o
4the preparation of nano particle
Get 90mgFe
3o
4nano particle joins in the there-necked flask filling 180mlTris (pH=8.5) solution, 20min is stirred on ultrasonic limit, limit, then getting 360mg dopamine joins in above-mentioned there-necked flask, 4h is stirred on ultrasonic limit, limit, then side Magneto separate, distilled water is washed till clear liquid in neutral, is made into 10ml/mg dispersion liquid, obtains the Fe of poly-dopamine modification with distilled water
3o
4nanoparticle dispersion liquid.
3. the preparation of nm of gold seed
Get 2%HAuCl
44H
2o aqueous solution 0.25mlHAuCl
44H
2o joins in 50ml water, and the sodium citrate solution adding 0.5ml1% under stirring after 1min adds, and adds 0.5mlNaBH after 1min
4the aqueous solution (37.5mgNaBH
4, be settled to 50ml with the sodium citrate solution of 1%), continue to stir 5min, after reaction terminates, put into refrigerator and preserve.
4. the Fe of loaded with nano gold seeds
3o
4the preparation of nano particle
Get the Fe that 1ml gathers dopamine modification
3o
4nanoparticle dispersion liquid, adds wherein by 10ml nm of gold seed solution, places 15min, Magneto separate after ultrasonic disperse 4min, and washing, adds 20ml distilled water and be configured to solution.
5. the preparation of core-shell magnetic/gold nanocomposite particles
Get 2%HAuCl
44H
2o aqueous solution 0.1ml joins in the particle dispersion of 4 gained, ultrasonic under room temperature, stirring 20min, Magneto separate, washing, adds 20ml distilled water and is configured to solution, repeats this experiment four times, obtain the dispersion liquid 20ml of core-shell magnetic/gold nanocomposite particles, Magneto separate is colourless to clear liquid, vacuum drying.
Above-mentioned example is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other field any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (2)
1. a preparation method for core-shell magnetic/gold nanocomposite particles, is characterized in that: this preparation method comprises the steps:
(1) Fe
3o
4the preparation of nano particle: by title 3.90 ~ 4.20gFeCl
35H
2o and 2.10 ~ 2.35gFeCl
26H
2o is dissolved in 80 ~ 120ml water, logical N
2deoxygenation, then fast drop ammoniacal liquor, logical N at 70 ~ 90 DEG C
2stirring reaction 40 ~ 60min, generates Fe
3o
4nano particle black precipitate, after reaction terminates, is cooled to room temperature, Magneto separate, is washed to clear liquid in neutral, vacuum drying;
(2) poly-dopamine MODIFIED Fe
3o
4the preparation of nano particle: be dissolved in by dopamine in the Tris-HCl cushioning liquid of pH=8.5, the concentration of dopamine controls to be 1 ~ 2mg/ml, gets the Fe obtained in (1)
3o
4nano particle 100 ~ 200mg is scattered in the above-mentioned dopamine cushioning liquid of 50 ~ 100ml, ultrasonic under room temperature, stirring 2 ~ 4h, and Magneto separate, after distilled water washing is neutrality to clear liquid, is made into 10ml/mg dispersion liquid with distilled water, obtains the Fe of poly-dopamine modification
3o
4nanoparticle dispersion liquid;
(3) preparation of nm of gold seed: get 2%HAuCl
44H
2o aqueous solution 0.25ml joins in 50ml water, and the sodium citrate solution adding 0.5ml1% under stirring adds, and then adds 0.5mlNaBH
4the aqueous solution, continues to stir 5min, after reaction terminates, puts into refrigerator and preserve; Wherein, NaBH
4the aqueous solution is for being taken from 37.5mgNaBH
4sodium citrate solution with 1% is settled to the solution that 50ml is formed;
(4) Fe of loaded with nano gold seeds
3o
4the preparation of nano particle: the Fe getting in 1ml (2) the poly-dopamine modification obtained
3o
4nanoparticle dispersion liquid, add wherein by nm of gold seed solution obtained in 10ml (3), ultrasonic disperse was placed 15 minutes after 2 ~ 4 minutes, Magneto separate, and washing, adds 20ml distilled water and be configured to solution;
(5) preparation of core-shell magnetic/gold nanocomposite particles: get 2%HAuCl
44H
2o aqueous solution 0.1ml joins in the particle dispersion of (4) gained, ultrasonic under room temperature, stirring 20 ~ 30min, Magneto separate, washing, add 20ml distilled water and be configured to solution, repeat this experiment four times, obtain the dispersion liquid 20ml of core-shell magnetic/gold nanocomposite particles, Magneto separate, vacuum drying.
2. the preparation method of a kind of core-shell magnetic/gold nanocomposite particles according to claim 1, it is characterized in that: described obtained core-shell magnetic/gold nanocomposite particles good dispersion in water, magnetic responsiveness is strong, this particle diameter is 30 ~ 100nm, saturation magnetization is 30.1 ~ 38.7emu/g, presents superparamagnetism.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9943487B2 (en) | 2015-05-26 | 2018-04-17 | The Board Of Trustees Of The University Of Illinois | Polydopamine-coated capsules |
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