CN102861921A - Preparation method of core-shell magnetic/gold nano particles - Google Patents
Preparation method of core-shell magnetic/gold nano particles Download PDFInfo
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Abstract
The invention discloses a preparation method of magnetic/gold nano particles. The preparation method comprises the following steps: firstly adopting a co-precipitation method to prepare the magnetic Fe3O4 nano particles; polymerizing the dopamine in-situ on the surfaces of the magnetic particles to obtain Fe3O4 nano particles modified by the poly dopamine; introducing polyphenol and amino groups to the surfaces of the Fe3O4 nano particles; absorbing the nano gold seeds on the surfaces of the modified magnetic particles through the static action; adopting the nano gold which is absorbed on the surfaces of the magnetic particles as the seed, adopting the polyphenol on the surfaces of the magnetic particles as a reducing agent, gradually adding the chloroauric acid liquid to gradually produce the gold layers on the surfaces of the magnetic particles to obtain the core-shell magnetic/gold nano particles. The nano particles have good water dispersion and strong magnetic respond performance. The diameters of the nano particles are 30-100 nanometers, the saturation magnetization is 30.1-38.7emu/g, and the nano particles are superparamagnetic. The nano particles have wide application prospect on the fields of targeted drug controlled release, thermal therapy, separation of protein and enzyme, etc.
Description
Technical field
The invention belongs to field of nanocomposite materials, particularly a kind of preparation of gold-magnetic nanoparticle (being the outer golden core/shell nanoparticles of tri-iron tetroxide magnetic nuclear membrane).
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 for life science and biotechnology provide multiple may, all be widely used at aspects such as bio-separation, target administration, thermotherapy and magnetic resonance radiography technology.In addition, in catalytic field, make catalyst carrier with it, not only can greatly improve catalyst activity, and be convenient to recovery and the recycling of catalyst.Reduce magnetic but nanomagnetic particle is easy oxidized, and the surface is difficult for modifying.Coat the layer of gold shell on its surface, form the magnetic/golden nanometer particle of nucleocapsid structure, can overcome the shortcoming of nanomagnetic particle.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 modify and the good characteristics such as biocompatibility.There is significant application value the aspects such as photo-thermal therapy at immunology detection, target drug-carrying, cancer cell.The mark that also can be used for 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, used reducing agent is generally azanol, natrium citricum, sodium borohydride etc.The core-shell particles dispersiveness of this method preparation is bad, and is difficult to obtain coating uniform particle, adds in addition reducing agent most of poisonous.Patent CN1736881 has reported with coprecipitation and has prepared the nanometer Fe that natrium citricum coats
3O
4Particle is made crystal seed with it again, under the boiling condition, reduces gold chloride with natrium citricum, makes nucleocapsid magnetic/golden nanometer particle, the nanometer Fe that this method obtains
3O
4Particle easy oxidized magnetic under the boiling condition reduces, and the nano particle dispersiveness that makes is bad.Adopted afterwards the seed mediator method, namely first to the magnetic nano-particle modifying surface, so that this particle surface can be positively charged, then with electronegative nm of gold seed by the electrostatic attraction used load on magnetic nano-particle, take this seed as organic centre, obtain core-shell particles by the method that drips one by one gold chloride and the reducing agent aqueous solution, although the particle that this method obtains coating is comparatively regular, the preparation process more complicated.
Recently, scientist find mussel can free adsorbing at wet body surface.Find by the research to its foot structure, the protein of mussel foot contains a large amount of dopamines in forming.Research finds that dopamine can be in a lot of inorganic or surperficial home position polymerization reaction that occur of organic polymer under alkali condition, and the poly-dopamine of formation has certain adhesiveness.Contain the functional groups such as ortho position phenolic hydroxyl group, amino, quinone in the poly-dopamine in addition, the poly-dopamine film of material surface can be used as the platform of secondary response, and material surface is carried out further modification.There are some researches show that poly-dopamine can be used as the metallization that a kind of active principle helps the surface.
Summary of the invention
The purpose of this invention is to provide a kind of green, the easy method for preparing nucleocapsid magnetic/gold nano compound particle, can obtain the nano-complex particle of fine dispersion in water with this preparation method.This nano-complex particle can be in fields such as the mark of biology and non-biological material, separation, detections.
(1) Fe
3O
4The preparation of nano particle: will claim 3.90～4.20g FeCl
35H
2O and 2.10～2.35g FeCl
26H
2O is dissolved in 80～120ml water, logical N
2Then deoxygenation drips ammoniacal liquor fast, in 70～90 ℃ of lower logical N
2Stirring reaction 40～60min generates Fe
3O
4The nano particle black precipitate after reaction finishes, is cooled to room temperature, and magnetic separates, and is washed to the stillness of night to be neutral, vacuum drying.
(2) poly-dopamine MODIFIED Fe
3O
4The preparation of nano particle: dopamine is dissolved in the Tris-HCl cushioning liquid of pH=8.5, the concentration of dopamine is controlled to be 1～2mg/ml, gets the Fe that obtains in (1)
3O
4Nano particle 100～200mg is scattered in the above-mentioned dopamine cushioning liquid of 50～100ml, and is ultrasonic under the room temperature, stir 2～4h, and magnetic separates, and distilled water is made into the 10ml/mg dispersion liquid with distilled water after washing and being neutrality to clear liquid, obtains the Fe of poly-dopamine modification
3O
4Nanoparticle dispersion liquid;
(3) preparation of nm of gold seed: get 0.25ml HAuCl
44H
2O (2%) aqueous solution joins in the 50ml water, and the sodium citrate solution that stirs the lower 0.5ml 1% of adding adds, and then adds 0.5ml NaBH
4The aqueous solution (37.5mgNaBH
4, be settled to 50ml with 1% sodium citrate solution), continue to stir 5min, reaction is put into refrigerator and is preserved after finishing.
(4) Fe of loaded with nano gold seeds
3O
4The preparation of nano particle: the Fe that gets resulting poly-dopamine modification among the 1ml (2)
3O
4Nanoparticle dispersion liquid adds the nm of gold seed solution that makes among the 10ml (3) wherein, and ultrasonic dispersion was placed 15 minutes after 2～4 minutes, and magnetic separates, and washing adds 20ml distilled water and is configured to solution;
(5) preparation of core-shell magnetic/gold nanocomposite particles: get 0.1ml HAuCl
44H
2O (2%) aqueous solution joins in the particle dispersion of (4) gained, ultrasonic under the room temperature, stirring 20～30min, magnetic separates, 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, magnetic separates, vacuum drying.
The prepared core-shell magnetic/gold nanocomposite particles of 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 the green easily row of the preparation condition of nucleocapsid magnetic/golden nanometer particle, has overcome 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 the 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, preparation condition is gentle in addition, ferriferrous oxide nano-particle is difficult for oxidized, and magnetic can not reduce.
Three of advantage of the present invention is that nucleocapsid magnetic/gold compound nano-particle that this method makes can stably be dispersed in water.
Description of drawings
Fig. 1 is the transmission electron microscope photo of the prepared core-shell magnetic/gold nanocomposite particles of the present invention.
Fig. 2 is the prepared poly-dopamine MODIFIED Fe of the present invention
3O
4(a) and the X-ray diffractogram of core-shell magnetic/gold nanocomposite particles (b).
Fig. 3 is the prepared poly-dopamine MODIFIED Fe of the present invention
3O
4(a) and the hysteresis curve figure of core-shell magnetic/gold nanocomposite particles (b).
The specific embodiment
The invention will be further described below in conjunction with embodiment, and subject area involved in the present invention is not limited only to this two examples.
Embodiment 1
This example is intended to illustrate the exploitativeness of nucleocapsid magnetic of the present invention/gold nano compound particle preparation.
1. magnetic nano-particle preparation:
Claim 4.1gFeCl
35H
2O and 2.35gFeCl
26H
2O adds the water-soluble solution of 100ml in flask, drip fast 10ml 30% ammoniacal liquor after 0.5 hour, is warming up to 80 ℃, and slaking is 1 hour under the vigorous stirring, be cooled to room temperature after magnetic separate, be washed to clear liquid and be neutral, the products therefrom vacuum drying.
2. gather the dopamine MODIFIED Fe
3O
4The preparation of nano particle
Get 90mg Fe
3O
4Nano particle joins in the there-necked flask that fills 180ml Tris (pH=8.5) solution, 20min is stirred on ultrasonic limit, limit, then getting the 360mg dopamine joins in the above-mentioned there-necked flask, 4h is stirred on ultrasonic limit, limit, then side magnetic separates, distilled water is washed till clear liquid and is neutral, is made into the 10ml/mg dispersion liquid with distilled water, obtains the Fe of poly-dopamine modification
3O
4Nanoparticle dispersion liquid.
3. the preparation of nm of gold seed
Get 0.25ml HAuCl
44H
2O (2%) aqueous solution joins in the 50ml water, and the sodium citrate solution that stirs the lower 0.5ml 1% of adding behind the 1min adds, and adds 0.5ml NaBH behind the 1min
4The aqueous solution (37.5mg NaBH
4, be settled to 50ml with 1% sodium citrate solution), continue to stir 5min, reaction is put into refrigerator and is preserved after finishing.
4. the Fe of loaded with nano gold seeds
3O
4The preparation of nano particle
Get the Fe of the poly-dopamine modification of 1ml
3O
4Nanoparticle dispersion liquid adds 10ml nm of gold seed solution wherein, places 15min behind the ultrasonic dispersion 4min, and magnetic separates, and washing adds 20ml distilled water and is configured to solution.
5. the preparation of core-shell magnetic/gold nanocomposite particles
Get 0.1ml HAuCl
44H
2O (2%) aqueous solution joins in the particle dispersion of 4 gained, ultrasonic under the room temperature, stirring 20min, magnetic separates, 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, it is colourless that magnetic is separated to clear liquid, vacuum drying.
Above-mentioned example is the better embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other field any do not deviate from change, the modification done under Spirit Essence of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (2)
1. the preparation method of a nuclear shell type magnet golden nanometer particle, it is characterized in that: this preparation method comprises the steps:
(1) Fe
3O
4The preparation of nano particle: will claim 3.90～4.20g FeCl
35H
2O and 2.10～2.35g FeCl
26H
2O is dissolved in 80～120ml water, logical N
2Then deoxygenation drips ammoniacal liquor fast, in 70～90 ℃ of lower logical N
2Stirring reaction 40～60min generates Fe
3O
4The nano particle black precipitate after reaction finishes, is cooled to room temperature, and magnetic separates, and is washed to the stillness of night to be neutral, vacuum drying.
(2) poly-dopamine MODIFIED Fe
3O
4The preparation of nano particle: dopamine is dissolved in the Tris-HCl cushioning liquid of pH=8.5, the concentration of dopamine is controlled to be 1～2mg/ml, gets the Fe that obtains in (1)
3O
4Nano particle 100～200mg is scattered in the above-mentioned dopamine cushioning liquid of 50～100ml, and is ultrasonic under the room temperature, stir 2～4h, and magnetic separates, and distilled water is made into the 10ml/mg dispersion liquid with distilled water after washing and being neutrality to clear liquid, obtains the Fe of poly-dopamine modification
3O
4Nanoparticle dispersion liquid;
(3) preparation of nm of gold seed: get 0.25ml HAuCl
44H
2O (2%) aqueous solution joins in the 50ml water, and the sodium citrate solution that stirs the lower 0.5ml 1% of adding adds, and then adds 0.5ml NaBH
4The aqueous solution (37.5mgNaBH
4, be settled to 50ml with 1% sodium citrate solution), continue to stir 5min, reaction is put into refrigerator and is preserved after finishing.
(4) Fe of loaded with nano gold seeds
3O
4The preparation of nano particle: the Fe that gets resulting poly-dopamine modification among the 1ml (2)
3O
4Nanoparticle dispersion liquid adds the nm of gold seed solution that makes among the 10ml (3) wherein, and ultrasonic dispersion was placed 15 minutes after 2～4 minutes, and magnetic separates, and washing adds 20ml distilled water and is configured to solution;
(5) preparation of core-shell magnetic/gold nanocomposite particles: get 0.1ml HAuCl
44H
2O (2%) aqueous solution joins in the particle dispersion of (4) gained, ultrasonic under the room temperature, stirring 20～30min, magnetic separates, 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, magnetic separates, vacuum drying.
2. according to the preparation method of claim 1 described a kind of core-shell magnetic/gold nanocomposite particles, it is characterized in that: the described core-shell magnetic/gold nanocomposite particles that makes 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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