CN101620910A - Preparation method and application of core-shell magnetic/gold nanocomposite particles - Google Patents
Preparation method and application of core-shell magnetic/gold nanocomposite particles Download PDFInfo
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- CN101620910A CN101620910A CN200810045427A CN200810045427A CN101620910A CN 101620910 A CN101620910 A CN 101620910A CN 200810045427 A CN200810045427 A CN 200810045427A CN 200810045427 A CN200810045427 A CN 200810045427A CN 101620910 A CN101620910 A CN 101620910A
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Abstract
The invention relates to a preparation method and application of core-shell magnetic/gold nanocomposite particles. The preparation method is characterized by preparing magnetic nanoparticles by using a coprecipitation method; transferring the magnetic nanoparticles to an organic solvent through a surfactant; and then reducing a gold precursor with organic amine by using the magnetic particles as seed crystals to form a gold shell layer on the surface of the magnetic particles. After adding a chain transfer agent, the nanoparticles can be transferred from the solvent into aqueous phase. The nanoparticles can be used for marking, separation, enrichment and detection of biological and non-biological, and can also be used in the fields of magnetic resonance contrast agents, targeting drug carriers, photothermal therapy for cancer cells and the like.
Description
Technical field
The present invention relates to a kind of preparation method and application thereof of nuclear shell type magnet/golden nanometer particle, belong to the nano magnetic material technical field.
Background technology
Magnetic nano-particle has characteristics such as magnetic field responsiveness, nanometer size effect, hypotoxicity and biocompatibility, is widely used in various fields.As: in the biomedical sector, can be used for the separation and concentration of magnetic target medicine carrier, magnetic resonance radiography technology, cell or NDA etc.; In the magnetic recording material field, replace traditional micron order magnetic, be used for the high density magnetic recording material; In the catalytic field, make catalyst carrier, not only can improve catalyst activity greatly, and be convenient to the recovery and the recycling of catalyst with it.Reduce magnetic but nanomagnetic particle is easily oxidized, and the surface is difficult for modifying.Coat one deck gold shell on its surface, form the magnetic/golden nanometer particle of nucleocapsid structure, both can overcome the limitation of nanomagnetic particle, can make nano-complex particle have the characteristic of nano Au particle concurrently again, as: excellent optical property, catalytic performance, surface are easy to modify and characteristic such as excellent biological compatibility.There is significant application value 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 detection of protein, cell, NDA etc.
At present, the preparation method of the nucleocapsid magnetic/golden nanometer particle of bibliographical information mainly is, with thermal decomposition process of preparing nano magnetic particle, is crystal seed with the magnetic particle more earlier, under the high temperature, reduces organic golden presoma with reducing agent, makes nucleocapsid magnetic/golden nanometer particle.In addition, the inside and outside oxidation-reduction method of high temperature also is the preparation method who uses always, this method is to prepare the elemental metals magnetic nano-particle with thermal decomposition method earlier, make crystal seed with it again, under hot conditions, with organic golden oxidation of precursor seed particles, golden presoma is reduced and forms golden shell simultaneously, makes nucleocapsid magnetic/golden nanometer particle.These methods mainly contain following shortcoming: (1) reaction temperature height, reaction temperature are usually about 200 ℃; (2) reaction time is long; (3) reactant toxicity height, common used reactant is toxic compounds such as iron pentacarbonyl, ferric acetyl acetonade.How to prepare nucleocapsid magnetic/golden nanometer particle under temperate condition is an important topic in this field.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.This method has overcome thermal decomposition method high temperature, highly toxic shortcoming, but nanometer Fe
3O
4Particle easy oxidized magnetic under the boiling condition reduces, and the nano particle dispersiveness that makes is bad.
Summary of the invention
The purpose of this invention is to provide a kind ofly under temperate condition, prepare the method for nucleocapsid magnetic/gold nano compound particle, this method can obtain the nano-complex particle of fine dispersion in decentralized medium.This nano-complex particle can be in mark, separation, the detection of biology and non-biological material.
For achieving the above object, the present invention takes following measure, a kind of preparation method of nuclear shell type magnet/golden nanometer particle and application thereof, and this method comprises the steps:
(1) adopts coprecipitation to prepare magnetic nano-particle, be warming up to 40-90 ℃ then under the vigorous stirring, drip low quantity of surfactant, obtain stable magnetic nano-particle aqueous dispersions;
(2) use is extracted into magnetic nano-particle in the organic facies with the immiscible organic solvent of water, and this magnetic fluid that takes a morsel adds organic reducing agent, and 15-50 ℃ is stirred 2-35h down;
(3) golden presoma is dissolved in the organic solvent, adds a small amount of organic reducing agent, splash in (2) middle magnetic fluid, under the vigorous stirring, 15-50 ℃ is reacted 10-36h down, with precipitation reagent nano particle is precipitated, and magnetic is dispersed in the organic solvent after separating again;
(4) nuclear shell type magnet/golden nanometer particle changes water over to consisting of phase-transferring agent in the organic solvent with being dispersed in of making in (3), the monitoring that is used for protein, NDA, cell, antibody with separate.
Used surfactant can be saturated or the unrighted acid and its esters of long-chain (8-24 carbochain) among the present invention, preferred unrighted acid and its esters, as: stearic acid, octadecenic acid (oleic acid) or its esters.And the volume fraction of surfactant in reactant mixture is 0.1-20%.
In the inventive method, used organic solvent is various and the immiscible solvent of water in the extraction process, preferred benzene and derivative, alkane, cycloalkane, halogenated hydrocarbons and ether compound, as: benzene,toluene,xylene, n-hexane, normal heptane, cyclohexane, carrene, chloroform etc.And the consumption of extractant be the water-based magnetic fluid volume 1-100 doubly.
In the inventive method, used organic solvent is polarity or non-polar organic solvent in the course of reaction, preferred benzene and derivative, alkane, cycloalkane, halogenated hydrocarbons and ether compound, as: benzene, toluene, carrene, chloroform etc.
Used organic reducing agent is saturated or unsaturated organic amine, the multicomponent alcoholics compound of long-chain (6-24 carbochain) among the present invention, preferred unsaturated organic amine compound, as: cetylamine, hexadecylene amine, octadecylamine, octadecenyl amine (oleyl amine), 1,2-hexadecane glycol etc.And the volume fraction of organic reducing agent in reactant mixture is 0.1-30%.
Used golden presoma can be inorganic gold-containing compound or organic gold-containing compound among the present invention.As: gold chloride, acetate gold etc.When selecting inorganic gold-containing compound for use, the reaction organic solvent is easily selected polarity or weakly polar organic solvent for use, and drips a small amount of organic reducing agent, and inorganic gold-containing compound is dissolved fully.
Used precipitation reagent is a poor solvent various and nano particle that dissolves each other of reaction organic solvent among the present invention, preferred alcohols compounds, ketone compounds, alkane, cycloalkane and halogenated hydrocarbons, as: methyl alcohol, ethanol, propyl alcohol, butanols, benzinum etc.
Used consisting of phase-transferring agent is ligand exchange reaction to take place on the nano-complex particle surface among the present invention, and nano particle can be changed over to the compound of water, preferably contain sulfydryl or amino polyethylene glycol compounds, organic carboxyl acid compounds and organic quaternary ammonium salt compounds.As: an end is the polyethylene glycol of sulfydryl, 11-sulfydryl undecanoic acid, 11-aminoundecanoic acid, bromination trimethyl-(11-sulfydryl)-undecyl ammonium.
The prepared nano-complex particle of the inventive method can be used for biomolecule or cell and non-biological materials such as marker enzyme, polysaccharide, polypeptide, nucleic acid, antigen, antibody, Avidin, streptavidin, also can be used for the aspects such as photo-thermal therapy of magnetic resonance contrast agent, target medicine carrier, cancer cell.
The prepared nano-complex particle of the inventive method can be used for biomolecular reaction system or complex-metal pollutant environmental monitorings such as ligand-receptor, antibody-antigen, DNA-DNA, NDA-oligonucleotides, Avidin-biotin, and the aspects such as enrichment, separation, purifying and detection of the biomolecule in field such as clinical pathogenic microorganisms such as bacterium, virus or food contaminant.
The present invention has following advantage:
One of advantage of the present invention is that the preparation condition of nucleocapsid magnetic/golden nanometer particle is simple, has overcome literature method severe reaction conditions, shortcoming that reaction reagent toxicity is high.
Two of advantage of the present invention is at ambient temperature, reduces golden presoma with the organic amine reducing agent, preparation nucleocapsid magnetic/gold compound nano-particle, and the preparation condition gentleness, 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 particle diameter of making of this method is little, good dispersion, can stable dispersion in decentralized medium.
Four of advantage of the present invention is that nucleocapsid magnetic/gold compound nano-particle that this method makes can change water over to from solvent mutually with consisting of phase-transferring agent, can be used for mark, separation, enrichment and the detection of biology and non-biological material.
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 three 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 4.1g FeCl
35H
2O and 2.35g FeCl
26H
2O adds that 100ml is water-soluble to be separated in flask, drip 10ml30% ammoniacal liquor after 0.5 hour, is warming up to 60 ℃, under the vigorous stirring, slowly drips 0.1ml oleic acid, after dropwising, this temperature slaking 1 hour, makes water-based magnetic fluid.Get this magnetic fluid of 30ml in separatory funnel, add 200ml toluene, shake up standing demix.The upper strata black liquor is the finish magnetic fluid.
2. the preparation of nucleocapsid magnetic/gold nano compound particle:
Get above-mentioned oil base magnetic fluid 0.6ml in two mouthfuls of flasks, add hexadecylene amine 0.3ml, carrene 2ml, room temperature vigorous stirring 3 hours.With the 0.1g gold chloride, 0.1ml hexadecylene amine is dissolved in the 2ml carrene, slowly is added drop-wise in the above-mentioned flask, and 30 ℃ were stirred 15 hours, and promptly got nucleocapsid magnetic/golden nanometer particle.Use the 50ml methanol extraction, magnetic is distributed in the 20ml toluene after separating again.
Embodiment 2
This example is intended to illustrate nucleocapsid magnetic of the present invention/gold nano compound particle can be from the solvent phase transfer to water.
The toluene dispersion liquid 5ml that gets nucleocapsid magnetic/golden nanometer particle adds 11-sulfydryl undecanoic acid 0.05g in flask, add water 5ml, stirred 1 hour, nano particle from the toluene phase transfer to aqueous phase.
Embodiment 3
This example is intended to illustrate nucleocapsid magnetic of the present invention/gold nano compound particle surface can pass through conventional method coupling antibody.
Get the aqueous dispersions 0.35ml of nucleocapsid magnetic/golden nanometer particle, add the Tris-HCl (pH=7.6) of 0.5ml0.05M, act on 10 minutes, magnetic divides the abandonment supernatant.Tris-HCl (PH=7.6) with 0.35ml0.05M is mixed with 0.2mg/ml with antibody stoste, gets 0.15ml then, adds in the aforesaid liquid, reacts 1 hour.With magnetic separator post reaction mixture is carried out magnetic and separate, magnetic/golden nanometer particle of the coated antibody that separation is obtained cleans with the PBS (pH=8.2) of 0.02M.
Claims (10)
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) adopts coprecipitation to prepare magnetic nano-particle, be warming up to 40-90 ℃ then under the vigorous stirring, drip low quantity of surfactant, obtain stable magnetic nano-particle aqueous dispersions;
(2) use is extracted into magnetic nano-particle in the organic facies with the immiscible organic solvent of water, and this magnetic fluid that takes a morsel adds organic reducing agent, and 15-50 ℃ is stirred 2-35h down;
(3) golden presoma is dissolved in the organic solvent, adds a small amount of organic reducing agent, splash in (2) middle magnetic fluid, under the vigorous stirring, 15-50 ℃ is reacted 10-36h down, with precipitation reagent nano particle is precipitated, and magnetic is dispersed in the organic solvent after separating again;
(4) nuclear shell type magnet/golden nanometer particle changes water over to hydrophilic consisting of phase-transferring agent in the organic solvent with being dispersed in of making in (3), the monitoring that is used for protein, NDA, cell, antibody with separate.
2. the preparation method of a kind of nuclear shell type magnet/golden nanometer particle according to claim 1, it is characterized in that: used surfactant can be saturated or the unrighted acid and its esters of long-chain (8-24 carbochain), preferred unrighted acid and its esters, and the volume fraction of surfactant in reactant mixture is 0.1-20%.
3. the preparation method of a kind of nuclear shell type magnet/golden nanometer particle according to claim 1, it is characterized in that: used organic solvent is various and the immiscible solvent of water in the extraction process, preferred benzene and derivative, alkane, cycloalkane, halogenated hydrocarbons and ether compound, and the consumption of extractant be the water-based magnetic fluid volume 1-100 doubly.
4. the preparation method of a kind of nuclear shell type magnet/golden nanometer particle according to claim 1, it is characterized in that: used organic solvent is polarity or non-polar organic solvent in the course of reaction, derivative, alkane, cycloalkane, halogenated hydrocarbons or the ether compound of preferred benzene, benzene.
5. the preparation method of a kind of nuclear shell type magnet/golden nanometer particle according to claim 1, it is characterized in that: used organic reducing agent is saturated or unsaturated organic amine, the multicomponent alcoholics compound of long-chain (6-24 carbochain), preferred unsaturated organic amine compound, and the volume fraction of organic reducing agent in reactant mixture is 0.1-30%.
6. the preparation method of a kind of nuclear shell type magnet/golden nanometer particle according to claim 1, it is characterized in that: used golden presoma is inorganic gold-containing compound or organic gold-containing compound.
7. the preparation method of a kind of nuclear shell type magnet/golden nanometer particle according to claim 1, it is characterized in that: used precipitation reagent is a poor solvent various and nano particle that dissolves each other of reaction organic solvent, preferred alcohols compounds, ketone compounds, alkane, cycloalkane or halogenated hydrocarbons.
8. the preparation method of a kind of nuclear shell type magnet/golden nanometer particle according to claim 1, it is characterized in that: ligand exchange reaction for taking place on the nano-complex particle surface in used consisting of phase-transferring agent, and nano particle can be changed over to the compound of water, preferably contain sulfydryl or amino polyethylene glycol compounds, organic carboxyl acid compounds or organic quaternary ammonium salt compounds.
9. application according to a kind of nuclear shell type magnet/golden nanometer particle of the described method preparation of claim 1, it is characterized in that: this nano-complex particle can be used for marker enzyme, polysaccharide, polypeptide, nucleic acid, antigen, antibody, Avidin, streptavidin biomolecule or cell and non-biological material, also can be used for the photo-thermal therapy aspect of magnetic resonance contrast agent, target medicine carrier, cancer cell.
10. application according to a kind of nuclear shell type magnet/golden nanometer particle of the described method preparation of claim 1, it is characterized in that: this nano-complex particle can be used for ligand-receptor, antibody-antigen, DNA-DNA, NDA-oligonucleotides, Avidin-biotin biomolecular reaction system or complex-metal pollutant environmental monitoring, and enrichment, separation, purifying and the context of detection of the biomolecule in bacterium, viral clinical pathogenic microorganisms or food contaminant field.
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| CN101776691A (en) * | 2010-02-09 | 2010-07-14 | 北京大学 | Method for immunoaffinity solid-phase extraction based on gold-coated ferroferric oxide nano-particles |
| CN102172411A (en) * | 2011-03-04 | 2011-09-07 | 中国人民解放军第二军医大学 | Nano complex particles with targeted MR (magnetic resonance) development and photothermal therapy performance and preparation method thereof |
| CN102463352A (en) * | 2010-11-11 | 2012-05-23 | 西北师范大学 | Method for synthesizing bimetallic Pd-Au core-shell hexahedron |
| CN102847493A (en) * | 2012-09-17 | 2013-01-02 | 北京科技大学 | Method for water-phase dispersion of metal magnetic nano particles |
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| CN101776691A (en) * | 2010-02-09 | 2010-07-14 | 北京大学 | Method for immunoaffinity solid-phase extraction based on gold-coated ferroferric oxide nano-particles |
| CN102463352A (en) * | 2010-11-11 | 2012-05-23 | 西北师范大学 | Method for synthesizing bimetallic Pd-Au core-shell hexahedron |
| CN102463352B (en) * | 2010-11-11 | 2013-08-21 | 西北师范大学 | Method for synthesizing bimetallic Pd-Au core-shell hexahedron |
| CN102172411B (en) * | 2011-03-04 | 2013-08-21 | 中国人民解放军第二军医大学 | Nano complex particles with targeted MR (magnetic resonance) development and photothermal therapy performance and preparation method thereof |
| CN102172411A (en) * | 2011-03-04 | 2011-09-07 | 中国人民解放军第二军医大学 | Nano complex particles with targeted MR (magnetic resonance) development and photothermal therapy performance and preparation method thereof |
| CN102847493A (en) * | 2012-09-17 | 2013-01-02 | 北京科技大学 | Method for water-phase dispersion of metal magnetic nano particles |
| CN103203451A (en) * | 2013-01-31 | 2013-07-17 | 河南大学 | Core-shell type La(1-x)SrxMnO3/Au nanometer composite particle and preparation method thereof |
| CN103203451B (en) * | 2013-01-31 | 2015-04-29 | 河南大学 | Core-shell type La(1-x)SrxMnO3/Au nanometer composite particle and preparation method thereof |
| CN105188765A (en) * | 2013-03-04 | 2015-12-23 | Mida科技有限公司 | Nanoparticle peptide compositions |
| CN103599794A (en) * | 2013-11-15 | 2014-02-26 | 深圳先进技术研究院 | Fe3O4-Au magnetic nano composite material, and preparation method and application thereof |
| CN103599794B (en) * | 2013-11-15 | 2016-02-24 | 深圳先进技术研究院 | Fe 3o 4-Au magnetic nanometer composite material and preparation method thereof and application |
| CN103862036A (en) * | 2014-01-24 | 2014-06-18 | 中国科学院长春光学精密机械与物理研究所 | Method for preparing silicon dioxide coated noble metal nanocrystalline |
| CN104028181A (en) * | 2014-04-24 | 2014-09-10 | 温州大学 | Precious metal/paramagnetic metal composite nanoparticle with core-shell structure and application thereof |
| CN104028181B (en) * | 2014-04-24 | 2016-04-06 | 温州大学 | There is noble metal/paramagnetic metal composite nanoparticle and the application thereof of nucleocapsid structure |
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| CN104258421B (en) * | 2014-09-12 | 2016-09-21 | 温州大学 | A kind of noble metal/paramagnetic metal composite nanoparticle and application thereof |
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| CN107030295A (en) * | 2017-03-24 | 2017-08-11 | 同济大学 | A kind of preparation method of magnetic/gold nanocomposite particle |
| CN107677817A (en) * | 2017-08-29 | 2018-02-09 | 山东师范大学 | A kind of salmonella typhimurium quick determination method based on immune magnetic Nano material photo-thermal effect |
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