CN104575908A - Dopamine modified magnetic nano-particle, method for preparing same and application of dopamine modified magnetic nano-particle - Google Patents
Dopamine modified magnetic nano-particle, method for preparing same and application of dopamine modified magnetic nano-particle Download PDFInfo
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- CN104575908A CN104575908A CN201510049780.3A CN201510049780A CN104575908A CN 104575908 A CN104575908 A CN 104575908A CN 201510049780 A CN201510049780 A CN 201510049780A CN 104575908 A CN104575908 A CN 104575908A
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Abstract
The invention discloses a dopamine modified magnetic nano-particle, a method for preparing the same and application of the dopamine modified magnetic nano-particle. Poly-dopamine is attached to the surface of a magnetic nano-particle to form the dopamine modified magnetic nano-particle. The method includes preparing the magnetic nano-particle by the aid of a chemical co-precipitation process; preparing a modified particle by the aid of a process for oxidizing, crosslinking and attaching dopamine to the surface of the magnetic nano-particle. The dopamine modified magnetic nano-particle, the method and the application have the advantages that technologies are simple, the prepared magnetic nano-particle is high in saturation magnetization intensity, small in particle size, good in stability and applicable to protein, cell and gene separation magnetic carriers and can be hopefully used in the biomedical field of target control release, magnetic resonance imaging, high-temperature thermal therapy, biosensors and the like.
Description
Technical field
The present invention relates to a kind of magnetic nano-particle and preparation method thereof, is a kind of dopamine modified magnetic nano particle and preparation method thereof in particular.
Background technology
Magnetic nano-particle is the magnetic material that a class has special character, when particle size lower than a critical value (usually at about 10-20nm), temperature higher than obstruct temperature time, show superparamagnetic behavior, namely particle performance such as a huge paramagnetic atoms has very fast response to externally-applied magnetic field, and after removing magnetic field, particle does not have remanent magnetism and magnetic coercive force.In recent years, due to magnetic property and the performance of its uniqueness, the synthesis of magnetic nano-particle and application study cause the concern of people day by day.
However, nano level particle is easily formed to assemble and reduces small-size effect and bring high surface energy.In addition, exposed metallic chemism is very high, and magnetic and the dispersiveness of oxidized rear system can reduce.Thus, surface modification carried out to it particularly important to strengthen its stability.Even more noteworthy, protective layer not only stable for nano particle under many circumstances, and can also be used for carrying out further functionalization with other particle or various part.
The shortcoming of current this kind of modified magnetic nano particle is: 1, particle is bigger than normal and uneven.2, disperse stability in aqueous inadequate, easily assemble sedimentation.3, magnetic targeted is not strong, and magnetic needs to improve further.
Summary of the invention
The object of the present invention is to provide a kind of dopamine modified magnetic nano particle, its good stability, particle are little, magnetic is high, be applicable to the magnetic carrier of protein, cell, Gene Isolation, and be expected to for biomedical sectors such as target Co ntrolled release, magnetic resonance imaging, Microwave biology sensors.
For the deficiency that existing modified magnetic nano particle preparation method exists, another object of the present invention is to provide a kind of preparation method of dopamine modified magnetic nano particle that is simple, that can obtain having special accumulation shape.
To achieve these goals, technical scheme of the present invention is: a kind of dopamine modified magnetic nano particle, the surface being attached to magnetic nano-particle by poly-dopamine is formed.
Described magnetic nano-particle is Fe
3o
4nano particle.
A preparation method for dopamine modified magnetic nano particle, is characterized in that: adopt chemical coprecipitation to prepare magnetic nano-particle, then adopts the oxidation cross-linked method being attached to magnetic nano particle sub-surface of dopamine to prepare modified particle.
The present invention has the following advantages compared with the prior art: technique is simple, prepared magnetic nano-particle disperses good stability in aqueous, saturation magnetization reaches as high as 53.01emu/g, the effective grain size of disperseing in water is minimum is 127.8nm, polydispersity coefficient is 0.127, and the particle diameter of particle is minimum is 7 ~ 15nm.Certain synthesis technique can synthesize the dopamine modified magnetic nano particle presenting peculiar accumulation shape, and the particle being embodied in about more than 20 tens nanometers assembles the aggregate forming about 200nm, as shown in Figure 4.The assay method of above data is: the saturation magnetization of magnetic nano-particle adopts magnetic property measuring system to measure, and effective grain size adopts dynamic light scattering to detect, and particle diameter and the pattern of particle are characterized by atomic force microscope.
The present invention is applicable to the magnetic carrier of protein, cell, Gene Isolation, and is expected to for biomedical sectors such as target Co ntrolled release, magnetic resonance imaging, Microwave biology sensors.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of dopamine oxidative crosslinking process;
Fig. 2 is the infrared spectrogram of the dopamine modified magnetic nano particle that the present invention obtains;
Fig. 3 is the magnetic hysteresis loop figure of the modified magnetic nano particle that the present invention obtains;
Fig. 4 is the atomic force microscope figure of the modified magnetic nano particle that the present invention obtains.
Embodiment
The present invention is a kind of dopamine modified magnetic nano particle, and the surface being attached to magnetic nano-particle by poly-dopamine is formed.Magnetic nano-particle is preferably Fe
3o
4nano particle.Dopamine (DOPA, 3,4-dihydroxy-L-phenylalanine) is modifier, and its structure is as follows:
Hydroxyl in dopamine structure formula and Fe
3o
4the hydroxyl of nanoparticle surface can form strong hydrogen bonding interaction, and it is exactly hydrogen bonding interaction that the attachment between them is combined except physisorption.
The preparation method of dopamine modified magnetic nano particle first adopts chemical coprecipitation to prepare magnetic nano-particle, then adopts the oxidation cross-linked method being attached to magnetic nano particle sub-surface of dopamine to prepare modified particle.
Preferably, specifically comprise the following steps:
(1) magnetic nano-particle is Fe
3o
4the synthesis of nano particle
At N
2under atmosphere, mechanical agitation, by Fe
2+, Fe
3+mixed salt solution and concentrated ammonia liquor react, wherein Fe
2+salt, Fe
3+the mol ratio of salt and ammoniacal liquor is 1:1.8 ~ 2:8 ~ 16, and mechanical agitation speed is 300 ~ 500rad/min, and reaction temperature is 50 ~ 80 DEG C, and the reaction time is 10 ~ 60min.Be cooled to room temperature.
(2) Fe
3o
4the washing of nano particle and the dispersion in water
With the Fe that distilled water cyclic washing is obtained by reacting
3o
4nano particle, and be separated with magnetic support, the excess charge of removing particle surface absorption; Finally product is scattered in water, stirs, with ultrasonic wave dispersion, obtain stable Fe
3o
4water-based magnetic fluid.Preferably, with the Fe that distilled water cyclic washing is obtained by reacting
3o
4nano particle, until supernatant liquor conductivity is less than 50 μ s/cm.Preferably, the Fe will obtained
3o
4collect supernatant liquid after the effect of water-based magnetic fluid magnetic support, after 1500 ~ 2500rad/min centrifugal treating, collect supernatant liquor, except the bulky grain generated in dereaction, then carry out the reaction of step (3).Preferably, the ultrasonic wave dispersion treatment time is 15 ~ 25min.
(3) Fe
3o
4the surface modification of magnetic nano-particle and the dispersion in water
By Fe
3o
4nano particle, modifier DOPA are according to Fe
3o
4: the mol ratio of DOPA is that 0.5 ~ 1:1 mixed dissolution is in 8 ~ 12mmol/L Tris-HCl cushioning liquid, react under 250 ~ 350rad/min mechanical agitation, then repeatedly clean with distilled water and be separated with magnetic support, until supernatant conductivity is 40 ~ 60 μ s/cm, distilled water is added in the magnetic-particle stayed, dispersed with stirring, sonic oscillation.Preferably, the pH of Tris-HCl cushioning liquid is 8.0 ~ 9.0.Preferably, reaction is reacted in normal temperature air atmosphere, and the reaction time is 15 ~ 30h.
Below in conjunction with drawings and Examples, the present invention is further elaborated, but the present invention is not limited to this specific examples.
Embodiment 1
Configuration concentration is 0.25mol/L FeCl
24H
2o and 0.5mol/L FeCl
36H
2the molysite mixed solution of O is in 200ml volumetric flask.Get 50ml molysite mixed solution and 250ml distilled water in three mouthfuls of round-bottomed flasks, then put it in 60 DEG C of thermostat water baths, under argon shield, 400rad/min mechanical agitation, add 20ml NH
3h
2o, sustained response 1h, generate the Fe of a large amount of black
3o
4magnetic particle, is cooled to room temperature.Obtain product with magnetic support effect, and wash product by massive laundering, until supernatant liquor becomes neutrality, conductivity is less than 50 μ s/cm.Product is scattered in 100ml water, stirs, disperse 20min with ultrasonic wave, then collect supernatant liquid after magnetic support effect 5min, collect supernatant liquid after the centrifugal 1h of 2000rad/min and be stable Fe
3o
4water-based magnetic fluid.By the Fe collected
3o
4water-based magnetic fluid sonic oscillation 20min.Get the Fe of the ultrasonic mistake of 2.5mL
3o
4water-based magnetic fluid, 0.1g DOPA and 50mL 10mmol/L Tris-HCl cushioning liquid, in 100mL there-necked flask, in 300rad/min mechanical agitation, react 15h under normal temperature air atmosphere.Repeatedly with distilled water cleaning, and be separated with magnetic support, until supernatant conductivity is 50 μ about s/cm, in the magnetic-particle stayed, add distilled water 50mL, dispersed with stirring, sonic oscillation 20min, obtain stable dopamine modified magnetic nanoparticle suspension.The oxidation cross-linked process of dopamine is as Fig. 1.The infrared spectrogram of dopamine modified magnetic nano particle, as Fig. 2, infrared spectrum has the characteristic peak of tri-iron tetroxide and poly-dopamine.The saturation magnetization of obtained dopamine modified magnetic nano particle reaches as high as 53.01emu/g, and its B-H loop is as Fig. 3.Obtained dopamine modified magnetic nano particle presents peculiar accumulation shape, assembles the aggregate forming about 200nm, as Fig. 4 by the particle of about more than 20 tens nanometers.
Embodiment 2
Fe
3o
4the synthesis of water-based magnetic fluid is with reference to embodiment 1.Get the Fe of the ultrasonic mistake of 5mL
3o
4water-based magnetic fluid, 0.1g DOPA and 50mL 10mmol/L Tris-HCl cushioning liquid, in 100mL there-necked flask, in 300rad/min mechanical agitation, react 15h under normal temperature air atmosphere.All the other steps are with embodiment 1.The saturation magnetization of the dopamine modified magnetic nano particle of synthesis reaches as high as 40.53emu/g.
Embodiment 3
Fe
3o
4the synthesis of water-based magnetic fluid is with reference to embodiment 1.Get the Fe of the ultrasonic mistake of 2.5mL
3o
4water-based magnetic fluid, 0.1g DOPA and 50mL 10mmol/L Tris-HCl cushioning liquid, in 100mL there-necked flask, in 300rad/min mechanical agitation, react 27h under normal temperature air atmosphere.All the other steps are with embodiment 1.The saturation magnetization of the dopamine modified magnetic nano particle of synthesis reaches as high as 38.83emu/g.
Embodiment 4
Fe
3o
4the synthesis of water-based magnetic fluid is with reference to embodiment 1.Get the Fe of the ultrasonic mistake of 5mL
3o
4water-based magnetic fluid, 0.1g DOPA and 50mL 10mmol/L Tris-HCl cushioning liquid, in 100mL there-necked flask, in 300rad/min mechanical agitation, react 27h under normal temperature air atmosphere.All the other steps are with embodiment 1.The saturation magnetization of the dopamine modified magnetic nano particle of synthesis reaches as high as 46.35emu/g.
Claims (10)
1. a dopamine modified magnetic nano particle, the surface being attached to magnetic nano-particle by poly-dopamine is formed.
2. dopamine modified magnetic nano particle according to claim 1, is characterized in that: described magnetic nano-particle is Fe
3o
4nano particle.
3. a preparation method for dopamine modified magnetic nano particle, is characterized in that: adopt chemical coprecipitation to prepare magnetic nano-particle, then adopts the oxidation cross-linked method being attached to magnetic nano particle sub-surface of dopamine to prepare modified particle.
4. the preparation method of dopamine modified magnetic nano particle according to claim 3, is characterized in that comprising the following steps:
(1) magnetic nano-particle is Fe
3o
4the synthesis of nano particle
At N
2under atmosphere, mechanical agitation, by Fe
2+, Fe
3+mixed salt solution and concentrated ammonia liquor react, wherein Fe
2+salt, Fe
3+the mol ratio of salt and ammoniacal liquor is 1:1.8 ~ 2:8 ~ 16, and mechanical agitation speed is 300 ~ 500rad/min, and reaction temperature is 50 ~ 80 DEG C, and the reaction time is 10 ~ 60min.Be cooled to room temperature;
(2) Fe
3o
4the washing of nano particle and the dispersion in water
With the Fe that distilled water cyclic washing is obtained by reacting
3o
4nano particle, and be separated with magnetic support, the excess charge of removing particle surface absorption; Finally product is scattered in water, stirs, with ultrasonic wave dispersion, obtain stable Fe
3o
4water-based magnetic fluid;
(3) Fe
3o
4the surface modification of magnetic nano-particle and the dispersion in water
By Fe
3o
4nano particle, modifier DOPA are according to Fe
3o
4: the mol ratio of DOPA is that 0.5 ~ 1:1 mixed dissolution is in 8 ~ 12mmol/L Tris-HCl cushioning liquid, react under 250 ~ 350rad/min mechanical agitation, then repeatedly clean with distilled water and be separated with magnetic support, until supernatant conductivity is less than 50 μ s/cm, distilled water is added in the magnetic-particle stayed, dispersed with stirring, sonic oscillation.
5. the preparation method of dopamine modified magnetic nano particle according to claim 4, is characterized in that: the Fe be obtained by reacting with distilled water cyclic washing in described step (2)
3o
4nano particle, until supernatant liquor conductivity is less than 50 μ s/cm.
6. the preparation method of dopamine modified magnetic nano particle according to claim 4, is characterized in that: in described step (2), by the stable Fe obtained
3o
4collect supernatant liquid after the effect of water-based magnetic fluid magnetic support, after 1500 ~ 2500rad/min centrifugal treating, collect supernatant liquor, except the bulky grain generated in dereaction, then carry out the reaction of step (3).
7. the preparation method of dopamine modified magnetic nano particle according to claim 4, is characterized in that: in described step (2), the ultrasonic wave dispersion treatment time is 15 ~ 25min.
8. the preparation method of dopamine modified magnetic nano particle according to claim 4, is characterized in that: in described step (3), the pH of Tris-HCl cushioning liquid is 8.0 ~ 9.0.
9. the preparation method of dopamine modified magnetic nano particle as claimed in claim 4, is characterized in that: described step (3) is reacted in normal temperature air atmosphere, and the reaction time is 15 ~ 30h.
10. dopamine modified magnetic nano particle described in claim 1 or 2 is applied to the preparation of magnetic carrier of protein, cell, Gene Isolation.
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| CN105921114A (en) * | 2016-04-26 | 2016-09-07 | 盐城工学院 | Paraquat magnetic adsorbent and preparation method thereof |
| CN107930592A (en) * | 2017-12-04 | 2018-04-20 | 郑州大学 | A kind of MOF magnetic graphenes hybrid material and its application in terms of chiral resolution and vitro cytotoxicity |
| CN109078761A (en) * | 2018-09-27 | 2018-12-25 | 江西理工大学 | A method of utilizing the difficult nickel sulfide ore flotation of magnetic hydrophobic particle strengthening |
| CN109091674A (en) * | 2018-09-14 | 2018-12-28 | 黄冈师范学院 | A kind of multi-functional drug carriers and the preparation method and application thereof |
| CN111383812A (en) * | 2018-12-27 | 2020-07-07 | 中国科学院理化技术研究所 | Novel liquid metal magnetofluid and preparation method thereof |
| CN112868668A (en) * | 2021-03-19 | 2021-06-01 | 常州英诺升康生物医药科技有限公司 | Fe3O4-DA-AMP nano composite antibacterial material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105921114A (en) * | 2016-04-26 | 2016-09-07 | 盐城工学院 | Paraquat magnetic adsorbent and preparation method thereof |
| CN105921114B (en) * | 2016-04-26 | 2019-04-23 | 盐城工学院 | A kind of paraquat magnetic adsorbent and preparation method thereof |
| CN107930592A (en) * | 2017-12-04 | 2018-04-20 | 郑州大学 | A kind of MOF magnetic graphenes hybrid material and its application in terms of chiral resolution and vitro cytotoxicity |
| CN107930592B (en) * | 2017-12-04 | 2020-11-06 | 郑州大学 | MOF-magnetic graphene hybrid material and application thereof in chiral resolution and in vitro cytotoxicity |
| CN109091674A (en) * | 2018-09-14 | 2018-12-28 | 黄冈师范学院 | A kind of multi-functional drug carriers and the preparation method and application thereof |
| CN109091674B (en) * | 2018-09-14 | 2021-05-25 | 黄冈师范学院 | Multifunctional drug carrier and preparation method and application thereof |
| CN109078761A (en) * | 2018-09-27 | 2018-12-25 | 江西理工大学 | A method of utilizing the difficult nickel sulfide ore flotation of magnetic hydrophobic particle strengthening |
| CN109078761B (en) * | 2018-09-27 | 2020-11-27 | 江西理工大学 | Method for reinforcing flotation of refractory nickel sulfide ore by using magnetic hydrophobic particles |
| CN111383812A (en) * | 2018-12-27 | 2020-07-07 | 中国科学院理化技术研究所 | Novel liquid metal magnetofluid and preparation method thereof |
| CN111383812B (en) * | 2018-12-27 | 2021-10-29 | 中国科学院理化技术研究所 | Novel liquid metal magnetofluid and preparation method thereof |
| CN112868668A (en) * | 2021-03-19 | 2021-06-01 | 常州英诺升康生物医药科技有限公司 | Fe3O4-DA-AMP nano composite antibacterial material and preparation method and application thereof |
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Application publication date: 20150429 |