CN103272267A - Preparation method of silk fibroin and Fe3O4 composite material - Google Patents
Preparation method of silk fibroin and Fe3O4 composite material Download PDFInfo
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- CN103272267A CN103272267A CN2013102285716A CN201310228571A CN103272267A CN 103272267 A CN103272267 A CN 103272267A CN 2013102285716 A CN2013102285716 A CN 2013102285716A CN 201310228571 A CN201310228571 A CN 201310228571A CN 103272267 A CN103272267 A CN 103272267A
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- fibroin albumen
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Abstract
The invention relates to a preparation method of a silk fibroin and Fe3O4 composite material, and concretely provides a preparation method of a silk fibroin and Fe3O4 composite functional material. The method has a simple technology and is convenient to process. The method concretely comprises the following steps: dissolving regenerated silk fibroins in a certain amount of an organic solvent or aqueous solution to realize a certain concentration of a solution; uniformly mixing the solution comprising the silk fibroins and the organic solvent or aqueous solution, adding a certain amount of nano-Fe3O4 powder, continuously stirring for uniform mixing to prepare a mixed solution comprising the silk fibroins and Fe3O4 particles; and using a certain amount of the mixed solution to prepare films or scaffolds or to prepare nanofibers or microspheres through an electrostatic spinning technology. The method has the advantages of low energy consumption, high biological safety, low price, simple and convenient operation, no pollution to the environment, and the like in the whole treatment process. Silk fibroin and Fe3O4 composite nanofibers prepared through the method have particulate protrusions which increase the body surface area ratio, and have a super-hydrophobic structure, and the prepared microspheres have a target drug carrier function under an external magnetic field.
Description
Technical field
The present invention relates to a kind of fibroin and nanometer Fe
3O
4The preparation method of composite belongs to the processing method of fibroin albumen.
Background technology
Silkworm albumen, tussah silk fibroin are fibrin, because of its special mechanical properties and excellent biological compatibility, degradability and stability, and essence is the construction features of protein, is widely used in fields such as medicine, biomaterial, is a kind of desirable bone renovating bracket material.And high-intensity mechanical property is one of essential condition of bone renovating bracket material.
Nanometer Fe
3O
4Dusty material shows as single domain structure, granule has very high coercivity, superparamagnetism, show as no remanent magnetism and coercivity on the hysteresis curve, these features make it have excellent magnetism energy, higher surface activity, significant magnetosensitive, the quick characteristic of air humidity and higher electric conductivity etc.And advantages such as preparation is simple relatively, biocompatibility is better make it become the normal a kind of important magnetic material that adopts of biomedical sector in addition.There are some researches show, with nanometer Fe
3O
4Granule is applied to tumor magnetic when crossing heating therapy, nanometer Fe
3O
4Granule to cancerous cell particularly the effects such as mechanical shock, diffusion of cell membrane play a part very important to the effect for the treatment of.In addition, magnetic Nano Fe
3O
4The gene transfection technology of granule mediation is that magnetic transfection (magnetofection) is applied to gene therapy research, these magnetic nanoparticles are made up of the polymer of magnetic oxide and biologically active usually, iron oxide particles is dispersed in the polymeric matrix, perhaps be aggregated the shell parcel that thing constitutes, final formation has magnetic and can stably be present in composite nanometer particle in the aqueous phase solution.
When regenerated silk solution and nanometer Fe
3O
4When powder mixes is even, have good super paramagnetic magnetic response and mechanical property by the homogeneous film of introducing the magnetic nano-particle preparation, its saturation magnetization and maximum stress strengthen with magnetic particle content; Add nanometer Fe
3O
4Timbering material in mineralization process, have certain advantage; It is a kind of super-drainage structure that the nanofiber of electrostatic spinning technique preparation has granular projection, and the microsphere of preparation has the target medicine carrier function.
Summary of the invention
The improvement that the present invention has done at the deficiencies in the prior art part just provides a kind of technology simple, and processing is convenient and fibroin albumen and nanometer Fe can be provided
3O
4The preparation method of compound multifunctional material.
To achieve these goals, technical scheme provided by the invention has 2 kinds, and is specific as follows:
The present invention is a kind of fibroin albumen and nanometer Fe
3O
4The granule blend prepares the method for novel biomaterial, and concrete preparation process is as follows:
(1), regenerated silk fibroin is dissolved in certain amount of organic solvent or the aqueous solution, be made into finite concentration;
(2), certain amount of nano Fe will be added behind fibroin albumen and organic solvent or the aqueous solution solution mix homogeneously
3O
4Powder, constantly stirring makes its mix homogeneously again, can make fibroin albumen and nanometer Fe
3O
4The mixed solution of granule;
(3), get a certain amount of mixed solution film processed, support or prepare nanofiber, microsphere by electrostatic spinning technique.
As further improvement, concrete preparation process of the present invention is, regenerated silk is dissolved in certain amount of organic solvent or the aqueous solution, is made into finite concentration.Treat to add certain amount of nano Fe again after regenerated silk dissolves fully
3O
4Granule constantly stirs and makes its mix homogeneously.Get a certain amount of mixed solution film processed or support.
As further improvement, concrete preparation process of the present invention is, regenerated silk is dissolved in certain amount of organic solvent or the aqueous solution, is made into finite concentration.Treat to add certain amount of nano Fe again after regenerated silk dissolves fully
3O
4, constantly stir and make its mix homogeneously.Get a certain amount of mixed solution and prepare nanofiber or microsphere by electrostatic spinning technique.
As further improvement, fibroin albumen of the present invention is: regeneration silk fibroin protein, regeneration tussah silk fibroin.
As further improvement, organic solvent of the present invention has: hexafluoroisopropanol, Hexafluoro acetone, formic acid, trifluoroacetic acid etc.
As further improvement, fibroin albumen of the present invention and nanometer Fe
3O
4The thin film that composite is made or support have function solenoid in the balanced body, and mineralising in the body is had certain advantage.
As further improvement, fibroin albumen of the present invention and nanometer Fe
3O
4Composite has super-drainage structure by the made nanofiber of electrostatic spinning technique, and microcapsule has the target medicine carrier function.
Compared with prior art, the present invention has following outstanding feature:
(1) it is low that the present invention has power consumption in the entire process process, and the biological safety height is cheap, simple to operation, advantages such as environmentally safe.
(2) biological fibroin and the nanometer Fe that makes by this invention
3O
4Composite membrane and timbering material have function solenoid in the good body.Because nanometer Fe
3O
4Particle has the electromagnetic field of certain magnetic in can balanced body, and produces heat because the generation energy loss is reset in the magnetization of low conduction magnetic domain under the effect that adds alternating magnetic field.This is general to use jointly with other cancer treatment methods, is a kind of compound tumor therapy, and its advantage is to add the growth that heat energy limits cancerous cell.And the biomineralization process had certain influence.
(3) biological fibroin and the nanometer Fe that makes by this invention
3O
4Composite nano fiber has granular projection, has increased the body surface area ratio, and is a kind of super-drainage structure, and the microsphere of preparation has the target medicine carrier function adding under the action of a magnetic field.
The specific embodiment
The present invention mainly implements by the following two kinds of programs:
(1) regenerated silk is dissolved in certain amount of organic solvent or the aqueous solution, is made into finite concentration.Treat to add certain amount of nano Fe again after regenerated silk dissolves fully
3O
4, constantly stir and make its mix homogeneously.Get a certain amount of mixed solution film processed or support.
(2) regenerated silk is dissolved in certain amount of organic solvent or the aqueous solution, is made into finite concentration.Treat to add certain amount of nano Fe again after regenerated silk dissolves fully
3O
4, constantly stir and make its mix homogeneously.Get a certain amount of mixed solution and prepare nanofiber or microsphere by electrostatic spinning technique.
Below by specific embodiment technical scheme of the present invention is described in further detail, following examples are explanation of the invention and the present invention is not limited to following examples.
Embodiment 1
Take by weighing regeneration silk fibroin protein 1g, place flat vial, add a certain amount of hexafluoroisopropanol solution, being made into concentration is 7.5% solution, treats that fibroin dissolves the nanometer Fe that the back adds 50mg fully
3O
4Powder constantly stirs.After treating its mix homogeneously, taking-up 2ml is applied on the diameter 10cm plastic plate and dries naturally; Or make the timbering material of certain pattern.By Mechanics Performance Testing, regenerated silk and nanometer Fe
3O
4The composite membrane of powder, timbering material are more eager to excel in whatever one does than single regenerated silk material mechanical performance.
Embodiment 2
Take by weighing regeneration silk fibroin protein 1g, place flat vial, add a certain amount of formic acid solution, being made into concentration is 7.5% solution, treats that fibroin dissolves the nanometer Fe that the back adds 50mg fully
3O
4Powder constantly stirs.After treating its mix homogeneously, mixed solution as for carrying out the electrospinning silk in the electrostatic spinning device, is obtained to have catenate nanofiber, this structure can increase the surface, and has ultra-hydrophobicity.
Embodiment 3
Take by weighing regeneration silk fibroin protein 1g, place flat vial, add a certain amount of formic acid solution, being made into concentration is 3% solution, treats that fibroin dissolves the nanometer Fe that the back adds 50mg fully
3O
4Powder constantly stirs.After treating its mix homogeneously, mixed solution as for carrying out the electrospinning silk in the electrostatic spinning device, is obtained uniform microsphere, this fibroin parcel nanometer Fe
3O
4Microsphere can be used as target medicine carrier adding under the action of a magnetic field.
At last, it is also to be noted that what more than enumerate only is several specific embodiment of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (7)
1. a fibroin albumen and nanometer Fe
3O
4The preparation method of compound multifunctional material is characterized in that, concrete preparation process is as follows:
(1), regenerated silk fibroin is dissolved in certain amount of organic solvent or the aqueous solution, be made into finite concentration;
(2), with fibroin albumen and organic solvent or the even back adding of aqueous solution certain amount of nano Fe
3O
4Powder, constantly stirring makes its mix homogeneously again, can make fibroin albumen and nanometer Fe
3O
4The mixed solution of powder;
(3), get a certain amount of mixed solution film processed, support or prepare nanofiber, microsphere by electrostatic spinning technique.
2. fibroin albumen according to claim 1 and nanometer Fe
3O
4The preparation method of compound multifunctional material is characterized in that, specifically preparation process is, regenerated silk is dissolved in certain amount of organic solvent or the aqueous solution, is made into finite concentration, treats to add certain amount of nano Fe again after regenerated silk dissolves fully
3O
4Powder constantly stirs and makes its mix homogeneously, gets a certain amount of mixed solution film processed or support.
3. fibroin albumen according to claim 1 and nanometer Fe
3O
4The preparation method of compound multifunctional material is characterized in that, specifically preparation process is, regenerated silk is dissolved in certain amount of organic solvent or the aqueous solution, is made into finite concentration, treats to add certain amount of nano Fe again after regenerated silk dissolves fully
3O
4Powder constantly stirs and makes its mix homogeneously, gets a certain amount of mixed solution and prepares nanofiber or microsphere by electrostatic spinning technique.
4. according to claim 1 or 2 or 3 described fibroin albumen and nanometer Fe
3O
4The preparation method of compound multifunctional material is characterized in that, described fibroin albumen is: regeneration silk fibroin protein or regeneration tussah silk fibroin.
5. according to claim 1 or 2 or 3 described fibroin albumen and nanometer Fe
3O
4The preparation method of compound multifunctional material is characterized in that, described organic solvent is: hexafluoroisopropanol or Hexafluoro acetone or formic acid or trifluoroacetic acid.
6. fibroin albumen according to claim 1 and 2 and nanometer Fe
3O
4The preparation method of compound multifunctional material is characterized in that, made thin film or support have function solenoid in the balanced body, and mineralising in the body is had certain advantage.
7. according to claim 1 or 3 described fibroin albumen and nanometer Fe
3O
4The preparation method of compound multifunctional material is characterized in that, made nanofiber has super-drainage structure, and microcapsule has the target medicine carrier function.
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103638554A (en) * | 2013-11-13 | 2014-03-19 | 浙江大学 | Preparation method of composite material of silk fibroin and marine mussel adhesion protein |
| CN103721295A (en) * | 2013-12-19 | 2014-04-16 | 浙江大学 | Method for increasing biocompatibility and mechanical property of fibroin biomaterials |
| CN105002658A (en) * | 2015-08-19 | 2015-10-28 | 哈尔滨工业大学 | Preparation method and driving method of remotely controllable multiple shape memory polymer composite fibrous membrane |
| CN107552095A (en) * | 2017-09-17 | 2018-01-09 | 钱景 | The silk three-dimensional porous material and preparation method of carried titanium dioxide Nano Silver |
| CN108976820A (en) * | 2018-05-11 | 2018-12-11 | 四川大学 | A kind of Ferroferric oxide/polypyrrole composite material and preparation method thereof |
| CN108976450A (en) * | 2018-04-23 | 2018-12-11 | 安徽工程大学 | Based on wax, growth prepares the method for super-hydrophobic fibroin protein film, a kind of super-hydrophobic fibroin protein film certainly |
| CN110448719A (en) * | 2019-06-28 | 2019-11-15 | 浙江大学 | A kind of fibroin-polypeptide electrospinning film and preparation method thereof promoting blood coagulation |
| CN111110912A (en) * | 2020-02-27 | 2020-05-08 | 东南大学 | Functional silk fibroin scaffold with cell response migration effect and preparation method thereof |
| CN111529759A (en) * | 2020-04-23 | 2020-08-14 | 东华大学 | Macroporous bone tissue engineering scaffold capable of sustainably releasing inorganic active ingredients and preparation method thereof |
| CN112980012A (en) * | 2021-02-22 | 2021-06-18 | 苏州大学 | Oriented material based on magnetic nanofiber and preparation method and application thereof |
| CN114209845A (en) * | 2021-12-18 | 2022-03-22 | 苏州健雄职业技术学院 | Preparation method of magnetic nanoparticles |
| CN114984313A (en) * | 2022-04-26 | 2022-09-02 | 江苏省中医药研究院(江苏省中西医结合医院) | Method for improving piezoelectric effect of silk fibroin scaffold |
| CN115068662A (en) * | 2022-05-18 | 2022-09-20 | 复旦大学附属中山医院 | Natural-source silk protein-tannic acid-ferroferric oxide nanoparticle hydrogel |
-
2013
- 2013-06-07 CN CN2013102285716A patent/CN103272267A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 樊宏鑫: "两种生物可降解复合材料的制备及其结构性能研究", 《中国优秀硕士学位论文全文数据库医药卫生科技辑》 * |
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103638554A (en) * | 2013-11-13 | 2014-03-19 | 浙江大学 | Preparation method of composite material of silk fibroin and marine mussel adhesion protein |
| CN103721295A (en) * | 2013-12-19 | 2014-04-16 | 浙江大学 | Method for increasing biocompatibility and mechanical property of fibroin biomaterials |
| CN105002658A (en) * | 2015-08-19 | 2015-10-28 | 哈尔滨工业大学 | Preparation method and driving method of remotely controllable multiple shape memory polymer composite fibrous membrane |
| CN105002658B (en) * | 2015-08-19 | 2017-11-03 | 哈尔滨工业大学 | The preparation method and driving method of remote-controllable Multiple Shape memory polymer composite cellulosic membrane |
| CN107552095A (en) * | 2017-09-17 | 2018-01-09 | 钱景 | The silk three-dimensional porous material and preparation method of carried titanium dioxide Nano Silver |
| CN108976450A (en) * | 2018-04-23 | 2018-12-11 | 安徽工程大学 | Based on wax, growth prepares the method for super-hydrophobic fibroin protein film, a kind of super-hydrophobic fibroin protein film certainly |
| CN108976820A (en) * | 2018-05-11 | 2018-12-11 | 四川大学 | A kind of Ferroferric oxide/polypyrrole composite material and preparation method thereof |
| CN110448719A (en) * | 2019-06-28 | 2019-11-15 | 浙江大学 | A kind of fibroin-polypeptide electrospinning film and preparation method thereof promoting blood coagulation |
| CN111110912A (en) * | 2020-02-27 | 2020-05-08 | 东南大学 | Functional silk fibroin scaffold with cell response migration effect and preparation method thereof |
| CN111529759A (en) * | 2020-04-23 | 2020-08-14 | 东华大学 | Macroporous bone tissue engineering scaffold capable of sustainably releasing inorganic active ingredients and preparation method thereof |
| CN112980012A (en) * | 2021-02-22 | 2021-06-18 | 苏州大学 | Oriented material based on magnetic nanofiber and preparation method and application thereof |
| CN114209845A (en) * | 2021-12-18 | 2022-03-22 | 苏州健雄职业技术学院 | Preparation method of magnetic nanoparticles |
| CN114209845B (en) * | 2021-12-18 | 2023-11-07 | 苏州健雄职业技术学院 | Preparation method of magnetic nano particles |
| CN114984313A (en) * | 2022-04-26 | 2022-09-02 | 江苏省中医药研究院(江苏省中西医结合医院) | Method for improving piezoelectric effect of silk fibroin scaffold |
| CN115068662A (en) * | 2022-05-18 | 2022-09-20 | 复旦大学附属中山医院 | Natural-source silk protein-tannic acid-ferroferric oxide nanoparticle hydrogel |
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Application publication date: 20130904 |