CN103184570A - Silk-fibroin-based antibacterial nanofiber and preparation method thereof - Google Patents
Silk-fibroin-based antibacterial nanofiber and preparation method thereof Download PDFInfo
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- CN103184570A CN103184570A CN2013101209700A CN201310120970A CN103184570A CN 103184570 A CN103184570 A CN 103184570A CN 2013101209700 A CN2013101209700 A CN 2013101209700A CN 201310120970 A CN201310120970 A CN 201310120970A CN 103184570 A CN103184570 A CN 103184570A
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Abstract
The invention discloses a silk-fibroin-based antibacterial nanofiber and a preparation method thereof. The nanofiber comprises the following components in parts by weight: 40-98 parts of silk fibroin, 1-10 parts of titanium dioxide and 1-60 parts of chitosan. The preparation method comprises the following steps: degumming and drying silk to obtain fibroin, processing fibroin to prepare a regenerated silk fibroin film, dissolving silk fibroin, titanium dioxide and chitosan in a polar solvent according to a certain mass ratio to prepare a spinning solution with the mass concentration of 0.01-80%, and preparing the silk fibroin-based antibacterial nanofiber with the average diameter of 10-1000 nm in a room-temperature state by electrostatic spinning equipment. The silk fibroin-based antibacterial nanofiber newly developed by the invention has an antibacterial ratio of more than 95%, has the characteristics of good biocompatibility and excellent mechanical performance while having the characteristic of long antibacterial property, and is suitable for biomedical materials.
Description
Technical field
The present invention relates to a kind of nano-fiber material and preparation method thereof, be specifically related to a kind of fibroin albumen base antibacterial nano fiber material and preparation method thereof, belong to field of medical materials.
Background technology
Nano anti-biotic material is the new material that a class possesses bacteriostasis property, because the high-specific surface area of antiseptic and the special effects of high reaction activity in the material, improved whole antibacterial effect greatly, can make microorganism comprise that the growth of bacterium, fungi, saccharomycete, algae and virus etc. and breeding keep lower level.The various goods made from anti-biotic material, has the health self-cleaning function, can effectively avoid the propagation of bacterium, and the mechanical property of anti-biotic material is strengthened, the nano-antibacterial product not only can effectively stop the bacterium cross infection of person to person, people and thing, thing and thing, can also guide people that the health care pattern is changed into ex ante forecasting and prevention from treat afterwards.Along with the raising of people's living standard and health environment consciousness, the production of nano anti-biotic material and products thereof has become important new industry.
Present most of anti-biotic material mainly adopts and directly adds material or the group that methods such as antiseptic or chemical graft will have antibacterial functions in the material and introduce, or is coated on the material that material surface becomes material to have anti-microbial property.The research of at present relevant anti-biotic material is in the majority with the anti-biotic material report that contains Nano Silver or silver ion, and the Nano Silver majority is powder additive, complicated process of preparation, and the processing cost height, and also Nano Silver is easily reunited, is combined with material matrix relatively poor when using; Chinese patent application CN102391738A discloses a kind of PVA-based nano composite antibacterial class coating material that contains silver ion and preparation method thereof, prepare PVA-based nanocomposite coating material earlier, again it is immersed in the liquor argenti nitratis ophthalmicus, stir, remove residual silver ion through washed with de-ionized water, drying at room temperature, acquisition contains the PVA-based nano composite antibacterial class coating material of silver ion, this method complex process, the antibiotic durability of class coating material prepared therefrom can not be guaranteed.
On the other hand, along with the develop rapidly of nano material technology, the nanofiber technology has become forward position and the research focus of fibre science, and is applied at industrial fields such as electronics, machinery, biomedicine, chemical industry, weavings.Nanofiber mainly comprises two concepts: the one, and proper nanofiber refers to that fibre diameter is less than the superfine fibre of 100 nm; Another concept is that nanoparticle is filled in the fiber, and fiber is carried out modification, adopts the different nanoparticle of performance, can develop various functional fibers such as antibiotic, fire-retardant, electromagnetic shielding.
Electrostatic spinning technique is to prepare the most important method of nanofiber at present.The core of this technology is charged Polymer Solution or melt to be flowed in electrostatic field and deformation takes place, and then through solvent evaporation or melt cooling and solidify, so obtain fibrous material, this process is called for short electrospinning.Adopt natural or synthetic high polymer is raw material, through the existing report of the nano-fiber material of electrostatic spinning preparation, for example: be the nano-fiber material of feedstock production with polyamide, polyvinyl alcohol, polypropylene, cellulose and derivative thereof etc., but the biocompatibility of above-mentioned material is poor, is unsuitable for as medical material.
Fibroin albumen is a kind of pure natural macromolecular material, with collagen equally have in the good body, the external biological compatibility (referring to Gregory H Altman, et al, Biomaterials, 2003,401-416), be suitable as biomaterial.Chinese patent application CN1348820A discloses a kind of Coremia-resisting wound protecting film and preparation method thereof, and this method adopts the method for fibroin and antiseptic blend to obtain the antimicrobial protection film; Chinese patent application CN102319448A discloses a kind of antibacterial hydrogel material for the preparation of medical wound dressing and preparation method thereof, this method adopts the interpolation n-trimethyl chitosan chloride to prepare the fibroin albumen anti-bacterial hydrogel, its preparation process is simple, but the mechanical property of material is very poor.
Simultaneously, as antibiotic material in medical use, not only to pay attention to its broad-spectrum antibacterial activity, more need to consider its biological safety, biocompatibility and degradability comprehensively, should avoid problems such as acute toxicity, allergic reaction.
Summary of the invention
The purpose of this invention is to provide a kind of fibroin albumen base antibacterial nano fiber and preparation method thereof, prepared nanofiber has mechanical property and the long-term antibacterial effect of excellent biological compatibility, excellence.
For achieving the above object, the technical solution used in the present invention is: a kind of fibroin albumen base antibacterial nano fiber by parts by mass, comprises following component:
40 ~ 98 parts of fibroin albumens
1 ~ 10 part of titanium dioxide
1 ~ 60 part of shitosan
Wherein, the particle diameter of described titanium dioxide is 5 ~ 1000nm; The diameter of described fibroin albumen base antibacterial nano fiber is 10 ~ 1000 nm.
In the technique scheme, the deacetylation of described shitosan is 50% ~ 100%, and molecular weight is 2 * 10
5~ 5 * 10
5, viscosity is 0.7 ~ 1Pa.s.
In the technique scheme, described fibroin albumen is one or more in tussah silk, mulberry silk, wild silk yarn, ricinus silk, camphor silk, cassava silkwormsilk, the willow silk.
The preparation method of above-mentioned fibroin albumen base antibacterial nano fiber may further comprise the steps:
(1) preparation of fibroin protein film: silk through come unstuck, dry fibroin fiber, the treated regenerated silk fibroin film that is prepared into of fibroin fiber of obtaining;
(2) preparation of spinning solution: fibroin protein film and the titanium dioxide with step (1) preparation is dissolved in the polar solvent earlier, shitosan is added in the solution again, and stirring at room is made uniform spinning solution, concentration of dope 0.01%～80% after fully mixing; Described polar solvent is one or more in anhydrous formic acid, glacial acetic acid, dimethyl formamide, glacial acetic acid, trifluoroacetic acid, the hexafluoroisopropanol;
(3) preparation of nanofiber: with the spinning solution electrostatic spinning apparatus spinning of step (2) preparation, obtain fibroin albumen base antibacterial nano fiber material.
In the technique scheme, the processing to fibroin fiber in the described step (1) comprises dissolving, dialysis, filtration, dry run; Wherein the solvent that adopts of course of dissolution is selected from LiBr, C
2H
5OH and H
2Mixed liquor (the LiBr:C of O
2H
5OH:H
2The O=45:44:11 mass ratio), LiBr and H
2Mixed liquor (the LiBr:H of O
2The O=40:60 mass ratio) or CaCl
2, C
2H
5OH and H
2Mixed liquor (the CaCl of O
2: C
2H
5OH:H
2The O=1:2:8 mol ratio).
In the technique scheme, in the described step (1) processing of fibroin fiber is comprised dissolving, drying, washing, dry run again, wherein the solvent that adopts of course of dissolution is selected from acid: the mass ratio of salt is acid/salt mixed liquor of 99:1～10:90; Described acid is selected from formic acid, phosphoric acid or both mixed liquors; Salt is selected from one or more in calcium chloride, calcium hydroxide, calcium carbonate, calcium nitrate, hydroxyapatite, tricalcium phosphate, tetracalcium phosphate, OCP, calcium monohydrogen phosphate, calcium phosphate, lithium bromide, barium chloride, copper chloride, zinc chloride, the magnesium chloride.
In the technique scheme, the technological parameter of electrostatic spinning is in the described step (3): 1～50 kilovolt of voltage, 1～50 centimetre of receiving range, liquid inventory are 0.01～20mL/h.
Because technique scheme is used, the present invention compared with prior art has following advantage:
1. the present invention has developed a kind of multicomponent fibroin albumen base antibacterial nano fiber material, antimicrobial component titanium dioxide and shitosan are dispersed in the nanofiber, the antibiotic rate of nanofiber reaches more than 95%, use in the prior art antibacterial effect of material of titanium dioxide or shitosan more lasting separately, antibiotic rate is higher.
2. the nano-fiber material of the present invention's preparation is matrix with the natural silk fibroin, has the biocompatibility of getting well, good degradability and excellent mechanical property, is a kind of desirable bio-medical material;
3. preparation method of the present invention is simple, and preparation condition is controlled, and can regulate material proportion as required, thereby obtains to satisfy the bio-medical material of respective performances, has a good application prospect.
Description of drawings
Fig. 1 is the sem photograph of fibroin albumen base antibacterial nano fiber in the embodiment of the invention one.
The specific embodiment
Be further described below in conjunction with the present invention of embodiment:
Embodiment one
A kind of fibroin albumen base antibacterial nano fiber, its preparation method comprises the steps:
(1) natural mulberry silk boils 30 min with the sodium carbonate liquor of mass fraction 0.05% and comes unstuck, and obtains pure mulberry silk fibroin fiber after repeating 3 times; This fibroin albumen is dissolved in LiBr:C
2H
5OH:H
2The O=45:44:11(mass ratio) in the mixed liquor, stirring and dissolving obtains regenerated silk fibroin solution in 70 ℃ of water-baths; Through dialysis, filtration, film forming, form regenerated silk fibroin film;
(2) regenerated silk fibroin film, titanium dioxide and shitosan being pressed mass ratio 95:3:2 prepares, earlier regenerated silk fibroin film and titanium dioxide are dissolved in the formic acid, then, shitosan are added in the above-mentioned solution again, stirring at room 4h is prepared into mass fraction and is 10% spinning solution;
(3) with the above-mentioned spinning solution that makes, under room temperature state, utilize electrospinning device to carry out spinning, can obtain fibroin albumen base antibacterial nano fiber.Technological parameter is during spinning: spinning speed is 0.2ml/h; Spinning voltage is 15kV; Receiving range is 10cm.
Accompanying drawing 1 is for the sem photograph of the above-mentioned fibroin albumen base antibacterial nano fiber that makes, and referring to Fig. 1, the diameter of antibacterial nano fiber is 99 ~ 173 nm.
Embodiment two
A kind of fibroin albumen base antibacterial nano fiber, its preparation method comprises the steps:
(1) natural mulberry silk boils 30 min with the sodium carbonate liquor of mass fraction 0.05% and comes unstuck, and obtains pure mulberry silk fibroin fiber after repeating 3 times; This fibroin albumen is dissolved in CaCl
2: C
2H
5OH:H
2The O=1:2:8(mol ratio) in the mixed liquor, stirring and dissolving obtains regenerated silk fibroin solution in 70 ℃ of water-baths; Through dialysis, filtration, film forming, form regenerated silk fibroin film;
(2) regenerated silk fibroin film, titanium dioxide and shitosan being pressed mass ratio 70:15:15 prepares, earlier regenerated silk fibroin film and titanium dioxide are dissolved in the formic acid, then, shitosan are added in the above-mentioned solution again, stirring at room 6h is prepared into mass fraction and is 20% spinning solution;
(3) with the above-mentioned spinning solution that makes, under room temperature state, utilize electrospinning device to carry out spinning, can obtain fibroin albumen base antibacterial nano fiber; Technological parameter is during spinning: spinning speed is 0.15ml/h; Spinning voltage is 20kV; Receiving range is 12cm.
Claims (6)
1. a fibroin albumen base antibacterial nano fiber is characterized in that, by parts by mass, comprises following component:
40～98 parts of fibroin albumens
1～10 part of titanium dioxide
1～60 part of shitosan
Wherein, the particle diameter of described titanium dioxide is 5～1000nm; The diameter of described fibroin albumen base antibacterial nano fiber is 10～1000 nm.
2. fibroin albumen base antibacterial nano fiber according to claim 1, it is characterized in that: the deacetylation of described shitosan is 50%～100%, molecular weight is 2 * 10
5～5 * 10
5, viscosity is 0.7 ~ 1Pas.
3. fibroin albumen base antibacterial nano fiber according to claim 1, it is characterized in that: described fibroin albumen is one or more in tussah silk, mulberry silk, wild silk yarn, ricinus silk, camphor silk, cassava silkwormsilk, the willow silk.
4. the preparation method of a fibroin albumen base antibacterial nano fiber as claimed in claim 1 is characterized in that, may further comprise the steps:
(1) preparation of fibroin protein film: silk through come unstuck, dry fibroin fiber, the treated regenerated silk fibroin film that is prepared into of fibroin fiber of obtaining;
(2) preparation of spinning solution: fibroin protein film and the titanium dioxide with step (1) preparation is dissolved in the polar solvent earlier, shitosan is added in the solution again, and stirring at room is made uniform spinning solution, concentration of dope 0.01%～80% after fully mixing; Described polar solvent is one or more in anhydrous formic acid, glacial acetic acid, dimethyl formamide, glacial acetic acid, trifluoroacetic acid, the hexafluoroisopropanol;
(3) preparation of nanofiber: with the spinning solution electrostatic spinning apparatus spinning of step (2) preparation, obtain fibroin albumen base antibacterial nano fiber material.
5. preparation method according to claim 4, it is characterized in that: the processing to fibroin fiber in the described step (1) comprises dissolving, dialysis, filtration, dry run; Wherein the solvent that adopts of course of dissolution is selected from LiBr, C
2H
5OH and H
2Mixed liquor (the LiBr:C of O
2H
5OH:H
2The O=45:44:11 mass ratio), LiBr and H
2Mixed liquor (the LiBr:H of O
2The O=40:60 mass ratio) or CaCl
2, C
2H
5OH and H
2Mixed liquor (the CaCl of O
2: C
2H
5OH:H
2The O=1:2:8 mol ratio).
6. preparation method according to claim 4, it is characterized in that: in the described step (1) processing of fibroin fiber is comprised dissolving, drying, washing, dry run again, wherein the solvent that adopts of course of dissolution is selected from acid: the mass ratio of salt is acid/salt mixed liquor of 99:1～10:90; Described acid is selected from formic acid, phosphoric acid or both mixed liquors; Salt is selected from one or more in calcium chloride, calcium hydroxide, calcium carbonate, calcium nitrate, hydroxyapatite, tricalcium phosphate, tetracalcium phosphate, OCP, calcium monohydrogen phosphate, calcium phosphate, lithium bromide, barium chloride, copper chloride, zinc chloride, the magnesium chloride.
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