CN107456607A - Guide Periodontal Tissue Regeneration film of new " sandwich " structure a kind of of difunctionalization and its preparation method and application - Google Patents

Guide Periodontal Tissue Regeneration film of new " sandwich " structure a kind of of difunctionalization and its preparation method and application Download PDF

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Publication number
CN107456607A
CN107456607A CN201710533099.5A CN201710533099A CN107456607A CN 107456607 A CN107456607 A CN 107456607A CN 201710533099 A CN201710533099 A CN 201710533099A CN 107456607 A CN107456607 A CN 107456607A
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China
Prior art keywords
tissue regeneration
polycaprolactone
film
preparation
periodontal tissue
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CN201710533099.5A
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Inventor
苗国厚
杨雪超
李正茂
赵世勇
叶上珠
夏娟
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Stomatological Hospital of Guangzhou Medical University
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Stomatological Hospital of Guangzhou Medical University
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Priority to CN201710533099.5A priority Critical patent/CN107456607A/en
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/54Biologically active materials, e.g. therapeutic substances
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/02Inorganic materials
    • A61L27/10Ceramics or glasses
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/14Macromolecular materials
    • A61L27/18Macromolecular materials obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/14Macromolecular materials
    • A61L27/22Polypeptides or derivatives thereof, e.g. degradation products
    • A61L27/227Other specific proteins or polypeptides not covered by A61L27/222, A61L27/225 or A61L27/24
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L27/00Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/20Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
    • A61L2300/252Polypeptides, proteins, e.g. glycoproteins, lipoproteins, cytokines
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/412Tissue-regenerating or healing or proliferative agents
    • A61L2300/414Growth factors
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2430/00Materials or treatment for tissue regeneration
    • A61L2430/02Materials or treatment for tissue regeneration for reconstruction of bones; weight-bearing implants
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2430/00Materials or treatment for tissue regeneration
    • A61L2430/12Materials or treatment for tissue regeneration for dental implants or prostheses
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L2430/00Materials or treatment for tissue regeneration
    • A61L2430/34Materials or treatment for tissue regeneration for soft tissue reconstruction

Abstract

The present invention relates to Guide Periodontal Tissue Regeneration film of new " sandwich " structure of a kind of difunctionalization and its preparation method and application, the Guide Periodontal Tissue Regeneration film includes internal layer, intermediate layer and outer layer, and the internal layer is polycaprolactone/fibroin albumen/mesopore bioactive glass microballoon tunica fibrosa;The intermediate layer is polycaprolactone/fibroin fiber film;The outer layer is polycaprolactone/fibroin fiber film of load platelet derived growth factor.Guide Periodontal Tissue Regeneration film provided by the invention is that trilamellar membrane structure can promote regeneration of periodontal soft tissue, has periodontal sclerous tissues and soft tissue double regeneration and repair function concurrently;Can also effectively prevent human gingival epithelial cells invasion and attack arrive Cranial defect area, for bone tissue regeneration reconstruction provide needed for space.In addition, Guide Periodontal Tissue Regeneration film provided by the invention also has preferable biocompatibility, degradability and bioactivity.

Description

A kind of Guide Periodontal Tissue Regeneration film of new " sandwich " structure of difunctionalization And its preparation method and application
Technical field
The invention belongs to biomaterial for medical purpose field, more particularly, to new " sandwich " of a kind of difunctionalization Guide Periodontal Tissue Regeneration film of structure and its preparation method and application.
Background technology
Periodontal disease is one of common disease and frequently-occurring disease in mouth disease, and according to statistics, the people in the whole world nearly 90% has different journeys The periodontal disease of degree(Predominantly periodontitis and gingivitis)If failing to treat in time, cause the forfeiture of connective tissue and bone tissue, Ultimately result in tooth mobility to come off, turn into the first cause that adult loses tooth.Therefore, prevention and treatment periodontal disease is to health It is particularly important.Traditional treatment method mainly has extraction, had a denture made with root canal etc..Extraction injures to damaging property of patient; Have a denture made and functionally had differences with natural teeth;Root canal treatments are complicated, cost is high, wound scale removal process easily to the tip of a root around Tissue causes to damage.
In recent years, paradenlal tissue regeneration therapy is induced to turn into the study hotspot and important development direction of periodontal disease treatment. Its principle is one layer of GTR of implantation between gum and root face(Guided tissue regeneration, GTR)Thin-film material, Prevent human gingival epithelial cells grow into defective region and can with root of the tooth formed certain interval, be periodontal ligament cell propagation, grow and Space needed for differentiation offer, so as to the periodontium of Regeneration and Repair defect.But Guide Periodontal Tissue Regeneration of the prior art Film such as GTR thin-film materials lack inductivity primarily directed to periodontal sclerous tissues to periodontal soft tissue.And paradenlal tissue regeneration reparation Not only include the sclerous tissues being made up of alveolar bone and cementum, in addition to the soft tissue such as parodontium and gum, if can not be complete Reparation periodontium, it is possible to cause the failure of whole Regeneration and Repair process.However, rarely have at present on soft tissue repair The report of paradenlal tissue regeneration film.
Therefore, New-type bifunctional a kind of while that there is mediation periodontal sclerous tissues and soft tissue regeneration effect is prepared Guide Periodontal Tissue Regeneration membrane material has great Research Significance and application value.
The content of the invention
It is an object of the invention to overcome Guide Periodontal Tissue Regeneration material shortage periodontal soft tissue induction in the prior art The defects of property, there is provided a kind of Guide Periodontal Tissue Regeneration film, Guide Periodontal Tissue Regeneration film provided by the invention are trilamellar membrane knot Structure, regeneration of periodontal soft tissue can be promoted, have periodontal sclerous tissues and soft tissue double regeneration and repair function concurrently;Can also effectively it prevent Human gingival epithelial cells invasion and attack arrive Cranial defect area, for bone tissue regeneration reconstruction provide needed for space.
Another object of the present invention is to provide the preparation method of above-mentioned Guide Periodontal Tissue Regeneration film.
Another object of the present invention is to provide above-mentioned Guide Periodontal Tissue Regeneration film in paradenlal tissue regeneration reparation Using
To achieve the above object, the present invention adopts the following technical scheme that:
A kind of Guide Periodontal Tissue Regeneration film, the Guide Periodontal Tissue Regeneration film includes internal layer, intermediate layer and outer layer, described interior Layer is polycaprolactone/fibroin albumen/mesopore bioactive glass microballoon tunica fibrosa;The intermediate layer is polycaprolactone/fibroin egg White fiber film;The outer layer is polycaprolactone/fibroin fiber film of load platelet derived growth factor.
Guide Periodontal Tissue Regeneration film provided by the invention has three-decker, and the regeneration for taking into account sclerous tissues and soft tissue is repaiied It is multiple.The intermediate layer of the regeneration membrane is polycaprolactone/fibroin fiber film, has and provides mechanical property support and barrier gum The function that cell is grown into;Polycaprolactone(PCL)It is a kind of excellent degradation material, good biocompatibility and degradation speed is fitted In;Fibroin albumen(SF)With preferable bioactivity, pla-pcl and fibroin albumen are combined to the guiding being prepared Paradenlal tissue regeneration material is while with suitable degradability with preferable bioactivity.Outer layer is platelet-derived by loading Growth factor(PDGF)Polycaprolactone/fibroin fiber film form, PDGF is as the potential schizogamy of fibroblast And chemotactic factor (CF), the synthesis of its collagen and non-collagen can be stimulated, promotes the generation and soft tissue healing of blood vessel.Internal layer For polycaprolactone/fibroin albumen/mesopore bioactive glass microballoon tunica fibrosa, mesopore bioactive glass microballoon is loaded with;With Other inorganic bios(Hydroxyapatite, calcium phosphate)Compare, mesopore bioactive glass microballoon has good biofacies Capacitive and degradability, be implanted into after human body surface can the formation of induced synthesis apatite and bone tissue chemically combined, pass through release Active ion(Soluble silicon ion)Activation and Bone formation-related gene, promotion organization differentiation and healing.
Guide Periodontal Tissue Regeneration film provided by the invention is three layers of similar " sandwich " structure, and intermediate layer and outer layer can Prevent human gingival epithelial cells attack arrive Cranial defect area, for bone tissue regeneration reconstruction provide needed for space;Internal layer and outer layer difference Periodontal sclerous tissues and soft tissue regeneration ability are assigned, so as to realize the dual-use function reparation of periodontium;And inventor passes through Material is carried out preferred so that present invention offer regeneration membrane has more preferable degradability, biocompatibility and bioactivity.
Preferably, the outer layer and internal layer are parallel-oriented fibre structure.Inventor has found by studying, outer layer and interior Parallel-oriented fibre structure possessed by layer can guide cell to be grown along fiber-wall-element model, promote the adhesion of cell, propagation with Differentiation and the secretion of extracellular matrix, be advantageous to accelerate tissue repair speed.
The preparation method of above-mentioned Guide Periodontal Tissue Regeneration film, including following preparation process:
S1:Fibroin albumen is freezed into powder to be completely dissolved in hexafluoroisopropanol with polycaprolactone, obtains intermediate layer spinning solution;
S2:Mesopore bioactive glass microballoon is added into intermediate layer spinning solution obtained by S1, stirring, concussion make mesoporous biological live Property glass microsphere, which is uniformly dispersed, produces internal layer spinning solution;
S3:Platelet derived growth factor solution is added into intermediate layer spinning solution obtained by S1, produces outer layer spinning solution;
S4:It is using method of electrostatic spinning that the outer layer, intermediate layer and internal layer spinning solution successively electrospinning, formation trilamellar membrane structure is dry It is dry to produce the Guide Periodontal Tissue Regeneration film.
The Guide Periodontal Tissue Regeneration film that this method is prepared has trilamellar membrane structure, has periodontal sclerous tissues and soft group concurrently The Regeneration and Repair effect knitted.
Preferably, the total mass concentration of polycaprolactone and fibroin albumen is 6% ~ 8% in the S1 steps, and fibroin albumen is with gathering The mass ratio of caprolactone is 1:3~3:1.
Preferably, the mass ratio of the fibroin albumen and polycaprolactone is 1:1.
Preferably, the mesopore bioactive glass microballoon in the S2 is radial meso-hole structure, particle diameter is 200 ~ 500nm.The microballoon has micro-nano appearance structure, bigger specific surface area and pore structure, has higher surface-active More macroion release performance, therefore more excellent cell compatibility and Cell differentiation inducing activity ability are shown, can be further The biocompatibility of Guide Periodontal Tissue Regeneration film is improved, and causes internal layer that there is mediation bone tissue Forming ability.
Preferably, the mesopore bioactive glass microballoon is by SiO2Formed with CaO, the SiO2Molar fraction be 60% ~ 90%, the CaO molar fraction are 10% ~ 40%.Inventor, which studies, to be found, is elected to the mesoporous life formed with above-mentioned molar fraction The paradenlal tissue regeneration film obtained during thing activity glass microballoon has more excellent biocompatibility.
Platelet derived growth factor can stimulate its collagen as the potential schizogamy of fibroblast and chemotactic factor (CF) The synthesis of albumen and non-collagen, promote the generation and soft tissue healing of blood vessel so that regeneration membrane provided by the invention has More preferable Regeneration and Repair function.
Preferably, the mass concentration of platelet derived growth factor is 50 ~ 100ng/mL in the S3.
Preferably, the mass concentration of the platelet derived growth factor is 80 ng/mL.
Preferably, it is 15 ~ 20 KV that high tension voltage is controlled in the method for electrostatic spinning.
Preferably, spinning flow velocity is 0.8 ~ 1.0 mL/h in the method for electrostatic spinning.
Preferably, the vertical range of syringe needle and reception device is 10 ~ 15 cm in the method for electrostatic spinning.
Preferably, reception device is roller reception device in the electrostatic silk spinning method.
Preferably, it is 2000 that outer layer and internal layer, which carry out roller reception device rotating speed during electrostatic silk spinning, in the electrostatic silk spinning method ~4000r/min.The rotating speed height of roller reception device will influence the orientation texture of tunica fibrosa, and roller receives dress in conventional method The rotating speed put typically selects 100 ~ 500 r/min, and the tunica fibrosa being prepared is random form;Received when greatly improving roller During the rotating speed of device, specific orientation structure can be formed.Inventor, which studies, to be found, when outer layer and internal layer silk spinning liquid are in electrostatic silk spinning Cheng Zhong, when setting roller reception device rotating speed as 2000 ~ 4000r/min, outer layer with parallel-oriented structure and interior can be made Layer.
Application of the above-mentioned Guide Periodontal Tissue Regeneration film in the Regeneration and Repair of periodontium is also in the protection model of the present invention Within enclosing.
Compared with prior art, the present invention has the advantages that:
Guide Periodontal Tissue Regeneration film provided by the invention is three layers of similar " sandwich " structure, can promote periodontal soft tissue again It is raw, have periodontal sclerous tissues and soft tissue double regeneration and repair function concurrently;Human gingival epithelial cells invasion and attack can be also effectively prevented to arrive bone Defective region, for bone tissue regeneration rebuild provide needed for space.In addition, Guide Periodontal Tissue Regeneration film provided by the invention also has There are preferable biocompatibility, degradability and bioactivity, use can be widely popularized in clinical practice.
Brief description of the drawings
Fig. 1 is the structural representation of Guide Periodontal Tissue Regeneration film provided by the invention;
Fig. 2 is schematic diagram of the random form with the Guide Periodontal Tissue Regeneration membrane material of parallel orientation texture;
Fig. 3 is the outer layer of random form and the microstructure figure of internal layer;
Fig. 4 is the outer layer of parallel-oriented structure and the microstructure figure of internal layer;
Fig. 5 is that the TEM of mesopore bioactive glass microballoon schemes.
Wherein 1 is internal layer;2 be intermediate layer;3 be outer layer.
Embodiment
With reference to embodiment, the present invention will be further described.These embodiments are only that the typical case of the present invention is retouched State, but the invention is not restricted to this.Test method used is conventional method unless otherwise specified in following embodiments;Made Raw material, reagent etc., unless otherwise specified, being can be from the raw material and reagent that the commercial sources such as conventional market obtain.
Embodiment 1
A kind of Guide Periodontal Tissue Regeneration film, wherein internal layer are that polycaprolactone/fibroin albumen/mesopore bioactive glass microballoon is fine Film is tieed up, mesopore bioactive glass microballoon is radial fiber pore structure, and its mole of composition is 80%SiO2- 20%CaO, quality point Number is 0.4%, particle diameter is 200 ~ 500nm;Intermediate layer is polycaprolactone/fibroin fiber film, and polycaprolactone/fibroin albumen is molten Solution both total mass concentrations after hexafluoroisopropanol are 6%, and the mass ratio of fibroin albumen and polycaprolactone is 1:3;Outer layer is negative Polycaprolactone/fibroin fiber film of platelet derived growth factor is carried, platelet derived growth factor is in outer layer silk spinning liquid In mass concentration be 50ng/mL.
Preparation method is as follows:
S1:Fibroin albumen is freezed into powder to be dissolved in hexafluoroisopropanol solution with polycaprolactone, fully dissolving, what is be configured to is mixed It is intermediate layer spinning solution to close solution;
S2:Mesopore bioactive glass microballoon is added in the spinning solution of intermediate layer, mechanical agitation, ultrasonic vibration, makes mesoporous life Thing activity glass microballoon is uniformly dispersed, and obtains internal layer spinning solution;
S3:The deionized water solution dissolved with platelet derived growth factor is added in the spinning solution of intermediate layer, is well mixed To outer layer spinning solution;
S4:Will be by outer layer, intermediate layer and internal layer spinning solution successively electrospinning using method of electrostatic spinning:Outer layer spinning solution is loaded and injected In device, syringe is fixed on microsyringe, front end of the syringe needle syringe needle(Internal diameter 1mm)As anode, roller reception device Surface is encased by the use of masking foil and is grounded as negative electrode, for receiving electricity spinning fibre.Syringe needle is placed with cathode vertical, sets voltage For 15 KV, spacing is 12 cm, spinning flow velocity 1mL/h, and roller reception device rotating speed is 3000r/min, the h of continuous electro-spinning 1, Obtain polycaprolactone/fibroin fiber film of parallel-oriented load platelet derived growth factor;During spinning solution is changed into Interbed spinning solution, setting voltage are 15 KV, and spacing is 12 cm, and spinning flow velocity 1mL/h, roller reception device rotating speed is 200 R/min, the h of continuous electro-spinning 1, obtain polycaprolactone/fibroin fiber film of random distribution;Spinning solution is changed into internal layer to spin Silk liquid, setting voltage is 15 KV, and spacing is 12 cm, and spinning flow velocity 1mL/h, roller reception device rotating speed is 2000r/min, The h of continuous electro-spinning 1, obtain parallel-oriented polycaprolactone/fibroin albumen/mesopore bioactive glass microballoon tunica fibrosa.By tinfoil Removed from roller reception device, drying at room temperature 3d, obtain the Guide Periodontal Tissue Regeneration film of difunctionalization.
The mesopore bioactive glass microballoon that the present invention is added can be made by microemulsion method, be specifically referred to 2014 years Li Xian et al. method(J Mater Chem B, 2014, 2(40): 7045-7054).Specifically, a mole composition is 80% SiO2- 20%CaO mesopore bioactive glass method for preparing microsphere is as follows:
0.3 g urea, 1 g bromide sixteen alkyls pyridines, 0.46 g isopropanols are added to 30 mL deionized waters and 30 mL In the mixed solution of hexamethylene, it is sufficiently stirred to form homogeneous emulsion, adds 2.5 g tetraethyl orthosilicates, the water nitre of 0.708g tetra- Sour calcium, after reacting 30 min under 30 °C, 70 °C are warming up to, continue to react 16 h, after being cooled to room temperature, reaction product 10000r/min centrifuges 20 min, is cleaned 3 times with acetone, absolute ethyl alcohol and deionized water successively, 60 °C of dryings, in 600 °C of heat 5 h are handled, it is 80%SiO to obtain a mole composition2- 20%CaO mesopore bioactive glass microballoon.
If changing the addition of corresponding material, the mesoporous biological that different moles of compositions are can obtain according to above-mentioned preparation method is lived Property glass microsphere.
Embodiment 2
In the Guide Periodontal Tissue Regeneration film that the present embodiment provides, a mole composition for mesopore bioactive glass microballoon is 60% SiO2- 40%CaO, mass fraction 0.6%, particle diameter are 200 ~ 500nm;The content of platelet derived growth factor is 80ng/ mL;It is 8% that the polycaprolactone/fibroin albumen in intermediate layer, which is dissolved in both total mass concentrations after hexafluoroisopropanol, fibroin albumen with The mass ratio of polycaprolactone is 1:3;Other components and dosage are consistent with embodiment 1.
For S1 ~ S3 in preparation method with consistent in embodiment 1, S4 is as follows:
Will be by outer layer, intermediate layer and internal layer spinning solution successively electrospinning using method of electrostatic spinning:Outer layer spinning solution is loaded into syringe In, syringe is fixed on microsyringe, front end of the syringe needle syringe needle(Internal diameter 1mm)As anode, roller reception device table Face is encased by the use of masking foil and is grounded as negative electrode, for receiving electricity spinning fibre.Syringe needle is placed with cathode vertical, and setting voltage is 16 KV, spacing are 15 cm, spinning flow velocity 0.8mL/h, and roller reception device rotating speed is 2000r/min, the h of continuous electro-spinning 1, Obtain polycaprolactone/fibroin fiber film of parallel-oriented load platelet derived growth factor;During spinning solution is changed into Interbed spinning solution, setting voltage are 18 KV, and spacing is 15 cm, spinning flow velocity 0.8mL/h, and roller reception device rotating speed is 300 r/min, the h of continuous electro-spinning 1, obtain polycaprolactone/fibroin fiber film of random distribution;Spinning solution is changed into interior Layer spinning solution, setting voltage is 18 KV, and spacing is 15 cm, spinning flow velocity 0.8mL/h, and roller reception device rotating speed is 2000r/min, the h of continuous electro-spinning 1, it is fine to obtain parallel-oriented polycaprolactone/fibroin albumen/mesopore bioactive glass microballoon Tie up film.Tinfoil is removed from roller reception device, drying at room temperature 3d, obtains the Guide Periodontal Tissue Regeneration film of difunctionalization.
Embodiment 3
In the Guide Periodontal Tissue Regeneration film that the present embodiment provides, a mole composition for mesopore bioactive glass microballoon is 90% SiO2- 10%CaO, mass fraction 0.8%, particle diameter are 200 ~ 500nm;The content of platelet derived growth factor is 100ng/ mL;It is 7% that the polycaprolactone/fibroin albumen in intermediate layer, which is dissolved in both total mass concentrations after hexafluoroisopropanol, fibroin albumen with The mass ratio of polycaprolactone is 1:3;Other components and dosage are consistent with embodiment 1.
For S1 ~ S3 in preparation method with consistent in embodiment 1, S4 is as follows:
Will be by outer layer, intermediate layer and internal layer spinning solution successively electrospinning using method of electrostatic spinning:Outer layer spinning solution is loaded into syringe In, syringe is fixed on microsyringe, front end of the syringe needle syringe needle(Internal diameter 1mm)As anode, roller reception device table Face is encased by the use of masking foil and is grounded as negative electrode, for receiving electricity spinning fibre.Syringe needle is placed with cathode vertical, and setting voltage is 15 KV, spacing are 15 cm, and spinning flow velocity 1mL/h, roller reception device rotating speed is 2000r/min, the h of continuous electro-spinning 1, is obtained To polycaprolactone/fibroin fiber film of parallel-oriented load platelet derived growth factor;Change spinning solution into centre Layer spinning solution, setting voltage are 20 KV, and spacing is 15 cm, and spinning flow velocity 1mL/h, roller reception device rotating speed is 300 R/min, the h of continuous electro-spinning 1, obtain polycaprolactone/fibroin fiber film of random distribution;Spinning solution is changed into internal layer to spin Silk liquid, setting voltage is 15 KV, and spacing is 15 cm, and spinning flow velocity 1mL/h, roller reception device rotating speed is 2000r/min, The h of continuous electro-spinning 1, obtain parallel-oriented polycaprolactone/fibroin albumen/mesopore bioactive glass microballoon tunica fibrosa.By tinfoil Removed from roller reception device, drying at room temperature 3d, obtain the Guide Periodontal Tissue Regeneration film of difunctionalization.
Embodiment 4
In the Guide Periodontal Tissue Regeneration film that the present embodiment provides, the polycaprolactone in intermediate layer/fibroin albumen is dissolved in hexafluoro is different Both total mass concentrations are 6% after propyl alcohol, and the mass ratio of fibroin albumen and polycaprolactone is 1:1, remaining component and dosage and system Preparation Method is consistent with embodiment 1.
Embodiment 5
In the Guide Periodontal Tissue Regeneration film that the present embodiment provides, the polycaprolactone in intermediate layer/fibroin albumen is dissolved in hexafluoro is different Both total mass concentrations are 6% after propyl alcohol, and the mass ratio of fibroin albumen and polycaprolactone is 3:1, remaining component and dosage and system Preparation Method is consistent with embodiment 1.
Embodiment 6
In the Guide Periodontal Tissue Regeneration film that the present embodiment provides, the tunica fibrosa of outer layer and internal layer does not have parallel-oriented structure, It is that 200 r/min are realized that roller, which receives speed, when mainly by controlling outer layer silk spinning liquid and internal layer silk spinning liquid electrostatic silk spinning, its Remaining component and dosage and preparation method are consistent with embodiment 1.
The structure of paradenlal tissue regeneration film and performance measurement
(1)The structure of Guide Periodontal Tissue Regeneration film
Guide Periodontal Tissue Regeneration film provided by the invention is the trilamellar membrane structure of similar " sandwich ", such as Fig. 1, is the present invention The structural representation of the Guide Periodontal Tissue Regeneration film of offer.1 is internal layer, i.e. polycaprolactone/fibroin albumen/mesopore bioactive Glass microsphere tunica fibrosa;2 be intermediate layer, i.e. polycaprolactone/fibroin fiber film;3 be outer layer, that is, loads platelet-derived life The polycaprolactone of the long factor/fibroin fiber film.Intermediate layer and outer layer can prevent human gingival epithelial cells invasion and attack from arriving Cranial defect area, For bone tissue regeneration rebuild provide needed for space;Internal layer and outer layer assign periodontal sclerous tissues and soft tissue regeneration ability respectively, So as to realize the dual-use function reparation of periodontium.
Fig. 2 is showing for random form provided by the invention and the Guide Periodontal Tissue Regeneration membrane material of parallel orientation texture It is intended to.Fig. 2(a)Outer layer/internal layer schematic diagram when being random form;Fig. 2(b)It is that there is the outer layer of parallel-oriented structure/interior Layer schematic diagram.
(2)The outer layer and internal layer of random form
The outer layer and internal layer of Guide Periodontal Tissue Regeneration film in the present embodiment 6 are random form, such as Fig. 2(a)And Fig. 2(b) It is shown.Fig. 2(a)For the microstructure figure of the outer layer of random form, Fig. 2(b)For the microstructure of the internal layer of random form Figure, it can be seen that outer layer and internal layer are disorderly arranged.
(3)Parallel-oriented structural outside layers and internal layer
The outer layer and internal layer of Guide Periodontal Tissue Regeneration film in the present embodiment 1 ~ 5 are respectively provided with parallel-oriented structure, its micro- knot Composition such as Fig. 3(a)And Fig. 3(b)It is shown.Fig. 3(a)For the microstructure figure of the outer layer with parallel-oriented structure, Fig. 3(b)For The microstructure figure of internal layer with parallel-oriented structure.By controlling roller in electrostatic silk spinning method to receive in the present embodiment 1 ~ 5 The speed of device so that outer layer and internal layer have parallel-oriented structure, cell can be guided to be grown along fiber-wall-element model, promote cell Adhesion, propagation and differentiation and extracellular matrix secretion, be advantageous to accelerate tissue repair speed.
(4)The structure of mesopore bioactive glass microballoon
The internal layer of the Guide Periodontal Tissue Regeneration film provided in the present invention is loaded with mesopore bioactive glass microballoon, and Fig. 5 is tool The TEM for having the porous structure mesoporous bioactivity glass microballoon of radial fiber schemes.As shown in Figure 5, the mesopore bioactive glass is micro- Ball has radial structure, and particle diameter is 200 ~ 500nm, has micro-nano appearance structure, bigger specific surface area and pore structure.

Claims (10)

1. the Guide Periodontal Tissue Regeneration film of new " sandwich " structure of a kind of difunctionalization, it is characterised in that described to draw Leading paradenlal tissue regeneration film includes internal layer, intermediate layer and outer layer, and the internal layer is that polycaprolactone/fibroin albumen/mesoporous biological is lived Property glass microsphere tunica fibrosa;The intermediate layer is polycaprolactone/fibroin fiber film;The outer layer is platelet-derived to load The polycaprolactone of growth factor/fibroin fiber film.
2. Guide Periodontal Tissue Regeneration film according to claim 1, it is characterised in that the outer layer and internal layer are parallel-oriented Fibre structure.
3. the preparation method of the Guide Periodontal Tissue Regeneration film of claim 1 or 2, it is characterised in that prepare step including following Suddenly:
S1:Fibroin albumen is freezed into powder to be completely dissolved in hexafluoroisopropanol with polycaprolactone, obtains intermediate layer spinning solution;
S2:Mesopore bioactive glass microballoon is added into intermediate layer spinning solution obtained by S1, stirring, concussion make mesoporous biological live Property glass microsphere, which is uniformly dispersed, produces internal layer spinning solution;
S3:Platelet derived growth factor solution is added into intermediate layer spinning solution obtained by S1, produces outer layer spinning solution;
S4:It is using method of electrostatic spinning that the outer layer, intermediate layer and internal layer spinning solution successively electrospinning, formation trilamellar membrane structure is dry It is dry to produce the Guide Periodontal Tissue Regeneration film.
4. preparation method according to claim 3, it is characterised in that in S1, the gross mass of polycaprolactone and fibroin albumen is dense Spend for 6% ~ 8%, the mass ratio of fibroin albumen and polycaprolactone is 1:3~3:1.
5. preparation method according to claim 4, it is characterised in that the mass ratio of the fibroin albumen and polycaprolactone is 1: 1。
6. preparation method according to claim 3, it is characterised in that in S2, the mesopore bioactive glass microballoon has Radial fiber pore structure, particle diameter are 200 ~ 500nm.
7. preparation method according to claim 6, it is characterised in that the mesopore bioactive glass microballoon is by SiO2And CaO Composition, the SiO2Molar fraction be 60% ~ 90%, the molar fraction of the CaO is 10% ~ 40%.
8. preparation method according to claim 3, it is characterised in that in S3, the quality of the platelet derived growth factor Concentration is 50 ~ 100ng/mL.
9. preparation method according to claim 8, it is characterised in that the mass concentration of the platelet derived growth factor is 80 ng/mL。
10. application of the Guide Periodontal Tissue Regeneration film of claim 1 or 2 in paradenlal tissue regeneration reparation.
CN201710533099.5A 2017-07-03 2017-07-03 Guide Periodontal Tissue Regeneration film of new " sandwich " structure a kind of of difunctionalization and its preparation method and application Pending CN107456607A (en)

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CN110075358A (en) * 2019-04-17 2019-08-02 苏州大学附属第二医院 Promote bone uptake composite membrane, preparation method and application
CN110193098A (en) * 2019-06-21 2019-09-03 四川大学 A kind of multi-gradient biomembrane and preparation method thereof
CN110193098B (en) * 2019-06-21 2021-07-13 四川大学 Multilayer gradient biological membrane and preparation method thereof
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CN112675361A (en) * 2020-12-28 2021-04-20 浙江大学 Preparation method of regional function specificity clinical periodontal defect repair module
CN113456885B (en) * 2021-05-28 2022-10-04 浙江大学 Gradient material for promoting repair of cartilage calcification layer and preparation method thereof
CN113456885A (en) * 2021-05-28 2021-10-01 浙江大学 Gradient material for promoting repair of cartilage calcified layer and preparation method thereof
CN113713184A (en) * 2021-07-13 2021-11-30 扬子江药业集团广州海瑞药业有限公司 Bone tissue regeneration guide membrane and preparation method thereof
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