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CN107158460A - A kind of preparation method of the composite regenerated fiber repair materials of acaudina molpadioidea collagen - Google Patents

A kind of preparation method of the composite regenerated fiber repair materials of acaudina molpadioidea collagen Download PDF

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Publication number
CN107158460A
CN107158460A CN201710405229.7A CN201710405229A CN107158460A CN 107158460 A CN107158460 A CN 107158460A CN 201710405229 A CN201710405229 A CN 201710405229A CN 107158460 A CN107158460 A CN 107158460A
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Prior art keywords
solution
preparation
film
repair materials
regenerated
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王吉鹏
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Hefei Create Technology Co Ltd
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Hefei Create Technology Co Ltd
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS 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
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/14—Macromolecular materials
    • A61L27/22—Polypeptides or derivatives thereof, e.g. degradation products
    • A61L27/24—Collagen
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS 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
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/14—Macromolecular materials
    • A61L27/20—Polysaccharides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS 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
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/14—Macromolecular materials
    • A61L27/22—Polypeptides or derivatives thereof, e.g. degradation products
    • A61L27/227—Other specific proteins or polypeptides not covered by A61L27/222, A61L27/225 or A61L27/24
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS 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
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/54—Biologically active materials, e.g. therapeutic substances
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS 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
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/56—Porous materials, e.g. foams or sponges
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS 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
    • A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
    • A61L27/50—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
    • A61L27/58—Materials at least partially resorbable by the body
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0015—Electro-spinning characterised by the initial state of the material
    • D01D5/003—Electro-spinning characterised by the initial state of the material the material being a polymer solution or dispersion
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0069—Electro-spinning characterised by the electro-spinning apparatus characterised by the spinning section, e.g. capillary tube, protrusion or pin
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0076—Electro-spinning characterised by the electro-spinning apparatus characterised by the collecting device, e.g. drum, wheel, endless belt, plate or grid
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/0007—Electro-spinning
    • D01D5/0061—Electro-spinning characterised by the electro-spinning apparatus
    • D01D5/0092—Electro-spinning characterised by the electro-spinning apparatus characterised by the electrical field, e.g. combined with a magnetic fields, using biased or alternating fields
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
    • D04H1/4382—Stretched reticular film fibres; Composite fibres; Mixed fibres; Ultrafine fibres; Fibres for artificial leather
    • D—TEXTILES; PAPER
    • D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
    • D04H1/72—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged
    • D04H1/728—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being randomly arranged by electro-spinning
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
    • A61L2300/23—Carbohydrates
    • A61L2300/232—Monosaccharides, disaccharides, polysaccharides, lipopolysaccharides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
    • A61L2300/252—Polypeptides, proteins, e.g. glycoproteins, lipoproteins, cytokines
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/412—Tissue-regenerating or healing or proliferative agents
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS 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
    • A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/60—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a special physical form
    • A61L2300/602—Type of release, e.g. controlled, sustained, slow
    • A61L2300/604—Biodegradation

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  • Health & Medical Sciences (AREA)
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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Veterinary Medicine (AREA)
  • Animal Behavior & Ethology (AREA)
  • Textile Engineering (AREA)
  • Dermatology (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Transplantation (AREA)
  • Epidemiology (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Biophysics (AREA)
  • Artificial Filaments (AREA)

Abstract

A kind of preparation method of the composite regenerated fiber repair materials of acaudina molpadioidea collagen, belongs to tissue renovation material preparing technical field, including：Repair materials are made in the preparation of acaudina molpadioidea collagen, the preparation of soybean protein isolate solution, the preparation of regenerated cellulose spinning solution, electrostatic spinning.Repair materials produced by the present invention have good anti-microbial property, mechanical performance, tissue repair performance and drug attachment.

Description

A kind of preparation method of the composite regenerated fiber repair materials of acaudina molpadioidea collagen
Technical field
The invention belongs to tissue renovation material preparing technical field, more particularly to a kind of acaudina molpadioidea collagen are composite regenerated The preparation method of fiber repair materials.
Background technology
Cellulose as natural biopolymer, with biodegradability, the physics of biocompatibility and uniqueness, Chemistry and mechanical performance, it has also become the study hotspot in new bio medical material field.And prior art is fine using regeneration mostly Dimension element is blended with other materials, and freeze-drying prepares composite membrane, using be combined made from the method film uniformity, stability compared with Difference, and tissue repairing ability and drug attachment need further raising.
The content of the invention
In order to solve problems of the prior art, the invention provides it is a kind of with good tissue repairing ability and The preparation method of the composite regenerated fiber repair materials of acaudina molpadioidea collagen of drug attachment.
The present invention uses following technical scheme：
A kind of preparation method of the composite regenerated fiber repair materials of acaudina molpadioidea collagen, comprises the following steps：
Step one：Fresh Haiti melon umbrella portion is cleaned with running water flowing water, shreds, is put into beaker, quality is added dense The 10 times of v aqueous sodium solutions spent for 9% take out natural air drying after soaking Haiti melon, stirring immersion 24h；
Step 2：Haiti melon 50g after being handled through step one is weighed, 100mL deionized waters, 2400U/g protease is added, It is 7.5 to carry out enzyme digestion reaction 3h, pH in 20 DEG C, and enzymolysis product is freeze-dried, and obtains acaudina molpadioidea collagen；
Step 3：2.5g soybean protein isolates are weighed, 50mL deionized waters and 1mL glycerine are measured in beaker, mixing is equal It is even, soybean protein isolate is added thereto while stirring, beaker is placed in constant temperature blender with magnetic force, temperature is transferred to 45 DEG C, to Mixed solution and dripping 1mol/L NaOH, the pH of solution is adjusted to 10, the glycerine of mass percent 2% is added, stirs Mix and 90 DEG C of continuation stirring 0.5h are warming up to after 3h, film liquid is made into, will be poured on into film liquid on glass plate, horizontal workbench is placed in On face, natural film forming at room temperature；
Step 4：Film made from step 3 is added in acetone, the solution of mass concentration 5% is made, under agitation slowly The acetic anhydride of mass percent 1% is added, pH controls take supernatant in 7-8,55 DEG C of reaction 1h after centrifugation, ultrasonically treated 20min, is made soybean protein isolate solution；
Step 5：Silk cocoon is removed into pupa, the mass concentration boiled is inserted in 0.5% aqueous sodium carbonate, bath raio is 1: 50, silk cocoon surface silk gum is removed, will pull out and wring out into thread silk cocoon, after repeating aforesaid operations once, use deionization Water is cleaned, and degumming fibroin is obtained after air-drying；
Step 6：By CaCl2It is dissolved under room temperature state in formic acid, stirs 30min, it is 5wt.%'s that concentration, which is made, CaCl2- FA solution, is then dissolved in CaCl by degumming fibroin2In-FA solution, magnetic agitation 3h obtains regenerated silk fibroin molten Liquid, drying and forming-film, soaks 3h, re-dry obtains regenerated silk fibroin film, by regenerated silk egg by film with deionized water at room temperature Tunica albuginea is secondary under room temperature state to be dissolved in formic acid, and bath raio is 1:10, dissolution time is 2h, obtains regenerated silk fibroin spinning Liquid；
Step 7：Cotton linter 5g is taken, is dissolved in formic acid, the cellulose solution of mass concentration 4% is configured to；
Step 8：By regenerated silk fibroin spinning solution and cellulose solution by weight 4:1 is well mixed to obtain regenerated fiber Plain spinning solution；
Step 9：By acaudina molpadioidea collagen, soybean protein isolate solution, regenerated cellulose spinning solution in mass ratio 3:5: 19 are well mixed, and it are disperseed using ultrasonic oscillation, magnetic agitation 1h under the conditions of 50 DEG C, then continue to stir at room temperature 8h, obtains viscous solution and is placed in the medical needle tubing being connected with high-pressure installation, and repair materials are made by electrostatic spinning, and height press-fits Voltage is put for 20kV, spinning flow 2ml/h, obtained material is placed in the ethanol of volumetric concentration 75% and soaks 30min, at 40 DEG C Lower vacuum drying.
It is preferred that, the capacity of the medical needle tubing described in step 9 is 20ml.
It is preferred that, the syringe needle of the medical needle tubing described in step 9 is fixed at electrostatic spinning receiver board 20cm.
It is preferred that, the syringe needle internal diameter of the medical needle tubing described in step 9 is 0.41mm.
The beneficial effects of the present invention are：
1) hydrophilic radicals, Er Qieyou such as multiple amino, carboxyl and hydroxyl are contained in the peptide chain of acaudina molpadioidea collagen polypeptide It is small in its molecular weight, there is good compatibility with skin, cuticula can be entered, not only with the water absorbing capacity for maintaining skin, also With tissue repair function.
2) soybean yields is very high, soybean protein isolate aboundresources, and nutritious, and machinability is strong, is made of it Biocompatibility it is good, low-carbon environment-friendly is a kind of raw material of good composite.Soybean protein isolate can with it is a variety of High molecular polymer is blended, and prepares soybean fiber, and these soybean fibers have a good mechanical performance, light specific gravity, Intensity is high, and Moisture absorption ＆ moisture conductivity is good.
3) fibroin albumen has good antibiotic property, biocompatibility and tissue repairing ability.
4) cellulose has good biocompatibility, degradability and excellent mechanical performance.
5) cellulose can improve the mechanical performance of material, and fibroin albumen can improve materials microstructure repair ability.
6) material prepared using electrostatic spinning technique, is further increased the porosity of material, is conducive to the attached of medicine .
Embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1
A kind of preparation method of the composite regenerated fiber repair materials of acaudina molpadioidea collagen, comprises the following steps：
Step one：Fresh Haiti melon umbrella portion is cleaned with running water flowing water, shreds, is put into beaker, quality is added dense The 10 times of v aqueous sodium solutions spent for 9% take out natural air drying after soaking Haiti melon, stirring immersion 24h；
Step 2：Haiti melon 50g after being handled through step one is weighed, 100mL deionized waters, 2400U/g protease is added, It is 7.5 to carry out enzyme digestion reaction 3h, pH in 20 DEG C, and enzymolysis product is freeze-dried, and obtains acaudina molpadioidea collagen；
Step 3：2.5g soybean protein isolates are weighed, 50mL deionized waters and 1mL glycerine are measured in beaker, mixing is equal It is even, soybean protein isolate is added thereto while stirring, beaker is placed in constant temperature blender with magnetic force, temperature is transferred to 45 DEG C, to Mixed solution and dripping 1mol/L NaOH, the pH of solution is adjusted to 10, the glycerine of mass percent 2% is added, stirs Mix and 90 DEG C of continuation stirring 0.5h are warming up to after 3h, film liquid is made into, will be poured on into film liquid on glass plate, horizontal workbench is placed in On face, natural film forming at room temperature；
Step 4：Film made from step 3 is added in acetone, the solution of mass concentration 5% is made, under agitation slowly The acetic anhydride of mass percent 1% is added, pH controls take supernatant in 7-8,55 DEG C of reaction 1h after centrifugation, ultrasonically treated 20min, is made soybean protein isolate solution；
Step 5：Silk cocoon is removed into pupa, the mass concentration boiled is inserted in 0.5% aqueous sodium carbonate, bath raio is 1: 50, silk cocoon surface silk gum is removed, will pull out and wring out into thread silk cocoon, after repeating aforesaid operations once, use deionization Water is cleaned, and degumming fibroin is obtained after air-drying；
Step 6：By CaCl2It is dissolved under room temperature state in formic acid, stirs 30min, it is 5wt.%'s that concentration, which is made, CaCl2- FA solution, is then dissolved in CaCl by degumming fibroin2In-FA solution, magnetic agitation 3h obtains regenerated silk fibroin molten Liquid, drying and forming-film, soaks 3h, re-dry obtains regenerated silk fibroin film, by regenerated silk egg by film with deionized water at room temperature Tunica albuginea is secondary under room temperature state to be dissolved in formic acid, and bath raio is 1:10, dissolution time is 2h, obtains regenerated silk fibroin spinning Liquid；
Step 7：Cotton linter 5g is taken, is dissolved in formic acid, the cellulose solution of mass concentration 4% is configured to；
Step 8：By regenerated silk fibroin spinning solution and cellulose solution by weight 4:1 is well mixed to obtain regenerated fiber Plain spinning solution；
Step 9：By acaudina molpadioidea collagen, soybean protein isolate solution, regenerated cellulose spinning solution in mass ratio 3:5: 19 are well mixed, and it are disperseed using ultrasonic oscillation, magnetic agitation 1h under the conditions of 50 DEG C, then continue to stir at room temperature 8h, obtains viscous solution and is placed in the medical needle tubing being connected with high-pressure installation, and repair materials are made by electrostatic spinning, and height press-fits Voltage is put for 20kV, spinning flow 2ml/h, obtained material is placed in the ethanol of volumetric concentration 75% and soaks 30min, at 40 DEG C Lower vacuum drying.
The capacity of medical needle tubing described in step 9 is 20ml, and the syringe needle of described medical needle tubing is fixed on apart from electrostatic At spinning receiver board 20cm, syringe needle internal diameter is 0.41mm.

Claims (4)

1. a kind of preparation method of the composite regenerated fiber repair materials of acaudina molpadioidea collagen, it is characterised in that including following step Suddenly：
Step one：Fresh Haiti melon umbrella portion is cleaned with running water flowing water, shreds, is put into beaker, adding mass concentration is 9% 10 times of v aqueous sodium solutions take out natural air drying after soaking Haiti melon, stirring immersion 24h；
Step 2：Haiti melon 50g after being handled through step one is weighed, 100mL deionized waters, 2400U/g protease are added, in 20 DEG C carry out enzyme digestion reaction 3h, pH be 7.5, enzymolysis product is freeze-dried, and obtains acaudina molpadioidea collagen；
Step 3：2.5g soybean protein isolates are weighed, 50mL deionized waters and 1mL glycerine are measured in beaker, are well mixed, side Soybean protein isolate is added thereto by stirring side, beaker is placed in constant temperature blender with magnetic force, temperature is transferred to 45 DEG C, molten to mixing 1mol/L NaOH is added dropwise in liquid, the pH of solution is adjusted to 10, adds after the glycerine of mass percent 2%, stirring 3h It is warming up to 90 DEG C to continue to stir 0.5h, film liquid is made into, will be poured on into film liquid on glass plate, is placed on horizontal work top, Natural film forming at room temperature；
Step 4：Film made from step 3 is added in acetone, the solution of mass concentration 5% is made, is added slowly with stirring The acetic anhydride of mass percent 1%, pH controls take supernatant in 7-8,55 DEG C of reaction 1h after centrifugation, ultrasonically treated 20min, is made soybean protein isolate solution；
Step 5：Silk cocoon is removed into pupa, the mass concentration boiled is inserted in 0.5% aqueous sodium carbonate, bath raio is 1:50, remove Silk cocoon surface silk gum is removed, will pull out and wring out into thread silk cocoon, after repeating aforesaid operations once, be washed with deionized water Only, degumming fibroin is obtained after air-drying；
Step 6：By CaCl2It is dissolved under room temperature state in formic acid, stirs 30min, the CaCl that concentration is 5wt.% is made2- FA solution, is then dissolved in CaCl by degumming fibroin2In-FA solution, magnetic agitation 3h obtains regenerated silk fibroin solution, room The lower drying and forming-film of temperature, soaks 3h, re-dry obtains regenerated silk fibroin film, by regenerated silk fibroin film by film with deionized water Secondary under room temperature state to be dissolved in formic acid, bath raio is 1:10, dissolution time is 2h, obtains regenerated silk fibroin spinning solution；
Step 7：Cotton linter 5g is taken, is dissolved in formic acid, the cellulose solution of mass concentration 4% is configured to；
Step 8：By regenerated silk fibroin spinning solution and cellulose solution by weight 4:1 is well mixed that regenerated cellulose is spun Silk liquid；
Step 9：By acaudina molpadioidea collagen, soybean protein isolate solution, regenerated cellulose spinning solution in mass ratio 3:5:19 mix Close uniform, it disperseed using ultrasonic oscillation, magnetic agitation 1h under the conditions of 50 DEG C, then continue to stir 8h at room temperature, Obtain viscous solution to be placed in the medical needle tubing being connected with high-pressure installation, repair materials, high-pressure installation are made by electrostatic spinning Voltage is 20kV, spinning flow 2ml/h, and obtained material is placed in the ethanol of volumetric concentration 75% and soaks 30min, at 40 DEG C Vacuum drying.
2. a kind of preparation method of the composite regenerated fiber repair materials of acaudina molpadioidea collagen according to claim 1, its It is characterised by：The capacity of medical needle tubing described in step 9 is 20ml.
3. a kind of preparation method of the composite regenerated fiber repair materials of acaudina molpadioidea collagen according to claim 1, its It is characterised by：The syringe needle of medical needle tubing described in step 9 is fixed at electrostatic spinning receiver board 20cm.
4. a kind of preparation method of the composite regenerated fiber repair materials of acaudina molpadioidea collagen according to claim 1, its It is characterised by：The syringe needle internal diameter of medical needle tubing described in step 9 is 0.41mm.
CN201710405229.7A 2017-06-01 2017-06-01 A kind of preparation method of the composite regenerated fiber repair materials of acaudina molpadioidea collagen Pending CN107158460A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103341209A (en) * 2013-07-08 2013-10-09 苏州大学 Silk fibroin nanofiber membrane and preparation method thereof
CN105400856A (en) * 2015-12-01 2016-03-16 雷春生 Extraction method of acaudina molpadioides collagen

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103341209A (en) * 2013-07-08 2013-10-09 苏州大学 Silk fibroin nanofiber membrane and preparation method thereof
CN105400856A (en) * 2015-12-01 2016-03-16 雷春生 Extraction method of acaudina molpadioides collagen

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