CN107261196A - A kind of antibacterial fibroin material and preparation method thereof - Google Patents
A kind of antibacterial fibroin material and preparation method thereof Download PDFInfo
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- CN107261196A CN107261196A CN201710341640.2A CN201710341640A CN107261196A CN 107261196 A CN107261196 A CN 107261196A CN 201710341640 A CN201710341640 A CN 201710341640A CN 107261196 A CN107261196 A CN 107261196A
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- fibroin
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- berberine
- albumen
- silk
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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
- A61L17/00—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
- A61L17/14—Post-treatment to improve physical properties
- A61L17/145—Coating
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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
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/20—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing organic materials
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- 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
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/32—Proteins, polypeptides; Degradation products or derivatives thereof, e.g. albumin, collagen, fibrin, gelatin
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- 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
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/44—Medicaments
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- 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
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
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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
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/64—Use of materials characterised by their function or physical properties specially adapted to be resorbable inside the body
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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
- A61L17/00—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
- A61L17/005—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters containing a biologically active substance, e.g. a medicament or a biocide
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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
- A61L17/00—Materials for surgical sutures or for ligaturing blood vessels ; Materials for prostheses or catheters
- A61L17/06—At least partially resorbable materials
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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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/04—Macromolecular materials
- A61L31/043—Proteins; Polypeptides; Degradation products thereof
- A61L31/047—Other specific proteins or polypeptides not covered by A61L31/044 - A61L31/046
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- 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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L31/148—Materials at least partially resorbable by the body
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- A—HUMAN NECESSITIES
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- 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
- A61L31/00—Materials for other surgical articles, e.g. stents, stent-grafts, shunts, surgical drapes, guide wires, materials for adhesion prevention, occluding devices, surgical gloves, tissue fixation devices
- A61L31/14—Materials characterised by their function or physical properties, e.g. injectable or lubricating compositions, shape-memory materials, surface modified materials
- A61L31/16—Biologically active materials, e.g. therapeutic substances
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- 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
- A61L2300/204—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials with nitrogen-containing functional groups, e.g. aminoxides, nitriles, guanidines
- A61L2300/208—Quaternary ammonium compounds
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- A—HUMAN NECESSITIES
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- 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
- A61L2300/236—Glycosaminoglycans, e.g. heparin, hyaluronic acid, chondroitin
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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
- 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
- A61L2300/30—Compounds of undetermined constitution extracted from natural sources, e.g. Aloe Vera
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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
- 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
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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
- 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
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- 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
Abstract
The invention discloses a kind of antibacterial fibroin material and preparation method thereof, the component of the antibacterial fibroin material includes fibroin albumen and berberine, and berberine is directly be combined with each other with fibroin albumen by intermolecular force.The step of this method, includes preparing silk fibroin protein solution, prepares fibroin albumen composite material, prepares the antibacterial fibroin material through steam treatment, and prepare the fibroin albumen composite material modified by glycerine.The antibacterial fibroin material of the present invention, by carrying out steam treatment and glycerine modification to fibroin albumen, to change fibroin albumen secondary structure, antibacterials berberine may be homogenously dispersed in fibroin albumen molecular absorbable material, being swelled and degrading with fibroin albumen molecular absorbable material, antibacterials slowly discharge, therefore there is the anti-microbial property of long-acting slow-release, the 3 days high-risk periods occurred especially for tissue infection, it is possible to effectively prevent wound infection, and promote healing, it can be coating material, biological dressing or medicine equipment provide new solution.
Description
Technical field
The invention belongs to biomedical materials field, it is related to a kind of antibiotic material in medical use and preparation method thereof, and in particular to one
Plant antibacterial fibroin material and preparation method thereof.
Background technology
Suture is most common surgery portable Biomedical Textiles, is widely used in all kinds of surgical operations
In, to sew up a wound, be coupled tissue and vascular ligation in terms of.However, the suture of braiding structure is in gap and single fiber
Easily adsorbed and harbor bacteria between dimension, each of which increases the incidence of surgical site infection.Surgical site infection not only influences
Wound healing, pain is brought to patient, extends the hospital stays, while also increasing the financial burden of patient and society, even
It is also the major reason for causing postoperative complications or even ultimately resulting in death.Suture is the passage that bacterium enters operative incision,
If suture has antibiotic property, can not only prevent bacterial adsorption from growing, moreover it is possible to by bacterial resistant within the specific limits not with
Wound contact, so as to reduce the incidence of surgical site infection.Therefore need to develop that a kind of histocompatbility is good, antibacterial effect
Really good antimicrobial coating material.
Silkworm silk is the natural animal albumen for being synthesized and being secreted by silkworm, and wide material sources, fibroin albumen is master in silk
The part wanted, accounts for the 70%~80% of silk quality, and remaining main component is sericin and carbohydrate etc..In reel silk from cocoons
In wire process, it is possible to achieve silk gum is removed, so as to obtain fibroin.Fibroin albumen has good compatibility, can by 20 kinds of human bodies
The amino acid composition of absorption, final catabolite is amino acid or small peptide molecule, is easily absorbed or is swallowed by cell, will not cause bright
Aobvious immune response.In China's clinical medicine, using boiled silk as operation suture thread, the history of existing decades.
The U.S., the unscoured silk fibroin again obtained by natural silk degumming, by food and medicine Surveillance Authority of the U.S.（US
Food and Drug Administration, FDA）It is approved as the bio-medical material that can be used in human body.Therefore, fibroin egg
White research and application in biomedical sector, increasingly causes interest and the attention of domestic and international researcher.Lot of documents table
Bright fibroin material can be also used for the sustained release agent of medicine, and its porous netted membrane structure inherently has extraordinary suction
The functions such as attached, sustained release.It recent studies have shown that, face coat is carried out to vancomycin and polycaprolactone by using fibroin albumen,
The release of vancomycin can effectively be extended and improve the anti-infection effect of vancomycin.Therefore, with other biological material phase
Than fibroin albumen is a kind of preferable carrier material.
At present, substantial amounts of antibiotic and synthetic drug are widely used in coating suture, such as triclosan, chlorohexidene, salt
Sour tetracycline etc., important function has been played in preventing and treating in terms of infection caused by suture.For example：（1）Using PCL
（Polycaprolactone）Carry antibacterials lavo-ofloxacin hydrochloride and prepare antimicrobial coating solution, coating is carried out to the silk thread of braiding, obtained
The suture with good antibacterial and sustained release performance is arrived（China Patent Publication No. CN204275113U）.But, it is international
On have strict management to the uses of antibioticses, it is to avoid abuse of antibiotics, to reduce the appearance of antibody-resistant bacterium；（2）Argentiferous
The antiseptic coating suture of ion（China Patent Publication No. CN1940168A and publication number CN102726448A）；However, by
In silver ion antimicrobial agent in preparation process, easily occur oxidation reaction and decline anti-microbial property, and the possibility of silver ion is deposited
In unstability, it is unfavorable for the health of human body；（3）Chinese herbal antibacterial agent coating suture（China Patent Publication No.
CN101584878A and publication number CN101584595A）, using the antibiotic property of Chinese medicine, have with Chinese medicine dipping or coating suture
There is antibiotic property, but the antibacterials slow-release time of antibacterial medical suture made from the technique is short, antibacterial effect is not obvious.
The content of the invention
It is an object of the invention to provide a kind of fibroin albumen material containing natural antibacterial agent, with continuation anti-microbial property
Material and preparation method thereof, a kind of new solution is provided for coating material, biological dressing or medical device industry.
To reach above-mentioned technical purpose and effect, the present invention is achieved through the following technical solutions：
A kind of antibacterial fibroin material, its component include fibroin albumen and antibacterials, the antibacterials directly with it is described
Fibroin albumen is be combined with each other by intermolecular force.
Further, the good medicine of the Antimicrobial drug choice clinical effectiveness, it is desirable to appropriate water-soluble, it is such as yellow
Lian Su, chitosan, chitin, aloe, radix scutellariae or honeysuckle etc..
It is preferred that, the mass ratio of the berberine and the fibroin albumen is 2~10/100.
A kind of preparation method of antibacterial fibroin material, comprises the following steps：
（1）It is 5~10% to prepare concentration（w/v）Silk fibroin protein solution；
（2）Prepare fibroin albumen composite material；The berberine that concentration is 3~6 mg/ml is added in deionized water, makes berberine
Dissolving is in deionized water；Then with the obtained deionized water dilution step for carrying berberine（1）In obtained fibroin albumen
Solution, makes the concentration of silk fibroin protein solution reach 5~10%（w/v）；Diluted silk fibroin protein solution is with being dissolved in deionization
After berberine in water is sufficiently mixed uniformly in proportion, the mixed solution of fibroin albumen and berberine is formed；Finally this is mixed
Solution is placed in fume hood and air-dried, and obtains antibacterial fibroin material；
（3）To step（2）Obtained antibacterial fibroin material carries out steam treatment, and processing time is 5~10 hours, processing
50~70 °C of temperature, obtains the antibacterial fibroin material after steam treatment；
（4）Prepare the fibroin albumen composite material of glycerine modification；The coptis that concentration is 3~6 mg/ml is added in deionized water
Element, makes berberine dissolving in deionized water；Then with the obtained deionized water dilution step for carrying berberine（1）In be made
Silk fibroin protein solution, the concentration of silk fibroin protein solution is reached 5~10%（w/v）；Add in silk fibroin protein solution after dilution
Enter glycerine, and stir, the glycerine accounts for 25~35% of fibroin albumen gross mass in silk fibroin protein solution（w/w）；Agitated
After berberine of the silk fibroin protein solution with dissolving in deionized water is sufficiently mixed uniformly in proportion, fibroin albumen, the coptis are formed
The mixed solution of element and glycerine；The mixed solution finally is placed in into fume hood to air-dry, the antibacterial fibroin modified by glycerine is obtained
Protein material.
Further, step（1）In the specific preparation method of silk fibroin protein solution be：Using silk, taken off respectively
After glue and dissolving, it is poured into bag filter, is then dialysed with deionized water, it is 5~10% that finally centrifugation, which obtains concentration,（w/v）'s
Silk fibroin protein solution.
Further, step（2）And step（4）In, the mass ratio of berberine and fibroin albumen in silk fibroin protein solution is 2
~10/100.
Further, step（2）And step（4）The curing of middle mixed solution for be placed in air dry cure in fume hood,
Oven for drying solidification, wet spinning solidification, electrostatic spinning solidification or the solidification of electrostatic differential method.
It is furthermore preferred that the mass ratio of berberine and fibroin albumen in silk fibroin protein solution is 5~10/100.
It is an advantage of the invention that：
1st, berberine is a kind of important isoquinoline alkaloid extracted from the medicinal plants such as the coptis, golden cypress, barberry, a kind of
Natural antibacterial agent, has the advantages that small toxicity, environmental protection, wide material sources, and berberine shows multiple pharmacological effect, including anti-
Bacterium, hypotensive, anti-inflammatory, hypoglycemic etc..Berberine can be carried by fibroin material of the present invention, directly played and killed
Bacterium or bacteria resistance function.
2nd, antibacterial fibroin material prepared by the present invention, by being repaiied to fibroin albumen progress steam treatment and glycerine
Decorations, to change fibroin albumen secondary structure, antibacterials berberine is dispersed in fibroin albumen high polymer material, with silk
Fibroin high polymer material being swelled and degrades, and antibacterials slowly discharge, therefore the antibacterial effect with long-acting slow-release.
3rd, the antibacterial fibroin material modified and handled by glycerine, flat using antibacterial GB/T20944.1-2007 agar
Ware diffusion method is to Gram-positive S staphylococcus（S.aureus）And Gram-E. coli（E.coli）Carry out
Antibacterial contrast test, antibacterial fibroin material can kill bacterium, and Durability of antimicrobial effect can be maintained more than 3~4 days, especially to group
3 days high-risk periods that infection occurs are knitted, are possible to effectively prevent different tissues wound infection, and promotion organization heals.
4th, the antibacterial fibroin material that prepared by the present invention is widely used, can be coating material, biological dressing or Medical treatment device
Tool provides new solution.
Described above, is only the general introduction of technical solution of the present invention, in order to better understand the technological means of the present invention,
And can be practiced according to the content of specification, below with the better embodiment of the present invention, and coordinate accompanying drawing to describe in detail.This
The embodiment of invention is shown in detail by following examples and its accompanying drawing.
Brief description of the drawings
Accompanying drawing described herein is used for providing a further understanding of the present invention, constitutes the part of the application, this hair
Bright schematic description and description is used to explain the present invention, does not constitute inappropriate limitation of the present invention.In the accompanying drawings：
Fig. 1 is steam treatment antibacterial fibroin material described in the embodiment of the present invention 1 and example 2, according to antibacterial GB/
T20944.1-2007 agar plates diffusion method is carried out to Gram-positive S staphylococcus and Gram-E. coli
Antibacterial experiment result figure.
Fig. 2 is glycerine modified antimicrobial fibroin material described in the embodiment of the present invention 3 and example 4, according to antibacterial GB/
T20944.1-2007 agar plates diffusion method is carried out to Gram-positive S staphylococcus and Gram-E. coli
Antibacterial experiment result figure.
Fig. 3 is that antibacterial fibroin material continues to Gram-E. coli antibacterial described in embodiment of the present invention
Property experimental result picture.
Embodiment
Embodiment one
A kind of preparation method of antibacterial fibroin material is as follows, weighs the Na that 30g silkworms unscoured silk seethes with excitement in 12L2CO3
（0.02M）Degumming 30 minutes in the aqueous solution, then with deionized water rinsing, clean fibroin fiber is placed in fume hood
Natural air drying overnight.Weigh dried 25g fibroin fibers and be dissolved in 100ml LiBr（9.3M）In solution, in 60 °C of baking oven
Dissolving 4 hours, during which takes out slight wobble to ensure that dissolving is complete per hour.Take out solution and pour into bag filter（Molecular cut off
3500）In, dialyse 36 hours in deionized water, change a water within every 4 hours.Solution after dialysis in supercentrifuge with
9000 r/min are centrifuged twice, 20 minutes every time, to go the removal of impurity, are finally obtained silk fibroin protein solution, are placed in 4 °C of refrigerators
It is stand-by.Utilize the mass fraction for evaporating weight method measure silk protein solution.Operation is as follows：It is put into after weighing disk is numbered in baking oven
Dry 0.5 hour, weigh to obtain W0（g）, then add 1ml silk protein solutions in weighing disk, weigh to obtain W1（g）, it is placed in baking oven
Took out and weigh every 20 minutes after drying 6 hours, until weight no longer changes, now write down data for W2（g）, it is public according to calculating
Formula, concentration C（%）=（W2-W0）/（W1-W0）× 100%, calculate the ultimate density for obtaining silk protein solution.Obtain silk after purification
The fibroin aqueous solution, and the silk fibroin protein solution concentration after dialysis is adjusted to 5~10%（w/v）.
Berberine is dissolved in deionized water, silk fibroin protein solution is then added, in the berberine and silk fibroin protein solution
The mass ratio of fibroin albumen is 10/100, is poured into after being well mixed in polystyrene dishes, is put into dried overnight in fume hood, takes
Go out to carry out steam treatment 5~10 hours, treatment temperature is 50~70 °C, obtains the antibacterial fibroin albumen by steam treatment
Material.
Embodiment two
A kind of preparation method of antibacterial fibroin material is as follows, uses the method in embodiment 1 to prepare concentration for 5~10%（w/
v）Silk fibroin protein solution, berberine is dissolved in deionized water, silk fibroin protein solution is then added, the berberine and fibroin egg
The mass ratio of fibroin albumen is 5/100 in white solution, is poured into after being well mixed in polystyrene dishes, is put into fume hood overnight
Dry, then, carry out steam treatment 5~10 hours, treatment temperature is 50~70 °C, obtains the antibacterial by steam treatment
Fibroin material.
Shown in Figure 1, Fig. 1 is the antibacterial fibroin material Jing Guo steam treatment described in embodiment 1 and example 2,
According to antibacterial GB/T20944.1-2007 agar plates diffusion method to Gram-positive S staphylococcus（S. aureus）With
Gram-E. coli（E. coli）The antibacterial experiment result figure of progress；Wherein, the mass ratio of berberine and fibroin albumen
Respectively 10/100 with the samples of 5/,100 two kinds of different drugloading rates.The anti-bacterial result shows that drugloading rate is higher, and antibacterial effect is got over
Good, different doses all show good anti-microbial property.
Embodiment three
A kind of preparation method of antibacterial fibroin material, uses the method in embodiment one to prepare concentration for 5~10%（w/v）
Silk fibroin protein solution, fibroin albumen quality in glycerine, glycerine and silk fibroin protein solution is added into above-mentioned silk fibroin protein solution
Than for 25~35/100,5-15 minute are stood after stirring, the then addition berberine aqueous solution, the berberine and fibroin albumen
The mass ratio of fibroin albumen in solution is 10/100, is poured into after being well mixed in polystyrene dishes, is put into mistake in fume hood
Night is dried, and obtains the antibacterial fibroin material modified by glycerine.
Example IV
A kind of preparation method of antibacterial fibroin material is as follows, uses the method in embodiment 1 to prepare concentration for 5~10%（w/
v）Silk fibroin protein solution, fibroin protein in glycerine, glycerine and silk fibroin protein solution is added into above-mentioned silk fibroin protein solution
Amount is placed 10 minutes after stirring than being 25~35/100, then adds the berberine aqueous solution, the berberine and fibroin albumen
The mass ratio of fibroin albumen in solution is 5/100, is poured into after being well mixed in polystyrene dishes, is put into fume hood overnight
Dry, obtain the antibacterial fibroin material modified by glycerine.
Shown in Figure 2, Fig. 2 is the antibacterial fibroin material modified described in embodiment 3 and example 4 by glycerine, is pressed
According to antibacterial GB/T20944.1-2007 agar plates diffusion method to Gram-positive S staphylococcus（S. aureus）And leather
Lan Shi negative bacteriums（E. coli）Carry out the result figure of antibacterial experiment；Wherein, the quality score of berberine and fibroin albumen
Not Wei 10/100 with the samples of 5/,100 two kinds of different drugloading rates.The anti-bacterial result shows that drugloading rate is higher, and antibacterial effect is better,
Different doses all show good anti-microbial property.
Shown in Figure 3, Fig. 3 is antibacterial fibroin material described in embodiment to Gram-E. coli
Antibacterial continuation experimental result picture.It can be seen that the antibacterial duration is more than 3~4 days, by steam treatment
Than the good anti-bacterial effect for the antibacterial fibroin material modified by glycerine, the antibacterial duration is longer；And drugloading rate is got over
Height, the antibacterial duration is longer.
In summary, the present invention proposes a kind of antibacterial fibroin material and preparation method thereof：By hydrolyzing and being blended
Method, natural antibacterial medicine berberine is mounted in fibroin albumen molecular absorbable material；By entering to fibroin albumen
Water-filling steam treated and glycerine modification, change the secondary structure of fibroin albumen so that natural antibacterial medicine is with fibroin albumen
The degraded of high polymer material and slowly discharge, so as to reach the effect of sustained anti-microbial.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Present disclosure can be understood and implemented according to this, it is not intended to limit the scope of the present invention.It is all main according to the present invention
The modification for wanting the Spirit Essence of technical scheme to be done, should all be included within the scope of the present invention.
Claims (8)
1. a kind of antibacterial fibroin material, its component includes fibroin albumen, it is characterised in that also include having water in its component
The antibacterials of dissolubility, the antibacterials are berberine, and the berberine is directly made with the fibroin albumen by intermolecular
Firmly it be combined with each other.
2. antibacterial fibroin material according to claim 1, it is characterised in that the berberine and the fibroin albumen
Mass ratio be 2~10/100.
3. antibacterial fibroin material according to claim 1, it is characterised in that the antibacterials also can be the coptis
Element, chitosan, chitin, aloe, radix scutellariae or honeysuckle.
4. a kind of preparation method of antibacterial fibroin material, it is characterised in that comprise the following steps：
（1）It is 5~10% to prepare concentration（w/v）Silk fibroin protein solution；
（2）Prepare fibroin albumen composite material；The berberine that concentration is 3~6 mg/ml is added in deionized water, makes berberine
Dissolving is in deionized water；Then with the obtained deionized water dilution step for carrying berberine（1）In obtained fibroin albumen
Solution, makes the concentration of silk fibroin protein solution reach 5~10%（w/v）；Diluted silk fibroin protein solution is with being dissolved in deionized water
In berberine be sufficiently mixed in proportion it is uniform after, form the mixed solution of fibroin albumen and berberine；It is finally that the mixing is molten
Liquid is placed in fume hood and air-dried, and obtains antibacterial fibroin material；
（3）To step（2）Obtained antibacterial fibroin material carries out steam treatment, and processing time is 5~10 hours, processing
50~70 °C of temperature, obtains the antibacterial fibroin material through steam treatment；
（4）Prepare the fibroin albumen composite material modified by glycerine；It is 3~6 mg/ml's to add concentration in deionized water
Berberine, makes berberine dissolving in deionized water；Then with the obtained deionized water dilution step for carrying berberine（1）In
Obtained silk fibroin protein solution, makes the concentration of silk fibroin protein solution reach 5~10%（w/v）；Silk fibroin protein solution toward after dilution
Middle addition glycerine, and stir, the glycerine accounts for 25~35% of fibroin albumen gross mass in silk fibroin protein solution（w/w）；Through stirring
After berberine of the silk fibroin protein solution mixed with dissolving in deionized water is sufficiently mixed uniformly in proportion, formation fibroin albumen,
The mixed solution of berberine and glycerine；The mixed solution finally is placed in into fume hood to air-dry, the antibacterial modified by glycerine is obtained
Fibroin material.
5. the preparation method of antibacterial fibroin material according to claim 4, it is characterised in that step（1）In silk
The specific preparation method of fibroin solution is：Using silk, carry out after degumming and dissolving, be poured into bag filter, then respectively
Dialysed with deionized water, it is 5~10% that finally centrifugation, which obtains concentration,（w/v）Silk fibroin protein solution.
6. the preparation method of antibacterial fibroin material according to claim 4, it is characterised in that step（2）And step
（4）In, the mass ratio of berberine and fibroin albumen in silk fibroin protein solution is 2~10/100.
7. the preparation method of antibacterial fibroin material according to claim 4, it is characterised in that step（2）And step
（4）The curing of middle mixed solution solidifies to be placed in air dry cure in fume hood, oven for drying, wet spinning solidifies, electrostatic
Spinning solidification or the solidification of electrostatic differential method.
8. the preparation method of antibacterial fibroin material according to claim 6, it is characterised in that berberine and fibroin egg
The mass ratio of fibroin albumen is 5~10/100 in white solution.
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| CN108316018A (en) * | 2018-03-15 | 2018-07-24 | 南通纺织丝绸产业技术研究院 | A kind of preparation method of fibroin albumen/chitosan functional solution |
| CN108904869A (en) * | 2018-07-20 | 2018-11-30 | 南通纺织丝绸产业技术研究院 | A kind of suture and preparation method thereof with natural antibacterial drug slow release function |
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| CN115350318A (en) * | 2022-07-22 | 2022-11-18 | 上海健康医学院 | Chitosan/fibroin nanofiber drug-loaded multilayer film and preparation method thereof |
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