CN101352580A - Method for preparing antimicrobial type epidermis repair material - Google Patents
Method for preparing antimicrobial type epidermis repair material Download PDFInfo
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- CN101352580A CN101352580A CNA2008100717413A CN200810071741A CN101352580A CN 101352580 A CN101352580 A CN 101352580A CN A2008100717413 A CNA2008100717413 A CN A2008100717413A CN 200810071741 A CN200810071741 A CN 200810071741A CN 101352580 A CN101352580 A CN 101352580A
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Abstract
The invention relates to a preparation method for an antibacterial epidermis repairing material, relating to a human body epidermis repairing material; the invention provides a preparation method for an antibacterial epidermis repairing material with antibacterial performance. The preparation method comprises the following steps: respectively dissolving collagen swelling solution and chitosan under acidic condition; respectively compounding collagen solution and chitosan solution according to weight percentage; adding an ag-series inorganic antibacterial agent to the chitosan solution, stirring and ultrasounding; mixing and stirring the mixture of the chitosan solution with antibacterial agent and the collagen solution so as to derive collagen/chitosan/antibacterial agent dispersion liquid; evenly spreading the collagen/chitosan/antibacterial agent dispersion liquid on a polyfluortetraethylene plate and drying; immersing with distilled water to separate the film and the polyfluortetraethylene plate; spreading the film on the surface of the polyfluortetraethylene plate once again and drying to derive collagen/chitosan/antibacterial agent complex film; immersing the collagen/chitosan/antibacterial agent complex film into a crosslinking agent to be cross-linked, washing and drying to derive the antibacterial epidermis repairing material.
Description
Technical field
The present invention relates to a kind of human epidermal repair materials, especially relate to a kind of preparation method of antimicrobial type epidermis repair material.
Background technology
Epidermis repair material is that a class is used for the medical dressing that various wounds and wound surface cover temporarily, and it can make wound exempt from the influence of bacterial infection and other foeign elements, has the effect of protection wound and wound surface.Therefore, seek ideal wound-surface cover and become both at home and abroad one of main direction of studying to all kinds of skin wound treatment.Collagen is the main component of extracellular matrix, has better biocompatibility than natural biologic materials such as albumin and gelatin, and helps adhesion, propagation and the differentiation of cell.The structure of chitosan is extremely similar to the intravital glycosaminoglycans of people, has good blood compatibility, degradability and antithrombotic.Can promote the synthetic of somatomedin and collagen, thereby quicken growth of fibroblasts.Chitosan can also improve the activity of macrophage, activates the immunization route that the host resists virus and bacterial infection.In addition, the adding of chitosan can also slow down the degradation speed of collagen.Therefore the composite membrane that utilizes the collagen-chitin preparation is the effective way that solves the wound covering problem.
Though chitosan has the effect of bacteria growing inhibiting, studies show that chitosan only just has antibiotic property under acid condition.In addition, the blend of chitosan and collagen has also limited the performance of chitosan anti-bacteria function, and amino cation easy because of the carboxyl in the collagen and chitosan generates polyelectrolyte or forms hydrogen bond, has reduced amino cationic antibacterial activity.Therefore, the wound surface that collagen-chitin dressing covers is easy to by bacterial invasion, and its antibacterial functions remains further to be improved.
Can cause the bacterial species of wound infection various, these antibacterials all have potential danger to wound and surrounding tissue thereof, reduce the most feasible approach of wound infection and use antibacterial exactly.Traditional antibacterial mainly is meant organic class antibacterial, mainly comprises alcohols, aldehydes, phenols, carboxylic acids, imidazoles and organic metal class etc.Though organic antibacterial agent has better anti-bacterial effect to fungus, its anti-bacterial effect is relatively poor, and heat stability is low, generally can only use at a lower temperature, and its decomposition or volatile matter also may cause certain harm to human body and environment.In addition, because the appearance of the extremely strong pathogenic bacteria of drug resistance in recent years makes the use of organic class antibacterial be restricted to a great extent.Therefore, using inorganic antiseptic replaces organic antibacterial agent imperative.Silver not only can be killed aerobe, anaerobe, gram negative bacteria, gram positive bacteria, yeast, fungus and virus ([14] Michael AA, George JV, Anthony EB.Antimicrobial properties of silver-containingwound dressings:a microcalorimetric study[J] .International Journal of Pharmaceutics, 2003,263:61-68:[15] Wright JB, Lam K, Hanson D, et al.Efficacy of topical silver against fungal bum wound pathogens[J] .Am JInf Cont, 1999,27:344-350; [16] lan AH, Paula D, Andrew PS.Assessment ofa silver-coated barrier dressing forpotential use with skin grafts on excised burns[J] .Burns, 2003,29:445-448.), and the effect of antiinflammatory in addition ([17] Demling RH, DeSanti L.Effects of silver on wound management[J] .Wounds, 2001,13:4-9.).
Summary of the invention
The object of the present invention is to provide a kind of preparation method with antimicrobial type epidermis repair material of anti-microbial property.
The present invention includes following steps:
1) under acid condition, dissolves collagen swelling solution and chitosan respectively, stir it is fully dissolved, be mixed with concentration by mass percentage respectively and be 0.2%～0.8% collagen solution and 0.2%～0.8% chitosan solution;
2) in chitosan solution, add 0.5%～7.5% silver base inorganic antibacterial agent by mass percentage, stir, ultrasonic;
3) with step 2) chitosan solution that is added with antibacterial that makes mixes stirring with collagen solution, promptly get collagen/chitosan/antibacterial dispersion liquid;
4) with collagen/chitosan/antibacterial dispersion liquid of making by 1～10cm
2The consumption of/g is evenly spread film, oven dry on polyfluortetraethylene plate;
5) with distilled water immersion film is separated with polyfluortetraethylene plate, once more film is laid on the polyfluortetraethylene plate surface, oven dry promptly gets collagen/chitosan/antibacterial composite membrane;
6) collagen/chitosan/antibacterial composite membrane is dipped in carries out crosslinkedly in the cross-linking agent, clean, oven dry promptly gets antimicrobial type epidermis repair material.
Silver base inorganic antibacterial agent can be silver-loaded zirconium phosphate, carry silver-colored salt of phosphoric acid, carry a kind of in silver-colored sodium hydroxide zirconium, the silver-loaded silica etc.
Be added with the chitosan solution of antibacterial by mass ratio: collagen solution is 1: (0.1～9).
Cross-linking agent can adopt glutaraldehyde or glycerol etc., and by mass percentage, the concentration of cross-linking agent is preferably 0.01%～10%, and the crosslinked time is preferably 1～24h, cleans and preferably uses washed with de-ionized water, the temperature of oven dry to be preferably 37 ℃.
Compare with the preparation method of existing epidermis repair material, because the antibiotic bactericide that the present invention adopts is compared with organic system antibacterial in the past, silver base inorganic antibacterial agent is that the silver ion that will have the high-efficiency antimicrobial ability is carried on the carrier of various inorganic natural or synthetic, thereby makes product have antibacterial effect.Characteristics such as that silver base inorganic antibacterial agent has is safe, has a broad antifungal spectrum, long action time, good heat resistance, not volatile and decomposition can overcome some common shortcomings of traditional organic antibacterial agent.Thereby use the stable material of physicochemical property to make, so its function can be not impaired because of processing, and solved the fast problem of import silver-based inorganic antibacterial agent migration velocity in the past.
Description of drawings
Fig. 1 is the influence (the antibiotic property assessment of collagen/chitosan/antibacterial composite membrane) of the antibacterial concentration of the embodiment of the invention 1 to the material antibiotic property.In Fig. 1, in same flat board, 1 of center is that sterilization filter paper is blank; Vertical two samples represent that HN-300 accounts for 10% (wt%) of composite membrane; The sample on the right represents that HN-300 accounts for 7.5% (wt%) of composite membrane; Following sample represents that HN-300 accounts for 5% (wt%) of composite membrane; The sample on the left side represents that HN-300 accounts for 2.5% (wt%) of composite membrane; 12h, 36h, 60h, 144h are incubation time.
Fig. 2 is the silver element release rate of collagen/chitosan/antibacterial composite membrane in PBS liquid of the embodiment of the invention 1 different HN-300 content.In Fig. 2, abscissa is time (day), and vertical coordinate is release rate (%); 2.5%, 5%, 7.5%, 10% is respectively HN-300 content in the composite membrane.
Fig. 3 contains the collagen of 10% (wt) FUMAT T200-4 for the glutaraldehyde cross-linking of the embodiment of the invention 2 variable concentrations: the degradation property of the composite membrane of chitosan=7: 3.In Fig. 3, abscissa is time (h), and vertical coordinate is degradation rate (%); 0.1%, 0.25%, 0.5%, 0.75%, 1%, 2.5% concentration that is respectively glutaraldehyde cross-linking liquid.
Fig. 4 is the electron scanning micrograph when the L292 cell is cultivated 4 days on the antimicrobial compound film surface of different content HN-300 in the embodiment of the invention 3.In Fig. 4,0%～10%, the mass percent of the HN-300 that adds in the composite membrane; A left side: * 200; Right: * 1000.
The specific embodiment
The invention will be further described below by embodiment.
Embodiment 1: antibacterial concentration is to the influence of material antibiotic property
Remove the infull collagen that terminal peptide obtains no antigen through enzyme digestion, acetic acid with 0.05M dissolves collagen swelling solution and chitosan respectively, being mixed with collagen solution and the concentration that concentration is 0.6% (wt) is the chitosan solution of 0.6% (wt), adding with phosphoric acid pick sodium crystal in chitosan solution then is the silver base inorganic antibacterial agent powder HN-300 of carrier, through stirring, ultrasonic, fully mix with 9: 1 mass ratio with chitosan solution behind the restir and obtain collagen/chitosan/HN-300 dispersion liquid, wherein the content of HN-300 is followed successively by 10%, 7.5%, 5%, 2.5% (wt), with the dispersion liquid that makes by 3cm
2/ g evenly spreads film on polyfluortetraethylene plate, place 37 ℃ of baking ovens to dry.With distilled water immersion film is separated with polyfluortetraethylene plate, once more composite membrane is laid on the plate surface and places 37 ℃ of baking oven oven dry promptly to get collagen/chitosan/HN-300 composite membrane.Estimate the influence of different content antibacterial to the composite membrane antibiotic property with the inhibition zone laboratory method, as shown in Figure 1, all samples have tangible inhibition zone appearance on every side except that blank.Each sample antibacterial circle diameter statistics is (referring to table 1: the antibacterial circle diameter testing result of embodiment 1 collagen/chitosan/antibacterial composite membrane) show, HN-300 content is that the antibacterial circle diameter around 2.5%～10% the composite membrane is compared with blank and had significance, and the antibacterial circle diameter of sample reduces with HN-300 concentration in the sample and reduces, and promptly the biocidal property of material weakens with the reduction of HN-300 concentration; Produce lixiviating solution in the composite membrane immersion PBS liquid with HN-300 content 2.5%～10%, the release rate of 1～7 day silver element as shown in Figure 2, this figure shows: through 24h, HN-300 content is that the release rate of silver element reaches 45% in 2.5% the composite membrane, show typical burst effect, and HN-300 content is that the release rate of silver element only reaches 12% in 10% the composite membrane, these phenomenons show, the burst effect at dispose procedure initial stage weakens with the increase of HN-300 content in the composite membrane, and the composite membrane that contains 2.5%HN-300 was through 7 days, the release rate of silver element only reaches 80%, so HN-300 content is that the release of silver element is a secular process in 2.5% the composite membrane, but the silver that 60h discharges later on, concentration is not enough to killing bacteria.In conjunction with as can be known, has lasting biocidal property in the time and the HN-300 addition of biological safety should be about 5% preferably at 144h to composite membrane leachate cytotoxicity assessment.
Table 1
Unit: millimeter
*: compare sample (P＜0.05) with significance with blank.mean±S.D.
Embodiment 2: crosslinker concentration is to the material degradation Effect on Performance
Remove the infull collagen that terminal peptide obtains no antigen through enzyme digestion, acetic acid with 0.5M dissolves collagen swelling solution and chitosan respectively, being mixed with collagen solution and the concentration that concentration is 0.8% (wt) is the chitosan solution of 0.8% (wt), adding with the zirconium phosphate in chitosan solution then is the silver base inorganic antibacterial agent powder FUMAT T200-4 of carrier, makes the content of FUMATT200-4 be 10% (wt).Obtain collagen/chitosan/FUMAT T200-4 dispersion liquid through stirring, fully mixing with 7: 3 mass ratio respectively with chitosan solution behind ultrasonic, the restir, obtain containing the collagen of 10% (wt) FUMATT200-4 after the drying: the composite membrane of chitosan=7: 3, crosslinked 12h obtains the different collagen/chitosan/FUMAT T200-4 composite membrane of the degree of cross linking in the glutaraldehyde water solution of 0.1%, 0.25%, 0.5%, 0.75%, 1% (w/w) respectively.As shown in Figure 3, the degradation resistant performance of crosslinked back composite membrane is significantly improved, at glutaraldehyde concentration is within 0.1%～1% scope, with this composite membrane of increase of glutaraldehyde concentration each the time phase the corresponding reduction of degradation rate, the stability that is composite membrane is good more, therefore can control the stability of this composite membrane by the concentration that changes glutaraldehyde according to concrete needs.
Embodiment 3: contain variable concentrations antibacterial composite membrane external biological safety evaluatio
Remove the infull collagen that terminal peptide obtains no antigen through enzyme digestion, acetic acid with 0.05M dissolves collagen swelling solution and chitosan respectively, being mixed with collagen solution and the concentration that concentration is 0.6% (wt) is the chitosan solution of 0.6% (wt), adding with phosphoric acid pick sodium crystal in chitosan solution then is the silver base inorganic antibacterial agent powder HN-300 of carrier, through stirring, ultrasonic, fully mix with 9: 1 mass ratio with chitosan solution behind the restir and obtain collagen/chitosan/HN-300 dispersion liquid, wherein the content of HN-300 is followed successively by 10%, 7.5%, 5%, 2.5% (wt), with the dispersion liquid that makes by 3cm
2/ g evenly spreads film on polyfluortetraethylene plate, place 37 ℃ of baking ovens to dry.With distilled water immersion film is separated with polyfluortetraethylene plate, once more composite membrane is laid on the plate surface and places 37 ℃ of baking oven oven dry promptly to get collagen/chitosan/HN-300 composite membrane.The l cell L929 (1 * 10 of plantation 1mL on each group composite membrane
4/ mL), 37 ℃ of following 5%CO
2Cultivate in the incubator, changed liquid once in per 2 days, after the continuous culture 4 days, (SEM) observes the cell on composite membrane surface with scanning electron microscope, as seen the HN-300 addition is that 10% composite membrane surface finds no the cell growth, and the HN-300 addition all has a large amount of cell growths on the composite membrane surface of 0%～7.5% (wt), and cell growth state is good, sees Fig. 4.
Embodiment 4
Under acid condition, dissolve collagen swelling solution and chitosan respectively, stir it is fully dissolved, be mixed with concentration by mass percentage respectively and be 0.2% collagen solution and 0.8% chitosan solution.In chitosan solution, add 1% silver-loaded zirconium phosphate by mass percentage, stir, ultrasonic.The chitosan solution that is added with antibacterial that makes is mixed stirring with collagen solution, promptly get collagen/chitosan/antibacterial dispersion liquid; Be added with the chitosan solution of antibacterial by mass ratio: collagen solution is 1: 1.5.With collagen/chitosan/antibacterial dispersion liquid of making by 3cm
2The consumption of/g is evenly spread film, oven dry on polyfluortetraethylene plate.With distilled water immersion film is separated with polyfluortetraethylene plate, once more film is laid on the polyfluortetraethylene plate surface, oven dry promptly gets collagen/chitosan/antibacterial composite membrane.Collagen/chitosan/antibacterial composite membrane is dipped in carries out crosslinked 10h in the cross-linking agent glutaraldehyde, clean,, promptly get antimicrobial type epidermis repair material 37 ℃ of oven dry down with ionized water.By mass percentage, the concentration of cross-linking agent is 0.1%.
Under acid condition, dissolve collagen swelling solution and chitosan respectively, stir it is fully dissolved, be mixed with concentration by mass percentage respectively and be 0.4% collagen solution and 0.20% chitosan solution.In chitosan solution, add 3% the silver-colored salt of phosphoric acid that carries by mass percentage, stir, ultrasonic.The chitosan solution that is added with antibacterial that makes is mixed stirring with collagen solution, promptly get collagen/chitosan/antibacterial dispersion liquid; Be added with the chitosan solution of antibacterial by mass ratio: collagen solution is 1: 3.With collagen/chitosan/antibacterial dispersion liquid of making by 1cm
2The consumption of/g is evenly spread film, oven dry on polyfluortetraethylene plate.With distilled water immersion film is separated with polyfluortetraethylene plate, once more film is laid on the polyfluortetraethylene plate surface, oven dry promptly gets collagen/chitosan/antibacterial composite membrane.Collagen/chitosan/antibacterial composite membrane is dipped in carries out crosslinked 15h in the cross-linking agent glutaraldehyde, clean,, promptly get antimicrobial type epidermis repair material 37 ℃ of oven dry down with ionized water.By mass percentage, the concentration of cross-linking agent is 2%.
Embodiment 6
Under acid condition, dissolve collagen swelling solution and chitosan respectively, stir it is fully dissolved, be mixed with concentration by mass percentage respectively and be 0.6% collagen solution and 0.4% chitosan solution.In chitosan solution, add 6% the silver-colored sodium hydroxide zirconium that carries by mass percentage, stir, ultrasonic.The chitosan solution that is added with antibacterial that makes is mixed stirring with collagen solution, promptly get collagen/chitosan/antibacterial dispersion liquid; Be added with the chitosan solution of antibacterial by mass ratio: collagen solution is 1: 5.With collagen/chitosan/antibacterial dispersion liquid of making by 5cm
2The consumption of/g is evenly spread film, oven dry on polyfluortetraethylene plate.With distilled water immersion film is separated with polyfluortetraethylene plate, once more film is laid on the polyfluortetraethylene plate surface, oven dry promptly gets collagen/chitosan/antibacterial composite membrane.Collagen/chitosan/antibacterial composite membrane is dipped in carries out crosslinked 20h in the cross-linking agent glutaraldehyde, clean,, promptly get antimicrobial type epidermis repair material 37 ℃ of oven dry down with ionized water.By mass percentage, the concentration of cross-linking agent is 6%.
Embodiment 7
Under acid condition, dissolve collagen swelling solution and chitosan respectively, stir it is fully dissolved, be mixed with concentration by mass percentage respectively and be 0.5% collagen solution and 0.6% chitosan solution.In chitosan solution, add 0.5% silver-loaded silica by mass percentage, stir, ultrasonic.The chitosan solution that is added with antibacterial that makes is mixed stirring with collagen solution, promptly get collagen/chitosan/antibacterial dispersion liquid; Be added with the chitosan solution of antibacterial by mass ratio: collagen solution is 1: 0.1.With collagen/chitosan/antibacterial dispersion liquid of making by 10cm
2The consumption of/g is evenly spread film, oven dry on polyfluortetraethylene plate.With distilled water immersion film is separated with polyfluortetraethylene plate, once more film is laid on the polyfluortetraethylene plate surface, oven dry promptly gets collagen/chitosan/antibacterial composite membrane.Collagen/chitosan/antibacterial composite membrane is dipped in carries out crosslinked 1h in the cross-linking agent glutaraldehyde, clean,, promptly get antimicrobial type epidermis repair material 37 ℃ of oven dry down with ionized water.By mass percentage, the concentration of cross-linking agent is 0.01%.
Embodiment 8
Under acid condition, dissolve collagen swelling solution and chitosan respectively, stir it is fully dissolved, be mixed with concentration by mass percentage respectively and be 0.8% collagen solution and 0.5% chitosan solution.In chitosan solution, add 7.5% silver-loaded zirconium phosphate by mass percentage, stir, ultrasonic.The chitosan solution that is added with antibacterial that makes is mixed stirring with collagen solution, promptly get collagen/chitosan/antibacterial dispersion liquid; Be added with the chitosan solution of antibacterial by mass ratio: collagen solution is 1: 9.With collagen/chitosan/antibacterial dispersion liquid of making by 7cm
2The consumption of/g is evenly spread film, oven dry on polyfluortetraethylene plate.With distilled water immersion film is separated with polyfluortetraethylene plate, once more film is laid on the polyfluortetraethylene plate surface, oven dry promptly gets collagen/chitosan/antibacterial composite membrane.Collagen/chitosan/antibacterial composite membrane is dipped in carries out crosslinked 24h in the cross-linking agent glutaraldehyde, clean,, promptly get antimicrobial type epidermis repair material 37 ℃ of oven dry down with ionized water.By mass percentage, the concentration of cross-linking agent is 10%.
Embodiment 9: contain the biological safety evaluation of the composite membrane of variety classes silver base inorganic antibacterial agent
Remove the infull collagen that terminal peptide obtains no antigen through enzyme digestion, acetic acid with 0.5M dissolves collagen swelling solution and chitosan respectively, being mixed with collagen solution and the concentration that concentration is 0.8% (wt) is the chitosan solution of 0.8% (wt), adding with phosphoric acid pick sodium crystal in chitosan solution respectively then is the silver base inorganic antibacterial agent powder HN-300 of carrier, with the zirconium phosphate is the silver base inorganic antibacterial agent SR1000 of carrier, with the zirconium phosphate is the silver-colored electrodeless antibacterial FUMAT T200-4 that carries of carrier, be the silver base inorganic antibacterial agent Novaron of carrier and be the silver base inorganic antibacterial agent MOD of carrier that with the sodium hydroxide zirconium concentration of various antibacterial in chitosan solution is 5% with silicon dioxide.Through stir, chitosan solution and collagen solution fully mix with 1: 9 mass ratio and obtain collagen/chitosan/HN-300 dispersion liquid, collagen/chitosan/SR1000 dispersion liquid, collagen/chitosan/FUMAT T200-4 dispersion liquid, collagen/chitosan/Novaron dispersion liquid and collagen/chitosan/MOD dispersion liquid behind ultrasonic, the restir, with above-mentioned several dispersion liquids of making by 10cm
2/ g evenly spreads film on polyfluortetraethylene plate, place 65 ℃ of baking ovens to dry.With distilled water immersion film is separated with polyfluortetraethylene plate, once more composite membrane is laid on the plate surface and places 65 ℃ of baking oven oven dry promptly to get the collagen/chitosan/antibacterial composite membrane that contains above-mentioned variety classes antibacterial.The l cell L929 (1 * 10 of plantation 1mL on each group composite membrane
4/ mL), 37 ℃ of following 5%CO
2Cultivate in the incubator, changed liquid once in per 2 days, continuous culture is after 4 days, and (SEM) observes the cell on composite membrane surface with scanning electron microscope, and as seen respectively organizing the composite membrane surface all has a large amount of cell growths, and cell growth state is good.
Remove the infull collagen that terminal peptide obtains no antigen through enzyme digestion, hydrochloric acid with 0.01M dissolves collagen swelling solution and chitosan respectively, being mixed with collagen solution and the concentration that concentration is 0.2% (wt) is the chitosan solution of 0.2% (wt), in chitosan solution, add then 0.5% be the silver base inorganic antibacterial agent SR1000 of carrier with the zirconium phosphate, obtain collagen/chitosan/SR1000 dispersion liquid through stirring, fully mixing with 1: 1 mass ratio with collagen solution behind ultrasonic, the restir, with the dispersion liquid that makes by 5cm
2/ g evenly spreads film on polyfluortetraethylene plate, place 45 ℃ of baking ovens to dry.With distilled water immersion film is separated with polyfluortetraethylene plate, once more composite membrane is laid on the plate surface and places 45 ℃ of baking oven oven dry promptly to get collagen/chitosan/SR1000 composite membrane.
Embodiment 11
Remove the infull collagen that terminal peptide obtains no antigen through enzyme digestion, acetic acid with 0.02M dissolves collagen swelling solution and chitosan respectively, being mixed with collagen solution and the concentration that concentration is 0.5% (wt) is the chitosan solution of 0.5% (wt), in chitosan solution, add then 1% be the silver base inorganic antibacterial agent SR1000 of carrier with the zirconium phosphate, obtain collagen/chitosan/SR1000 dispersion liquid through stirring, fully mixing with 2: 8 mass ratio with collagen solution behind ultrasonic, the restir, with the dispersion liquid that makes by 18cm
2/ g evenly spreads film on polyfluortetraethylene plate, place 37 ℃ of baking ovens to dry.With distilled water immersion film is separated with polyfluortetraethylene plate, once more composite membrane is laid on the plate surface and places 37 ℃ of baking oven oven dry promptly to get collagen/chitosan/SR1000 composite membrane.
Embodiment 12
Remove the infull collagen that terminal peptide obtains no antigen through enzyme digestion, hydrochloric acid with 0.01M dissolves collagen swelling solution and chitosan respectively, being mixed with collagen solution and the concentration that concentration is 0.5% (wt) is the chitosan solution of 0.5% (wt), in chitosan solution, add then 2% be the silver base inorganic antibacterial agent Novaron of carrier with the sodium hydroxide zirconium, obtain collagen/chitosan/Novaron dispersion liquid through stirring, fully mixing with 3: 7 mass ratio with collagen solution behind ultrasonic, the restir, with the dispersion liquid that makes by 10cm
2/ g evenly spreads film on polyfluortetraethylene plate, place 37 ℃ of baking ovens to dry.With distilled water immersion film is separated with polyfluortetraethylene plate, once more composite membrane is laid on the plate surface and places 37 ℃ of baking oven oven dry promptly to get collagen/chitosan/Novaron composite membrane.
Claims (8)
1. the preparation method of an antimicrobial type epidermis repair material is characterized in that may further comprise the steps:
1) under acid condition, dissolves collagen swelling solution and chitosan respectively, stir it is fully dissolved, be mixed with concentration by mass percentage respectively and be 0.2%～0.8% collagen solution and 0.2%～0.8% chitosan solution;
2) in chitosan solution, add 0.5%～7.5% silver base inorganic antibacterial agent by mass percentage, stir, ultrasonic;
3) with step 2) chitosan solution that is added with antibacterial that makes mixes stirring with collagen solution, promptly get collagen/chitosan/antibacterial dispersion liquid;
4) with collagen/chitosan/antibacterial dispersion liquid of making by 1～10cm
2The consumption of/g is evenly spread film, oven dry on polyfluortetraethylene plate;
5) with distilled water immersion film is separated with polyfluortetraethylene plate, once more film is laid on the polyfluortetraethylene plate surface, oven dry promptly gets collagen/chitosan/antibacterial composite membrane;
6) collagen/chitosan/antibacterial composite membrane is dipped in carries out crosslinkedly in the cross-linking agent, clean, oven dry promptly gets antimicrobial type epidermis repair material.
2. the preparation method of a kind of antimicrobial type epidermis repair material as claimed in claim 1 is characterized in that silver base inorganic antibacterial agent is silver-loaded zirconium phosphate, carries silver-colored salt of phosphoric acid, carries a kind of in silver-colored sodium hydroxide zirconium, the silver-loaded silica.
3. the preparation method of a kind of antimicrobial type epidermis repair material as claimed in claim 1, it is characterized in that being added with by mass ratio the chitosan solution of antibacterial: collagen solution is 1: 0.1～9.
4. the preparation method of a kind of antimicrobial type epidermis repair material as claimed in claim 1 is characterized in that cross-linking agent is glutaraldehyde or glycerol.
5. as the preparation method of claim 1 or 4 described a kind of antimicrobial type epidermis repair materials, it is characterized in that by mass percentage that the concentration of cross-linking agent is 0.01%～10%.
6. the preparation method of a kind of antimicrobial type epidermis repair material as claimed in claim 1 is characterized in that the crosslinked time is 1～24h.
7. the preparation method of a kind of antimicrobial type epidermis repair material as claimed in claim 1 is characterized in that cleaning and uses washed with de-ionized water.
8. the preparation method of a kind of antimicrobial type epidermis repair material as claimed in claim 1 is characterized in that in step 6), and the temperature of oven dry is 37 ℃.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101791425A (en) * | 2010-03-30 | 2010-08-04 | 赵雪林 | Antibacterial heal-promoting gel material used for preparing medical wound dressing and preparation method thereof |
| CN102552963A (en) * | 2011-11-21 | 2012-07-11 | 北京科技大学 | Preparation method of starch/nano-silver antibacterial composite film |
| CN103146006A (en) * | 2013-03-02 | 2013-06-12 | 福建农林大学 | Medical agar dressing with high strength and high antibacterial property and preparation method thereof |
| CN105532731A (en) * | 2016-02-02 | 2016-05-04 | 江苏时空涂料有限公司 | Preparation method of sustained-release zirconium phosphate silver-carrying antibacterial agent |
| CN108295298A (en) * | 2018-01-25 | 2018-07-20 | 四川大学 | A kind of calcium alginate perforated membrane of the basic zirconium phosphate containing carrying metal ion and preparation method thereof |
| CN113563643A (en) * | 2021-08-05 | 2021-10-29 | 常熟理工学院 | Slow-release antibacterial cross-linked chitosan/montmorillonite film and preparation method thereof |
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2008
- 2008-09-08 CN CNA2008100717413A patent/CN101352580A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101791425A (en) * | 2010-03-30 | 2010-08-04 | 赵雪林 | Antibacterial heal-promoting gel material used for preparing medical wound dressing and preparation method thereof |
| CN101791425B (en) * | 2010-03-30 | 2013-04-10 | 赵雪林 | Antibacterial heal-promoting gel material used for preparing medical wound dressing and preparation method thereof |
| CN102552963A (en) * | 2011-11-21 | 2012-07-11 | 北京科技大学 | Preparation method of starch/nano-silver antibacterial composite film |
| CN102552963B (en) * | 2011-11-21 | 2013-09-25 | 北京科技大学 | Preparation method of starch/nano-silver antibacterial composite film |
| CN103146006A (en) * | 2013-03-02 | 2013-06-12 | 福建农林大学 | Medical agar dressing with high strength and high antibacterial property and preparation method thereof |
| CN103146006B (en) * | 2013-03-02 | 2015-05-27 | 福建农林大学 | Medical agar dressing with high strength and high antibacterial property and preparation method thereof |
| CN105532731A (en) * | 2016-02-02 | 2016-05-04 | 江苏时空涂料有限公司 | Preparation method of sustained-release zirconium phosphate silver-carrying antibacterial agent |
| CN105532731B (en) * | 2016-02-02 | 2018-06-19 | 浙江华德新材料有限公司 | A kind of preparation method of slow-release phosphonic acids zirconium carrying silver antimicrobials |
| CN108295298A (en) * | 2018-01-25 | 2018-07-20 | 四川大学 | A kind of calcium alginate perforated membrane of the basic zirconium phosphate containing carrying metal ion and preparation method thereof |
| CN113563643A (en) * | 2021-08-05 | 2021-10-29 | 常熟理工学院 | Slow-release antibacterial cross-linked chitosan/montmorillonite film and preparation method thereof |
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Application publication date: 20090128 |