CN106620832A - Transparent antibacterial hydrogel dressing as well as preparation method and application thereof - Google Patents
Transparent antibacterial hydrogel dressing as well as preparation method and application thereof Download PDFInfo
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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
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0061—Use of materials characterised by their function or physical properties
- A61L26/0085—Porous materials, e.g. foams or sponges
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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
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0004—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form containing inorganic 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
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0009—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form containing macromolecular materials
- A61L26/0014—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form containing macromolecular materials obtained by reactions only involving carbon-to-carbon unsaturated bonds
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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
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0009—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form containing macromolecular materials
- A61L26/0023—Polysaccharides
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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
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0061—Use of materials characterised by their function or physical properties
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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
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0061—Use of materials characterised by their function or physical properties
- A61L26/0066—Medicaments; Biocides
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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
- A61L26/00—Chemical aspects of, or use of materials for, wound dressings or bandages in liquid, gel or powder form
- A61L26/0061—Use of materials characterised by their function or physical properties
- A61L26/008—Hydrogels or hydrocolloids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
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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
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
- A61L2300/104—Silver, e.g. silver sulfadiazine
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/28—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety
- C08F220/281—Esters containing oxygen in addition to the carboxy oxygen containing no aromatic rings in the alcohol moiety and containing only one oxygen, e.g. furfuryl (meth)acrylate or 2-methoxyethyl (meth)acrylate
Abstract
The invention discloses transparent antibacterial hydrogel dressing and a preparation method thereof. Bacterial cellulose crystal whiskers are compounded with a polymer of gel monomers by adopting an in-situ compositing method; a composite transparent antibacterial gel material is prepared under the action of an initiator, namely ammonium persulfate; the composite transparent antibacterial gel material is used as medical dressing and has high moisture content; a preparation process of the dressing is simple, short in duration and low in cost; the dressing has good elasticity and flexibility and good moisture retention property. By adopting the transparent dressing, lesion and healing conditions of wounds can be clearly observed and pains caused by the fact that the dressing is replaced can be avoided.
Description
Technical field
The invention belongs to the field such as biomaterial, macromolecular material, in particular it relates to one kind is applied to promote wound to heal
Close, prevent transparent anti-bacterial hydrogel dressing, its preparation method and the application of wound infection.
Background technology
The function medical dressing of humectant and antibiotic property is played over the course for the treatment of as a kind of temporary skin substitute
Important function.When skin histology is subject to wound, such as burn, scratch is festered, and cells of superficial layer resistivity declines, golden yellow
The gram- bacteria such as color staphylococcus and Escherichia coli is easily bred on wound, causes the further expansion of wound scope.Wound
Once being infected by bacterial, just it is not easy healing.What at present Clinical practice was most is sterile gauze, low cost, there is certain every bacterium
Effect, but when wound suppuration or when having body fluid to flow out, easily it is bonded together with gauze, when changing gauze, easy brokenization new life
Skin, is unfavorable for wound healing, while patient obtains be subjected to again pain.
Early it is proved under moist environment to be more beneficial for the healing of wound, bacteria cellulose has that wettability power is strong, promotes to heal
Close, mitigate pain and reduce the advantages of changing number of times, especially in accordance with the difference of condition of culture, the membrane material of various trait can be obtained
Material, is a kind of great potential " ideal " wound dressing materials to tackle the wound case that difference oozes out liquid measure and microbiological contamination degree.
Simultaneously aerogel dressing becomes the hot topic of current research, and hydrogel water content is high, can keep the moist environment of wound, swelling behavior
It is good, when wound body fluid oozes out, diffusate can be absorbed, to wound, one is cleaned clean environment.Transparent aquagel dressing can also
The healing state of wound is observed at any time, if wound deterioration, can be taken measures in time.The side for preparing hydrogel the most frequently used at present
Method is chemical method, and a small amount of crosslinking agent is added in gel monomers.The hydrogel performance of chemical method synthesis receives gel monomers, crosslinking
The impact of agent, amount of initiator and reaction condition.
In the current existing dressing patent document with regard to bacteria cellulose, Chinese patent CN 103205863 discloses one
The method of kind of bacterial cellulose slow-release dressing, using the method for electrostatic spinning by bacteria cellulose and polymeric medicine slow release nanometer
Fiber composite.The oil phase organic solvent used during electrostatic spinning is poisonous, and is sustained dressing and need to frequently change, reduction it is negative
Carry the utilization rate of medicine.
Patent CN 203138849 provides a kind of bacteria cellulose moist dressing, does not have in dressing antibacterial or sterilized
, there is infectivity in composition.
With regard in the patent document of aerogel dressing, Chinese patent CN 102675651 discloses a kind of aquagel
The method for preparing antiseptic dressing.The modification of chitosan hydrogel containing antiseptic is prepared, the aerogel dressing has antibiotic property, gram
The problem of wound infection has been taken, but material mechanical performance is poor, and water-resistance is poor, there is certain limitation in application.
Patent CN 101502607 announces a kind of preparation method of medical chitosan transparent hydrogel wound dressing.In dressing
Preservative is with the addition of in preparation process, can resisting mycotic infection of superficial part.But additive best results, human body pH=in pH slant acidities
7.35-7.45, antibacterial effect has suppressed.
The relevant transparent aquagel patent application in the U.S. is as follows：
The open and clear polym eric gel wound dressings of the A1 of United States Patent (USP) US 2009/0326496, it is therefore an objective to absorb wound
Diffusate can at any time observe wound healing situation simultaneously.Hydrogel layer is mainly the cellulose after chemical modification, such as carboxylic first
Base cellulose gel, hydroxyethylcellulose gel, hydroxypropyl methyl cellulose, modified propylene acid amides etc..
United States Patent (USP) United States Patent No.4909244. design a kind of transparent dressing, and dressing mainly includes
Gel layer and bacterial isolation layer, clear gel layer is ethylene vinyl acetate, and material is free from moisture, the polymerization of 100% solid meltability
Thing, flexibility and elasticity are good.Resistance bacterium layer is elasticity and the good polyurethane of caking property, as bacterial isolation layer, stops that bacterium invades wound
Place.The moisture content of the dressing is not high, it is impossible to provide a moist environment for promoting to repair for wound.
The content of the invention
For the disadvantages described above or Improvement requirement of prior art, the invention provides a kind of transparent anti-bacterial hydrogel dressing and
Its preparation method, its object is to by adopting in-situ compositing, and bacteria cellulose whisker and hydrogel monomer I are entered
Row is compound, and is immersed in silver nitrate and NaBH4In solution, preparing surface attachment has the transparent antibacterial of nano-Ag particles
Aerogel dressing, thus solves the technical problem that aerogel dressing water content is low, antibacterial effect is poor of prior art.
For achieving the above object, it is described according to one aspect of the present invention, there is provided a kind of transparent anti-bacterial hydrogel dressing
Aerogel dressing includes bacteria cellulose whisker and clear gel, wherein the bacteria cellulose whisker be dispersed in it is described transparent solidifying
In glue.
Preferably, the clear gel has the general structure shown in formula (I),
Wherein, R1For hydrogen, methyl or ethyl, R2For hydroxyl, amido, methyl esters, ethyl ester, propyl ester, butyl ester, different monooctyl ester, hydroxyl second
Ester, polyglycidyl, diformazan ammonia ethyl ester, hexadecyl ester or octadecyl ester.
Preferably, the water content of the bacteria cellulose whisker is 95%～99.6%, the bacteria cellulose whisker
Length is 100～300nm, a diameter of 5～50nm.
Preferably, the aerogel dressing is loose structure, and the pore size of the loose structure is 2 μm～5.5 μm.
Preferably, the water content of the aerogel dressing is 50%～70%.
Preferably, the aerogel dressing also includes the antiseptic nano-Ag particles on its surface, the nano-Ag particles
Size is 40～70nm.
It is according to another aspect of the present invention, there is provided a kind of preparation method of described aerogel dressing including as follows
Step：
(1) by produce bacteria cellulose microbionation liquid medium within, in 25 DEG C～30 DEG C static cultures at least
Week obtains cellulose membrane, by the cellulose membrane for obtaining distilled water immersion 2～4 days, then puts it into concentration for 0.1mol/L
Boil in NaOH solution 30 minutes, then deionized water is rinsed to neutrality and obtains bacterial cellulose film；
(2) bacterial cellulose film that step (1) is obtained is smashed to pieces, centrifuging and taking upper strata, the cellulose after being centrifuged, will
Cellulose after centrifugation is added to volumetric concentration in 40%～60% sulfuric acid, under the conditions of 40 DEG C～60 DEG C, to be hydrolyzed anti-
Answer 8 hours to 12 hours, hydrolysis is centrifuged, is dialysed, being centrifuged obtain bacteria cellulose whisker again after completing；
(4) the bacteria cellulose whisker for obtaining clear gel monomer and step (2) is according to volume ratio 1～9:1 is mixed
Close, preferred volume ratio is 2.25～9:1, add crosslinking agent GDMA and catalyst n, N, N', N'- tetramethyl
Base ethylenediamine, polymerizing curable is formed after gel, adds 15%～30% ammonium persulfate aqueous solution, is well mixed, and stands 2～4
Hour forms transparent aquagel, and it is washed in the ethanol solution of variable concentrations, the clear gel after being washed；
The concrete steps of the washing are preferably：Carry out in 50%, 40%, 30%, 20%, 10% and 5% ethanol solution respectively
Drop gradient wash, washs four hours every time；
(4) transparent aquagel that step (3) is obtained is immersed in into AgNO31 hour in solution, then with alcohol rinse, then
By it in NaBH4Solution soaks 10 minutes, obtains adhering to the transparent anti-bacterial hydrogel of nano-Ag particles after ultra-pure water cleaning.
Preferably, the bacterium of the product bacteria cellulose described in step (1) is glucose acetobacter xylinum, produces acetobacter, acetifies bar
One or more in bacterium, Pasteur's acetobacter, Agrobacterium, rhizobium and/or sarcine.
Preferably, the fluid nutrient medium described in step (1) is that bacterium produces Membrance cuiture base, and its composition includes the grape of 20g/L
The Na of sugar, the dusty yeast of 5g/L, the dusty yeast of 5g/L, the citric acid of 1.5g/L and 6.8g/L2HPO4。
According to another aspect of the present invention, there is provided a kind of application of described anti-bacterial hydrogel dressing, the antibacterial
Aerogel dressing is applied to medical dressing.
In general, by the contemplated above technical scheme of the present invention compared with prior art, can obtain down and show
Beneficial effect.
(1) in-situ compositing is adopted, bacteria cellulose whisker is combined with the polymer of transparent gel monomers, caused
In the presence of agent ammonium persulfate, compound transparent antibacterial gel material is prepared, as medical dressing, water content is high；
(2) aerogel dressing that the present invention is prepared has preferable mechanical strength and pliability, and its tensile strength can
To reach 0.35MPa-0.55MPa；
(3) aerogel dressing that prepared by the present invention is transparent, can at any time observe wound healing and deterioration, can also extend deposited
The use time of material, after attachment nano-Ag particles, the anti-microbial property of dressing is improved；
(4) aerogel dressing of the invention is loose structure, can provide enough skies in material surface growth for cell
Between, be conducive to the adhesion of cell；
(5) present invention is time-consuming short, and test operation is simple, can as needed prepare various transparent wounds of different shapes and apply
Material.
Description of the drawings
Structural representation after the antibacterial transparent aquagel dressing incision of Fig. 1 present invention；
Fig. 2 is for poly hydroxy ethyl acrylate in embodiment 1 and embodiment 2 with bacteria cellulose whisker in different volumes ratio
The transparency sign of lower composite aquogel；
Fig. 3 is that poly hydroxy ethyl acrylate contains with bacteria cellulose whisker composite aquogel in embodiment 1 and embodiment 2
Water yield figure；
Fig. 4 is that poly hydroxy ethyl acrylate resists with bacteria cellulose whisker composite aquogel in embodiment 1 and embodiment 2
Bacterium design sketch；
Fig. 5 is proliferative conditions of the l cell on the aerogel dressing material that embodiment 1 is prepared；
Fig. 6 is that the aerogel dressing surface SEM that embodiment 1 is prepared is characterized；
Fig. 7 is the SEM figures of the aerogel dressing attachment nano-Ag particles material prepared in embodiment 1；
Fig. 8 is the SEM photograph of the bacteria cellulose whisker that step (2) is prepared in embodiment 1.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, it is right below in conjunction with drawings and Examples
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, and
It is not used in the restriction present invention.As long as additionally, technical characteristic involved in invention described below each embodiment
Not constituting conflict each other just can be mutually combined.
The transparent anti-bacterial hydrogel dressing as shown in Figure 1 that the present invention is provided, including bacteria cellulose whisker and transparent solidifying
Glue, wherein the bacteria cellulose whisker is dispersed in the clear gel.
The clear gel be with the general structure shown in formula (I),
Wherein, R1For hydrogen, methyl or ethyl, R2For hydroxyl, amido, methyl esters, ethyl ester, propyl ester, butyl ester, different monooctyl ester, hydroxyl second
Ester, polyglycidyl, diformazan ammonia ethyl ester, hexadecyl ester or octadecyl ester.
Clear gel for and preparation method thereof be prior art, transparent gel pair is become after all gel monomers are aggregated
All it is feasible in transparent aquagel dressing of the invention is prepared, its polymerization degree n is existing transparent gel monomers polymer
The scope of arbitrarily feasible n, preferred n is 100～10000.
The water content of the bacteria cellulose whisker is 95%～99.6%, and the length of the bacteria cellulose whisker is
100～300nm, a diameter of 5-50nm.
The aerogel dressing is loose structure, and the pore size of the loose structure is 2 μm～5 μm.Loose structure can
To provide enough spaces in material surface growth as cell, be conducive to the adhesion of cell.
The water content of the aerogel dressing is 50%～70%.
Also including the antiseptic nano-Ag particles on its surface, the size of the nano-Ag particles is 40 to the aerogel dressing
～70nm.
The preparation method of described aerogel dressing, comprises the steps：
(1) by produce bacteria cellulose microbionation liquid medium within, in 25 DEG C～30 DEG C static cultures at least
Week obtains cellulose membrane, by the cellulose membrane for obtaining distilled water immersion 2～4 days, then puts it into concentration for 0.1mol/L
30 minutes are boiled in NaOH solution, it is therefore an objective to remove the thalline and culture medium of remaining, then deionized water is rinsed to neutral and obtained
To bacterial cellulose film；
(2) bacterial cellulose film that step (1) is obtained is smashed to pieces, centrifuging and taking upper strata, the cellulose after being centrifuged, will
Cellulose after centrifugation is added to volumetric concentration in 40%～60% sulfuric acid, under the conditions of 40 DEG C～60 DEG C, to be hydrolyzed anti-
Answer 8 hours to 12 hours, hydrolysis is centrifuged, is dialysed, being centrifuged obtain bacteria cellulose whisker again after completing；
(3) the bacteria cellulose whisker for obtaining clear gel monomer and step (2) is according to volume ratio 1～9:1 mixing is equal
It is even, add crosslinking agent GDMA and catalyst n, N, N', N'- tetramethylethylenediamine, polymerizing curable to be formed
15%～30% ammonium persulfate aqueous solution is added after gel, is well mixed, stood 2～4 hours and form transparent aquagel, and will
It carries out gradient wash, the clear gel after being washed in the ethanol solution of variable concentrations；
(5) transparent aquagel that step (3) is obtained is immersed in into AgNO31 hour in solution, then with alcohol rinse, then
By it in NaBH4Solution soaks 10 minutes, obtains adhering to the transparent anti-bacterial hydrogel of nano-Ag particles after ultra-pure water cleaning.
The bacterium of the product bacteria cellulose described in step (1) is glucose acetobacter xylinum, produces acetobacter, acetifies bacillus, Pasteur
One or more in acetobacter, Agrobacterium, rhizobium and/or sarcine.
Fluid nutrient medium described in step (1) is that bacterium produces film HS culture mediums, and its composition is：Glucose 20g/L, dusty yeast
5g/L, dusty yeast 5g/L, citric acid 1.5g/L, Na2HPO4 6.8g/L。
The addition of sulfuric acid is that 150～400 milliliters of volume integrals are added in the cellulose per 100 grams after centrifugation in step (2)
It is 40%～60% sulfuric acid to count, preferably 200 milliliters.
For the first time centrifugation is that, in order to remove the concentrated sulfuric acid, dialysis is to be further purified to step (2), and the ion for removing residual is molten
Liquid, final step centrifugation is to take supernatant, that is, finely dispersed bacteria cellulose whisker in aqueous.
The bacteria cellulose whisker mixed volume ratio that step (3) the clear gel monomer is obtained with step (2) is preferably
2.25～9:1.
Step (3) crosslinking agent quality is the 0.5%～3%, preferably 1% of the gel monomers quality, described to urge
Agent is the 0.5%～1.5% of the gel monomers quality, preferably 1.4%.
It is solidifying that the concrete operations of step (3) polymerizing curable formation gel standing 24h preferably at 4 DEG C forms polymerizing curable
Glue.
The gel monomers mix with the mixed liquor of bacteria cellulose whisker with ammonium persulfate, and the amount of ammonium persulfate is mixing
0.2wt%～the 1wt% of liquid measure, wherein 0.5wt% are optimum.
The bacteria cellulose whisker that step (3) prepares gel monomers and step (2) is according to certain volume than mixing
Uniformly, add crosslinking agent and catalyst to promote gel monomers polymerization, add ammonium persulfate initiated gel monomer and bacterial fibers
The gelation of plain whisker, so that bacteria cellulose whisker and gel monomers polymer together form transparent aquagel, and
Bacteria cellulose whisker is dispersed in clear gel monomer-polymer.
Gradient wash is carried out in the ethanol solution of variable concentrations described in step (3), its objective is to remove ammonium persulfate
(APS).Concretely comprising the following steps for gradient wash is carried out in ethanol solution：Respectively 50%, 40%, 30%, 20%, 10% and 5%
Ethanol solution in carry out drop gradient wash, each washing four hours.
The difficulty of the present invention is how bacteria cellulose to be hydrolyzed to into the cellulose whiskers of nanostructured, and retain bacterium
The high-moisture of cellulose, increases its photopermeability, while the cellulose whiskers of nanostructured are required can be uniform with gel monomers
Mixing.
Specific difficulty is to temperature, sulfuric acid concentration, the addition of sulfuric acid and the control in reaction time.Different is anti-
The bacteria cellulose whisker size obtained with temperature between seasonable is of different sizes.Sulfuric acid concentration is too high to cause cellulose to be carbonized, sulphur
Acid concentration is too low to be unable to acidolysis cellulose.
The anti-bacterial hydrogel dressing that the present invention is prepared can be applicable to medical dressing.
It is below embodiment：
Embodiment 1
(1) it is gluconacetobacter to test bacterium used, and gluconacetobacter is seeded in HS culture mediums, in 30 DEG C of biochemical trainings
Static culture one week in foster case, obtains the bacteria cellulose film that thickness is about 10 millimeters.Half is boiled with 0.1mol/L NaOH solutions
Hour remove culture medium in bacterium residual, then deionized water soak one week it is neutral to pH, you can obtain fiber after purification
Plain film.
(2) smash into bacterial fibers film to pieces slurry, (10000 revs/min, the 10 minutes) moisture removed in homogenate are centrifuged, take
Upper strata, the cellulose after being centrifuged；The configuration concentrated sulfuric acids of 200ml 50%, weigh the cellulose after centrifugation, fine according to every 100g
The concentrated sulfuric acids of 200ml 50%, water-bath 60 DEG C 8 hours or so are added in dimension element.Centrifugal treating (10000 is first carried out after the completion of hydrolysis
Rev/min, 10 minutes), upper strata is taken, dialyse, then supernatant liquor is centrifuged, obtain bacteria cellulose whisker.
(3) hydroxyethyl methacrylate is well mixed with bacteria cellulose whisker, wherein hydroxyethyl methacrylate with
Bacteria cellulose whisker volume ratio is 7:3, add crosslinking agent GDMA quality to be hydroxyethyl methacrylate second
The 0.1% of ester, adds catalyst n, and N, N', N'- tetramethylethylenediamine (TEMED) are hydroxyethyl methacrylate quality
1.4%, it is well mixed and adds 20% ammonium persulfate after standing 24 hours under the conditions of 4 DEG C.Hydroxyethyl methacrylate with it is thin
Fungin whisker mixed liquor is 13 with the volume ratio of ammonium persulfate:1.Mixing after uniform is transferred in 24 orifice plates, quiet at 10 DEG C
Put to form clear gel.Gel is placed in gradient wash in the ethanol solution of variable concentrations, i.e., respectively concentration be 50%,
40%, 30%, 20%, 10%, gradient wash drops in 5% ethanol solution, and every time washing four hours, concretely comprise the following steps：First
By hydrogel in 50% alcohol solution dipping 4 hours, afterwards the hydrogel of the ethanol solution of saturated absorption 50% is placed in into concentration is
40% ethanol solution 4 hours, it is therefore intended that the ethanol in dilution hydrogel, repeats the above and operates to concentration of alcohol to be down to
10%, then hydrogel is immersed in 4 hours in 5% ethanol solution, finally hydrogel is put and is soaked 4 hours in deionized water,
Changing deionized water guarantees for 5 times ethanol all except clean.
(4) clear gel after above-mentioned process is immersed in into concentration for 0.001mol/L AgNO3In one hour and then use wine
Fine is washed 30 seconds, then is immersed in concentration for 0.1mol/L NaBH4In 10 minutes.Obtain adhering to the antibacterial of nano-Ag particles
Property clear gel dressing.
Embodiment 2
Repeat embodiment 1 with the same steps, difference is, in step (3), hydroxyethyl methacrylate is fine with bacterium
The plain whisker volume ratio of dimension is 1:1.
Embodiment 3
Repeat embodiment 1 with the same steps, difference is, in step (3), prepare acrylic acid brilliant with bacteria cellulose
Must mixed liquor：Acrylic monomers is 7 with bacteria cellulose whisker volume ratio:3, crosslinking agent GDMA quality
For acrylic acid 0.1%, catalyst n, N, N', N'- tetramethylethylenediamine (TEMED) are the 1.4% of acrylic acid quality, and mixing is equal
It is even and add 20% ammonium persulfate after standing 24 hours under the conditions of 4 DEG C.Mixed liquor is 13 with the volume ratio of ammonium persulfate:1.
Embodiment 4
Repeat embodiment 1 with the same steps, difference is that 60% concentrated sulfuric acid acidolysis bacterium of configuration is fine in step (2)
Dimension element, water-bath 40 DEG C 12 hours.
Embodiment 5
Repeat embodiment 1 with the same steps, difference is, in step (1), experiment bacteria used thereby is product acetobacter.
Embodiment 6
Repeat embodiment 1 with the same steps, difference is, in step (4), AgNO3Concentration is 0.001mol/L,
NaBH4Concentration is 0.01mol/L.
Embodiment 7
Antibacterial effect detection is carried out to material in embodiment 1, experiment bacteria used thereby is Escherichia coli, and experimental technique is as follows：System
Standby concentration is about 104The E. coli suspension of cfu/ml, takes 2ml bacterium solutions, and material is immersed in bacterium solution, and material size is circle
Column 2cm2×0.5cm.After cultivating 1 day and 2 days at 37 DEG C, with 10ml PBS flushing materials surface bacterium solution.After bacterium solution is mixed
Appropriate dilution is done, 3 dilution factors are done.0.1ml dilution factor bacterium solution uniform applications are removed on solid agar flat board, 37 DEG C of cultures are placed in
24h is cultivated in case.Clump count in observation flat board.
Embodiment 8
Biological assessment is carried out to material in embodiment 1, cell used by cell experiment is MEC
(3T3), cell suspending liquid is prepared, and is inoculated in and is equipped with 24 orifice plates of the material of embodiment 1；Control group is without the material of embodiment 1
Lower inoculating cell is in 96 orifice plates.10000 cells are inoculated with per hole.37 DEG C are placed in, 5%CO2Under the conditions of incubator trained
Support, a fresh culture is changed per 24h, and carry out a CCK-8 cells propagation detection.The OD values surveyed under 450nm wavelength, OD values
It is higher, illustrate that cell quantity is more.
Interpretation：
Fig. 1 cuts later structural representation open for antibacterial transparent aquagel dressing.Dressing inside and bacteria cellulose whisker
It is well mixed, adsorbs the nano-Ag particles on composite aquogel surface and be easy to release, plays antibacterial effect.
Fig. 2 is embodiment 1, and poly hydroxy ethyl acrylate is combined with bacteria cellulose whisker under different volumes ratio in 2
The transparency sign of hydrogel.At visible wavelengths, the transparency of composite aquogel can be up to more than 85%.
Fig. 3 is poly hydroxy ethyl acrylate and the aqueous spirogram of bacteria cellulose whisker composite aquogel in embodiment 1.It is multiple
The water content of Heshui gel is between 60%-70%.
Fig. 4 is poly hydroxy ethyl acrylate and bacteria cellulose whisker composite aquogel antibacterial effect figure in embodiment 1.
Experiment bacteria used thereby is Escherichia coli, and antibacterial effect can reach 70% at first day, as nano-Ag particles discharge, antibacterial effect
Also progressively strengthen, antibiotic rate is up to 80% within second day.
Fig. 5 is proliferative conditions of the l cell on the aerogel dressing material that embodiment 1 is prepared.OD values
It is higher, illustrate that cell quantity is more.Cells On day and second day it is good in the material proliferative conditions of embodiment 1, it can be seen that it is real
Apply and have good biocompatibility between the aerogel dressing and l cell that example 1 prepares.
Fig. 6 is that the aerogel dressing material surface prepared in embodiment 1 characterizes SEM figures, and the aerogel dressing is porous
Structure, the pore size of the loose structure is 2 μm～5.5 μm.
Fig. 7 is the SEM figures of the aerogel dressing attachment nano-Ag particles material prepared in embodiment 1.Nano-Ag particles
Size is 40～70nm.
Fig. 8 is the SEM photograph of the bacteria cellulose whisker that step (2) is prepared in embodiment 1.Bacteria cellulose whisker
Length be 100～300nm, a diameter of 5-50nm.
As it will be easily appreciated by one skilled in the art that the foregoing is only presently preferred embodiments of the present invention, not to
The present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc. are limited, all should be included
Within protection scope of the present invention.
Claims (10)
1. a kind of transparent anti-bacterial hydrogel dressing, it is characterised in that the aerogel dressing includes bacteria cellulose whisker and thoroughly
Bright gel, wherein the bacteria cellulose whisker is dispersed in the clear gel.
2. aerogel dressing as claimed in claim 1, it is characterised in that the clear gel has the structure shown in formula (I)
Formula,
Wherein, R1For hydrogen, methyl or ethyl, R2For hydroxyl, amido, methyl esters, ethyl ester, propyl ester, butyl ester, different monooctyl ester, hydroxyl ethyl ester, ring
Oxygen propyl ester, diformazan ammonia ethyl ester, hexadecyl ester or octadecyl ester.
3. aerogel dressing as claimed in claim 1 or 2, it is characterised in that the water content of the bacteria cellulose whisker is
95%～99.6%, the length of the bacteria cellulose whisker is 100～300nm, a diameter of 5～50nm.
4. aerogel dressing as claimed in claim 1, it is characterised in that the aerogel dressing is loose structure, described many
The pore size of pore structure is 2 μm～5.5 μm.
5. aerogel dressing as claimed in claim 1, it is characterised in that the water content of the aerogel dressing is 50%～
70%.
6. aerogel dressing as claimed in claim 1, it is characterised in that the aerogel dressing is also including the antibacterial on its surface
Agent nano-Ag particles, the size of the nano-Ag particles is 40～70nm.
7. the preparation method of the aerogel dressing as described in claim 1～6 any one, it is characterised in that including following step
Suddenly：
(1) by the microbionation liquid medium within for producing bacteria cellulose, obtain within least one week in 25 DEG C～30 DEG C static cultures
To cellulose membrane, by the cellulose membrane for obtaining distilled water immersion 2～4 days, then to put it into concentration molten for 0.1mol/L NaOH
Boil in liquid 30 minutes, then deionized water is rinsed to neutrality and obtains bacterial cellulose film；
(2) bacterial cellulose film that step (1) is obtained is smashed to pieces, centrifuging and taking upper strata, the cellulose after being centrifuged will be centrifuged
Cellulose afterwards is added to volumetric concentration in 40%～60% sulfuric acid, under the conditions of 40 DEG C～60 DEG C, the reaction 8 that is hydrolyzed is little
When by 12 hours, hydrolysis is centrifuged, is dialysed, being centrifuged obtain bacteria cellulose whisker again after completing；
(3) the bacteria cellulose whisker for obtaining clear gel monomer and step (2) is according to volume ratio 1～9:1 is mixed, excellent
Volume ratio is selected to be 2.25～9:1, add crosslinking agent GDMA and catalyst n, N, N', N'- tetramethyl second
Diamines, polymerizing curable is formed after gel, adds 15%～30% ammonium persulfate aqueous solution, is well mixed, and stands 2～4 hours
Transparent aquagel is formed, and it is washed in the ethanol solution of variable concentrations, the clear gel after being washed；It is described
The concrete steps of washing are preferably：Carry out drop ladder in 50%, 40%, 30%, 20%, 10% and 5% ethanol solution respectively
Degree washing, washs four hours every time；
(4) transparent aquagel that step (3) is obtained is immersed in into AgNO31 hour in solution, then with alcohol rinse, then by its
NaBH4Solution soaks 10 minutes, obtains adhering to the transparent anti-bacterial hydrogel of nano-Ag particles after ultra-pure water cleaning.
8. preparation method as claimed in claim 7, it is characterised in that the bacterium of the product bacteria cellulose described in step (1) is
Glucose acetobacter xylinum, produce acetobacter, the one kind acetified in bacillus, Pasteur's acetobacter, Agrobacterium, rhizobium and/or sarcine
Or it is various.
9. preparation method as claimed in claim 7, it is characterised in that the fluid nutrient medium described in step (1) is that bacterium produces film
Culture medium, the glucose of its composition including 20g/L, the dusty yeast of 5g/L, the dusty yeast of 5g/L, the citric acid of 1.5g/L and
The Na of 6.8g/L2HPO4。
10. the application of the anti-bacterial hydrogel dressing as described in claim 1～6 any one, it is characterised in that the antibacterial water
Gel dressing is applied to medical dressing.
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