CN115252872A - Antibacterial dressing based on ferroelectric material and preparation method and application thereof - Google Patents
Antibacterial dressing based on ferroelectric material and preparation method and application thereof Download PDFInfo
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- 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
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- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
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- 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
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- A61L15/42—Use of materials characterised by their function or physical properties
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Abstract
The invention discloses an antibacterial dressing based on a ferroelectric material, and a preparation method and application thereof. The ferroelectric material comprises ferroelectric high molecular polymer and/or inorganic ferroelectric particles, wherein the inorganic ferroelectric particles account for 0-20% of the volume fraction of the ferroelectric high molecular polymer, and the diameter of the inorganic ferroelectric particles is 50 nm-500 nm. The invention further provides a preparation method of the antibacterial dressing based on the ferroelectric material, which comprises the following steps: preparing a composite material by using a ferroelectric high molecular polymer, ferroelectric ceramic particles and an inorganic pore-foaming agent; and subjecting the composite material to high-temperature treatment, corona polarization treatment and acid liquor treatment in sequence; or sequentially carrying out corona polarization treatment, high-temperature treatment and acid liquor treatment. Experiments prove that the prepared antibacterial dressing has the capability of promoting the regeneration of infectious tissues and the anti-infection function in vivo.
Description
Technical Field
The invention relates to the field of antibacterial dressings, in particular to an antibacterial dressing based on ferroelectric materials and a preparation method and application thereof.
Background
The current clinical evaluation and research show that the wound dressing, the collagen film and the like which are commonly used in the market have certain defects. For example, transparent dressings are prone to adhesion to wounds, have an unsatisfactory antimicrobial effect, lack tissue regeneration-inducing activity, and require external force to generate an electrical signal in the current piezoelectric materials. PTFE is a barrier membrane commonly used in clinical severe periodontitis for inducing bone tissue regeneration, but due to lack of antibacterial activity, repair failure is often caused by exposure to easily-induced infection complications, and such nonabsorbable membrane tissue regeneration-inducing activity and anti-adhesive adhesion to newly-born soft and hard tissues are not ideal. Therefore, there is a need to develop a novel antibacterial biomaterial that is effective in promoting the regeneration of infectious tissues.
The information in this background is only for the purpose of illustrating the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art that is already known to a person skilled in the art.
Disclosure of Invention
In order to solve at least part of technical problems in the prior art, the invention provides an antibacterial dressing based on a ferroelectric material, and a preparation method and application thereof. Specifically, the present invention includes the following.
In a first aspect of the present invention, an antibacterial dressing based on ferroelectric material is provided, wherein the ferroelectric material comprises ferroelectric high molecular polymer and/or inorganic ferroelectric particles, and the inorganic ferroelectric particles occupy 0-20% of the volume fraction of the ferroelectric high molecular polymer, and the diameter of the inorganic ferroelectric particles is 50 nm-500 nm.
In certain embodiments, an antimicrobial dressing based on ferroelectric material according to the present invention comprises ferroelectric high molecular polymer and ferroelectric ceramic particles, and further comprises a porous structure located inside the dressing.
In a second aspect of the present invention, a method for preparing an antibacterial dressing based on a ferroelectric material is provided, which comprises the following steps:
(1) Preparing a composite material by using a ferroelectric high molecular polymer, ferroelectric ceramic particles and an inorganic pore-foaming agent; and
(2) Carrying out high-temperature treatment, corona polarization treatment and acid liquor treatment on the composite material in sequence; or sequentially carrying out corona polarization treatment, high-temperature treatment and acid liquor treatment.
In certain embodiments, the method for preparing an antibacterial dressing based on a ferroelectric material according to the present invention, wherein the inorganic porogen comprises zinc oxide and/or calcium carbonate.
In certain embodiments, the method of making an antimicrobial dressing based on ferroelectric material according to the present invention, wherein the ferroelectric ceramic particles comprise one or more of barium titanate, barium strontium titanate, bismuth ferrite, potassium sodium niobate, and lithium niobate.
In certain embodiments, the preparation method of the antibacterial dressing based on ferroelectric material according to the present invention, wherein the high temperature treatment condition comprises treatment at a temperature of 80 ℃ to 150 ℃ for 5min to 2h in air or vacuum, followed by natural cooling.
In certain embodiments, the conditions of the corona polarization treatment include a polarization field strength of 0.1kV/mm to 10kV/mm, a polarization time of 1min to 60min, air or vacuum as a polarization medium, and a polarization temperature of 25 ℃ to 100 ℃.
In certain embodiments, the method for preparing an antibacterial dressing based on a ferroelectric material according to the present invention, wherein the acid treatment comprises a treatment with an aqueous solution selected from hydrochloric acid, sulfuric acid, nitric acid, and carbonic acid for 3 to 30 hours.
In a third aspect of the invention, there is provided the use of an antimicrobial dressing based on a ferroelectric material in the manufacture of an antimicrobial product.
In certain embodiments, the antimicrobial products include products for combating infections caused by skin defects, mucosal lesions, oral ulcers, according to the uses of the present invention.
Aiming at common skin infections represented by staphylococcus aureus and porphyromonas gingivalis, experiments prove that the prepared antibacterial dressing can effectively resist bacteria without applying external force and promote the regeneration capability of infectious tissues in skin infection diseases. The tissue bacteria content of a mouse at 3 days and 8 days is detected, the regeneration capacity of the BTO/P (VDF-TrFE) electroactive composite membrane tissue is evaluated by comparing the healing speed of a skin wound and observing the tissue morphology through histological staining, the result shows that the charged membrane has more excellent result, and immunofluorescence assay further shows that the expression of the IL-6 in the high-charged group is far lower than that of other groups, which shows that the material has the anti-inflammatory effect and confirms the anti-infection effect of the charged dressing in vivo. In addition, the expression activity of important molecules CD31 and KRT5 related to epithelial repair further verifies the capability of the charged membrane material to effectively promote tissue regeneration.
Drawings
FIG. 1 shows the charge values (piezoelectric constants d) of different materials prepared in example 1 of the present invention 33 ) And (5) characterizing the result.
FIG. 2 is a photograph of colonies of Staphylococcus aureus and Porphyromonas gingivalis cultured on the surface of materials with different charges according to example 1 of the present invention.
FIG. 3 is a photograph showing the structural morphology of Staphylococcus aureus and Porphyromonas gingivalis cultured on the surface of materials with different charge amounts in example 1 of the present invention.
FIG. 4 shows the results of the antibacterial rate of the surface of the material with different charge amounts against Staphylococcus aureus and Porphyromonas gingivalis in example 1 of the present invention.
Figure 5 mouse skin healing wound changes. (a) an image of the healing of a mouse skin wound within 0-8 days; (b) a quantitative statistical plot of wound diameter size; (c) number of bacterial colony units in the tissue at 3 and 8 days. In fig. 5 (b), each group diagram corresponding to each day includes a Blank group (Blank), a non-charged group (NC), and a charged group (HC) in this order from left to right.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that the upper and lower limits of the range, and each intervening value therebetween, is specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control. Unless otherwise indicated, "%" is percent by weight.
As used herein, the term "breathability" characterizes breathability by the water vapor transmission measured at 38 ℃,90% RH.
Herein, the term "antibacterial" refers to the antibacterial effect based on the charged property of the ferroelectric material itself, and is not based on chemical components, nor is it based on the case where electricity is generated by external force action to realize antibacterial.
In a first aspect of the invention, an antibacterial dressing based on a ferroelectric material is provided, wherein the ferroelectric material comprises a ferroelectric high molecular polymer and/or inorganic ferroelectric particles, the inorganic ferroelectric particles account for 0-20% of the volume fraction of the ferroelectric high molecular polymer, and the diameter of the inorganic ferroelectric particles is 50 nm-500 nm.
In an exemplary embodiment, the antimicrobial dressing of the present invention comprises ferroelectric high molecular polymers and ferroelectric ceramic particles, and further comprises a porous structure located inside the dressing.
In the present invention, the form of the antimicrobial dressing is not particularly limited, and may be any form, for example, a film material form, a gel form, and the like.
In a second aspect of the present invention, there is provided a method for preparing an antibacterial dressing based on ferroelectric material, comprising the steps of:
(1) Preparing a composite material from a ferroelectric high molecular polymer, ferroelectric ceramic particles and an optional inorganic pore-foaming agent (used for preparing the porous antibacterial material);
(2) The composite material is sequentially subjected to high-temperature treatment, corona polarization treatment and acid liquor treatment.
In the present invention, the step (1) may specifically include (1-1) dissolving the ferroelectric polymer in an organic solvent to form a ferroelectric polymer mixed solution; (1-2) adding an inorganic pore-foaming agent and an inorganic ferroelectric material into the ferroelectric high-molecular polymer mixed solution, and mixing to form a dispersion solution; and (1-3) preparing a thin film by casting the dispersion to obtain a primary film.
In the present invention, the size of the inorganic ferroelectric particles is not limited, but generally the average diameter thereof is 50 nm to 500 nm, preferably 100 to 400nm, more preferably 200 to 300nm.
In the present invention, examples of the inorganic ferroelectric material include, but are not limited to, one or more of barium titanate, barium strontium titanate, bismuth ferrite, potassium sodium niobate, and lithium niobate.
In the invention, the particle size of the inorganic pore-foaming agent is generally 40 nm-100 nm, preferably 50-90 nm. This particle size range facilitates uniform dispersion of the porogen in the polymer mixture. If the particle diameter of the inorganic porogen is too large, although the gas permeability of the resulting membrane material is improved, the antibacterial property after polarization becomes poor, and further the strength of the resulting membrane material becomes low, and the inorganic porogen particles tend to precipitate in the polymer, which is not favorable for dispersion. On the other hand, if the particle diameter of the inorganic porogen particles is too small, the gas permeability tends to be poor, and the inorganic porogen particles are easily agglomerated when the polymer mixture is added, and also are not conducive to dispersion, thereby affecting the gas permeability and strength of the obtained membrane material.
In the present invention, the inorganic pore-forming particles are preferably used in an amount of 5 to 15% based on the weight of the dispersion. If the amount is too low, the gas permeability becomes poor, and the gas permeability of, for example, tissues in the body cannot be achieved. On the other hand, if the amount is too high, the antibacterial property after polarization becomes poor, and the strength of the film material is affected.
The inorganic porogen particles are selected from zinc oxide and/or calcium carbonate. In the present invention, one kind of the above particles may be used, or two or more kinds thereof may be used in combination.
In the present invention, the ferroelectric high molecular polymer is not limited, and includes polyvinylidene fluoride or a copolymer thereof, and examples thereof include, but are not limited to, polyvinylidene fluoride-hexafluoropropylene, and polyvinylidene fluoride-trifluoroethylene, and polylactic acid. In the present invention, one or a combination of two or more of the above polymers may be used. In the case of using two or more kinds in combination, the amount of each polymer or the ratio of the amounts of the polymers is not particularly limited and can be freely set by those skilled in the art according to actual needs. The molecular weight of the ferroelectric high molecular polymer is not limited, and is generally between 20 and 100 kilodalton, preferably between 30 and 80 kilodalton, and more preferably between 40 and 60 kilodalton.
In the present invention, the organic solvent is not particularly limited, and an aprotic polar solvent is preferred, and examples thereof include, but are not limited to, one or more of N, N-dimethylformamide, toluene, chloroform, dichloromethane, methanol and ethyl acetate, and N, N-dimethylformamide is particularly preferably contained. The solvent of the present invention may be a single solvent, or a mixed solvent such as a mixed solvent of N, N-dimethylformamide and toluene, or a mixed solvent of N, N-dimethylformamide and chloroform may be used. The ratio of each solvent in the solvent mixture is not particularly limited, and may be any ratio as long as the object of the present invention is not impaired.
In the present invention, the ferroelectric polymer is used in an amount ratio to the organic solvent such that the ferroelectric polymer is 5 to 40% by weight, preferably 10 to 30% by weight. If the proportion of the ferroelectric high molecular polymer is too low, the charging performance of the resulting repair film tends to be lowered. On the other hand, if the proportion of the ferroelectric high molecular polymer is too high, the gas permeability becomes poor.
In the present invention, in order to promote mixing between the ferroelectric polymer and the organic solvent, for example, stirring may be performed during mixing. The stirring conditions are not limited, and the stirring can be carried out by any known stirring method, the stirring time is not special, and the stirring can be carried out by only fully mixing or completely dissolving the two. In addition, in order to promote the mixing between the two, it is conceivable to increase the temperature at the time of mixing the ferroelectric high molecular polymer and the organic solvent, but the temperature should be lower than the boiling point of the organic solvent and at the same time lower than the lowest temperature at the time of the subsequent high-temperature treatment, that is, lower than 80 ℃, preferably lower than 70 ℃.
In the present invention, the treatment of the material comprises a corona polarization treatment followed by an acid treatment, optionally followed by a high temperature treatment prior to the acid treatment. The acid treatment of the present invention cannot precede the polarization treatment. In an exemplary embodiment, the treatment sequence is a high temperature treatment, a corona polarization treatment, an acid treatment in that order.
In the present invention, the acid treatment is a treatment of immersing the material in an acidic solution for 5 to 30 hours, for example, 6 hours, 7 hours, 8 hours, 10 hours, 12 hours, 14 hours, 16 hours, 18 hours, or even 24 hours or more.
In the present invention, the acidic solution is not particularly limited, and examples thereof include, but are not limited to, aqueous solutions of hydrochloric acid, sulfuric acid, nitric acid, carbonic acid, and the like. In the present invention, one or a combination of two or more of the above acids may be used. In the case of the combination, the ratio of each acid is not particularly limited. The concentration of the acid in the acidic solution is not particularly limited as long as the pH in the solution can be made lower than 7, preferably 6, more preferably 5. In general, the concentration of the acid in the aqueous solution is 5 to 60% by mass, preferably 6 to 50% by mass, more preferably 10 to 40% by mass. The time for the treatment with the acidic solution is not limited, but is generally 5 hours or more, for example, 10 hours, 12 hours, 15 hours, 20 hours, 25 hours, 30 hours, or the like. The permeability of the membrane material is improved by treatment with an acidic solution. The concentration of acid and treatment time are generally related to the content of inorganic porogen particles, the concentration of high molecular weight polymer, etc.
In the present invention, the high temperature treatment is generally to treat the antibacterial material at 80-100 ℃ for 5-30 minutes. The elevated temperature may be, for example, 85 ℃,90 ℃, 95 ℃, 100 ℃ and the like. If the temperature is too low, the effect on reducing the adverse effects of corona polarization tends to be weak or even non-functional. If the temperature is too high, the gas permeability of the membrane material tends to deteriorate, even failing to meet the oxygen exchange requirement of the in vivo tissue.
In the invention, the parameters of the corona polarization treatment comprise that the polarization medium is one of air and methyl silicone oil, and the polarization voltage is 1kV to 30kV, more preferably 2 kV to 25 kV. The distance between the pole head and the sample is set to be 1mm to 50mm, for example, 5mm, 10mm, 15mm, 20mm, 25mm, 30mm, 35mm, and the like. The polarisation temperature is 20 ℃ to 50 ℃, for example 25, 30, 35 or 40 ℃. The polarization time is 1 minute to 60 minutes, for example, 5 minutes, 10 minutes, 15 minutes, 20 minutes, 30 minutes, 40 minutes, and the like.
Example 1
This example is a preparation example of an exemplary antimicrobial dressing, and specifically includes the following steps:
1. putting the nano barium titanate particles into dopamine aqueous solution, heating and stirring in a water bath at 60 ℃ for 12 h, and centrifugally drying to obtain barium titanate nano particle filler;
2. dispersing a proper amount of the barium titanate nano-particle filler prepared in the step (1) in a 3 ml organic solvent DMF, and stirring 3 h by adopting stirring and ultrasonic oscillation to obtain a barium titanate particle filler dispersion liquid;
3. dispersing 1 g polymer P (VDF-TrFE) powder in 7 ml organic solvent DMF, and stirring 3 h to completely dissolve the polymer P (VDF-TrFE) solution;
4. mixing the barium titanate particle filler dispersion liquid formed in the step (2) and the polymer P (VDF-TrFE) solution formed in the step (3), and stirring 24h to obtain a mixed liquid with uniformly dispersed particle fillers;
5. respectively taking the mixed solution obtained in the step (4) to be cast into a film in a casting container, and drying the film at the temperature of 55 ℃ to obtain 4h so as to completely volatilize the solvent;
6. will step withAnnealing the composite membrane prepared in the step (5) on a heating platform at 100 ℃ and 125 ℃ for 30min to obtain two ferroelectric composite membranes which are not subjected to annealing treatment in the step (5) and are treated at different temperatures, then respectively placing the ferroelectric composite membranes on sample platforms of a corona polarization device, wherein the polarization medium is air, the voltage is applied to the ferroelectric composite membranes at 21kV, the distance between a polarization head and a sample is set to be 15mm, the polarization temperature is 25 ℃, and the polarization time is 30min to obtain two BaTiO materials with different charge quantities 3 a/P (VDF-TrFE) antibacterial composite film material with a piezoelectric constant d 33 8pC/N, 15 pC/N and 21pC/N, respectively (as shown in FIG. 1). The water vapor transmission capacity of the catalyst is about 54g/m 2 ·24h。
Examples 2 to 4
An antibacterial film material was prepared in the same manner as in example 1, except that the material composition or the treatment pattern was changed as shown in table 1.
TABLE 1
Example 5
This example is an exemplary preparation of a porous antimicrobial dressing. When an inorganic pore-forming agent is used for preparing the porous antibacterial dressing, the inventor finds that the ferroelectric inorganic particles in the composite film can be corroded by acid liquor treatment, different ferroelectric materials have different resistances to acid liquor, the influence of barium titanate BTO is minimal, and the influence of potassium sodium niobate KNN and barium strontium titanate BST on acid liquor treatment is large. In addition, it has been found that corrosion of the ferroelectric material affects the improvement of the piezoelectric constant of the composite material during polarization, and further affects the antibacterial property.
TABLE 2
In order to avoid the above influence, the inventor improves the preparation process of the porous antibacterial dressing, and the preparation process specifically comprises the following steps:
1. putting the nano ferroelectric material particles shown in the table 2 into a dopamine aqueous solution, heating and stirring in a water bath at 60 ℃ for 12 h, and centrifugally drying to obtain a nano particle filler;
2. dispersing a proper amount of the nanoparticle filler prepared in the step (1) and 10wt% of an inorganic pore-forming agent (with an average particle size of 80 nm) shown in Table 2 in a 3 ml organic solvent DMF, and stirring 3 h by adopting stirring and ultrasonic oscillation to obtain a dispersion liquid;
3. taking 1 g polymer P (VDF-TrFE) powder to disperse in 7 ml organic solvent DMF, stirring 3 h to completely dissolve the powder to form a polymer P (VDF-TrFE) solution;
4. mixing the dispersion liquid formed in the step (2) with the polymer P (VDF-TrFE) solution formed in the step (3), and stirring 24h to obtain a mixed liquid with uniformly dispersed particle fillers;
5. respectively taking the mixed solution obtained in the step (4) to be cast into a film in a casting container, and drying the film at the temperature of 55 ℃ to obtain 4h so as to completely volatilize the solvent;
6. annealing the composite film prepared in the step (5) on a heating platform at 125 ℃ for 30min, then placing the composite film on a sample platform of a corona polarization device, wherein a polarization medium is air, a voltage is applied to 21kV, the distance between a polarization pole head and a sample is set to be 15mm, the polarization temperature is 25 ℃, and polarization is carried out for 30min to obtain an antibacterial composite film material, and then soaking the antibacterial composite film material in a 37% hydrochloric acid solution for 12 hours;
7. and (4) taking out the film prepared in the step (6), washing the film for a plurality of times by using deionized water, and taking out the film to be blown for 3 hours at 37 ℃.
Comparative example 1
1. Putting the nano ferroelectric material particles into dopamine aqueous solution, heating and stirring in water bath at 60 ℃ for 12 h, and centrifugally drying to obtain nano particle filler;
2. dispersing a proper amount of the nano-particle filler prepared in the step (1) and 10wt% of inorganic particle ZnO (with the average particle size of 80 nm) in 3 ml organic solvent DMF, and stirring 3 h by adopting stirring and ultrasonic oscillation to obtain a dispersion liquid;
3. dispersing 1 g polymer P (VDF-TrFE) powder in 7 ml organic solvent DMF, and stirring 3 h to completely dissolve the polymer P (VDF-TrFE) solution;
4. mixing the dispersion liquid formed in the step (2) with the polymer P (VDF-TrFE) solution formed in the step (3), and stirring 24h to obtain a mixed liquid with uniformly dispersed particle fillers;
5. respectively taking the mixed solution obtained in the step (4) to be cast into a film in a casting container, and drying the film at the temperature of 55 ℃ to obtain 4h so as to completely volatilize the solvent;
6. soaking the composite membrane prepared in the step (5) in a 37% hydrochloric acid solution for 12 hours, taking out, washing with deionized water for several times, taking out, and purging at 37 ℃ for 3 hours;
7. and (3) annealing the material obtained in the step (6) on a heating platform at 125 ℃ for 30min, then placing the material on a sample platform of a corona polarization device, wherein a polarization medium is air, a voltage is 21kV, the distance between a polarization head and a sample is 15mm, the polarization temperature is 25 ℃, and polarization is carried out for 30min to obtain the antibacterial composite membrane material.
Comparative example 2
1. Putting the nano ferroelectric material particles into a dopamine aqueous solution, heating and stirring in a water bath at 60 ℃ for 12 h, and centrifugally drying to obtain a nano particle filler;
2. dispersing a proper amount of the nano-particle filler prepared in the step (1) and 10wt% of inorganic particle ZnO (with the average particle size of 80 nm) in 3 ml organic solvent DMF, and stirring 3 h by adopting stirring and ultrasonic oscillation to obtain a dispersion liquid;
3. dispersing 1 g polymer P (VDF-TrFE) powder in 7 ml organic solvent DMF, and stirring 3 h to completely dissolve the polymer P (VDF-TrFE) solution;
4. mixing the dispersion liquid formed in the step (2) with the polymer P (VDF-TrFE) solution formed in the step (3), and stirring 24h to obtain a mixed liquid with uniformly dispersed particle fillers;
5. respectively taking the mixed solution obtained in the step (4) to be cast into a film in a casting container, and drying the film at the temperature of 55 ℃ to obtain 4h so as to completely volatilize the solvent;
6. soaking the composite membrane prepared in the step (5) in a 37% hydrochloric acid solution for 12 hours, taking out, washing with deionized water for several times, taking out, and purging at 37 ℃ for 3 hours;
7. and (3) placing the material obtained in the step (6) on a sample table of a corona polarization device, wherein a polarization medium is air, applying a voltage of 21kV, setting the distance between a polarization head and a sample to be 15mm, polarizing at the temperature of 25 ℃, and polarizing for 30min to obtain the antibacterial composite membrane material.
Test example
1. Antibacterial experiments
The obtained ferroelectric composite membranes with different charge amounts and bacteria (gram-negative bacteria, namely, porphyromonas gingivalis and gram-positive bacteria, namely, staphylococcus aureus) are cultured together, the growth activity and the structural change of the bacteria are detected after 24 hours, the antibacterial rate is analyzed, and unpolarized uncharged composite membranes are used as a control group. Fig. 2, fig. 3 and fig. 4 show the detection results of this example, and the experimental results show that the antibacterial activity is closely related to the charge amount, and the charged group has obvious antibacterial activity compared with the uncharged group, and increases with the increase of the charge amount, which confirms that the high-efficiency antibacterial activity can be realized by regulating and controlling the charge amount.
2. Skin defect infection test
2.1 model preparation
The mice were acclimatized for 7 days, anesthetized with 1% pentobarbital, injected at a dose of 50mg/Kg, shaved, and a circular full-thickness skin wound (. Phi.8 mm) was prepared on the back of each mouse, followed by 20. Mu.L of a Staphylococcus aureus solution (10. Mu.L) 7 CFU/mL) was evenly applied to the wound area in two separate passes, covered with an air-impermeable plastic film and fixed, and after 24h, whether the model construction was successful was observed (success flag: wound suppuration was observed). After the model is successfully established, a BTO/P (VDF-TrFE) composite membrane is added to the wound for treatment, and is fixed by a hollow Tegaderm breathable dressing patch and a 3M adhesive tape, and the control conditions of the blank group are consistent with those of the experimental group except that no material is placed. Daily body weight and wound diameter changes of the mice were recorded daily, and the wound size (%) was calculated by the following formula: wound size = wound area of a day/wound area of a wound 0 day x 100% day. And (5) counting the results. Mice were sacrificed at treatment 3d and 8d, respectively. Homogenizing half of the tissue, diluting with PBS to appropriate ratio, coating on a flat plate, and taking a picture for recording; fixing half of the tissues by using paraformaldehyde, and observing the pathological change condition of the tissues by using HE staining and Masson staining; the immune tissue fluorescence detects the expression of IL-6, CD31, KRT5 in the tissue.
2.2 Data analysis
All results were statistically analyzed using SPSS17.0 software using analysis of variance (ANOVA) and expressed as mean ± standard deviation, with P <0.05 as significant difference, denoted P <0.05, denoted P <0.01, and denoted P <0.001.
2.3 Results of the experiment
The wound condition of the mice is shown in fig. 5, and at 0 day, the suppuration of the mouse wound and the red swelling around the wound can be observed, which indicates that the staphylococcus aureus successfully infects the mouse wound and the skin defect infection model is successfully prepared. At 0d-8d, the wound healing speed of the mice treated by the highly charged dressing (HC) obtained in example 1 is obviously faster than that of the blank group and the non-charged group (NC) in fig. 5 (a), the wound diameter within 8 days is counted and analyzed, and the result shows that the wound of the highly charged group in example 1 is obviously reduced after the next day, the wound healing of the blank group and the non-charged group is not obvious, the wound of the highly charged group mice in example 1 is basically replaced by new skin at the 8 th day, and the wound healing of the skin of the infected mice can be promoted by the charged surface (b in fig. 5). Half of the tissues were taken at 3 and 8 days after treatment to thin-coat the plates to verify the antibacterial effect of the charged membrane, and the results are shown in fig. 5, panel c, which shows that the bacterial colony units in the highly charged group are significantly reduced compared to the non-charged and blank groups at both 3 and 8 days, indicating that the charged surface can promote wound healing of infected skin in mice by inhibiting bacterial growth.
Three markers, IL-6, KRT5 and CD31, were selected to evaluate the healing of skin wounds in mice. Immunofluorescence results show that the expression of the IL-6 in the high-charge group is far lower than that in the non-charge group and the blank group at 3 days and 8 days, and the IL-6 always shows a descending trend, which indicates that the charged membrane inhibits the inflammation of infected wounds of mice; in addition, the expression of the keratin KRT5 is obviously increased in the high-charged group at 3 days, which shows that the high-charged group accelerates the proliferation and differentiation of epithelial cells and promotes the healing of skin wounds, and the KRT5 expression is reduced at 8 days, but the overall level is still higher than that of the non-charged group and the blank group, and accords with the trend reported in the literature; CD31 also showed higher activity in the high-charged group for 3 days, and no obvious difference was observed between the groups at 8 days, indicating that the repair of the early high-charged group promoted the formation of new blood vessels, which also indicates that the wound of the high-charged group healed better.
3. Air permeability test
The resulting dressings were tested for water vapor transmission using a C360M water vapor Transmission test System at 38 deg.C, 90% RH, with emphasis on observing water vapor transmission.
4. Piezoelectric constant
With ZJ-3AN quasistatic d 33 The tester measures the piezoelectric constant of the dressing.
TABLE 3
While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments. Many modifications and variations may be made to the exemplary embodiments of the present description without departing from the scope or spirit of the present invention. The scope of the claims is to be accorded the broadest interpretation so as to encompass all modifications and equivalent structures and functions.
Claims (10)
1. An antibacterial dressing based on a ferroelectric material, which is characterized in that the ferroelectric material comprises a ferroelectric high molecular polymer and/or inorganic ferroelectric particles, the inorganic ferroelectric particles account for 0-20% of the volume fraction of the ferroelectric high molecular polymer, and the diameter of the inorganic ferroelectric particles is 50 nm-500 nm.
2. The ferroelectric-material-based antimicrobial dressing of claim 1, comprising ferroelectric high molecular polymers and ferroelectric ceramic particles, and further comprising a porous structure located inside the dressing.
3. A preparation method of an antibacterial dressing based on a ferroelectric material is characterized by comprising the following steps:
(1) Preparing a composite material by using a ferroelectric high molecular polymer, ferroelectric ceramic particles and an inorganic pore-foaming agent; and
(2) Carrying out high-temperature treatment, corona polarization treatment and acid liquor treatment on the composite material in sequence; or sequentially carrying out corona polarization treatment, high-temperature treatment and acid liquor treatment.
4. The method for preparing an antibacterial dressing based on ferroelectric material according to claim 3, wherein the inorganic pore-forming agent comprises zinc oxide and/or calcium carbonate.
5. The method for preparing an antibacterial dressing based on ferroelectric material according to claim 3, wherein the ferroelectric ceramic particles comprise one or more of barium titanate, barium strontium titanate, bismuth ferrite, potassium sodium niobate, and lithium niobate; the ferroelectric high molecular polymer is at least one selected from the group consisting of polyvinylidene fluoride, polyvinylidene fluoride-hexafluoropropylene, polyvinylidene fluoride-trifluoroethylene, and polylactic acid.
6. The method for preparing an antibacterial dressing based on ferroelectric material according to claim 3, wherein the conditions of the high temperature treatment include treatment at a temperature of 80-150 ℃ for 5min-2h in air or vacuum, followed by natural cooling.
7. The method for preparing an antibacterial dressing based on ferroelectric material according to claim 3, wherein the conditions of the corona polarization treatment include a polarization field strength of 0.1kV/mm-10kV/mm, a polarization time of 1min-60min, a polarization medium of air or vacuum, and a polarization temperature of 25 ℃ -100 ℃.
8. The method for preparing an antibacterial dressing based on a ferroelectric material according to claim 3, wherein the acid treatment comprises treatment with an aqueous solution selected from hydrochloric acid, sulfuric acid, nitric acid, and carbonic acid for 3-30 hours.
9. Use of an antimicrobial dressing based on a ferroelectric material according to claim 1 or 2 for the preparation of an antimicrobial product.
10. Use according to claim 9, wherein the antibacterial product comprises a product for infections caused by skin defects, mucosal lesions, canker sores.
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| CN115634158A (en) * | 2022-12-21 | 2023-01-24 | 北京大学口腔医学院 | Long-acting antibacterial flowing composite resin or pit and fissure sealant composition for dentistry and application |
| CN115634159A (en) * | 2022-12-16 | 2023-01-24 | 北京大学口腔医学院 | Antibacterial toothpaste |
| CN115636666A (en) * | 2022-12-23 | 2023-01-24 | 北京大学口腔医学院 | Temperature change antibacterial composition, preparation method and application |
| CN115844736A (en) * | 2022-12-23 | 2023-03-28 | 北京大学口腔医学院 | Adhesive composition based on pyroelectric principle and application thereof |
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