CN113274539B - Self-powered wound patch and preparation method thereof - Google Patents
Self-powered wound patch and preparation method thereof Download PDFInfo
- Publication number
- CN113274539B CN113274539B CN202110476569.5A CN202110476569A CN113274539B CN 113274539 B CN113274539 B CN 113274539B CN 202110476569 A CN202110476569 A CN 202110476569A CN 113274539 B CN113274539 B CN 113274539B
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/70—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres
- D04H1/74—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres characterised by the method of forming fleeces or layers, e.g. reorientation of fibres the fibres being orientated, e.g. in parallel (anisotropic fleeces)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/20—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing organic materials
- A61L2300/23—Carbohydrates
- A61L2300/232—Monosaccharides, disaccharides, polysaccharides, lipopolysaccharides
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/41—Anti-inflammatory agents, e.g. NSAIDs
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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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/04—Materials for stopping bleeding
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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
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
Abstract
The invention discloses a self-powered wound patch, which comprises a PVDF/CNTs fiber patch, wherein drug-loaded PDA-CS hydrogel is coated on the PVDF/CNTs fiber patch; the drug-loaded PDA-CS hydrogel comprises the following components: dopamine DA hydrochloride, chitosan, curcumin or epidermal growth factor or asiaticoside, ammonium persulfate APS, N-methylene bisacrylamide MBA, azobisisobutyronitrile AIBN, deionized water and acetic acid solution. The invention achieves the aims of stopping bleeding and absorbing exudates through the water absorption characteristic of the hydrogel, and in the inflammation period, the chitosan hydrogel not only can improve a good microenvironment for wound healing through the anti-inflammatory antibacterial and moisturizing characteristics of the chitosan hydrogel, but also can trigger human macrophages to generate necrosis factor alpha, thereby triggering inflammation signals to trigger macrophage activities, increasing the level of cytokines in the wound and promoting wound healing. The invention also discloses a preparation method of the self-powered wound patch.
Description
Technical Field
The invention belongs to the technical field of medical biomaterials, relates to a self-powered wound patch, and further relates to a preparation method of the self-powered wound patch.
Background
Worldwide, acute and chronic wounds, such as war wounds, burns and diabetic foot ulcers, place a significant burden on patients and healthcare systems, respectively. In order to reduce the economic burden on patients and society, extensive research is currently being conducted to develop a technology capable of effectively treating wounds in a short time. Among the appropriate treatment strategies are the use of high-healing-rate wound dressings, which not only prevent infection, prevent adverse consequences of prolonged wound healing, reduce costs, and alleviate patient suffering. Wound dressings are an important component of the world's wound care industry and trade. The wound dressing is a key part for treating wounds which are difficult to heal, such as diabetic foot ulcer and the like, is widely used for wound nursing, and can protect the wounds and promote the healing of the wounds.
The traditional dressings such as gauze, cotton, bandages, hydrogel and the like which are widely applied clinically have the advantages of good biocompatibility, strong wound absorption capacity and capability of improving moist environment and being beneficial to repairing wound cell growth, but still have the defects of poor air permeability, poor antibacterial effect and the like, and most importantly, the healing of the wound is also dependent on the self recovery capacity of a patient and cannot play a role in promoting the accelerated healing of the wound. In order to accelerate wound healing, research shows that wound repair is closely related to the endogenous Electric Field (EF) of the wound, an endogenous direct current electric field is generated due to the disappearance of trans-epithelial potential difference after the wound is formed, the electric field is the most important direction signal for guiding epidermal cells to migrate to the center of the wound in the wound healing process, and the electric field can enhance cell migration and proliferation and is very important for a plurality of skin regeneration activities (such as collagen deposition, angiogenesis and re-epithelialization). Electrical Stimulation (ES) therapy simulates and enhances the effects of endogenous EF in the wound by applying an outer membrane to the wound site and is used to accelerate the healing of cutaneous wounds; its application in clinical practice is often limited by the bulky size of the device and the difficulty of achieving real-time treatment. In summary, it is not only necessary to prepare an outer membrane that can be applied to a wound surface to simulate and enhance an endogenous electric field of the wound surface to accelerate the healing of the skin wound surface, but also the material should have the characteristics of good biocompatibility and moisture retention and antibacterial property of the conventional dressing, so as to improve a good microenvironment for wound healing and further accelerate the healing rate of the wound.
Therefore, on the one hand, to meet the external environmental requirements for wound healing (moist, breathable), and on the other hand, to enhance efficient cell proliferation and migration to accelerate skin wound healing and facilitate clinical operation. This patent wants through combining piezoelectric material and natural hydrogel material to reach and to provide good microenvironment for wound healing, can also effectively strengthen cell migration and proliferation rate, and then reach the purpose that improves wound healing rate.
Chinese patent application No. 202011495354.X, published date: 2021.04.02, publication No. CN 112587712A discloses a composite bacterial cellulose dressing based on controllable nanofiber spatial structure and a preparation method thereof, and the composite bacterial cellulose dressing based on controllable nanofiber spatial structure and the preparation method thereof.
Chinese patent "preparation method of a bacteria-proof polylactic acid superfine nanofiber wound dressing" (application No. CN 201910307469.2, publication No. CN 110067036A, published date 2019.07.30) discloses a preparation method of a bacteria-proof polylactic acid superfine nanofiber wound dressing, wherein the pore diameter of the fiber of the polylactic acid superfine nanofiber wound dressing is smaller than the diameter of thallus, so that the bacteria-proof and anti-infection effects can be effectively achieved; and the polylactic acid superfine fiber has porous small gaps to promote hemostasis, and the high specific surface area can promote liquid absorption and enhance the release of drugs or antibiotics, so that the wound healing can be promoted while the inevitable secondary damage in the conventional dressing replacement is eliminated. However, the wound dressing prepared by the method is limited in large-area wounds and deep wounds due to yield problems, and the ultrafine pores may block oxygen components necessary for the wounds.
Chinese patent application No. 202011340886.6, published Japanese 2021.02.09, published Japanese CN 112336912A discloses a preparation method of a monatomic antibacterial, disinfectant and hemostatic hydrogel, which is prepared by mixing 40-75% of sodium hydroxymethyl cellulose, 5-10% of monatomic antibacterial disinfectant and 20-50% of deionized water. Compared with the traditional antibacterial, disinfectant and hemostatic material, the monoatomic antibacterial, disinfectant and hemostatic hydrogel has more excellent antibacterial, disinfectant and hemostatic performances. However, it can only play a role in antisepsis, disinfection and hemostasis, and cannot play a fundamental role in treating various diseases.
Chinese patent "A fibrous wound dressing for promoting wound healing and its preparation method" (application No. CN 202010886847.X, publication No. CN 111956858A, published: 2020.11.20) discloses a preparation method of a fibrous wound dressing for promoting wound healing, the method takes polyglutamic acid, Arabic gum, ferulic acid, keratin and procyanidine as main raw materials to prepare a fibrous wound dressing which is convenient to carry according to a proper proportion and processing mode, and the fibrous wound dressing has the advantages of resisting bacteria and diminishing inflammation, promoting healing, repairing skin, reducing scars and being convenient to use. However, the material prepared by the method cannot provide a moisture-preserving microenvironment for wound healing for the material, and the means for promoting wound healing is passive promotion, and cannot induce automatic healing of cells.
Disclosure of Invention
The invention aims to provide a self-powered wound patch, which achieves the purposes of stopping bleeding and absorbing exudates through the water absorption characteristic of hydrogel, and in the inflammation period, the chitosan hydrogel can improve a good microenvironment for wound healing through the anti-inflammatory, antibacterial and moisturizing characteristics of the chitosan hydrogel, and can trigger human macrophages to generate necrosis factor alpha, so that inflammation signals are triggered to trigger macrophage activities, the cytokine level in the wound is increased, and the wound healing is promoted.
Another object of the invention is to provide a method for manufacturing a self-powered wound patch.
The technical scheme adopted by the invention is that the self-powered wound patch comprises a PVDF/CNTs fiber patch, wherein drug-loaded PDA-CS hydrogel is coated on the PVDF/CNTs fiber patch;
the PVDF/CNTs fiber patch comprises the following components: polyvinylidene fluoride PVDF 4.5-7.5 g, modified carbon nano tube CNTs 0.5-3.21 g, acetone C3H6O7.5ml to 12ml, N, N-dimethylformamide DMF18ml to 22.5 ml;
the drug-loaded PDA-CS hydrogel comprises the following components: 0.01 to 0.05g of acid dopamine DA, 0.5 to 2g of chitosan CS, 0.01 to 0.05g of curcumin or epidermal growth factor or asiaticoside, 0.005 to 0.02g of ammonium persulfate APS, 0.005 to 0.02g of N, N-methylene bisacrylamide MBA, 0.005 to 0.02g of azobisisobutyronitrile AIBN, 5 to 15ml of deionized water and 15 to 50ml of 1 to 2 weight percent acetic acid solution.
The first aspect of the present invention is also characterized in that,
the modified carbon nano tube CNTs comprise the following components: 2-5 g of carbon nano tube CNT, 50-100 ml of concentrated nitric acid and 10-30 ml of concentrated sulfuric acid.
The invention also provides a preparation method of the self-powered wound patch, which is implemented by the following steps:
step 1, preparing modified carbon nano tube CNTs;
step 2, preparing PVDF/CNTs fiber, wherein the PVDF/CNTs fiber comprises the following components: polyvinylidene fluoride PVDF 4.5-7.5 g, modified carbon nano tube CNTs 0.5-3.21 g, acetone C3H6O7.5ml-12 ml, N-dimethylformamide DMF18 ml-22.5 ml;
step 3, weaving the PVDF/CNTs fiber prepared in the step 2 into a patch material with certain fiber orientation and porosity through a weaving process;
step 4, preparing the drug-loaded PDA-CS hydrogel, wherein the drug-loaded PDA-CS hydrogel comprises the following components: 0.01-0.05 g of acid dopamine DA, 0.5-2 g of chitosan CS, 0.01-0.05 g of curcumin or epidermal growth factor or asiaticoside, 0.005-0.02 g of ammonium persulfate APS, 0.005g-0.02 g of N, N-methylene bisacrylamide MBA0.005, 0.005-0.02 g of azobisisobutyronitrile AIBN, 5-15 ml of deionized water and 15-50 ml of 1-2 wt% acetic acid solution;
and 5, coating the drug-loaded PDA-CS hydrogel prepared in the step 4 on the patch material with certain fiber orientation and porosity in the step 3 to obtain the self-powered wound patch.
Another solution according to the invention is also characterised in that,
the step 1 specifically comprises the following steps:
step 1.1, measuring the following components: 2 g-5 g of carbon nano tube CNT, 50 ml-100 ml of concentrated nitric acid and 10 ml-30 ml of concentrated sulfuric acid;
step 1.2, mixing the concentrated nitric acid and the concentrated sulfuric acid which are measured in the step 1, adding the measured carbon nano tube, and dissolving by adopting ultrasonic waves;
and step 1.3, adding deionized water into the solution obtained after ultrasonic dissolution in the step 1.2, performing centrifugal washing until the pH value is 6.5, performing suction filtration on the obtained product, and drying in a vacuum furnace at 50 ℃ for 12-24 hours to obtain the modified carbon nanotube CNTs.
The ultrasonic dissolution in the step 1.2 is ultrasonic dissolution for 8 to 12 hours at the temperature of between 20 and 40 ℃.
The step 2 specifically comprises the following steps:
step 2.1, measuring the following components: polyvinylidene fluoride PVDF 4.5-7.5 g, modified carbon nano tube CNTs 0.5-3.21 g, acetone C3H6O7.5ml to 12ml, N-dimethylformamide DMF18ml ml to 22.5 ml;
step 2.2, uniformly dispersing the weighed modified carbon nano tube in acetone C3H6Stirring uniformly at room temperature in a mixed solution of O and N, N-dimethylformamide solution DMF, then adding the weighed polyvinylidene fluoride PVDF, and stirring uniformly at a constant temperature of 50-80 ℃ to prepare a spinning solution;
and 2.3, preparing the PVDF/CNTs fiber from the spinning solution prepared in the step 2.2 in a coagulating bath at 40-70 ℃ through a wet spinning device according to a certain draw ratio.
Acetone C in step 2.23H6The volume ratio of the O to the N, N-dimethylformamide solution DMF is 6:4 or 6: 2.
the step 4 specifically comprises the following steps:
step 4.1, measuring the following components: 0.01-0.05 g of acid dopamine DA, 0.5-2 g of chitosan CS, 0.01-0.05 g of curcumin or epidermal growth factor or asiaticoside, 0.005-0.02 g of ammonium persulfate APS, 0.005-0.02 g of N, N-methylene bisacrylamide MBA, 0.005g-0.02 g of azodiisobutyronitrile AIBNB, 5-15 ml of deionized water and 15-50 ml of 1-2 wt% acetic acid solution;
step 4.2, adding the chitosan CS measured in the step 4.1 into an acetic acid solution, and stirring and dissolving at the temperature of 30-60 ℃ to obtain a light yellow transparent liquid;
step 4.3, adding acid dopamine DA into deionized water with the pH value of 11, and stirring at room temperature to enable the acid dopamine DA to be self-polymerized into a PDA solution;
and 4.4, adding the light yellow transparent liquid prepared in the step 4.2 and curcumin or epidermal growth factor or asiaticoside into the PDA solution prepared in the step 4.3, stirring at normal temperature to uniformly disperse the liquid, then adding ammonium persulfate APS, N-methylene bisacrylamide MBA and azobisisobutyronitrile AIBN, and stirring at constant temperature of 50-90 ℃ to fully crosslink the liquid, thereby obtaining the drug-loaded PDA-CS hydrogel.
The invention has the beneficial effects that:
in the wound healing hemostasis period, the purposes of hemostasis and exudate absorption are achieved through the water absorption characteristic of the hydrogel, in the inflammation period, the chitosan hydrogel can improve a good microenvironment for wound healing through the anti-inflammatory antibacterial and wetting characteristics of the chitosan hydrogel, and can trigger human body macrophages to generate necrosis factor alpha (TNF-alpha), so that an inflammation signal is triggered to trigger macrophage activity, the level of cytokines in the wound is increased, and the wound healing is promoted; on the other hand, during the proliferation phase of wound healing, local electric field EFs can be provided by PVDF/CNTs with piezoelectric properties, which, in combination with oriented weaving technology, can allow oriented and ordered growth of cells, which is an important condition for the final formation of tissue or for the repair of tissue. In addition, the oriented superfine fiber bundle prepared by wet spinning is combined with a weaving technology, so that on one hand, the air permeability is realized by regulating and controlling the size of pores, and on the other hand, the oriented fiber is beneficial to promoting cell migration and proliferation and promoting wound healing to a certain extent. The piezoelectric repairing function is to convert mechanical force into electric signal, provide exogenous electric field, stimulate the directional migration, proliferation and differentiation of fibroblast, and further realize the accelerated healing of wound. Therefore, the invention realizes the purpose of accelerating wound healing by the synergistic effect of the regulation and control of the material structure and the piezoelectric performance of the material, has low production cost and no special requirement on production equipment, and has good application prospect in the field of biomedical materials.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a self-powered wound patch, which comprises a PVDF/CNTs fiber patch, wherein drug-loaded PDA-CS hydrogel is coated on the PVDF/CNTs fiber patch;
the PVDF/CNTs fiber patch comprises the following components: polyvinylidene fluoride PVDF 4.5-7.5 g, modified carbon nano tube CNTs 0.5-3.21 g, acetone C3H6O7.5ml to 12ml, N, N-dimethylformamide DMF18ml to 22.5ml, wherein the modified carbon nano tube CNTs comprise the following components: 2 g-5 g of carbon nano tube CNT, 50 ml-100 ml of concentrated nitric acid and 10 ml-30 ml of concentrated sulfuric acid;
the drug-loaded PDA-CS hydrogel comprises the following components: 0.01 to 0.05g of acid dopamine DA, 0.5 to 2g of chitosan CS, 0.01 to 0.05g of curcumin or epidermal growth factor or asiaticoside, 0.005 to 0.02g of ammonium persulfate APS, 0.005 to 0.02g of N, N-methylene bisacrylamide MBA, 0.005 to 0.02g of azobisisobutyronitrile AIBN, 5 to 15ml of deionized water and 15 to 50ml of 1 to 2 weight percent acetic acid solution.
The invention relates to a preparation method of a self-powered wound patch, which is implemented by the following steps:
step 1, preparing modified carbon nano tube CNTs; the method specifically comprises the following steps:
step 1.1, measuring the following components: 2 g-5 g of carbon nano tube CNT, 50 ml-100 ml of concentrated nitric acid and 10 ml-30 ml of concentrated sulfuric acid;
step 1.2, mixing the concentrated nitric acid and the concentrated sulfuric acid which are measured in the step 1, adding the measured carbon nano tube, and then ultrasonically dissolving for 8-12 h at the temperature of 20-40 ℃;
step 1.3, adding deionized water into the solution obtained after ultrasonic dissolution in the step 1.2, performing centrifugal washing until the pH value is 6.5, performing suction filtration on the obtained product, and drying in a vacuum furnace at 50 ℃ for 12-24 hours to obtain modified carbon nanotube CNTs;
step 2, preparing PVDF/CNTs fiber, wherein the PVDF/CNTs fiber comprises the following components: polyvinylidene fluoride PVDF 4.5-7.5 g, modified carbon nano tube CNTs 0.5-3.21 g, acetone C3H6O7.5ml-12 ml, N-dimethylformamide DMF18 ml-22.5 ml; the method specifically comprises the following steps:
step 2.1, measuring the following components: polyvinylidene fluoride PVDF 4.5-7.5 g, modified carbon nano tube CNTs 0.5-3.21 g, acetone C3H6O7.5ml to 12ml, N-dimethylformamide DMF18ml ml to 22.5 ml;
step 2.2, uniformly dispersing the weighed modified carbon nano tube in acetone C3H6Stirring uniformly at room temperature in a mixed solution of O and N, N-dimethylformamide solution DMF, adding the weighed polyvinylidene fluoride PVDF, stirring uniformly at a constant temperature of 50-80 ℃ to prepare a spinning solution, wherein acetone C3H6The volume ratio of the O to the N, N-dimethylformamide solution DMF is 6:4 or 6: 2;
and 2.3, preparing the PVDF/CNTs fiber from the spinning solution prepared in the step 2.2 in a coagulating bath at 40-70 ℃ through a wet spinning device according to a certain draw ratio.
Step 3, weaving the PVDF/CNTs fiber prepared in the step 2 into a patch material with certain fiber orientation and porosity through a weaving process;
step 4, preparing the drug-loaded PDA-CS hydrogel, wherein the drug-loaded PDA-CS hydrogel comprises the following components: 0.01-0.05 g of acid dopamine DA, 0.5-2 g of chitosan CS, 0.01-0.05 g of curcumin or epidermal growth factor or asiaticoside, 0.005-0.02 g of ammonium persulfate APS, 0.005-0.02 g of N, N-methylene bisacrylamide MBA, 0.005-0.02 g of azobisisobutyronitrile AIBN, 5-15 ml of deionized water and 15-50 ml of 1-2 wt% acetic acid solution; the method specifically comprises the following steps:
step 4.1, measuring the following components: 0.01-0.05 g of acid dopamine DA, 0.5-2 g of chitosan CS, 0.01-0.05 g of curcumin or epidermal growth factor or asiaticoside, 0.005-0.02 g of ammonium persulfate APS, 0.005-0.02 g of N, N-methylene bisacrylamide MBA, 0.005g-0.02 g of azodiisobutyronitrile AIBNB, 5-15 ml of deionized water and 15-50 ml of 1-2 wt% acetic acid solution;
step 4.2, adding the chitosan CS measured in the step 4.1 into an acetic acid solution, and stirring and dissolving at the temperature of 30-60 ℃ to obtain a light yellow transparent liquid;
step 4.3, adding acid dopamine DA into ph 11 deionized water, and stirring at room temperature to enable the acid dopamine DA to be self-polymerized into a PDA solution;
step 4.4, adding the light yellow transparent liquid prepared in the step 4.2 and curcumin or epidermal growth factor or asiaticoside into the PDA solution prepared in the step 4.3, stirring at normal temperature to uniformly disperse the liquid, then adding ammonium persulfate APS, N-methylene bisacrylamide MBA and azobisisobutyronitrile AIBN, and then stirring at constant temperature of 50-90 ℃ to fully crosslink the liquid, thereby obtaining the drug-loaded PDA-CS hydrogel;
and 5, coating the drug-loaded PDA-CS hydrogel prepared in the step 4 on the patch material with certain fiber orientation and porosity in the step 3 to obtain the self-powered wound patch.
The PVDF with piezoelectric property is combined with the drug-loaded PDA-CS hydrogel, on one hand, the purposes of stopping bleeding and absorbing exudates can be achieved through the water absorption property of the hydrogel in the wound healing hemostasis period, and in the inflammation period, the chitosan hydrogel not only can improve a good microenvironment for wound healing through the anti-inflammatory, antibacterial and wetting properties of the chitosan hydrogel, but also can trigger human body macrophages to generate necrosis factor alpha (TNF-alpha), so that an inflammation signal is triggered to trigger macrophage activity, the cytokine level in the wound is increased, and the wound healing is promoted; on the other hand, the local electric field EFs is provided by PVDF with piezoelectric property in the multiplication phase of wound healing, and the directional weaving technology is combined, so that cells can directionally and orderly grow, which is an important condition for finally forming tissues or repairing tissues. In addition, the oriented superfine fiber bundle prepared by wet spinning is combined with a weaving technology, so that on one hand, the air permeability is realized by regulating and controlling the size of pores, and on the other hand, the oriented fiber is beneficial to promoting cell migration and proliferation and promoting wound healing to a certain extent. The piezoelectric repairing function is to convert mechanical force into electric signal, provide exogenous electric field, stimulate the directional migration, proliferation and differentiation of fibroblast, and further realize the accelerated healing of wound. Therefore, the invention realizes the purpose of accelerating wound healing through the synergistic effect of the regulation and control of the material structure and the regulation and control of the piezoelectric property of the material.
Example 1
Step 1, preparation of modified CNTs:
adding 2g of CNT into 100ml of concentrated nitric acid-sulfuric acid solution with the volume ratio of 3:1 in a container, ultrasonically dissolving at 20 ℃ for 8h to remove impurities and amorphous carbon, introducing hydrophilic functional groups, then centrifugally washing with deionized water until the pH value is 6.5, filtering the obtained product, and drying in a vacuum furnace at 50 ℃ for 12h to obtain the modified CNT, namely CNTs.
Step 2, preparing PVDF/CNTs fiber:
0.5g of CNTs are homogeneously dispersed in 100ml of DMF C with a volume ratio of 6:43H6Adding 4.5g of PVDF powder into the O solution at room temperature after assisting magnetic stirring or mechanical stirring uniformly, dispersing uniformly at a constant temperature of 60 ℃ by assisting magnetic stirring or mechanical stirring to obtain a uniform spinning solution precursor, and preparing the PVDF/CNTs fiber in a deionized water coagulation bath at 60 ℃ by a wet spinning device under the condition that the draft ratio is 4;
step 3, weaving the PVDF/CNTs fiber prepared in the step 2 into a patch material with certain fiber orientation and porosity through a weaving process;
step 4, preparing medicine-carrying PDA-CS hydrogel;
firstly, 2.5g of chitosan is added into 12.5ml of 1wt% acetic acid solution in a container, and the mixture is stirred and dissolved under the assistance of magnetic stirring at the constant temperature of 30 ℃ to obtain light yellow transparent liquid; secondly, adding 0.02g of DA into 11.2ml of deionized water with the pH value of 11, and carrying out self-polymerization to obtain PDA by magnetic stirring or mechanical stirring at room temperature; adding 0.0025g of curcumin into the mixed solution of the two solutions, stirring for 30min, adding 0.01g of APS, 0.01g of MBA and 0.01g of AIBN, and carrying out magnetic stirring or mechanical stirring at the constant temperature of 60 ℃ to ensure that the curcumin is fully crosslinked and polymerized, thus obtaining the self-adhesive medicine-carrying PDA-CS hydrogel.
And 5, coating the self-adhesive hydrogel in the step 4 on the patch material with certain fiber orientation and porosity in the step 3, thereby obtaining the self-powered wound patch material.
Example 2
Step 1, preparation of modified CNTs:
adding 2g of CNT into 100ml of concentrated nitric acid-sulfuric acid solution with the volume ratio of 3:1 in a container, ultrasonically dissolving for 10h at 30 ℃ to remove impurities and amorphous carbon, introducing hydrophilic functional groups, then centrifugally washing with deionized water until the pH value is 6.5, filtering the obtained product, and drying in a vacuum furnace at 50 ℃ for 12h to obtain the modified CNT, namely CNTs.
Step 2, preparing PVDF/CNTs fiber:
1.125g CNTs are uniformly dispersed in 100ml DMF C with the volume ratio of 6:23H6Adding 4.5g of PVDF powder into the O solution at room temperature after assisting magnetic stirring or mechanical stirring uniformly, dispersing uniformly at a constant temperature of 60 ℃ by assisting magnetic stirring or mechanical stirring to obtain a uniform spinning solution precursor, and preparing the PVDF/CNTs fiber in a deionized water coagulation bath at 60 ℃ by a wet spinning device under the condition that the draft ratio is 5;
step 3, weaving the PVDF/CNTs fiber prepared in the step 2 into a patch material with certain fiber orientation and porosity through a weaving process;
step 4, preparing medicine-carrying PDA-CS hydrogel;
firstly, 2.5g of chitosan is added into 12.5ml of 1wt% acetic acid solution in a container, and the mixture is stirred and dissolved under the assistance of magnetic stirring at the constant temperature of 40 ℃ to obtain light yellow transparent liquid; secondly, adding 0.02g of DA into 11.2ml of deionized water with the pH value of 11, and carrying out self-polymerization to obtain PDA by magnetic stirring or mechanical stirring at room temperature; adding 0.0025g of epidermal growth factor into the mixed solution of the two solutions, stirring for 30min, adding 0.01g of APS, 0.02g of MBA and 0.02g of AIBN, and carrying out magnetic stirring or mechanical stirring at the constant temperature of 60 ℃ to ensure that the mixture is fully crosslinked and polymerized more fully, thus obtaining the self-adhesive medicine-carrying PDA-CS hydrogel.
And 5, coating the self-adhesive hydrogel in the step 4 on the patch material with certain fiber orientation and porosity in the step 3, thereby obtaining the self-powered wound patch material.
Example 3
Step 1, preparation of modified CNTs:
adding 2g of CNT into 100ml of concentrated nitric acid-sulfuric acid solution with the volume ratio of 3:1 in a container, ultrasonically dissolving for 10h at 30 ℃ to remove impurities and amorphous carbon, introducing hydrophilic functional groups, then centrifugally washing with deionized water until the pH value is 6.5, filtering the obtained product, and drying in a vacuum furnace at 50 ℃ for 24h to obtain the modified CNT, namely CNTs.
Step 2, preparing PVDF/CNTs fiber:
0.667g of CNTs were uniformly dispersed in 100ml of DMF C with a volume ratio of 6:43H6Adding 6g of PVDF powder into O solution at room temperature after assisting magnetic stirring or mechanical stirring uniformly, dispersing uniformly at a constant temperature of 60 ℃ by assisting magnetic stirring or mechanical stirring to obtain a uniform spinning solution precursor, and preparing the PVDF/CNTs fiber in a deionized water coagulation bath at 70 ℃ by a wet spinning device under the condition that the drafting ratio is 4;
step 3, weaving the PVDF/CNTs fiber prepared in the step 2 into a patch material with certain fiber orientation and porosity through a weaving process;
step 4, preparing medicine-carrying PDA-CS hydrogel;
firstly, 2.5g of chitosan is added into 12.5ml of 1wt% acetic acid solution in a container, and the mixture is stirred and dissolved under the assistance of magnetic stirring at the constant temperature of 30 ℃ to obtain light yellow transparent liquid; secondly, adding 0.02g of DA into 11.2ml of deionized water with the pH value of 11, and carrying out self-polymerization to obtain PDA by magnetic stirring or mechanical stirring at room temperature; adding 0.0025g of asiaticoside into the mixed solution of the two solutions, stirring for 50min, adding 0.01g of APS, 0.02g of MBA and 0.02g of AIBN, and carrying out magnetic stirring or mechanical stirring at the constant temperature of 60 ℃ to ensure that the two solutions are fully crosslinked and polymerized more fully, thus obtaining the self-adhesive medicament-carrying PDA-CS hydrogel.
And 5, coating the self-adhesive hydrogel in the step 4 on the patch material with certain fiber orientation and porosity in the step 3, thereby obtaining the self-powered wound patch material.
Example 4
Step 1, preparation of modified CNTs:
adding 2g of CNT into 100ml of concentrated nitric acid-sulfuric acid solution with the volume ratio of 3:1 in a container, ultrasonically dissolving for 10h at 30 ℃ to remove impurities and amorphous carbon, introducing hydrophilic functional groups, then centrifugally washing with deionized water until the pH value is 6.5, filtering the obtained product, and drying in a vacuum furnace at 50 ℃ for 24h to obtain the modified CNT, namely CNTs.
Step 2, preparing PVDF/CNTs fiber:
0.833g of CNTs are homogeneously dispersed in 100ml of DMF C with a volume ratio of 6:43H6Adding 7.5g of PVDF powder into the O solution at room temperature after assisting magnetic stirring or mechanical stirring uniformly, dispersing uniformly at a constant temperature of 60 ℃ by assisting magnetic stirring or mechanical stirring to obtain a uniform spinning solution precursor, and preparing the PVDF/CNTs fiber in a deionized water coagulation bath at 60 ℃ by a wet spinning device under the condition that the draft ratio is 6;
step 3, weaving the PVDF/CNTs fiber prepared in the step 2 into a patch material with certain fiber orientation and porosity through a weaving process;
step 4, preparing medicine-carrying PDA-CS hydrogel;
firstly, 2.5g of chitosan is added into 12.5ml of 1wt% acetic acid solution in a container, and the mixture is stirred and dissolved under the assistance of magnetic stirring at the constant temperature of 30 ℃ to obtain light yellow transparent liquid; secondly, adding 0.02g of DA into 11.2ml of deionized water with the pH value of 11, and carrying out self-polymerization to obtain PDA by magnetic stirring or mechanical stirring at room temperature; adding 0.0025g of curcumin into the mixed solution of the two solutions, stirring for 50min, adding 0.01g of APS, 0.02g of MBA and 0.02g of AIBN, and carrying out magnetic stirring or mechanical stirring at the constant temperature of 60 ℃ to ensure that the curcumin is fully crosslinked and polymerized, thus obtaining the self-adhesive medicine-carrying PDA-CS hydrogel.
And 5, coating the self-adhesive hydrogel in the step 4 on the patch material with certain fiber orientation and porosity in the step 3, thereby obtaining the self-powered wound patch material.
Example 5
Step 1, preparation of modified CNTs:
adding 2g of CNT into 100ml of concentrated nitric acid-sulfuric acid solution with the volume ratio of 3:1 in a container, ultrasonically dissolving for 10h at 30 ℃ to remove impurities and amorphous carbon, introducing hydrophilic functional groups, then centrifugally washing with deionized water until the pH value is 6.5, filtering the obtained product, and drying in a vacuum furnace at 50 ℃ for 24h to obtain the modified CNT, namely CNTs.
Step 2, preparing PVDF/CNTs fiber:
1.5g of CNTs are homogeneously dispersed in 100ml of DMF C with a volume ratio of 6:43H6Adding 6g of PVDF powder into O solution at room temperature after assisting magnetic stirring or mechanical stirring uniformly, dispersing uniformly at a constant temperature of 60 ℃ by assisting magnetic stirring or mechanical stirring to obtain a uniform spinning solution precursor, and preparing the PVDF/CNTs fiber in a deionized water coagulation bath at 60 ℃ by a wet spinning device under the condition that the drafting ratio is 5;
step 3, weaving the PVDF/CNTs fiber prepared in the step 2 into a patch material with certain fiber orientation and porosity through a weaving process;
step 4, preparing medicine-carrying PDA-CS hydrogel;
firstly, 2.5g of chitosan is added into 12.5ml of 1wt% acetic acid solution in a container, and the mixture is stirred and dissolved under the assistance of magnetic stirring at the constant temperature of 30 ℃ to obtain light yellow transparent liquid; secondly, adding 0.02g of DA into 11.2ml of deionized water with the pH value of 11, and carrying out self-polymerization to obtain PDA by magnetic stirring or mechanical stirring at room temperature; adding 0.0025g of asiaticoside into the mixed solution of the two solutions, stirring for 30min, adding 0.01g of APS, 0.02g of MBA and 0.02g of AIBN, and carrying out magnetic stirring or mechanical stirring at the constant temperature of 60 ℃ to ensure that the two solutions are fully crosslinked and polymerized more fully, thus obtaining the self-adhesive medicament-carrying PDA-CS hydrogel.
And 5, coating the self-adhesive hydrogel in the step 4 on the patch material with certain fiber orientation and porosity in the step 3, thereby obtaining the self-powered wound patch material.
Claims (6)
1. A self-powered wound patch is characterized by comprising a PVDF/CNTs fiber patch, wherein drug-loaded PDA-CS hydrogel is coated on the PVDF/CNTs fiber patch;
the PVDF/CNTs fiber patch comprises the following components: polyvinylidene fluoride PVDF4.5g-7.5 g, modified carbon nano tube CNTs0.5g-3.21 g, acetone C3H6O7.5ml-12 ml, N, N-dimethylformamide DMF18 ml-22.5 ml;
the drug-loaded PDA-CS hydrogel comprises the following components: 0.01g-0.05 g of dopamine hydrochloride (DAD), 0.5g-2 g of Chitosan (CSS), 0.01 g-0.05 g of curcumin or epidermal growth factor or asiaticoside, 0.005g-0.02 g of Ammonium Persulfate (APS), 0.005g-0.02 g of N, N-Methylene Bisacrylamide (MBA), 0.005g-0.02 g of Azodiisobutyronitrile (AIBNB), 5 ml-15 ml of deionized water, and 15ml-50ml of 1wt% l-2 wt% acetic acid solution;
the preparation method of the self-powered wound patch is implemented according to the following steps:
step 1, preparing modified carbon nano tube CNTs;
step 2, preparing PVDF/CNTs fiber, wherein the PVDF/CNTs fiber comprises the following components: polyvinylidene fluoride PVDF4.5g-7.5 g, modified carbon nano tube CNTs0.5g-3.21 g, acetone C3H6O7.5ml-12 ml, N-dimethylformamide DMF18 ml-22.5 ml;
the method specifically comprises the following steps:
step 2.1, measuring the following components: polyvinylidene fluoride PVDF4.5g-7.5 g, modified carbon nano tube CNTs0.5g-3.21 g, acetone C3H6O7.5ml-12 ml, N-dimethylformamide DMF18 ml-22.5 ml;
step 2.2, uniformly dispersing the weighed modified carbon nano tube in acetone C3H6Stirring uniformly at room temperature in a mixed solution of O and N, N-dimethylformamide solution DMF, then adding the weighed polyvinylidene fluoride PVDF, and stirring uniformly at a constant temperature of 50-80 ℃ to prepare a spinning solution;
step 2.3, preparing the PVDF/CNTs fiber from the spinning solution prepared in the step 2.2 in a coagulating bath at 40-70 ℃ through a wet spinning device according to a certain draw ratio;
step 3, weaving the PVDF/CNTs fiber prepared in the step 2 into a patch material with certain fiber orientation and porosity through a weaving process;
step 4, preparing the drug-loaded PDA-CS hydrogel, wherein the drug-loaded PDA-CS hydrogel comprises the following components: 0.01g-0.05 g of dopamine hydrochloride (DAD), 0.5g-2 g of Chitosan (CSS), 0.01 g-0.05 g of curcumin or epidermal growth factor or asiaticoside, 0.005g-0.02 g of Ammonium Persulfate (APS), 0.005g-0.02 g of N, N-Methylene Bisacrylamide (MBA), 0.005g-0.02 g of Azodiisobutyronitrile (AIBNB), 5 ml-15 ml of deionized water and 15ml-50ml of 1wt% -2wt% acetic acid solution;
and 5, coating the drug-loaded PDA-CS hydrogel prepared in the step 4 on the patch material with certain fiber orientation and porosity in the step 3 to obtain the self-powered wound patch.
2. A self-powered wound patch according to claim 1, wherein the modified carbon nanotube CNTs comprise the following composition: carbon nano tube CNT2 g-5 g, concentrated nitric acid 50 ml-100 ml, concentrated sulfuric acid 10 ml-30 ml.
3. A self-powered wound patch according to claim 1, wherein step 1 is in particular:
step 1.1, measuring the following components: carbon nano tube CNT2 g-5 g, concentrated nitric acid 50 ml-100 ml, concentrated sulfuric acid 10 ml-30 ml;
step 1.2, mixing the concentrated nitric acid and the concentrated sulfuric acid which are measured in the step 1, adding the measured carbon nano tube, and dissolving by adopting ultrasonic waves;
and step 1.3, adding deionized water into the solution subjected to ultrasonic dissolution in the step 1.2, performing centrifugal washing until the pH is =6.5, performing suction filtration on the obtained product, and drying in a vacuum furnace at 50 ℃ for 12-24 hours to obtain the modified carbon nanotube CNTs.
4. A self-powered wound patch according to claim 3, wherein the ultrasonic dissolution in step 1.2 is ultrasonic dissolution at 20-40 ℃ for 8-12 h.
5. A self-powered wound patch according to claim 4, wherein acetone C in step 2.23H6The volume ratio of the O to the N, N-dimethylformamide solution DMF is 6:4 or 6: 2.
6. a self-powered wound patch according to claim 5, wherein step 4 is in particular:
step 4.1, measuring the following components: 0.01g-0.05 g of dopamine hydrochloride (DAD), 0.5g-2 g of Chitosan (CSS), 0.01 g-0.05 g of curcumin or epidermal growth factor or asiaticoside, 0.005g-0.02 g of Ammonium Persulfate (APS), 0.005g-0.02 g of N, N-Methylene Bisacrylamide (MBA), 0.005g-0.02 g of Azodiisobutyronitrile (AIBNB), 5 ml-15 ml of deionized water and 15ml-50ml of 1wt% -2wt% acetic acid solution;
step 4.2, adding the chitosan CS measured in the step 4.1 into an acetic acid solution, and stirring and dissolving at the temperature of 30-60 ℃ to obtain a light yellow transparent liquid;
step 4.3, adding acid dopamine DA into deionized water with pH =11, and stirring at room temperature to enable the acid dopamine DA to be self-polymerized into a PDA solution;
and 4.4, adding the light yellow transparent liquid prepared in the step 4.2 and curcumin or epidermal growth factor or asiaticoside into the PDA solution prepared in the step 4.3, stirring at normal temperature to uniformly disperse the liquid, then adding ammonium persulfate APS, N-methylene bisacrylamide MBA and azobisisobutyronitrile AIBN, and stirring at constant temperature of 50-90 ℃ to fully crosslink the liquid, thereby obtaining the drug-loaded PDA-CS hydrogel.
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