CN115501376A - Gel type antibacterial medical band-aid and preparation method thereof - Google Patents
Gel type antibacterial medical band-aid and preparation method 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
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
- A61L15/46—Deodorants or malodour counteractants, e.g. to inhibit the formation of ammonia or bacteria
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- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/26—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/28—Polysaccharides or their derivatives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/32—Proteins, polypeptides; Degradation products or derivatives thereof, e.g. albumin, collagen, fibrin, gelatin
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- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/42—Use of materials characterised by their function or physical properties
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- 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
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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
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- 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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- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
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- 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
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Abstract
The invention relates to the technical field of medical band-aid, and particularly discloses a gel type antibacterial medical band-aid and a preparation method thereof, wherein the scheme is that components such as chitosan, gelatin, epidermal cell growth factor and the like are coated and dried on the surface of a medical adhesive tape to form the gel type medical band-aid; during preparation of the scheme, firstly, carrying out sulfhydrylation modification on chitosan, modifying the chitosan by using N-acetylcysteine to obtain sulfhydrylated chitosan, modifying gelatin by using methacrylic anhydride to obtain methacrylic gelatin containing double-bond groups, and polymerizing the methacrylic gelatin and the sulfhydrylated chitosan under the action of ultraviolet light to obtain antibacterial gel; the medical adhesive bandage has the advantages that the process design is reasonable, the component distribution is proper, the prepared medical adhesive bandage has excellent antibacterial performance, the wound healing can be promoted, the medical adhesive bandage has great potential in the field of wound care, and the practicability is high.
Description
Technical Field
The invention relates to the technical field of medical band-aid, in particular to a gel type antibacterial medical band-aid and a preparation method thereof.
Background
The adhesive bandage is commonly called as sterilizing elastic adhesive bandage, and is one of the most common medical articles for emergency treatment. The band-aid mainly comprises a plain cloth adhesive tape and a water absorption pad, has the functions of stopping bleeding and protecting wound, and can be used by patients according to different requirements.
Most of the band-aids purchased in the market adopt water-absorbing cloth pads, but the nursing effect is poor, and the antibacterial performance cannot meet the requirements of people, so that the technical problem to be solved urgently is how to improve the antibacterial performance of the band-aids and promote wound healing.
Disclosure of Invention
The invention aims to provide a gel-type antibacterial medical band-aid and a preparation method thereof, and aims to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of a gel type antibacterial medical band-aid comprises the following steps:
(1) Mixing 0.5g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 2mL of deionized water, stirring for 20-30 min, adding 150g of N-acetylcysteine after stirring uniformly, continuing stirring for 20-30 min, adding 6mL of polylysine aqueous solution, reacting for 4-6 h at 25-30 ℃, washing and drying to obtain thiolated polylysine;
(2) Mixing thiolated chitosan, thiolated polylysine and deionized water, and uniformly stirring to obtain a solution A; mixing methacrylic acid gelatin and deionized water, and uniformly stirring to obtain a solution B; mixing the solution A and the solution B with a photoinitiator, and adding an epidermal cell growth factor to obtain an antibacterial gel solution;
(3) Coating the antibacterial gel liquid on the middle part of the medical adhesive tape, irradiating by ultraviolet light for 20-25 min, standing for 3-4 h, and packaging to obtain a finished product.
According to an optimized scheme, in the step (2), the concentration of the solution A is 2.5-3 wt%, wherein the mass ratio of the thiolated chitosan to the thiolated polylysine is 4:1; the concentration of the solution B is 2.5-3 wt%.
According to an optimized scheme, in the step (3), the mass ratio of the solution A to the solution B is 1:1; the dosage of the photoinitiator is 3 to 4 weight percent of the antibacterial gel liquid; the dosage of the epidermal cell growth factor is 8-10 wt% of the antibacterial gel liquid.
In the optimized scheme, in the step (2), the preparation steps of the thiolated chitosan are as follows: mixing 1g of chitosan, 0.7g of 1-hydroxybenzotriazole and 100mL of deionized water, stirring uniformly, adding a mixed solution of N-acetylcysteine, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 50mL of deionized water, adjusting the pH value to 5 by sodium hydroxide, stirring and reacting for 2-3 h at 25-30 ℃, separating out ethanol, washing and drying to obtain the thiolated chitosan.
In an optimized scheme, the molar ratio of the chitosan to the N-acetyl cysteine is 1:2; the mol ratio of the N-acetyl cysteine to the 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide hydrochloride is 2:1.
according to a more optimized scheme, in the step (2), the preparation steps of the methacrylic acid gelatin are as follows: taking 5g of gelatin and 50mL of PBS buffer solution, stirring the gelatin and the 50mL of PBS buffer solution at 45-55 ℃ until the gelatin is dissolved, adding sodium hydroxide to adjust the pH value to 7, adding 5mL of methacrylic anhydride, keeping the temperature and stirring the mixture for 12-16 h, dialyzing the mixture for 2 days in a dialysis bag, and freeze-drying the dialyzed mixture to obtain the methacrylic gelatin.
According to an optimized scheme, in the step (2), adding acryloyl chitosan into the solution B, mixing methacrylic acid gelatin, acryloyl chitosan and deionized water, and uniformly stirring to obtain the solution B, wherein the mass ratio of the acryloyl chitosan to the methacrylic acid gelatin is 3:2.
in an optimized scheme, in the step (2), the preparation steps of the acryloyl chitosan are as follows: mixing 5g of chitosan and 30mL of methanesulfonic acid, stirring at 25-35 ℃ for 25-30 min, cooling to 0 ℃, stirring for 1-2 h, adding 10mL of acryloyl chloride, continuously stirring for 7-8 h to obtain a reaction solution, and settling through an acetone-ether mixed solution, performing centrifugal separation, washing and drying to obtain the acryloyl chitosan.
According to an optimized scheme, the adhesive bandage is prepared by the preparation method of the gel-type antibacterial medical adhesive bandage.
Compared with the prior art, the invention has the following beneficial effects:
the invention discloses a gel type antibacterial medical band-aid and a preparation method thereof, wherein the scheme is that components such as chitosan, gelatin, epidermal cell growth factor and the like are coated and dried on the surface of a medical adhesive tape to form the gel type medical band-aid; during preparation of the scheme, firstly, carrying out sulfhydrylation modification on chitosan, modifying the chitosan by using N-acetylcysteine to obtain sulfhydrylated chitosan, modifying gelatin by using methacrylic anhydride to obtain methacrylic gelatin containing double-bond groups, and polymerizing the methacrylic gelatin and the sulfhydrylated chitosan under the action of ultraviolet light to obtain antibacterial gel; the gelatin can exist as protein, on one hand, the gelatin and the epidermal growth factor are matched with each other to promote the healing of the wound, on the other hand, the existence of the gelatin can also improve the adhesion performance between the antibacterial gel and the medical adhesive tape, and by utilizing the mutual cross-linking and matching of the methacrylic acid gelatin and the thiolated chitosan, the obtained medical band-aid has excellent antibacterial performance and biocompatibility, and can promote the healing of the wound.
In the scheme, in order to further improve the antibacterial performance of the medical band-aid, other antibacterial particles are generally introduced in the prior art, but the introduction of the single antibacterial particles can influence the mechanical performance of the gel, and the particles are easy to fall off in the gel, so that the antibacterial performance is relatively unstable, and in order to avoid the technical problem, the scheme introduces thiolated polylysine, and the thiolate is grafted on the surface of the polylysine after being activated by 1-ethyl- (3-dimethylaminopropyl) carbodiimide, so that the polylysine participates in a crosslinking reaction under the action of ultraviolet light, and the comprehensive antibacterial performance of the product is ensured; in the scheme, the mass ratio of thiolated chitosan to thiolated polylysine is defined to be 4: 1', under the parameter, the scheme can further improve the antibacterial property while ensuring the mechanical property, and the comprehensive effect is more excellent.
The scheme also discloses another more excellent scheme in practical development, and the acryloyl chitosan is introduced into the system, and the mass ratio of the acryloyl chitosan to the methacrylic acid gelatin is defined as 3: 2', part of acryloyl chitosan is used for replacing methacrylic acid gelatin, so that the adaptability of the acryloyl chitosan and thiolated chitosan is more excellent, and the antibacterial performance of the product can be further improved.
The invention discloses a gel type antibacterial medical band-aid and a preparation method thereof, the process design is reasonable, the component distribution is proper, the prepared medical band-aid not only has excellent antibacterial performance, but also can promote wound healing, and has great potential and high practicability in the field of wound care.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In this example, chitosan was purchased from Sigma-Aldrich chemical reagents ltd; 1-hydroxybenzotriazole was purchased from Ron's reagent; n-acetyl cysteine was purchased from McClin Biochemical Co., ltd; 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, 1-ethyl- (3-dimethylaminopropyl) carbodiimide, polylysine were purchased from Sasa chemical technology (Shanghai) Co., ltd; gelatin is purchased from national pharmaceutical chemicals reagents, ltd; methacrylic anhydride, PBS buffer solution was purchased from alatin. The medical adhesive tape is a commercially available medical adhesive tape and can be replaced according to actual requirements.
Example 1:
a preparation method of a gel type antibacterial medical band-aid comprises the following steps:
(1) Mixing 1g of chitosan, 0.7g of 1-hydroxybenzotriazole and 100mL of deionized water, stirring uniformly, adding a mixed solution of N-acetylcysteine, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 50mL of deionized water, adjusting the pH value to 5 by using sodium hydroxide, stirring for reacting for 3 hours at 25 ℃, separating out ethanol, washing and drying to obtain the thiolated chitosan. The molar ratio of the chitosan to the N-acetyl cysteine is 1:2; the mol ratio of the N-acetyl cysteine to the 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide hydrochloride is 2:1.
mixing 0.5g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 2mL of deionized water, stirring for 20min, adding 150g of N-acetylcysteine after stirring uniformly, continuing stirring for 20min, adding 6mL of polylysine aqueous solution, reacting for 6h at 25 ℃, washing and drying to obtain the thiolated polylysine. The concentration of the polylysine aqueous solution is 0.5g/mL; the mass ratio of the N-acetylcysteine to the polylysine aqueous solution is 50:1.
(2) Taking 5g of gelatin and 50mL of PBS buffer solution, stirring the mixture at 45 ℃ until the gelatin and the 50mL of PBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH value to 7, adding 5mL of methacrylic anhydride, keeping the temperature and stirring the mixture for 12 hours, dialyzing the mixture in a dialysis bag for 2 days, and freeze-drying the dialyzed mixture to obtain the methacrylic gelatin.
(3) Mixing thiolated chitosan, thiolated polylysine and deionized water, and uniformly stirring to obtain a solution A; the concentration of the solution A is 3wt%, wherein the mass ratio of thiolated chitosan to thiolated polylysine is 4:1. mixing methacrylic acid gelatin and deionized water, and uniformly stirring to obtain a solution B; the concentration of the solution B was 3wt%. Mixing the solution A, the solution B and a photoinitiator, and adding epidermal cell growth factors to obtain an antibacterial gel solution; the mass ratio of the solution A to the solution B is 1:1; the dosage of the photoinitiator is 4wt% of the antibacterial gel liquid; the dosage of the epidermal cell growth factor is 10wt% of the antibacterial gel liquid.
(4) Coating antibacterial gel solution on the middle part of the medical adhesive tape, irradiating with 365nm ultraviolet light for 20min, standing for 3h, and packaging to obtain the final product. The coating thickness of the antibacterial gel liquid is 2mm.
Example 2:
a preparation method of a gel type antibacterial medical band-aid comprises the following steps:
(1) Mixing 1g of chitosan, 0.7g of 1-hydroxybenzotriazole and 100mL of deionized water, stirring uniformly, adding a mixed solution of N-acetylcysteine, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 50mL of deionized water, adjusting the pH value to 5 by using sodium hydroxide, stirring and reacting for 2.5h at 28 ℃, separating out ethanol, washing and drying to obtain the thiolated chitosan. The molar ratio of the chitosan to the N-acetylcysteine is 1:2; the mol ratio of the N-acetyl cysteine to the 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide hydrochloride is 2:1.
mixing 0.5g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 2mL of deionized water, stirring for 25min, adding 150g of N-acetylcysteine after stirring uniformly, continuing stirring for 25min, adding 6mL of polylysine aqueous solution, reacting for 5h at 28 ℃, washing and drying to obtain the thiolated polylysine. The concentration of the polylysine aqueous solution is 0.5g/mL; the mass ratio of the N-acetylcysteine to the polylysine aqueous solution is 50:1.
(2) Taking 5g of gelatin and 50mL of PBS buffer solution, stirring the mixture at 50 ℃ until the gelatin and the 50mL of PBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH value to 7, adding 5mL of methacrylic anhydride, keeping the temperature and stirring the mixture for 14 hours, dialyzing the mixture for 2 days in a dialysis bag, and freeze-drying the dialyzed mixture to obtain the methacrylic gelatin.
(3) Mixing thiolated chitosan, thiolated polylysine and deionized water, and uniformly stirring to obtain a solution A; the concentration of the solution A is 3wt%, wherein the mass ratio of thiolated chitosan to thiolated polylysine is 4:1. mixing methacrylic acid gelatin and deionized water, and uniformly stirring to obtain a solution B; the concentration of the solution B was 3wt%. Mixing the solution A, the solution B and a photoinitiator, and adding epidermal cell growth factors to obtain an antibacterial gel solution; the mass ratio of the solution A to the solution B is 1:1; the dosage of the photoinitiator is 4wt% of the antibacterial gel liquid; the dosage of the epidermal cell growth factor is 10wt% of the antibacterial gel liquid.
(4) Coating antibacterial gel solution on the middle part of the medical adhesive tape, irradiating with 365nm ultraviolet light for 25min, standing for 3.5h, and packaging to obtain the final product. The coating thickness of the antibacterial gel liquid is 2mm.
Example 3:
a preparation method of a gel type antibacterial medical band-aid comprises the following steps:
(1) Mixing 1g of chitosan, 0.7g of 1-hydroxybenzotriazole and 100mL of deionized water, uniformly stirring, adding a mixed solution of N-acetylcysteine, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 50mL of deionized water, adjusting the pH value to 5 by using sodium hydroxide, stirring and reacting for 2 hours at the temperature of 30 ℃, precipitating ethanol, washing and drying to obtain the thiolated chitosan. The molar ratio of the chitosan to the N-acetyl cysteine is 1:2; the molar ratio of the N-acetylcysteine to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 2:1.
and (2) mixing 0.5g of 1-ethyl- (3-dimethylaminopropyl) carbonyldiimine with 2mL of deionized water, stirring for 30min, adding 150g of N-acetylcysteine after stirring uniformly, continuing stirring for 30min, adding 6mL of polylysine aqueous solution, reacting for 4h at 30 ℃, washing and drying to obtain thiolated polylysine. The concentration of the polylysine aqueous solution is 0.5g/mL; the mass ratio of the N-acetylcysteine to the polylysine aqueous solution is 50:1.
(2) Taking 5g of gelatin and 50mL of PBS buffer solution, stirring the mixture at 55 ℃ until the gelatin and the 50mL of PBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH value to 7, adding 5mL of methacrylic anhydride, keeping the temperature and stirring the mixture for 12 hours, dialyzing the mixture for 2 days in a dialysis bag, and freeze-drying the dialyzed mixture to obtain the methacrylic gelatin.
(3) Mixing thiolated chitosan, thiolated polylysine and deionized water, and uniformly stirring to obtain a solution A; the concentration of the solution A is 3wt%, wherein the mass ratio of thiolated chitosan to thiolated polylysine is 4:1. mixing methacrylic acid gelatin and deionized water, and uniformly stirring to obtain a solution B; the concentration of the solution B was 3wt%. Mixing the solution A, the solution B and a photoinitiator, and adding epidermal cell growth factors to obtain an antibacterial gel solution; the mass ratio of the solution A to the solution B is 1:1; the dosage of the photoinitiator is 4wt% of the antibacterial gel liquid; the dosage of the epidermal cell growth factor is 10wt% of the antibacterial gel liquid.
(4) Coating antibacterial gel solution on the middle part of the medical adhesive tape, irradiating with 365nm ultraviolet light for 25min, standing for 4h, and packaging to obtain the final product. The coating thickness of the antibacterial gel liquid is 2mm.
Example 4: the acryloyl chitosan is introduced on the basis of the example 3.
A preparation method of a gel type antibacterial medical band-aid comprises the following steps:
(1) Mixing 1g of chitosan, 0.7g of 1-hydroxybenzotriazole and 100mL of deionized water, uniformly stirring, adding a mixed solution of N-acetylcysteine, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 50mL of deionized water, adjusting the pH value to 5 by using sodium hydroxide, stirring and reacting for 2 hours at the temperature of 30 ℃, precipitating ethanol, washing and drying to obtain the thiolated chitosan. The molar ratio of the chitosan to the N-acetyl cysteine is 1:2; the mol ratio of the N-acetyl cysteine to the 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide hydrochloride is 2:1.
mixing 0.5g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 2mL of deionized water, stirring for 30min, adding 150g of N-acetylcysteine after stirring uniformly, continuing stirring for 30min, adding 6mL of polylysine aqueous solution, reacting for 4h at 30 ℃, washing and drying to obtain the thiolated polylysine. The concentration of the polylysine aqueous solution is 0.5g/mL; the mass ratio of the N-acetylcysteine to the polylysine aqueous solution is 50:1.
(2) Taking 5g of gelatin and 50mL of PBS buffer solution, stirring the mixture at 55 ℃ until the gelatin and the 50mL of PBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH value to 7, adding 5mL of methacrylic anhydride, keeping the temperature and stirring the mixture for 12 hours, dialyzing the mixture for 2 days in a dialysis bag, and freeze-drying the dialyzed mixture to obtain the methacrylic gelatin.
Mixing 5g of chitosan and 30mL of methanesulfonic acid, stirring at 35 ℃ for 25min, cooling to 0 ℃, stirring for 1.5h, adding 10mL of acryloyl chloride, continuously stirring for 7.5h to obtain a reaction solution, settling by using a mixed solution of acetone and diethyl ether, performing centrifugal separation, washing and drying to obtain the acryloyl chitosan.
(3) Mixing thiolated chitosan, thiolated polylysine and deionized water, and uniformly stirring to obtain a solution A; the concentration of the solution A is 3wt%, wherein the mass ratio of the thiolated chitosan to the thiolated polylysine is 4:1. mixing methacrylic acid gelatin, acryloyl chitosan and deionized water, and uniformly stirring to obtain a solution B; the concentration of the solution B is 3wt%, wherein the mass ratio of the acryloyl chitosan to the methacrylic acid gelatin is 3:2.
mixing the solution A, the solution B and a photoinitiator, and adding epidermal cell growth factors to obtain an antibacterial gel solution; the mass ratio of the solution A to the solution B is 1:1; the dosage of the photoinitiator is 4wt% of the antibacterial gel liquid; the dosage of the epidermal cell growth factor is 10wt% of the antibacterial gel liquid.
(4) Coating antibacterial gel solution on the middle part of the medical adhesive tape, irradiating with 365nm ultraviolet light for 25min, standing for 4h, and packaging to obtain the final product. The coating thickness of the antibacterial gel liquid is 2mm.
Comparative example 1: with example 4 as a control, no thiolated polylysine was introduced in comparative example 1.
A preparation method of a gel type antibacterial medical band-aid comprises the following steps:
(1) Mixing 0.5g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 2mL of deionized water, stirring for 30min, adding 150g of N-acetylcysteine after stirring uniformly, continuing stirring for 30min, adding 6mL of polylysine aqueous solution, reacting for 4h at 30 ℃, washing and drying to obtain the thiolated polylysine. The concentration of the polylysine aqueous solution is 0.5g/mL; the mass ratio of the N-acetylcysteine to the polylysine aqueous solution is 50:1.
(2) Taking 5g of gelatin and 50mL of PBS buffer solution, stirring the mixture at 55 ℃ until the gelatin and the 50mL of PBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH value to 7, adding 5mL of methacrylic anhydride, keeping the temperature and stirring the mixture for 12 hours, dialyzing the mixture for 2 days in a dialysis bag, and freeze-drying the dialyzed mixture to obtain the methacrylic gelatin.
Mixing 5g of chitosan and 30mL of methanesulfonic acid, stirring at 35 ℃ for 25min, cooling to 0 ℃, stirring for 1.5h, adding 10mL of acryloyl chloride, continuously stirring for 7.5h to obtain a reaction solution, settling by using a mixed solution of acetone and diethyl ether, performing centrifugal separation, washing and drying to obtain the acryloyl chitosan.
(3) Mixing thiolated chitosan with deionized water, and uniformly stirring to obtain a solution A; the concentration of the solution A was 3wt%. Mixing methacrylic acid gelatin, acryloyl chitosan and deionized water, and uniformly stirring to obtain a solution B; the concentration of the solution B is 3wt%, wherein the mass ratio of the acryloyl chitosan to the methacrylic acid gelatin is 3:2.
mixing the solution A, the solution B and a photoinitiator, and adding epidermal cell growth factors to obtain an antibacterial gel solution; the mass ratio of the solution A to the solution B is 1:1; the dosage of the photoinitiator is 4wt% of the antibacterial gel liquid; the dosage of the epidermal cell growth factor is 10wt% of the antibacterial gel liquid.
(4) Coating antibacterial gel solution on the middle part of the medical adhesive tape, irradiating with 365nm ultraviolet light for 25min, standing for 4h, and packaging to obtain the final product. The coating thickness of the antibacterial gel liquid is 2mm.
Comparative example 2: in comparative example 2, no epidermal growth factor was introduced, using example 4 as a control.
A preparation method of a gel type antibacterial medical band-aid comprises the following steps:
(1) Mixing 1g of chitosan, 0.7g of 1-hydroxybenzotriazole and 100mL of deionized water, uniformly stirring, adding a mixed solution of N-acetylcysteine, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and 50mL of deionized water, adjusting the pH value to 5 by using sodium hydroxide, stirring and reacting for 2 hours at the temperature of 30 ℃, precipitating ethanol, washing and drying to obtain the thiolated chitosan. The molar ratio of the chitosan to the N-acetyl cysteine is 1:2; the mol ratio of the N-acetyl cysteine to the 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide hydrochloride is 2:1.
mixing 0.5g of 1-ethyl- (3-dimethylaminopropyl) carbodiimide and 2mL of deionized water, stirring for 30min, adding 150g of N-acetylcysteine after stirring uniformly, continuing stirring for 30min, adding 6mL of polylysine aqueous solution, reacting for 4h at 30 ℃, washing and drying to obtain the thiolated polylysine. The concentration of the polylysine aqueous solution is 0.5g/mL; the mass ratio of the N-acetylcysteine to the polylysine aqueous solution is 50:1.
(2) Taking 5g of gelatin and 50mL of PBS buffer solution, stirring the mixture at 55 ℃ until the gelatin and the 50mL of PBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH value to 7, adding 5mL of methacrylic anhydride, keeping the temperature and stirring the mixture for 12 hours, dialyzing the mixture in a dialysis bag for 2 days, and freeze-drying the dialyzed mixture to obtain the methacrylic gelatin.
Mixing 5g of chitosan and 30mL of methanesulfonic acid, stirring at 35 ℃ for 25min, cooling to 0 ℃, stirring for 1.5h, adding 10mL of acryloyl chloride, continuously stirring for 7.5h to obtain a reaction solution, settling by using a mixed solution of acetone and diethyl ether, performing centrifugal separation, washing and drying to obtain the acryloyl chitosan.
(3) Mixing thiolated chitosan, thiolated polylysine and deionized water, and uniformly stirring to obtain a solution A; the concentration of the solution A is 3wt%, wherein the mass ratio of thiolated chitosan to thiolated polylysine is 4:1. mixing methacrylic acid gelatin, acryloyl chitosan and deionized water, and uniformly stirring to obtain a solution B; the concentration of the solution B is 3wt%, wherein the mass ratio of the acryloyl chitosan to the methacrylic acid gelatin is 3:2.
mixing the solution A, the solution B and a photoinitiator to obtain an antibacterial gel solution; the mass ratio of the solution A to the solution B is 1:1; the dosage of the photoinitiator is 4wt% of the antibacterial gel liquid.
(4) Coating antibacterial gel solution on the middle part of the medical adhesive tape, irradiating with 365nm ultraviolet light for 25min, standing for 4h, and packaging to obtain the final product. The coating thickness of the antibacterial gel liquid is 2mm.
Detection experiment:
1. and (3) antibacterial experiments: taking Escherichia coli, performing activated culture at 37 deg.C and 220rpm, culturing for 12 hr, diluting bacterial suspension, and diluting to 10% concentration 8 cfu/mL, an equal volume of the UV-crosslinked gel sample (prepared according to examples 1-4 and comparative examples 1-2) was added, and the size of the zone of inhibition was recorded after 12h of culture to characterize the antibacterial performance.
2. Cytotoxicity: taking a gel sample (prepared according to examples 1-4 and comparative examples 1-2) after ultraviolet crosslinking, soaking the sample in a DMEM culture solution for 24 hours to obtain a leaching solution, culturing a 3T3 cell suspension (a 96-well plate) through the leaching solution for 24 hours, performing MTT test after culture, and recording the cell survival rate.
3. Selecting 30 SPF SD rats with the weight of about 200g, dividing the SD rats into 6 groups, feeding 5 rats in each group for 2 weeks, anesthetizing the rats, unhairing the backs, creating wounds with the length of 2mm and the depth of 2mm, fixing band aids (prepared according to examples 1-4 and comparative examples 1-2) at the wounds, replacing the wounds every day, and observing the healing rate of the wounds after 5 days; the average value is recorded for each group.
And (4) conclusion: the invention discloses a gel type antibacterial medical band-aid and a preparation method thereof, the process design is reasonable, the component distribution is proper, the prepared medical band-aid not only has excellent antibacterial performance, but also can promote wound healing, and the gel type antibacterial medical band-aid has great potential and high practicability in the field of wound care.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described above, or equivalents may be substituted for elements thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation method of a gel type antibacterial medical band-aid is characterized by comprising the following steps: the method comprises the following steps:
(1) Mixing 1-ethyl- (3-dimethylaminopropyl) carbodiimide and deionized water, stirring for 20-30 min, adding N-acetylcysteine after uniformly stirring, continuing stirring for 20-30 min, adding a polylysine aqueous solution, reacting for 4-6 h at 25-30 ℃, washing and drying to obtain thiolated polylysine;
(2) Mixing thiolated chitosan, thiolated polylysine and deionized water, and uniformly stirring to obtain a solution A; mixing methacrylic acid gelatin and deionized water, and uniformly stirring to obtain a solution B; mixing the solution A and the solution B with a photoinitiator, and adding an epidermal cell growth factor to obtain an antibacterial gel solution;
(3) Coating the antibacterial gel liquid on the middle part of the medical adhesive tape, irradiating by ultraviolet light for 20-25 min, standing for 3-4 h, and packaging to obtain a finished product.
2. The method for preparing the gel-type antibacterial medical band-aid according to claim 1, characterized in that: in the step (2), the concentration of the solution A is 2.5-3 wt%, wherein the mass ratio of the thiolated chitosan to the thiolated polylysine is 4:1; the concentration of the solution B is 2.5-3 wt%.
3. The method for preparing the gel-type antibacterial medical band-aid according to claim 1, characterized in that: in the step (3), the mass ratio of the solution A to the solution B is 1:1; the dosage of the photoinitiator is 3 to 4 weight percent of the antibacterial gel liquid; the dosage of the epidermal cell growth factor is 8-10 wt% of the antibacterial gel liquid.
4. The method for preparing the gel-type antibacterial medical band-aid according to claim 1, characterized in that: in the step (2), the preparation of the thiolated chitosan comprises the following steps: mixing chitosan, 1-hydroxybenzotriazole and deionized water, stirring uniformly, adding a mixed solution of N-acetylcysteine, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and deionized water, adjusting the pH value to 5 with sodium hydroxide, stirring and reacting for 2-3 h at 25-30 ℃, separating out ethanol, washing and drying to obtain the thiolated chitosan.
5. The method for preparing the gel-type antibacterial medical band-aid according to claim 4, characterized in that: the molar ratio of the chitosan to the N-acetylcysteine is 1:2; the mol ratio of the N-acetyl cysteine to the 1- (3-dimethylaminopropyl) -3-ethyl carbodiimide hydrochloride is 2:1.
6. the method for preparing the gel-type antibacterial medical band-aid according to claim 1, characterized in that: in the step (2), the preparation of the methacrylic acid gelatin comprises the following steps: taking gelatin and PBS buffer solution, stirring the solution at 45-55 ℃ until the gelatin and the PBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH value to 7, adding methacrylic anhydride, stirring the solution for 12-16 h under the condition of heat preservation, dialyzing the solution for 2 days by a dialysis bag, and freeze-drying the solution to obtain the methacrylic gelatin.
7. The method for preparing the gel-type antibacterial medical band-aid according to claim 1, characterized in that: in the step (2), adding acryloyl chitosan into the solution B, mixing methacrylic acid gelatin, acryloyl chitosan and deionized water, and uniformly stirring to obtain the solution B, wherein the mass ratio of the acryloyl chitosan to the methacrylic acid gelatin is 3:2.
8. the method for preparing the gel-type antibacterial medical band-aid according to claim 7, characterized in that: in the step (2), the preparation of the acryloyl chitosan comprises the following steps: mixing chitosan and methanesulfonic acid, stirring for 25-30 min at 25-35 ℃, cooling to 0 ℃, stirring for 1-2 h, adding acryloyl chloride, continuously stirring for 7-8 h to obtain a reaction solution, settling by using a mixed solution of acetone and diethyl ether, performing centrifugal separation, washing and drying to obtain the acryloyl chitosan.
9. The adhesive bandage prepared by the preparation method of the gel-type antibacterial medical adhesive bandage according to any one of claims 1 to 8.
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