CN115501376B - 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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- 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
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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
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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
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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
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Abstract
The invention relates to the technical field of medical band-aids, and particularly discloses a gel type antibacterial medical band-aid and a preparation method thereof, wherein the gel type antibacterial medical band-aid is prepared by coating and drying components such as chitosan, gelatin, epidermal cell growth factor and the like on the surface of a medical adhesive tape; firstly, carrying out sulfhydrylation modification on chitosan, modifying the chitosan by utilizing N-acetylcysteine to obtain sulfhydrylation chitosan, modifying gelatin by utilizing methacrylic anhydride to obtain methacrylic acid gelatin containing double bond groups, and polymerizing the methacrylic acid gelatin and the sulfhydrylation chitosan under the action of ultraviolet light to obtain antibacterial gel; the process design is reasonable, the component proportion is proper, and the prepared medical band-aid has excellent antibacterial performance, can promote wound healing, has great potential in the field of wound care, and has high practicability.
Description
Technical Field
The invention relates to the technical field of medical band-aids, in particular to a gel-type antibacterial medical band-aid and a preparation method thereof.
Background
The adhesive bandage is commonly called as a sterilizing elastic adhesive bandage, and is a necessary medical product for emergency treatment most commonly used in life of people. The band-aid mainly comprises a flat cloth adhesive tape and a water absorbing pad, has the function of stopping bleeding and protecting wound, and is available for patients in various shapes according to different requirements.
Most of the prior commercially available band-aids adopt water-absorbing cloth pads, but the nursing effect is poor, and the antibacterial performance can not meet the demands of people, so how to improve the antibacterial performance of the band-aids and promote wound healing is one of the technical problems to be solved urgently.
Disclosure of Invention
The invention aims to provide a gel-type antibacterial medical band-aid and a preparation method thereof, which are used for solving the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
a preparation method of 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, continuously stirring for 20-30 min, adding 6mL of polylysine aqueous solution, reacting for 4-6 h at 25-30 ℃, washing and drying to obtain sulfhydryl polylysine;
(2) Mixing sulfhydrylation chitosan, sulfhydrylation polylysine and deionized water, and stirring uniformly to obtain a solution A; mixing methacrylic acid gelatin and deionized water, and uniformly stirring to obtain a solution B; mixing the solution A, the solution B and the photoinitiator, and adding the epidermal cell growth factor to obtain an antibacterial gel solution;
(3) The middle part of the medical adhesive tape is coated with an antibacterial gel liquid, irradiated by ultraviolet light for 20-25 min, stood for 3-4 h and packaged to obtain a finished product.
In the more optimized scheme, in the step (2), the concentration of the solution A is 2.5-3 wt%, wherein the mass ratio of the sulfhydryl chitosan to the sulfhydryl polylysine is 4:1, a step of; the concentration of the solution B is 2.5-3 wt%.
In the more optimized scheme, in the step (3), the mass ratio of the solution A to the solution B is 1:1, a step of; the dosage of the photoinitiator is 3-4wt% of the antibacterial gel solution; the dosage of the epidermal cell growth factor is 8-10wt% of the antibacterial gel solution.
In the more optimized scheme, in the step (2), the preparation steps of the sulfhydrylation 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, regulating the pH to 5 by sodium hydroxide, stirring at 25-30 ℃ for reacting for 2-3 hours, precipitating ethanol, washing and drying to obtain the sulfhydryl chitosan.
In a more optimized scheme, the molar ratio of the chitosan to the N-acetylcysteine is 1:2; the molar ratio of the N-acetylcysteine to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 2:1.
in a more optimized scheme, in the step (2), the preparation steps of the methacrylic acid gelatin are as follows: 5g of gelatin and 50mLPBS buffer solution are taken, stirred at 45-55 ℃ until the gelatin is dissolved, sodium hydroxide is added to adjust the pH to 7, 5mL of methacrylic anhydride is added, the temperature is kept, the stirring is carried out for 12-16 h, dialysis is carried out for 2 days by a dialysis bag, and the methacrylic gelatin is obtained by freeze drying.
In the more optimized scheme, in the step (2), adding acryl chitosan into the solution B, mixing methacrylic acid gelatin, acryl chitosan and deionized water, and uniformly stirring to obtain the solution B, wherein the mass ratio of acryl chitosan to methacrylic acid gelatin is 3:2.
in a more optimized scheme, in the step (2), the preparation steps of the acryl chitosan are as follows: mixing 5g of chitosan with 30mL of methanesulfonic acid, stirring for 25-30 min at 25-35 ℃, cooling to 0 ℃, stirring for 1-2 h, adding 10mL of acryloyl chloride, continuously stirring for 7-8 h to obtain a reaction solution, settling the reaction solution through acetone and diethyl ether mixed solution, centrifuging, separating, washing and drying to obtain the acryl chitosan.
According to the more optimized scheme, the adhesive bandage prepared by the preparation method of the gel type antibacterial medical adhesive bandage is prepared according to any one of the above.
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 gel type antibacterial medical band-aid is formed by coating and drying components such as chitosan, gelatin, epidermal cell growth factors and the like on the surface of a medical adhesive tape; firstly, carrying out sulfhydrylation modification on chitosan, modifying the chitosan by utilizing N-acetylcysteine to obtain sulfhydrylation chitosan, modifying gelatin by utilizing methacrylic anhydride to obtain methacrylic acid gelatin containing double bond groups, and polymerizing the methacrylic acid gelatin and the sulfhydrylation chitosan under the action of ultraviolet light to obtain antibacterial gel; the gelatin can be used as protein, on one hand, the gelatin and the epidermal cell growth factor are matched with each other to promote the healing of wounds, on the other hand, the gelatin can also improve the adhesion performance between the antibacterial gel and the medical adhesive tape, and the medical adhesive bandage obtained by the mutual cross-linking and matching of the methacrylic acid gelatin and the sulfhydrylation chitosan has excellent antibacterial performance and excellent biocompatibility and can promote the healing of wounds.
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 pure 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, in order to avoid the technical problem, the scheme introduces sulfhydryl polylysine, and sulfydryl is grafted on the surface of the polylysine after the activation by using 1-ethyl- (3-dimethylaminopropyl) carbodiimide, so that the polylysine participates in the crosslinking reaction under the action of ultraviolet light, and the comprehensive antibacterial performance of the product is ensured; the scheme defines that the mass ratio of the sulfhydryl chitosan to the sulfhydryl polylysine is 4:1", under this parameter, the scheme can further improve antibacterial property when guaranteeing mechanical properties, and comprehensive effect is more excellent.
The scheme also discloses another more excellent scheme when actually developing, acryl chitosan is introduced into the system, and the mass ratio of acryl chitosan to methacrylic acid gelatin is defined as 3: 2', partial acryl chitosan is used for replacing the methacrylic acid gelatin, so that on one hand, the suitability of acryl chitosan and sulfhydrylation chitosan is more excellent, and on the other hand, 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, which are reasonable in process design and relatively suitable in component proportion, and the prepared medical band-aid not only has relatively excellent antibacterial performance, but also can promote wound healing, and has relatively great potential in the field of wound care and relatively high practicability.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In this example, chitosan was purchased from Sigma-Aldrich chemical Co., ltd; 1-hydroxybenzotriazole was purchased from rohn's reagent; n-acetylcysteine was purchased from microphone Lin Shenghua Co., ltd; 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, 1-ethyl- (3-dimethylaminopropyl) carbodiimide, and polylysine were all available from Sachs chemical technology (Shanghai) Inc.; gelatin is purchased from national pharmaceutical and chemical reagents, inc; methacrylic anhydride, PBS buffer was purchased from aladine. The medical adhesive tape is a commercial medical adhesive tape and can be replaced according to actual requirements.
Example 1:
a preparation method of 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, regulating the pH to 5 by sodium hydroxide, stirring at 25 ℃ for reaction for 3 hours, precipitating ethanol, washing and drying to obtain the sulfhydryl chitosan. The molar ratio of the chitosan to the N-acetylcysteine is 1:2; the molar ratio of the N-acetylcysteine to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide 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, continuously stirring for 20min, adding 6mL of polylysine aqueous solution, reacting for 6h at 25 ℃, washing and drying to obtain sulfhydryl 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 50mLPBS buffer solution, stirring at 45 ℃ until the gelatin and 50mLPBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH to 7, adding 5mL of methacrylic anhydride, keeping the temperature and stirring for 12h, dialyzing by a dialysis bag for 2 days, and freeze-drying to obtain the methacrylic gelatin.
(3) Mixing sulfhydrylation chitosan, sulfhydrylation polylysine and deionized water, and stirring uniformly to obtain a solution A; the concentration of the solution A is 3wt%, wherein the mass ratio of the sulfhydryl chitosan to the sulfhydryl 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 the photoinitiator, and adding the epidermal cell growth factor to obtain an antibacterial gel solution; the mass ratio of the solution A to the solution B is 1:1, a step of; the photoinitiator is 4wt% of the antibacterial gel solution; the amount of the epidermal growth factor is 10wt% of the antibacterial gel solution.
(4) The medical adhesive tape is coated with an antibacterial gel solution in the middle, irradiated by 365nm ultraviolet light for 20min, stood for 3h and packaged to obtain a finished product. The thickness of the coating of the antibacterial gel solution was 2mm.
Example 2:
a preparation method of 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, regulating the pH to 5 by sodium hydroxide, stirring at 28 ℃ for reacting for 2.5 hours, precipitating ethanol, washing and drying to obtain the sulfhydryl chitosan. The molar ratio of the chitosan to the N-acetylcysteine is 1:2; the molar ratio of the N-acetylcysteine to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide 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, continuously stirring for 25min, adding 6mL of polylysine aqueous solution, reacting for 5h at 28 ℃, washing and drying to obtain sulfhydryl 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 50mLPBS buffer solution, stirring at 50 ℃ until the gelatin and 50mLPBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH to 7, adding 5mL of methacrylic anhydride, keeping the temperature and stirring for 14h, dialyzing by a dialysis bag for 2 days, and freeze-drying to obtain the methacrylic gelatin.
(3) Mixing sulfhydrylation chitosan, sulfhydrylation polylysine and deionized water, and stirring uniformly to obtain a solution A; the concentration of the solution A is 3wt%, wherein the mass ratio of the sulfhydryl chitosan to the sulfhydryl 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 the photoinitiator, and adding the epidermal cell growth factor to obtain an antibacterial gel solution; the mass ratio of the solution A to the solution B is 1:1, a step of; the photoinitiator is 4wt% of the antibacterial gel solution; the amount of the epidermal growth factor is 10wt% of the antibacterial gel solution.
(4) The medical adhesive tape is coated with an antibacterial gel liquid in the middle, irradiated by 365nm ultraviolet light for 25min, stood for 3.5h and packaged to obtain a finished product. The thickness of the coating of the antibacterial gel solution was 2mm.
Example 3:
a preparation method of 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, regulating the pH to 5 by sodium hydroxide, stirring at 30 ℃ for reacting for 2 hours, precipitating ethanol, washing and drying to obtain the sulfhydryl chitosan. The molar ratio of the chitosan to the N-acetylcysteine is 1:2; the molar ratio of the N-acetylcysteine to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide 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, continuously stirring for 30min, adding 6mL of polylysine aqueous solution, reacting for 4h at 30 ℃, washing and drying to obtain sulfhydryl 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 50mLPBS buffer solution, stirring at 55 ℃ until the gelatin and 50mLPBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH to 7, adding 5mL of methacrylic anhydride, keeping the temperature and stirring for 12h, dialyzing by a dialysis bag for 2 days, and freeze-drying to obtain the methacrylic gelatin.
(3) Mixing sulfhydrylation chitosan, sulfhydrylation polylysine and deionized water, and stirring uniformly to obtain a solution A; the concentration of the solution A is 3wt%, wherein the mass ratio of the sulfhydryl chitosan to the sulfhydryl 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 the photoinitiator, and adding the epidermal cell growth factor to obtain an antibacterial gel solution; the mass ratio of the solution A to the solution B is 1:1, a step of; the photoinitiator is 4wt% of the antibacterial gel solution; the amount of the epidermal growth factor is 10wt% of the antibacterial gel solution.
(4) The medical adhesive tape is coated with an antibacterial gel solution in the middle, irradiated by 365nm ultraviolet light for 25min, stood for 4h and packaged to obtain a finished product. The thickness of the coating of the antibacterial gel solution was 2mm.
Example 4: acryl chitosan was introduced on the basis of example 3.
A preparation method of 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, regulating the pH to 5 by sodium hydroxide, stirring at 30 ℃ for reacting for 2 hours, precipitating ethanol, washing and drying to obtain the sulfhydryl chitosan. The molar ratio of the chitosan to the N-acetylcysteine is 1:2; the molar ratio of the N-acetylcysteine to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide 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, continuously stirring for 30min, adding 6mL of polylysine aqueous solution, reacting for 4h at 30 ℃, washing and drying to obtain sulfhydryl 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 50mLPBS buffer solution, stirring at 55 ℃ until the gelatin and 50mLPBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH to 7, adding 5mL of methacrylic anhydride, keeping the temperature and stirring for 12h, dialyzing by a dialysis bag for 2 days, and freeze-drying to obtain the methacrylic gelatin.
Mixing 5g of chitosan with 30mL of methanesulfonic acid, stirring for 25min at 35 ℃, cooling to 0 ℃, stirring for 1.5h, adding 10mL of acryloyl chloride, continuing stirring for 7.5h to obtain a reaction solution, settling by using a mixed solution of acetone and diethyl ether, centrifuging, separating, washing and drying to obtain the acryloyl chitosan.
(3) Mixing sulfhydrylation chitosan, sulfhydrylation polylysine and deionized water, and stirring uniformly to obtain a solution A; the concentration of the solution A is 3wt%, wherein the mass ratio of the sulfhydryl chitosan to the sulfhydryl polylysine is 4:1. mixing methacrylic acid gelatin, acryl 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 acryl chitosan to the methacrylic acid gelatin is 3:2.
mixing the solution A, the solution B and the photoinitiator, and adding the epidermal cell growth factor to obtain an antibacterial gel solution; the mass ratio of the solution A to the solution B is 1:1, a step of; the photoinitiator is 4wt% of the antibacterial gel solution; the amount of the epidermal growth factor is 10wt% of the antibacterial gel solution.
(4) The medical adhesive tape is coated with an antibacterial gel solution in the middle, irradiated by 365nm ultraviolet light for 25min, stood for 4h and packaged to obtain a finished product. The thickness of the coating of the antibacterial gel solution was 2mm.
Comparative example 1: in comparative example 1, thiolated polylysine was not introduced using example 4 as a control.
A preparation method of 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, continuously stirring for 30min, adding 6mL of polylysine aqueous solution, reacting for 4h at 30 ℃, washing and drying to obtain sulfhydryl 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 50mLPBS buffer solution, stirring at 55 ℃ until the gelatin and 50mLPBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH to 7, adding 5mL of methacrylic anhydride, keeping the temperature and stirring for 12h, dialyzing by a dialysis bag for 2 days, and freeze-drying to obtain the methacrylic gelatin.
Mixing 5g of chitosan with 30mL of methanesulfonic acid, stirring for 25min at 35 ℃, cooling to 0 ℃, stirring for 1.5h, adding 10mL of acryloyl chloride, continuing stirring for 7.5h to obtain a reaction solution, settling by using a mixed solution of acetone and diethyl ether, centrifuging, separating, washing and drying to obtain the acryloyl chitosan.
(3) Mixing sulfhydrylation chitosan and deionized water, and stirring uniformly to obtain a solution A; the concentration of the solution A was 3% by weight. Mixing methacrylic acid gelatin, acryl 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 acryl chitosan to the methacrylic acid gelatin is 3:2.
mixing the solution A, the solution B and the photoinitiator, and adding the epidermal cell growth factor to obtain an antibacterial gel solution; the mass ratio of the solution A to the solution B is 1:1, a step of; the photoinitiator is 4wt% of the antibacterial gel solution; the amount of the epidermal growth factor is 10wt% of the antibacterial gel solution.
(4) The medical adhesive tape is coated with an antibacterial gel solution in the middle, irradiated by 365nm ultraviolet light for 25min, stood for 4h and packaged to obtain a finished product. The thickness of the coating of the antibacterial gel solution was 2mm.
Comparative example 2: in comparative example 2, no epidermal growth factor was introduced in example 4 as a control group.
A preparation method of 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, regulating the pH to 5 by sodium hydroxide, stirring at 30 ℃ for reacting for 2 hours, precipitating ethanol, washing and drying to obtain the sulfhydryl chitosan. The molar ratio of the chitosan to the N-acetylcysteine is 1:2; the molar ratio of the N-acetylcysteine to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide 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, continuously stirring for 30min, adding 6mL of polylysine aqueous solution, reacting for 4h at 30 ℃, washing and drying to obtain sulfhydryl 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 50mLPBS buffer solution, stirring at 55 ℃ until the gelatin and 50mLPBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH to 7, adding 5mL of methacrylic anhydride, keeping the temperature and stirring for 12h, dialyzing by a dialysis bag for 2 days, and freeze-drying to obtain the methacrylic gelatin.
Mixing 5g of chitosan with 30mL of methanesulfonic acid, stirring for 25min at 35 ℃, cooling to 0 ℃, stirring for 1.5h, adding 10mL of acryloyl chloride, continuing stirring for 7.5h to obtain a reaction solution, settling by using a mixed solution of acetone and diethyl ether, centrifuging, separating, washing and drying to obtain the acryloyl chitosan.
(3) Mixing sulfhydrylation chitosan, sulfhydrylation polylysine and deionized water, and stirring uniformly to obtain a solution A; the concentration of the solution A is 3wt%, wherein the mass ratio of the sulfhydryl chitosan to the sulfhydryl polylysine is 4:1. mixing methacrylic acid gelatin, acryl 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 acryl chitosan to the methacrylic acid gelatin is 3:2.
mixing the solution A, the solution B and the photoinitiator to obtain an antibacterial gel solution; the mass ratio of the solution A to the solution B is 1:1, a step of; the photoinitiator was used in an amount of 4wt% of the antimicrobial gel solution.
(4) The medical adhesive tape is coated with an antibacterial gel solution in the middle, irradiated by 365nm ultraviolet light for 25min, stood for 4h and packaged to obtain a finished product. The thickness of the coating of the antibacterial gel solution was 2mm.
Detection experiment:
1. antibacterial experiment: activating and culturing Escherichia coli at 37deg.C and 220rpm, and diluting the bacterial suspension after culturing for 12 hr to give a concentration of 10 8 cfu/mL, an equal volume of the gel sample after ultraviolet crosslinking (prepared according to examples 1-4 and comparative examples 1-2) was added, and after 12 hours of culture, the size of the inhibition zone was recorded to characterize the antibacterial performance.
2. Cytotoxicity: taking a gel sample after ultraviolet crosslinking (prepared according to examples 1-4 and comparative examples 1-2), soaking the sample in a DMEM culture solution for 24 hours to obtain a leaching solution, culturing a 3T3 cell suspension (96-well plate) by the leaching solution, culturing for 24 hours, performing an MTT test after culturing, and recording the cell survival rate.
3. 30 SD rats with SPF grade are selected, the weight is about 200g, the rats are divided into 6 groups, 5 rats in each group are respectively fed for 2 weeks and then anesthetized, the backs of the rats are dehaired, wounds with the length of 2mm and the depth of 2mm are created, a band-aid (prepared according to examples 1-4 and comparative examples 1-2) is fixed at the wounds, the wounds are replaced every day, and the wound healing rate is observed after 5 days; the average value was recorded for each group.
Conclusion: the invention discloses a gel-type antibacterial medical band-aid and a preparation method thereof, which are reasonable in process design and relatively suitable in component proportion, and the prepared medical band-aid not only has relatively excellent antibacterial performance, but also can promote wound healing, and has relatively great potential in the field of wound care and relatively high practicability.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A preparation method of 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 stirring uniformly, continuously stirring for 20-30 min, adding a polylysine aqueous solution, reacting for 4-6 h at 25-30 ℃, washing and drying to obtain sulfhydryl polylysine;
(2) Mixing sulfhydrylation chitosan, sulfhydrylation polylysine and deionized water, and stirring uniformly to obtain a solution A; mixing methacrylic acid gelatin and deionized water, and uniformly stirring to obtain a solution B; mixing the solution A, the solution B and the photoinitiator, and adding the epidermal cell growth factor to obtain an antibacterial gel solution;
in the step (2), the concentration of the solution A is 2.5-3 wt%, wherein the mass ratio of the sulfhydryl chitosan to the sulfhydryl polylysine is 4:1, a step of; the concentration of the solution B is 2.5-3wt%;
(3) The middle part of the medical adhesive tape is coated with an antibacterial gel liquid, irradiated by ultraviolet light for 20-25 min, stood for 3-4 h and packaged to obtain a finished product.
2. The method for preparing the gel-type antibacterial medical band-aid according to claim 1, which is characterized in that: in the step (3), the mass ratio of the solution A to the solution B is 1:1, a step of; the dosage of the photoinitiator is 3-4wt% of the antibacterial gel solution; the dosage of the epidermal cell growth factor is 8-10wt% of the antibacterial gel solution.
3. The method for preparing the gel-type antibacterial medical band-aid according to claim 1, which is characterized in that: in the step (2), the preparation steps of the sulfhydrylation chitosan are as follows: 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, regulating the pH to 5 by sodium hydroxide, stirring and reacting for 2-3 hours at 25-30 ℃, precipitating by ethanol, washing and drying to obtain the sulfhydryl chitosan.
4. The method for preparing the gel-type antibacterial medical band-aid according to claim 3, which is characterized in that: the molar ratio of the chitosan to the N-acetylcysteine is 1:2; the molar ratio of the N-acetylcysteine to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride is 2:1.
5. the method for preparing the gel-type antibacterial medical band-aid according to claim 1, which is characterized in that: in the step (2), the preparation steps of the methacrylic acid gelatin are as follows: and (3) taking gelatin and PBS buffer solution, stirring at 45-55 ℃ until the gelatin and PBS buffer solution are dissolved, adding sodium hydroxide to adjust the pH to 7, adding methacrylic anhydride, carrying out heat preservation and stirring for 12-16 h, dialyzing for 2 days by using a dialysis bag, and freeze-drying to obtain the methacrylic gelatin.
6. The method for preparing the gel-type antibacterial medical band-aid according to claim 1, which is characterized in that: in the step (2), adding acryl chitosan into the solution B, mixing methacrylic acid gelatin, acryl chitosan and deionized water, and uniformly stirring to obtain the solution B, wherein the mass ratio of acryl chitosan to methacrylic acid gelatin is 3:2.
7. the method for preparing the gel-type antibacterial medical band-aid according to claim 6, which is characterized in that: in the step (2), the preparation steps of the acryl chitosan are as follows: mixing chitosan and methylsulfonic acid, stirring for 25-30 min at 25-35 ℃, cooling to 0 ℃, stirring for 1-2 h, adding acryloyl chloride, continuing stirring for 7-8 h to obtain a reaction solution, settling the reaction solution by using acetone and diethyl ether mixed solution, centrifuging, separating, washing and drying to obtain the acryl chitosan.
8. A wound plaster prepared by the method for preparing a gel-type antibacterial medical wound plaster according to any one of claims 1 to 7.
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