CN109010897B - Preparation method of medical antibacterial gel dressing - Google Patents
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- CN109010897B CN109010897B CN201811046922.0A CN201811046922A CN109010897B CN 109010897 B CN109010897 B CN 109010897B CN 201811046922 A CN201811046922 A CN 201811046922A CN 109010897 B CN109010897 B CN 109010897B
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- A61L15/18—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
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- A61L15/00—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
- A61L15/20—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing organic materials
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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
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- 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
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
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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 discloses a preparation method of a medical antibacterial gel dressing, and belongs to the technical field of medical high polymer materials. The invention adopts quaternary ammonium cationic etherifying agent to react with starch to prepare quaternary ammonium cationic starch, and silver nano particles are loaded on the surface of the quaternary ammonium cationic starch as an antibacterial agent of the medical antibacterial gel dressing; the antibacterial agent is mainly characterized in that negative charged bacteria are adsorbed and gathered on cell walls by cations under the actions of electrostatic force, hydrogen bond force, hydrophobic combination between surfactant molecules and protein molecules and the like, and a chamber resistance effect is generated, so that the bacteria are inhibited in growth and die; the hydrophobic alkyl group of the cell lysis inhibitor reacts with the hydrophilic group of bacteria to cause cell lysis and cell structure destruction, so that cell lysis and cell death are caused; the prepared medical antibacterial gel dressing material has good air permeability and mechanical strength, can provide a moist tissue contact environment, has good cell compatibility, can absorb wound exudate, and is not adhered to tissues, so that secondary damage caused by dressing change is avoided.
Description
Technical Field
The invention relates to a preparation method of a medical antibacterial gel dressing, and belongs to the technical field of medical high polymer materials.
Background
At present, the most effective method for treating the wound surface of large-area burn and scald is a skin transplantation method, and the wound must be treated and protected by adopting the skin transplantation method. The gel covering is a better protection method, and the medical gel dressing material has the following functions: preventing loss of moisture and body fluids; covering and protecting the wound surface from infection; good biocompatibility; the air permeability and the moisture retention are good; has better adhesive force with the wound surface and does not generate deformation; sufficient mechanical strength to support cell differentiation and proliferation; the surface has enough cell adsorption capacity, which is beneficial to the salary and growth of cells; can promote the normal growth of epithelial tissues and granulation, promote the healing of wounds and leave no scars; the material source is sufficient, and the preparation, the processing and the like are easy. In addition to this, medical gel materials are also required to be non-toxic, non-irritating and non-allergenic. However, the existing gel has a complex preparation process and high process control difficulty, so that a medical gel material which has a simple preparation method and a good antibacterial effect is needed.
The common medical wound dressing is prepared by matching gauze or non-woven fabrics and cotton with medicines, can protect wounds from mechanical damage and prevent the wounds from being infected, but has unsatisfactory performances of antibiosis, liquid absorption, inflammation diminishing and the like.
The medical gel dressing material has the following functions: preventing loss of moisture and body fluids; covering and protecting the wound surface from infection; good biocompatibility; the air permeability and the moisture retention are good; has better adhesive force with the wound surface and does not generate deformation; sufficient mechanical strength to support cell differentiation and proliferation; the surface has enough cell adsorption capacity, which is beneficial to the salary and growth of cells; can promote the normal growth of epithelial tissues and granulation, promote the healing of wounds and leave no scars; the material source is sufficient, and the preparation, the processing and the like are easy. The main indicators for evaluating dressing performance are as follows: (1) mechanical properties; (2) bacterial barrier action: the ideal wound dressing should have the function of blocking the invasion of microorganisms, effectively protect the wound and prevent infection. (3) Adhesion: i.e. the ability of the dressing to adhere uniformly and tightly to the wound bed, expressed as the peel force. (4) Absorption capacity: the dressing with large absorption capacity can prevent wound surface effusion and reduce bacterial growth, thereby promoting healing. (5) Water vapor transmission rate: the proper water vapor transmission rate can keep the wound surface in an ideal humidity environment, prevent hydrops and keep the wound surface moist, thereby being beneficial to promoting healing. (6) Oxygen permeability: oxygen can improve the activity of fibroblasts, and is beneficial to the synthesis of collagen of epithelial tissue components and the growth of epidermal cells.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the problem of poor air permeability and mechanical strength of the traditional medical gel dressing, the preparation method of the medical antibacterial gel dressing is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
(1) weighing 100-120 parts by weight of deionized water, 20-30 parts by weight of 20% sodium hydroxide solution, 40-50 parts by weight of starch and 10-22 parts by weight of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, mixing the deionized water, the 20% by weight of sodium hydroxide solution, the starch and the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, stirring to obtain a composite solution, adjusting the pH value to obtain a suspension, carrying out suction filtration to obtain filter residues, washing with the deionized water for 3-5 times, and drying in an oven at 60-70 ℃ to constant weight to obtain modified starch;
(2) mixing modified starch, anhydrous methanol and a silver nitrate solution with the mass fraction of 10% according to the mass ratio of 2: 1, stirring for 6-8 hours in a dark place at the rotating speed of 100-150 r/min to obtain a blend, adding a trisodium citrate solution with the mass fraction of 5%, stirring to obtain a mixed solution, performing centrifugal separation to obtain a precipitate, washing for 3-5 times by using anhydrous ethanol and deionized water respectively, and drying to constant weight to obtain an antibacterial agent;
(3) respectively weighing 20-40 parts of an antibacterial agent, 1-10 parts of a quaternary ammonium salt cationic surfactant, 10-16 parts of hyaluronic acid, 1-4 parts of epoxy chloropropane and 50-60 parts of deionized water according to parts by weight, mixing the antibacterial agent, the quaternary ammonium salt cationic surfactant, the hyaluronic acid, the epoxy chloropropane and the deionized water, stirring at a constant temperature, and cooling to room temperature to obtain the medical antibacterial gel dressing.
The stirring treatment in the step (1) is to mix deionized water, a sodium hydroxide solution with the mass fraction of 20% and starch, stir the mixture evenly at room temperature at the rotating speed of 200-300 r/min to obtain emulsion, add 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, continue stirring for 5-10 min, heat the mixture to 40-50 ℃ and stir the mixture for reaction for 8-12 h.
And (2) adjusting the pH value in the step (1) to 5.5-6.5 by using a hydrochloric acid solution with the mass fraction of 7%.
And (3) stirring in a dark place in the step (2) at the rotating speed of 100-150 r/min for 6-8 h.
The mass ratio of the trisodium citrate solution with the mass fraction of 5 percent to the blend in the step (2) is 1: 10.
The stirring treatment in the step (2) is stirring for 30-50 min at the speed of 400-500 r/min.
The constant-temperature stirring treatment in the step (3) is stirring for 2-4 hours at the temperature of 60-80 ℃ and the rotating speed of 800-1000 r/min.
Compared with other methods, the method has the beneficial technical effects that:
(1) the invention adopts quaternary ammonium salt cationic etherifying agent to react with starch under the action of catalyst to prepare quaternary ammonium type cationic starch, and silver nano particles are loaded on the surface of the quaternary ammonium type cationic starch as an antibacterial agent of the medical antibacterial gel dressing, the prepared antibacterial agent is mainly characterized in that the cations adsorb negatively charged bacteria through the actions of electrostatic force, hydrogen bond force, hydrophobic combination between surfactant molecules and protein molecules and the like, and the negatively charged bacteria are gathered on cell walls to generate a chamber resistance effect, so that the bacteria are inhibited in growth and die; meanwhile, the hydrophobic alkyl can also act with the hydrophilic group of bacteria to change the permeability of the membrane, so that the lysis is generated, the cell structure is damaged, and the cell is dissolved and killed; silver nanoparticles may interfere with the permeability of cells and their respiratory function by attaching to the surface of cell membranes; under the condition of the same mass, the nano silver particles can have larger surface area than other large particles, so that the nano silver particles have larger space for interaction with microorganisms; the silver nanoparticles can interact with sulfur-containing proteins on the bacterial membrane and simultaneously interact with phosphorus-containing compounds on DNA, so that the bacteria are inactivated; the nano silver particles can release silver ions in bacteria, so that the antibacterial activity of the nano silver particles can be improved;
(2) the medical antibacterial gel dressing material prepared by the invention can provide a moist tissue contact environment, has good cell compatibility, can absorb wound exudate, is not adhered to tissues so as to avoid secondary damage caused by dressing change, and the prepared gel dressing has good air permeability and good mechanical strength because the starch in the antibacterial agent is used as a pore-forming agent and the epichlorohydrin is used as a starch cross-linking agent in the preparation process.
Detailed Description
Weighing 100-120 parts by weight of deionized water, 20-30 parts by weight of 20% sodium hydroxide solution, 40-50 parts by weight of starch and 10-22 parts by weight of 3-chloro-2-hydroxypropyltrimethylammonium chloride respectively, mixing the deionized water, the 20% by weight of sodium hydroxide solution and the starch, uniformly stirring at the room temperature at the rotating speed of 200-300 r/min to obtain emulsion, adding the 3-chloro-2-hydroxypropyltrimethylammonium chloride, continuously stirring for 5-10 min, heating to 40-50 ℃, stirring and reacting for 8-12 h to obtain a composite solution, adjusting the pH value to 5.5-6.5 by using a 7% by weight hydrochloric acid solution to obtain turbid liquid, performing suction filtration to obtain filter residues, washing 3-5 times by using the deionized water, and drying in an oven at the temperature of 60-70 ℃ to constant weight to obtain modified starch; mixing modified starch, anhydrous methanol and a silver nitrate solution with the mass fraction of 10% according to the mass ratio of 2: 1, stirring for 6-8 hours in the dark at the rotating speed of 100-150 r/min to obtain a blend, adding a trisodium citrate solution with the mass fraction of 5% according to the mass ratio of 1: 10, stirring for 30-50 minutes at the rotating speed of 400-500 r/min to obtain a mixed solution, performing centrifugal separation to obtain a precipitate, washing for 3-5 times by using anhydrous ethanol and deionized water respectively, and drying to constant weight to obtain an antibacterial agent; respectively weighing 20-40 parts of an antibacterial agent, 1-10 parts of a quaternary ammonium salt cationic surfactant, 10-16 parts of hyaluronic acid, 1-4 parts of epoxy chloropropane and 50-60 parts of deionized water according to parts by weight, mixing the antibacterial agent, the quaternary ammonium salt cationic surfactant, the hyaluronic acid, the epoxy chloropropane and the deionized water, stirring for 2-4 hours at the temperature of 60-80 ℃ and the rotating speed of 800-1000 r/min, and cooling to room temperature to obtain the medical antibacterial gel dressing.
Weighing 100 parts of deionized water, 20 parts of 20 mass percent sodium hydroxide solution, 40 parts of starch and 10 parts of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride respectively, mixing the deionized water, the 20 mass percent sodium hydroxide solution and the starch, uniformly stirring at the room temperature of the rotation speed of 200r/min to obtain emulsion, adding the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, continuously stirring for 5min, heating to 40 ℃, stirring and reacting for 8h to obtain composite liquid, regulating the pH value to 5.5 by using 7 mass percent hydrochloric acid solution to obtain suspension, performing suction filtration to obtain filter residue, washing 3 times by using the deionized water, and placing in an oven at 60 ℃ to dry to constant weight to obtain modified starch; mixing modified starch, anhydrous methanol and 10% silver nitrate solution according to the mass ratio of 2: 1, stirring for 6h in the dark at the rotating speed of 100r/min to obtain a blend, adding 5% trisodium citrate solution according to the mass ratio of 1: 10, stirring for 30min at the speed of 400r/min to obtain a mixed solution, performing centrifugal separation to obtain a precipitate, washing for 3 times by using anhydrous ethanol and deionized water respectively, and drying to constant weight to obtain an antibacterial agent; respectively weighing 20 parts of antibacterial agent, 1 part of quaternary ammonium salt cationic surfactant, 10 parts of hyaluronic acid, 1 part of epichlorohydrin and 50 parts of deionized water, mixing the antibacterial agent, the quaternary ammonium salt cationic surfactant, the hyaluronic acid, the epichlorohydrin and the deionized water, stirring for 2 hours at the temperature of 60 ℃ and the rotating speed of 800r/min, and cooling to room temperature to obtain the medical antibacterial gel dressing.
Respectively weighing 110 parts of deionized water, 25 parts of 20% sodium hydroxide solution by mass fraction, 45 parts of starch and 16 parts of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, mixing the deionized water, the 20% sodium hydroxide solution by mass fraction and the starch, uniformly stirring at the room temperature of 250r/min to obtain emulsion, adding the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, continuously stirring for 7min, heating to 45 ℃, stirring and reacting for 10h to obtain composite liquid, regulating the pH value to 6.0 by using 7% hydrochloric acid solution by mass fraction to obtain suspension, performing suction filtration to obtain filter residue, washing with the deionized water for 4 times, and placing in a 65 ℃ drying oven to dry to constant weight to obtain modified starch; mixing modified starch, anhydrous methanol and 10% silver nitrate solution according to the mass ratio of 2: 1, stirring for 7h in the dark at the rotating speed of 125r/min to obtain a blend, adding 5% trisodium citrate solution according to the mass ratio of 1: 10, stirring for 40min at the speed of 450r/min to obtain a mixed solution, performing centrifugal separation to obtain a precipitate, washing for 4 times by using anhydrous ethanol and deionized water respectively, and drying to constant weight to obtain an antibacterial agent; respectively weighing 30 parts of antibacterial agent, 5 parts of quaternary ammonium salt cationic surfactant, 13 parts of hyaluronic acid, 2 parts of epichlorohydrin and 55 parts of deionized water according to parts by weight, mixing the antibacterial agent, the quaternary ammonium salt cationic surfactant, the hyaluronic acid, the epichlorohydrin and the deionized water, stirring for 3 hours at the temperature of 70 ℃ and the rotating speed of 900r/min, and cooling to room temperature to obtain the medical antibacterial gel dressing.
Respectively weighing 120 parts of deionized water, 30 parts of 20% sodium hydroxide solution by mass fraction, 50 parts of starch and 22 parts of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, mixing the deionized water, the 20% sodium hydroxide solution by mass fraction and the starch, uniformly stirring at the room temperature of 300r/min to obtain emulsion, adding the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, continuously stirring for 10min, heating to 50 ℃, stirring and reacting for 12h to obtain composite liquid, regulating the pH value to 6.5 by using 7% hydrochloric acid solution by mass fraction to obtain suspension, performing suction filtration to obtain filter residue, washing 5 times with the deionized water, and placing in an oven at 70 ℃ to dry to constant weight to obtain modified starch; mixing modified starch, anhydrous methanol and 10% silver nitrate solution according to the mass ratio of 2: 1, stirring for 8h in the dark at the rotating speed of 150r/min to obtain a blend, adding 5% trisodium citrate solution according to the mass ratio of 1: 10, stirring for 50min at the speed of 500r/min to obtain a mixed solution, performing centrifugal separation to obtain a precipitate, washing for 5 times by using anhydrous ethanol and deionized water respectively, and drying to constant weight to obtain an antibacterial agent; respectively weighing 40 parts of antibacterial agent, 10 parts of quaternary ammonium salt cationic surfactant, 16 parts of hyaluronic acid, 4 parts of epichlorohydrin and 60 parts of deionized water, mixing the antibacterial agent, the quaternary ammonium salt cationic surfactant, the hyaluronic acid, the epichlorohydrin and the deionized water, stirring for 4 hours at the temperature of 80 ℃ and the rotating speed of 1000r/min, and cooling to room temperature to obtain the medical antibacterial gel dressing.
The medical antibacterial gel dressing and the commercially available antibacterial gel dressing prepared by the invention are detected, and the specific detection is as follows:
and (3) testing mechanical strength:
and (3) performing compression mechanical test on hydrogel samples with different parameters by using a universal mechanical testing machine, and compressing at the speed of 1mm/min until the samples are broken.
Swelling property test: soaking the prepared hydrogel sample in a centrifuge tube containing 15ml PBS, placing the centrifuge tube in a constant humidity culture table with the temperature of 37 ℃ and the rpm of 70rpm, testing the swelling performance, taking out after 1h, absorbing the surface moisture by using filter paper and weighing. After the swelling experiment is finished, the hydrogel is taken out, freeze-dried and weighed to obtain the mass of the dry gel.
Calculation formula of swelling degreeThe following were used: degree of swelling = (W)i-Wd)/Wd
Wherein WiThe mass of the gel after swelling after absorption of water, WdIs the mass of the gel in the dry state.
And (3) testing air permeability: the air permeability of the medical antibacterial gel dressing is measured by using a computer type air permeability tester, the set pressure difference is 100.0Pa, and the test area is 20cm2The number of the nozzle is 0.8.
The specific test results are shown in table 1.
Table 1 comparative table of property characterization
Item | Example 1 | Example 2 | Example 3 | Comparative example |
Tangent modulus (MPa) | 211 | 213 | 209 | 185 |
Degree of swelling (%) | 3000 | 3400 | 3200 | 4000 |
Air permeability (%) | 2.81 | 2.75 | 2.77 | 1.98 |
As can be seen from Table 1, the medical antibacterial gel dressing prepared by the invention has the advantages of good mechanical strength, good air permeability and wide application prospect.
Claims (6)
1. A preparation method of medical antibacterial gel dressing is characterized by comprising the following specific preparation steps:
(1) weighing 100-120 parts by weight of deionized water, 20-30 parts by weight of 20% sodium hydroxide solution, 40-50 parts by weight of starch and 10-22 parts by weight of 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, mixing the deionized water, the 20% by weight of sodium hydroxide solution, the starch and the 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, stirring to obtain a composite solution, adjusting the pH value to obtain a suspension, carrying out suction filtration to obtain filter residues, washing with the deionized water for 3-5 times, and drying in an oven at 60-70 ℃ to constant weight to obtain modified starch;
(2) mixing modified starch, anhydrous methanol and a silver nitrate solution with the mass fraction of 10% according to the mass ratio of 2: 1, stirring for 6-8 hours in a dark place at the rotating speed of 100-150 r/min to obtain a blend, adding a trisodium citrate solution with the mass fraction of 5%, stirring to obtain a mixed solution, performing centrifugal separation to obtain a precipitate, washing for 3-5 times by using anhydrous ethanol and deionized water respectively, and drying to constant weight to obtain an antibacterial agent;
(3) respectively weighing 20-40 parts of an antibacterial agent, 1-10 parts of a quaternary ammonium salt cationic surfactant, 10-16 parts of hyaluronic acid, 1-4 parts of epoxy chloropropane and 50-60 parts of deionized water according to parts by weight, mixing the antibacterial agent, the quaternary ammonium salt cationic surfactant, the hyaluronic acid, the epoxy chloropropane and the deionized water, stirring at a constant temperature, and cooling to room temperature to obtain the medical antibacterial gel dressing.
2. The method for preparing the medical antibacterial gel dressing according to claim 1, wherein the method comprises the following steps: the stirring treatment in the step (1) is to mix deionized water, a sodium hydroxide solution with the mass fraction of 20% and starch, stir the mixture evenly at room temperature at the rotating speed of 200-300 r/min to obtain emulsion, add 3-chloro-2-hydroxypropyl trimethyl ammonium chloride, continue stirring for 5-10 min, heat the mixture to 40-50 ℃ and stir the mixture for reaction for 8-12 h.
3. The method for preparing the medical antibacterial gel dressing according to claim 1, wherein the method comprises the following steps: and (2) adjusting the pH value in the step (1) to 5.5-6.5 by using a hydrochloric acid solution with the mass fraction of 7%.
4. The method for preparing the medical antibacterial gel dressing according to claim 1, wherein the method comprises the following steps: the mass ratio of the trisodium citrate solution with the mass fraction of 5 percent to the blend in the step (2) is 1: 10.
5. The method for preparing the medical antibacterial gel dressing according to claim 1, wherein the method comprises the following steps: the stirring treatment in the step (2) is stirring for 30-50 min at the speed of 400-500 r/min.
6. The method for preparing the medical antibacterial gel dressing according to claim 1, wherein the method comprises the following steps: the constant-temperature stirring treatment in the step (3) is stirring for 2-4 hours at the temperature of 60-80 ℃ and the rotating speed of 800-1000 r/min.
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CN102585021B (en) * | 2012-02-21 | 2014-06-11 | 芜湖迅腾新材料有限公司 | Method for synthesizing composite modified starch slurry |
CN103520767B (en) * | 2013-10-28 | 2016-08-17 | 山东赛克赛斯药业科技有限公司 | A kind of antibacterial heal-promoting aerogel dressing and preparation method thereof |
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