CN112972750B - Antibacterial and disinfectant nanofiber medical dressing and preparation method thereof - Google Patents
Antibacterial and disinfectant nanofiber medical dressing 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
- A61L15/44—Medicaments
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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
- A61L15/18—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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- 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
- A61L15/42—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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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/10—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
- A61L2300/102—Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2300/00—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
- A61L2300/40—Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
- A61L2300/404—Biocides, antimicrobial agents, antiseptic agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2400/00—Materials characterised by their function or physical properties
- A61L2400/12—Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
Abstract
The invention relates to the technical field of medical dressings and discloses an antibacterial and disinfectant nanofiber medical dressing, nano zinc oxide is a multifunctional inorganic nano material, has a series of advantages of high temperature resistance, antibiosis and the like, is a multifunctional semiconductor oxide with antimicrobial activity, can be excited to generate active oxygen species such as superoxide anion or active hydroxyl and the like, generates active groups such as hydrogen peroxide and the like, thereby causing the damage of bacterial cell membrane, protein and the like, causing the cell death and achieving the purpose of sterilization, the imidazole group carried by the side chain of histidine makes the histidine become basic amino acid with positive charge, the positive charge of cellulose is increased by the grafting method, the antibacterial activity of the cellulose is improved, meanwhile, the nano-fiber medical dressing is grafted to a cellulose substrate, so that the dispersibility of nano-zinc oxide can be effectively improved, and the antibacterial effect is improved, thereby obtaining the nano-fiber medical dressing with good antibacterial and disinfection performance.
Description
Technical Field
The invention relates to the technical field of medical dressings, in particular to an antibacterial and disinfectant nanofiber medical dressing and a preparation method thereof.
Background
The rapid development of the economic level effectively improves the medical care consciousness of residents, and meanwhile, medical resources of China are gradually enriched and improved, but with the increasing severity of environmental pollution and the abuse of various medicines, people face more and more health threats, the skin is taken as the tissue of the epidermis of the human body, the important role of protecting the inside of the human body is played, the faced threats and injuries cannot be avoided, medical dressings can form a wound healing environment by covering damaged skin, play a role in protecting the skin, are common medical instruments, and have wide prospects and research spaces.
The medical dressings are various, the traditional dressings mainly comprise sterile gauze, absorbent cotton and the like, the early medical dressings mainly keep the wound dry by absorbing the effusion at the wound to accelerate the wound healing, but the dressings are easy to adhere to the wound to cause secondary injury and have great defects, the nano fiber is a raw material of the medical dressings with better advanced and good effect, can well isolate the external pollution to the wound, simulate extracellular matrix, can achieve the effect of antibacterial disinfection on the wound by grafting effective antibacterial and disinfectant groups or substances, provide favorable environment for the wound healing, wherein the cellulose is taken as a novel material and has good application prospect in the field of medical dressings, is polysaccharide with the largest content and the widest distribution in nature and is a renewable resource, meanwhile, the antibacterial nano-fiber medical dressing has biocompatibility and is easy to degrade, the antibacterial nano-fiber medical dressing is a green and environment-friendly material, antibacterial agents such as quaternary ammonium salt, quaternary phosphonium salt, imidazole and the like are grafted after cellulose is modified, and nano-particle zinc oxide, silver, copper and the like are compounded with a matrix, so that the excellent antibacterial and disinfection effect is shown, the antibacterial and disinfection capacity of the matrix is improved, and the antibacterial and disinfection nano-fiber medical dressing is obtained.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides an antibacterial and disinfectant nanofiber medical dressing and a preparation method thereof, and solves the problem of poor antibacterial effect of the traditional medical dressing.
(II) technical scheme
In order to achieve the purpose, the invention provides the following technical scheme: an antibacterial and disinfectant nanofiber medical dressing comprises the following components in parts by weight:
(1) using toluene as a solvent, using 3-aminopropyltriethoxysilane to modify the surface of the nano zinc oxide, and obtaining aminated zinc oxide after the reaction is finished;
(2) adding aminated zinc oxide into deionized water, performing ultrasonic dispersion, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, N-hydroxysuccinimide and histidine, stirring and mixing uniformly, performing amidation reaction, dialyzing and drying after the reaction is finished, thereby obtaining histidine modified zinc oxide;
(3) adding sodium periodate and nano-cellulose into a deionized water solvent, uniformly stirring and mixing, carrying out selective oxidation under a dark condition, after the reaction is finished, carrying out suction filtration, centrifuging, washing and drying to obtain aldehyde cellulose;
(4) adding histidine modified zinc oxide into a methanol solvent, performing ultrasonic dispersion, adding aldehyde cellulose, stirring and mixing uniformly, adding sodium hydroxide to perform Schiff base reaction, and after the reaction is finished, washing, filtering and drying to obtain histidine modified zinc oxide grafted cellulose;
(5) and adding histidine modified zinc oxide grafted cellulose into deionized water again, stirring, mixing uniformly, dissolving, standing for 2-6h, adding the mixed solution into an electrostatic spinning machine, carrying out electrostatic spinning, and obtaining the antibacterial and disinfectant nanofiber medical dressing after spinning is finished.
Preferably, the mass ratio of the zinc oxide amide, the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, the N-hydroxysuccinimide and the histidine in the step (2) is 100:2.5-4:2-5: 200-.
Preferably, the temperature of the amidation reaction in the step (2) is 15-45 ℃, and the time of the amidation reaction is 24-48 h.
Preferably, the temperature of the selective oxidation in the step (3) is 35-50 ℃, and the time of the selective oxidation is 15-30 min.
Preferably, the mass ratio of the histidine-modified zinc oxide to the aldehyde cellulose to the sodium hydroxide in the step (4) is 5-10:100: 4-8.
Preferably, the temperature of the Schiff base reaction in the step (4) is 20-40 ℃, and the time of the Schiff base reaction is 5-10 h.
Preferably, the flow rate of the electrostatic spinning in the step (5) is 0.2-0.8mL/h, and the voltage of the electrostatic spinning is 7-10 kV.
(III) advantageous technical effects
Compared with the prior art, the invention has the following beneficial technical effects:
in the synthesis process of the antibacterial and disinfectant nanofiber medical dressing, 3-aminopropyltriethoxysilane is firstly used for modifying nano zinc oxide to obtain aminated zinc oxide, in deionized water, amido on aminated zinc oxide and carboxyl on histidine are amidated under the action of 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride and N-hydroxysuccinimide to modify zinc oxide with histidine, in a methanol solvent, performing Schiff base reaction on an amido group on histidine modified zinc oxide and an aldehyde group on aldehydized cellulose obtained by modifying sodium periodate under the action of sodium hydroxide to obtain histidine modified zinc oxide grafted cellulose, in an electrostatic spinning machine, histidine modified zinc oxide grafted cellulose is used as a raw material, and electrostatic spinning is carried out to obtain the antibacterial and disinfectant nanofiber medical dressing.
The antibacterial and disinfectant nanofiber medical dressing is a multifunctional inorganic nano material, has a series of advantages of high temperature resistance, antibiosis and the like, is a multifunctional semiconductor oxide with antimicrobial activity, can excite to generate active oxygen species such as superoxide anion or active hydroxyl and the like, and further generates active groups such as hydrogen peroxide and the like through a series of reactions, so that cell membranes, proteins and the like of bacteria are damaged, cell death is caused, and the purpose of sterilization is achieved, histidine serves as a biological functional macromolecule, imidazole groups are arranged on side chains, the histidine is made into basic amino acid with positive charge, the basic amino acid is grafted onto cellulose through a grafting method, the positive charge of the cellulose can be theoretically increased, the bacteriostasis of the cellulose is improved, and meanwhile, the histidine is grafted onto a cellulose matrix, the dispersibility of the nano zinc oxide can be effectively improved, the antibacterial effect is improved, so that the nanofiber medical dressing with good antibacterial and disinfection performance is obtained.
Drawings
FIG. 1 is a diagram showing the synthetic mechanism of histidine-modified zinc oxide.
FIG. 2 is a diagram showing the synthetic mechanism of histidine-modified zinc oxide-grafted cellulose.
Detailed Description
To achieve the above object, the present invention provides the following embodiments and examples: the preparation method of the antibacterial and disinfectant nanofiber medical dressing comprises the following steps:
(1) adding a toluene solvent into a flask, carrying out surface modification on the nano zinc oxide by using 3-aminopropyltriethoxysilane, and obtaining aminated zinc oxide after the reaction is finished;
(2) adding deionized water and aminated zinc oxide into a flask, performing ultrasonic dispersion, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, N-hydroxysuccinimide and histidine, stirring and mixing the added aminated zinc oxide, 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, N-hydroxysuccinimide and histidine uniformly at a mass ratio of 100:2.5-4:2-5:200 and 280, performing amidation reaction at 15-45 ℃, wherein the amidation reaction time is 24-48h, after the reaction is finished, putting the mixture into deionized water for dialysis, and performing vacuum freeze drying to obtain histidine modified zinc oxide;
(3) adding a deionized water solvent, sodium periodate and nano-cellulose into a flask, stirring and mixing uniformly, carrying out selective oxidation at 35-50 ℃ in a dark condition for 15-30min, after the reaction is finished, carrying out suction filtration, centrifuging, washing with deionized water, and drying to obtain aldehyde cellulose;
(4) adding methanol solvent and histidine modified zinc oxide into a three-neck flask, performing ultrasonic dispersion, adding formylated cellulose, stirring and mixing uniformly, adding sodium hydroxide, wherein the mass ratio of the added histidine modified zinc oxide to the formylated cellulose to the sodium hydroxide is 5-10:100:4-8, performing Schiff base reaction at 20-40 ℃ for 5-10h, and after the reaction is finished, washing, filtering and drying to obtain histidine modified zinc oxide grafted cellulose;
(5) adding deionized water and histidine modified zinc oxide grafted cellulose into a beaker, stirring, mixing uniformly, dissolving, standing for 2-6h, adding the mixed solution into an electrostatic spinning machine, carrying out electrostatic spinning, wherein the flow rate of electrostatic spinning is 0.2-0.8mL/h, the voltage of electrostatic spinning is 7-10kV, and obtaining the antibacterial and disinfectant nanofiber medical dressing after spinning.
Example 1
(1) Adding a toluene solvent into a flask, carrying out surface modification on the nano zinc oxide by using 3-aminopropyltriethoxysilane, and obtaining aminated zinc oxide after the reaction is finished;
(2) adding deionized water and aminated zinc oxide into a flask, performing ultrasonic dispersion, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, N-hydroxysuccinimide and histidine, wherein the mass ratio of the added aminated zinc oxide to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to the N-hydroxysuccinimide to the histidine is 100:2.5:2:200, uniformly stirring and mixing, performing amidation reaction at 15 ℃, wherein the amidation reaction time is 24 hours, after the reaction is finished, dialyzing in deionized water, and performing vacuum freeze drying to obtain histidine modified zinc oxide;
(3) adding a deionized water solvent, sodium periodate and nano-cellulose into a flask, stirring and mixing uniformly, carrying out selective oxidation at 35 ℃ in a dark condition for 15min, after the reaction is finished, carrying out suction filtration, centrifuging, washing with deionized water, and drying to obtain aldehyde cellulose;
(4) adding methanol solvent and histidine modified zinc oxide into a three-neck flask, performing ultrasonic dispersion, adding aldehyde cellulose, stirring and mixing uniformly, adding sodium hydroxide, wherein the mass ratio of the added histidine modified zinc oxide to the aldehyde cellulose to the sodium hydroxide is 5:100:4, performing Schiff base reaction at 20 ℃, the Schiff base reaction time is 5 hours, and after the reaction is finished, washing, filtering and drying to obtain histidine modified zinc oxide grafted cellulose;
(5) adding deionized water and histidine modified zinc oxide grafted cellulose into a beaker, stirring, mixing uniformly, dissolving, standing for 2h, adding the mixed solution into an electrostatic spinning machine, carrying out electrostatic spinning, wherein the flow rate of the electrostatic spinning is 0.2mL/h, the voltage of the electrostatic spinning is 7kV, and obtaining the antibacterial and disinfectant nanofiber medical dressing after the spinning is finished.
Example 2
(1) Adding a toluene solvent into a flask, carrying out surface modification on the nano zinc oxide by using 3-aminopropyltriethoxysilane, and obtaining aminated zinc oxide after the reaction is finished;
(2) adding deionized water and aminated zinc oxide into a flask, performing ultrasonic dispersion, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, N-hydroxysuccinimide and histidine, wherein the mass ratio of the added aminated zinc oxide to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to the N-hydroxysuccinimide to the histidine is 100:3:3:220, uniformly stirring and mixing, performing amidation reaction at 20 ℃, wherein the amidation reaction time is 30 hours, after the reaction is finished, dialyzing in deionized water, and performing vacuum freeze drying to obtain histidine modified zinc oxide;
(3) adding a deionized water solvent, sodium periodate and nano-cellulose into a flask, stirring and mixing uniformly, carrying out selective oxidation at 40 ℃ in a dark condition for 20min, after the reaction is finished, carrying out suction filtration, centrifuging, washing with deionized water, and drying to obtain aldehyde cellulose;
(4) adding methanol solvent and histidine modified zinc oxide into a three-neck flask, performing ultrasonic dispersion, adding aldehyde cellulose, stirring and mixing uniformly, adding sodium hydroxide, wherein the mass ratio of the added histidine modified zinc oxide to the aldehyde cellulose to the sodium hydroxide is 7:100:5, performing Schiff base reaction at 25 ℃, the Schiff base reaction time is 6 hours, and after the reaction is finished, washing, filtering and drying to obtain histidine modified zinc oxide grafted cellulose;
(5) adding deionized water and histidine modified zinc oxide grafted cellulose into a beaker, stirring, mixing uniformly, dissolving, standing for 4h, adding the mixed solution into an electrostatic spinning machine, carrying out electrostatic spinning, wherein the flow rate of the electrostatic spinning is 0.4mL/h, the voltage of the electrostatic spinning is 8kV, and obtaining the antibacterial and disinfectant nanofiber medical dressing after the spinning is finished.
Example 3
(1) Adding a toluene solvent into a flask, carrying out surface modification on the nano zinc oxide by using 3-aminopropyltriethoxysilane, and obtaining aminated zinc oxide after the reaction is finished;
(2) adding deionized water and aminated zinc oxide into a flask, performing ultrasonic dispersion, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, N-hydroxysuccinimide and histidine, wherein the mass ratio of the added aminated zinc oxide to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to the N-hydroxysuccinimide to the histidine is 100:3.5:4:260, uniformly stirring and mixing, performing amidation reaction at 35 ℃, wherein the amidation reaction time is 45 hours, after the reaction is finished, dialyzing in deionized water, and performing vacuum freeze drying to obtain histidine modified zinc oxide;
(3) adding a deionized water solvent, sodium periodate and nano-cellulose into a flask, stirring and mixing uniformly, carrying out selective oxidation at 45 ℃ in a dark condition for 25min, after the reaction is finished, carrying out suction filtration, centrifuging, washing with deionized water, and drying to obtain aldehyde cellulose;
(4) adding methanol solvent and histidine modified zinc oxide into a three-neck flask, performing ultrasonic dispersion, adding aldehyde cellulose, stirring and mixing uniformly, adding sodium hydroxide, wherein the mass ratio of the added histidine modified zinc oxide to the aldehyde cellulose to the sodium hydroxide is 9:100:7, performing Schiff base reaction at 35 ℃, the Schiff base reaction time is 8 hours, and after the reaction is finished, washing, filtering and drying to obtain histidine modified zinc oxide grafted cellulose;
(5) adding deionized water and histidine modified zinc oxide grafted cellulose into a beaker, stirring, mixing uniformly, dissolving, standing for 5h, adding the mixed solution into an electrostatic spinning machine, carrying out electrostatic spinning, wherein the flow rate of the electrostatic spinning is 0.6mL/h, the voltage of the electrostatic spinning is 9kV, and obtaining the antibacterial and disinfectant nanofiber medical dressing after the spinning is finished.
Example 4
(1) Adding a toluene solvent into a flask, carrying out surface modification on the nano zinc oxide by using 3-aminopropyltriethoxysilane, and obtaining aminated zinc oxide after the reaction is finished;
(2) adding deionized water and aminated zinc oxide into a flask, performing ultrasonic dispersion, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, N-hydroxysuccinimide and histidine, wherein the mass ratio of the added aminated zinc oxide to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to the N-hydroxysuccinimide to the histidine is 100:4:5:280, uniformly stirring and mixing, performing amidation reaction at 45 ℃, wherein the amidation reaction time is 48 hours, after the reaction is finished, putting the mixture into deionized water for dialysis, and performing vacuum freeze drying to obtain histidine modified zinc oxide;
(3) adding a deionized water solvent, sodium periodate and nano-cellulose into a flask, stirring and mixing uniformly, carrying out selective oxidation at 50 ℃ in a dark condition for 30min, after the reaction is finished, carrying out suction filtration, centrifuging, washing with deionized water, and drying to obtain aldehyde cellulose;
(4) adding methanol solvent and histidine modified zinc oxide into a three-neck flask, performing ultrasonic dispersion, adding aldehyde cellulose, stirring and mixing uniformly, adding sodium hydroxide, wherein the mass ratio of the added histidine modified zinc oxide to the aldehyde cellulose to the sodium hydroxide is 10:100:8, performing Schiff base reaction at 40 ℃, the Schiff base reaction time is 10 hours, and after the reaction is finished, washing, filtering and drying to obtain histidine modified zinc oxide grafted cellulose;
(5) adding deionized water and histidine modified zinc oxide grafted cellulose into a beaker, stirring, mixing uniformly, dissolving, standing for 6h, adding the mixed solution into an electrostatic spinning machine, carrying out electrostatic spinning, wherein the flow rate of the electrostatic spinning is 0.8mL/h, the voltage of the electrostatic spinning is 10kV, and obtaining the antibacterial and disinfectant nanofiber medical dressing after the spinning is finished.
Comparative example 1
(1) Adding a toluene solvent into a flask, carrying out surface modification on the nano zinc oxide by using 3-aminopropyltriethoxysilane, and obtaining aminated zinc oxide after the reaction is finished;
(2) adding deionized water and aminated zinc oxide into a flask, performing ultrasonic dispersion, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, N-hydroxysuccinimide and histidine, wherein the mass ratio of the added aminated zinc oxide to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to the N-hydroxysuccinimide to the histidine is 100:1.5:1:150, uniformly stirring and mixing, performing amidation reaction at 30 ℃, wherein the amidation reaction time is 30h, after the reaction is finished, dialyzing in deionized water, and performing vacuum freeze drying to obtain histidine modified zinc oxide;
(3) adding a deionized water solvent, sodium periodate and nano-cellulose into a flask, stirring and mixing uniformly, carrying out selective oxidation at 40 ℃ in a dark condition for 20min, after the reaction is finished, carrying out suction filtration, centrifuging, washing with deionized water, and drying to obtain aldehyde cellulose;
(4) adding methanol solvent and histidine modified zinc oxide into a three-neck flask, performing ultrasonic dispersion, adding aldehyde cellulose, stirring and mixing uniformly, adding sodium hydroxide, wherein the mass ratio of the added histidine modified zinc oxide to the aldehyde cellulose to the sodium hydroxide is 3.5:100:3, performing Schiff base reaction at 30 ℃, the Schiff base reaction time is 7 hours, and after the reaction is finished, washing, filtering and drying to obtain histidine modified zinc oxide grafted cellulose;
(5) adding deionized water and histidine modified zinc oxide grafted cellulose into a beaker, stirring, mixing uniformly, dissolving, standing for 4h, adding the mixed solution into an electrostatic spinning machine, carrying out electrostatic spinning, wherein the flow rate of the electrostatic spinning is 0.1mL/h, the voltage of the electrostatic spinning is 8kV, and obtaining the antibacterial and disinfectant nanofiber medical dressing after the spinning is finished.
Comparative example 2
(1) Adding a toluene solvent into a flask, carrying out surface modification on the nano zinc oxide by using 3-aminopropyltriethoxysilane, and obtaining aminated zinc oxide after the reaction is finished;
(2) adding deionized water and aminated zinc oxide into a flask, performing ultrasonic dispersion, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, N-hydroxysuccinimide and histidine, wherein the mass ratio of the added aminated zinc oxide to the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride to the N-hydroxysuccinimide to the histidine is 100:5:5.5:320, uniformly stirring and mixing, performing amidation reaction at 40 ℃, wherein the amidation reaction time is 45 hours, after the reaction is finished, dialyzing in deionized water, and performing vacuum freeze drying to obtain histidine modified zinc oxide;
(3) adding a deionized water solvent, sodium periodate and nano-cellulose into a flask, stirring and mixing uniformly, carrying out selective oxidation at 45 ℃ in a dark condition for 25min, after the reaction is finished, carrying out suction filtration, centrifuging, washing with deionized water, and drying to obtain aldehyde cellulose;
(4) adding methanol solvent and histidine modified zinc oxide into a three-neck flask, performing ultrasonic dispersion, adding aldehyde cellulose, stirring and mixing uniformly, adding sodium hydroxide, wherein the mass ratio of the added histidine modified zinc oxide to the aldehyde cellulose to the sodium hydroxide is 15:100:14, performing Schiff base reaction at 30 ℃, the Schiff base reaction time is 9 hours, and after the reaction is finished, washing, filtering and drying to obtain histidine modified zinc oxide grafted cellulose;
(5) adding deionized water and histidine modified zinc oxide grafted cellulose into a beaker, stirring, mixing uniformly, dissolving, standing for 5h, adding the mixed solution into an electrostatic spinning machine, carrying out electrostatic spinning, wherein the flow rate of the electrostatic spinning is 0.9mL/h, the voltage of the electrostatic spinning is 9kV, and obtaining the antibacterial and disinfectant nanofiber medical dressing after the spinning is finished.
Testing antibacterial property of sample by antibacterial ring method, preparing liquid culture medium and plate culture medium, inoculating Escherichia coli into seed culture medium, culturing at constant temperature for 12 hr to obtain seed solution, diluting with normal saline to 10%7CFU/mL, absorbing seed liquid into a solid plate culture medium, uniformly coating, respectively spreading the antibacterial and disinfectant nanofiber medical dressing synthesized in the embodiment and the comparative example at the center of a plate, carrying out inverted culture for 24 hours in a constant temperature environment of 37 ℃, checking whether an inhibition zone exists, measuring the difference between the radiuses of the inhibition zone and the antibacterial and disinfectant nanofiber medical dressing, testing each sample for three times, and measuring the diameter of the inhibition zone.
Claims (7)
1. An antibacterial and disinfectant nanofiber medical dressing is characterized in that: the preparation method of the antibacterial and disinfectant nanofiber medical dressing comprises the following steps:
(1) using toluene as a solvent, using 3-aminopropyltriethoxysilane to modify the surface of the nano zinc oxide, and obtaining aminated zinc oxide after the reaction is finished;
(2) adding aminated zinc oxide into deionized water, performing ultrasonic dispersion, adding 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, N-hydroxysuccinimide and histidine, stirring and mixing uniformly, performing amidation reaction, dialyzing and drying after the reaction is finished, thereby obtaining histidine modified zinc oxide;
(3) adding sodium periodate and nano-cellulose into a deionized water solvent, uniformly stirring and mixing, carrying out selective oxidation under a dark condition, after the reaction is finished, carrying out suction filtration, centrifuging, washing and drying to obtain aldehyde cellulose;
(4) adding histidine modified zinc oxide into a methanol solvent, performing ultrasonic dispersion, adding aldehyde cellulose, stirring and mixing uniformly, adding sodium hydroxide to perform Schiff base reaction, and after the reaction is finished, washing, filtering and drying to obtain histidine modified zinc oxide grafted cellulose;
(5) and adding histidine modified zinc oxide grafted cellulose into deionized water again, stirring, mixing uniformly, dissolving, standing for 2-6h, adding the mixed solution into an electrostatic spinning machine, carrying out electrostatic spinning, and obtaining the antibacterial and disinfectant nanofiber medical dressing after spinning is finished.
2. The medical dressing of claim 1, wherein the antibacterial and antiseptic nanofiber dressing comprises: the mass ratio of the zinc oxide amide, the 1- (3-dimethylaminopropyl) -3-ethylcarbodiimide hydrochloride, the N-hydroxysuccinimide and the histidine in the step (2) is 100:2.5-4:2-5: 200-280.
3. The medical dressing of claim 1, wherein the antibacterial and antiseptic nanofiber dressing comprises: the temperature of the amidation reaction in the step (2) is 15-45 ℃, and the time of the amidation reaction is 24-48 h.
4. The medical dressing of claim 1, wherein the antibacterial and antiseptic nanofiber dressing comprises: the temperature of the selective oxidation in the step (3) is 35-50 ℃, and the time of the selective oxidation is 15-30 min.
5. The medical dressing of claim 1, wherein the antibacterial and antiseptic nanofiber dressing comprises: in the step (4), the mass ratio of the histidine modified zinc oxide to the aldehyde cellulose to the sodium hydroxide is 5-10:100: 4-8.
6. The medical dressing of claim 1, wherein the antibacterial and antiseptic nanofiber dressing comprises: the temperature of the Schiff base reaction in the step (4) is 20-40 ℃, and the time of the Schiff base reaction is 5-10 h.
7. The medical dressing of claim 1, wherein the antibacterial and antiseptic nanofiber dressing comprises: the flow rate of electrostatic spinning in the step (5) is 0.2-0.8mL/h, and the voltage of electrostatic spinning is 7-10 kV.
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| CN102091346A (en) * | 2010-01-15 | 2011-06-15 | 东华大学 | Bacterial cellulose-based antibacterial dry film for acute trauma and preparation method and application thereof |
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| CN102091346A (en) * | 2010-01-15 | 2011-06-15 | 东华大学 | Bacterial cellulose-based antibacterial dry film for acute trauma and preparation method and application thereof |
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