CN116251223A - Rare earth metal-based dressing for wound surface sterilization and preparation method thereof - Google Patents

Rare earth metal-based dressing for wound surface sterilization and preparation method thereof Download PDF

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CN116251223A
CN116251223A CN202310513553.6A CN202310513553A CN116251223A CN 116251223 A CN116251223 A CN 116251223A CN 202310513553 A CN202310513553 A CN 202310513553A CN 116251223 A CN116251223 A CN 116251223A
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rare earth
dressing
earth metal
base cloth
preparation
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CN116251223B (en
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张春霞
张光睿
李璐
孙丕智
刘岗
赵长玉
彭维
阚丽欣
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Tianjin Baogang Rare Earth Research Institute Co Ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/20Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing organic materials
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/18Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing inorganic materials
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L15/00Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
    • A61L15/16Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
    • A61L15/42Use of materials characterised by their function or physical properties
    • A61L15/44Medicaments
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/10Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices containing or releasing inorganic materials
    • A61L2300/102Metals or metal compounds, e.g. salts such as bicarbonates, carbonates, oxides, zeolites, silicates
    • A61L2300/104Silver, e.g. silver sulfadiazine
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2300/00Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices
    • A61L2300/40Biologically active materials used in bandages, wound dressings, absorbent pads or medical devices characterised by a specific therapeutic activity or mode of action
    • A61L2300/404Biocides, antimicrobial agents, antiseptic agents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS 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
    • A61L2400/00Materials characterised by their function or physical properties
    • A61L2400/12Nanosized materials, e.g. nanofibres, nanoparticles, nanowires, nanotubes; Nanostructured surfaces
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

A rare earth metal-based dressing for wound surface sterilization and a preparation method thereof are provided, wherein the sterilization dressing comprises a base cloth and a dressing liquid, and the base cloth is a hydrophobic base cloth; the dressing liquid is prepared from the following components: rare earth Eu-loaded nanoparticles: 4-8wt%; glycerol: 0.5-2wt%; butanediol: 0.5-2wt%; zinc gluconate: 1-6wt%; 0.1-0.5wt% of potassium persulfate; triethanolamine: 3-10wt%; phenoxyethanol: 1-2wt%; the balance of water. The dressing provided by the invention has good stability and good air permeability, and can play a role in killing bacteria in the air after contacting the bacteria. Proved by verification, the dressing provided by the invention has obvious inhibition and killing effects on two common and representative infectious bacteria, namely escherichia coli and staphylococcus aureus.

Description

Rare earth metal-based dressing for wound surface sterilization and preparation method thereof
Technical Field
The invention belongs to the field of sterilization dressing, and particularly relates to a rare earth metal-based dressing for wound surface sterilization and a preparation method thereof.
Background
Wound surface refers to the damage of healthy human skin or tissue caused by internal or external factors, and the damage of normal tissue or the damage of damaged human skin is lost. The common wound surface in clinic and life mainly comprises burn wound surface, electric wound surface, chemical corrosion wound surface and the like. The wound surface is directly contacted with the external environment, and has the environmental characteristics of warmth, humidity and the like, so that the bacteria can be quickly propagated on the wound surface, and the bacteria are easy to infect and possibly cause other complications due to invasion and quick propagation of microorganisms such as escherichia coli, staphylococcus aureus and the like. Among them, the development of antibacterial dressings for wound surfaces has also become one of the hot spots of medical research in recent years.
The traditional medical dressing is cotton gauze, and has the main effects of stopping bleeding, sterilizing and absorbing wound surface exudates, but has the defects of easy adhesion to wound surfaces, injury again, strong gauze air permeability, high probability of bacterial infection, high usage amount and frequent replacement. In the prior art, high polymer material medical dressings are adopted to replace the traditional gauze, but the medical dressings have the defects of poor antibacterial and anti-infection performances, poor air permeability and further improved biocompatibility, and can not accelerate wound healing. The existing antibacterial dressing on the market generally uses antibiotics or soaking antibiotic solution to achieve the antibacterial purpose, but a large amount of antibiotics are used, so that not only can the environment be polluted, but also the antibiotic resistance of bacteria can be improved, so that the antibiotics are invalid, and some bacteria become superbacteria after being subjected to mutation under the influence of the antibiotics, so that the national biosafety is endangered. In addition, pregnant women and the elderly can have a certain influence on their health after using these antibiotic-containing dressings. Therefore, the development of the medical antibacterial dressing with lasting and efficient sterilization and bacteriostasis meets the market demand, and has very important significance for efficient treatment of skin wounds.
Disclosure of Invention
In view of the above, the present invention aims to overcome the defects in the prior art, and proposes a rare earth metal-based dressing for wound surface sterilization and a preparation method thereof.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
in a first aspect, the present invention provides a rare earth metal-based dressing for wound surface sterilization, the dressing being made from a base fabric impregnated with a dressing liquid; the base cloth is hydrophobic base cloth, and the warp yarn number is 75+/-35 per 100 mm; the number of weft yarns per 100 mm is 65+/-30; the dressing liquid is prepared from the following components in percentage by mass: rare earth Eu-loaded nanoparticles: 4-8wt%; glycerol: 0.5-2wt%; butanediol: 0.5-2wt%; zinc gluconate: 1-6wt%; 0.1-0.5wt% of potassium persulfate; triethanolamine: 3-10wt%; phenoxyethanol: 1-2wt%; the balance of water.
Preferably, the rare earth Eu-loaded nanoparticle consists of a Eu-containing reagent, chloroauric acid (HAuCl) 4 ) Silver nitrate (AgNO) 3 ) The raw materials of Glutathione (GSH) and sodium Citrate (CA) are prepared.
Preferably, the Eu-containing reagent, chloroauric acid (HAuCl) 4 ) Silver nitrate (AgNO) 3 ) The molar concentration ratio of Glutathione (GSH) to sodium Citrate (CA) is 1: (8-9): (4-5): (30-32): (200-205).
More preferably, the Eu-containing reagent, chloroauric acid (HAuCl) 4 ) Silver nitrate (AgNO) 3 ) The molar concentration ratio of Glutathione (GSH) to sodium Citrate (CA) is 1:8:4:32:200.
preferably, the Eu-containing reagent is Na x [EuW 10 O 36 ]•yH 2 O, wherein x is taken from 8, 9, 10, y is taken from 30,31、32、33、34、35。
Preferably, the Eu-containing reagent is Na 9 [EuW 10 O 36 ]·32H 2 O。
In a second aspect, the invention also provides a preparation method of the rare earth metal-based dressing for wound surface sterilization, which specifically comprises the following steps:
1) Preparation of glutathione protected gold and silver nanoclusters (Au-AgNCs@GSH)
Sequentially to HAuCl 4 AgNO is added into the solution 3 Mixing GSH and CA uniformly, reacting at 100-120 ℃ for 2-3h, taking out, cooling to room temperature, collecting a crude product, adding ethanol into the crude product, mixing uniformly, centrifuging at 8000 rpm for not less than 30 min, removing the supernatant, washing the precipitate, and collecting the glutathione-protected gold and silver nanocluster concentrate for later use;
2) Preparation of rare earth Eu-loaded nanoparticles
Adding Na into the purified glutathione-protected gold-silver nanocluster concentrated solution 9 [EuW 10 O 36 ]•32H 2 O, reacting the obtained mixed solution for 2-3 hours at 65-75 ℃ to obtain rare earth Eu-loaded nano particles, and refrigerating for later use;
3) Preparation of dressing liquid
Mixing rare earth Eu-loaded nano particles, glycerol, butanediol, zinc gluconate, potassium persulfate, triethanolamine, phenoxyethanol and water, and stirring at 35-45deg.C for 20-30 min to obtain a dressing liquid;
4) Preparation of rare earth metal-based dressing
Coating the dressing liquid on a base cloth, and drying at 55-70 ℃; then, the dried base cloth is coated with the dimethyl silicone oil, wherein the coating standard of the dimethyl silicone oil is 0.6-1g/100cm 2 The base cloth is sealed and packaged after being coated; finally, the base cloth is irradiated for 10 to 40 minutes with the irradiation intensity of 10 to 50kGy, and the final rare earth metal base dressing is obtained.
Compared with the prior art, the invention has the following advantages:
(1) The dressing provided by the invention contains rare earth Eu-loaded nano particles, has the characteristic of 805-nm near infrared emission under visible light irradiation, can effectively exert a thermal effect in the process of illumination sterilization, and has a better antibacterial effect compared with other antibacterial medical dressings.
(2) The rare earth Eu-loaded nano particles used in the invention can be used as a substrate to uniformly disperse the metal nanoclusters on the particle surface through electrostatic action.
(3) The dressing provided by the invention has the advantages of no pollution to gram-negative bacteria such as escherichia coliE.coli) And gram positive bacteria staphylococcus aureusS.aureus) Has stronger inhibiting and killing effect.
Drawings
FIG. 1 is a graph showing the DLS dynamic light scattering particle size contrast of the glutathione-protected gold nanoclusters of example 3 (Au-AgNCs@GSH) and the glutathione-protected gold nanoclusters prepared in example 2 (AuNCs@GSH);
FIG. 2 is an SEM image of rare earth Eu-supported metal nanoparticles prepared in example 4;
FIG. 3 shows the dressing of example 10 against E.coliE.coli) And staphylococcus aureus @ andS.aureus) Is a bacterial inhibition of the formula (I);
FIG. 4 shows the E.coli strain using the single material and composite material dressing of example 12E.coli) And staphylococcus aureus @ sS.aureus) The test result of the antibacterial effect coated board.
Detailed Description
Unless defined otherwise, the technical terms used in the following examples have the same meanings as commonly understood by those skilled in the art to which the invention pertains, and the test reagents used in the following examples are as follows:
Na 2 WO 4 •2H 2 O、Eu(NO 3 ) 3 •6H 2 o, hydrochloric acid (HCl), chloroauric acid (HAuCl) 4 ) Glutathione (GSH), sodium Citrate (CA) were purchased from Aba Ding Huaxue Co., ltd, all chemicals were used without further treatment, distilled water [ ]ρ=18.2M Ω·cm, 25 ℃) from Millipore milli-Q water purification system, stock was diluted to the required concentration according to different experimental requirements. Luria Broth (LB) from Sigma-Aldrich, wicklow, ireland. Coli @E.coli) And staphylococcus aureus @ sS.aureus) From Beijing four-ring biopharmaceutical Co. If not specified, the biochemical reagents are all conventional biochemical reagents; the experimental methods are conventional methods unless otherwise specified.
The invention will be described in detail with reference to examples.
Example 1 Na 9 [EuW 10 O 36 ]·32H 2 Preparation and purification of O (EuW 10)
8.3 g of Na 2 WO 4 ·2H 2 O was dissolved in 20 mL distilled water using acetic acid (CH 3 COOH) to adjust the pH to 7.0 to 7.5. Will contain 1.1 g Eu (NO) 3 ) 3 ·6H 2 Dropwise adding O2 mL water solution into the solution, stirring at 80-90 ℃, and cooling to room temperature to obtain crystallized Na 9 [EuW 10 O 36 ]·32H 2 O, after filtration, is dried in air to obtain Na 9 [EuW 10 O 36 ]·32H 2 O。
Example 2 preparation of glutathione protected gold nanoclusters (AuNCs@GSH)
Preparation of HAuCl 4 Stock solutions of GSH and CA were 10 mM, 10 mM and 500 mM, respectively. 0.4 mL 10 mM HAuCl is added to 10 groups of polytetrafluoroethylene lining with total volume of 20 and mL respectively 4 Taking 8.48 and mL secondary distilled water, vibrating while adding, mixing the solutions uniformly, sequentially adding 0.32 mL 100 mM GSH and 0.4 mL of 500 mM CA into the solutions, vibrating uniformly, putting the mixed solutions into a reaction kettle, screwing, performing parallel experiments for 10 groups, transferring into a 110 ℃ oven, reacting for 2.5 h, taking out, and cooling to room temperature.
Purifying: pouring out the solution in the polytetrafluoroethylene lining, collecting the crude product into a 50 mL centrifuge tube, and storing the crude product in 2 tubes for later use. Taking 6 50 mL empty centrifuge tubes, sequentially adding 10 mL crude products into the centrifuge tubes, adding 20 mL ethanol into the centrifuge tubes, vibrating the centrifuge tubes uniformly on a vortex oscillator, transferring the 6 centrifuge tubes into the centrifuge, centrifuging at 8000 rpm for 30 min, removing the supernatant, repeatedly washing the precipitate with secondary distilled water and collecting the precipitate, and operating the remaining 40 mL crude products according to the process flow to finally obtain 10 mL concentrated solution for later use.
Example 3 preparation of glutathione protected gold and silver nanoclusters (Au-AgNCs@GSH)
Preparation of HAuCl 4 、AgNO 3 Stock solutions of GSH and CA at concentrations of 10 mM, 10 mM, 10 mM, 500 mM, respectively; 0.4 mL 10 mM HAuCl is added to 10 groups of polytetrafluoroethylene lining with total volume of 20 and mL respectively 4 Adding 8.48. 8.48 mL secondary distilled water and vibrating to uniformly mix the solutions, sequentially adding 0.3 mL 10 mM AgNO to the above solutions 3 And 0.32 mL 100 mM GSH and 0.4 mL of 500 mM CA, shaking the mixed solution uniformly, putting the mixed solution into a reaction kettle, screwing, carrying out parallel experiments for 10 groups, transferring the mixed solution into a 110 ℃ oven, taking out the mixed solution after reacting 2.5 h, and cooling to room temperature.
Pouring out the solution in the polytetrafluoroethylene lining, collecting the crude product into a 50 mL centrifuge tube, and storing the crude product in 2 tubes for later use. Taking 6 50 mL empty centrifuge tubes, sequentially adding 10 mL crude products into the centrifuge tubes, adding 20 mL ethanol into the centrifuge tubes, vibrating the centrifuge tubes uniformly on a vortex oscillator, transferring the 6 centrifuge tubes into a centrifuge, centrifuging at 8000 rpm for 30 min, removing the supernatant, repeatedly washing the precipitate with secondary distilled water and collecting the precipitate, and operating the remaining 40 mL crude products according to the process flow to finally obtain 10 mL Au-AgNCs@GSH concentrated solution for later use.
The invention uses Ag + Is synthesized into a gold and silver nano cluster (Au-AgNCs@GSH) by a hydrothermal method due to the introduction of Ag + In the figure, the DLS dynamic light scattering spectrum of the glutathione-protected gold and silver nanocluster (Au-AgNCs@GSH) is shown in the figure, and the microsphere particle size is at the nanometer level, so that the monodispersity of the compound is better, and the particle size of about 350 nm of the original gold nanocluster (AuNCs@GSH) is changed into the particle size of about 670 nm of the gold and silver nanocluster (Au-AgNCs@GSH), thereby indicating that Ag+ is well combined with the gold nanocluster.
Example 4 preparation of Eu-loaded nanoparticle additive containing rare earth
Weighing 33.51 mg Na 9 [EuW 10 O 36 ]•32H 2 O in15 Adding 10 mL redistilled water into a mL centrifuge tube to obtain Na with concentration of 10 mM 9 [EuW 10 O 36 ]•32H 2 O stock solution.
To the purified Au-AgNCs@GSH concentrate was added 1 mL of 10 mM Na 9 [EuW 10 O 36 ]•32H 2 O, the obtained mixed solution reacts for 2 hours at 70 ℃ to obtain rare earth Eu-loaded nano particles. Transferring the solution into a centrifuge tube, wrapping with tinfoil, and placing in a refrigerator at 4deg.C for use. Fig. 2 shows a scanning electron microscope image of rare earth Eu-loaded nano-particles, and it can be seen that rare earth Eu is uniformly distributed after being loaded on glutathione-protected gold and silver nanoclusters, which indicates that the surface of the rare earth Eu nano-particles regularly adsorbs the metal nanoclusters on the surface thereof through electrostatic interaction.
EXAMPLE 5 preparation of dressing solution
In a beaker, the following components were mixed in mass percent: rare earth Eu-loaded nanoparticles: 7wt%; glycerol: 1.0wt%; butanediol: 1.0wt%; zinc gluconate: 3wt%; 0.1wt% of potassium persulfate; triethanolamine: 5wt%; phenoxyethanol: 1wt%; and mixing the rest water uniformly to obtain the dressing liquid.
EXAMPLE 6 preparation of rare earth Metal-based dressing for wound surface Sterilization
Coating the dressing liquid on a base cloth, and drying at 60 ℃; then, the dried base cloth is coated with the dimethyl silicone oil, wherein the coating standard of the dimethyl silicone oil is 0.8g/100cm 2 The base cloth is sealed and packaged after being coated; finally, the base cloth is irradiated for 30 minutes with irradiation intensity of 50kGy, so that the final sterilization dressing is obtained, and the base cloth can be cut into different sizes for use according to the needs, wherein 5 mm multiplied by 5 mm dressings are cut for standby for bacteriostasis experiment convenience.
EXAMPLE 7 preparation of the Medium
Liquid LB medium: adding 10g NaCl, 10g peptone and 5g yeast extract into 1L pure water, stirring, packaging into 4 conical flasks, and sterilizing in high pressure steam sterilizing pot at 121deg.C for 25 min.
Solid LB medium: adding 10g of NaCl, 10g peptone, 5g yeast extract and 15g of agar powder into 1L pure water, placing into a high-pressure steam sterilizing pot for sterilizing at 121 ℃ for 25 min, pouring into a disposable culture dish when the temperature is cooled to 55-60 ℃, cooling and solidifying, sealing by a sealing film, and placing into a 4 ℃ refrigerator for standby.
EXAMPLE 8 Escherichia coliE.coli) And staphylococcus aureus @ sS.aureus) Resuscitating and passaging of (a)
To be purchased fromE.coliUniformly mixing the freeze-dried powder and resuscitating solution, inoculating to LB culture solution prepared in advance, placing in a constant-temperature shaking table for culturing 6 h, and sucking 500 μl of cultured second generation in an ultra-clean workbenchE.coliThe bacterial solution was then aspirated 500. Mu.L of 50% glycerol, mixed well in a 2 mL EP tube and stored in a-80℃freezer. Third generationE.coliThe passage method of the strain is the same as the second generation.S.aureusAnd (3) withE.coliResuscitation and passaging were performed using the same method.
Example 9 antibacterial Performance test of zone of inhibition
Will be third generationE.coliInoculating glycerol bacteria into prepared LB culture solution, and performing third generationS.aureusInoculating glycerol bacteria into prepared LB culture solution, placing into a constant temperature shaking table for culturing 5 h, diluting the bacterial solution with PBS solution in an ultra-clean workbench for 10 5 After doubling, 100. Mu.L of diluted solution was aspirated separatelyE.coliAndS.aureusthe bacterial liquid is put into LB agar medium, evenly coated by using a sterile coating rod, then a dressing coating plate of 5 mm multiplied by 5 mm is put in the center of the LB agar medium, a blank control experiment is carried out at the same time, the medium is put into a constant temperature incubator for incubation of 24 h, and the bacteriostasis effect around the coating plate is observed by naked eyes.
Example 10 antibacterial test results of zone of inhibition
Figure 3 shows a macroscopic photograph of the dressing panel after incubation with two bacteria for 24 h. Both control groups had no killing effect on bacteria,E.coliandS.aureusthe growth state is good. At the position ofE.coliThe periphery of the middle dressing test plate generates a bacteriostasis ring of about 2 mm, and the bacteria inhibition ring is arranged onS.aureusThe four sides of the test plate of the middle dressing generate about 3 mm antibacterial rings, and experiments prove that the novel antibacterial dressing has stronger antibacterial effect, so that the novel antibacterial dressing is emptyWhen bacteria in the air contact the antibacterial dressing, more bacteria can be inhibited from growing and even dying.
Example 11 scanning electron microscope observations of the bacteriocidal Effect of the sterilizing and purifying dressing on bacteria
Glycerol was stored in Ep tubesE.coliAndS.aureusthe second generation strain was inoculated in 5 mL of Luria-Bertani (LB) medium, shaken at 37℃overnight, and then 10. Mu.L of the bacterial culture was transferred to 4X 5 mL fresh LB medium for further experiments. After adding 100. Mu.L of dressing solution to each of the above two strains, culturing the cultures in an incubator at 37℃for 24 hours under illumination, transferring 10. Mu.L of the solution onto a silicon wafer and air-drying to prepare samples, and then Scanning Electron Microscopy (SEM) imaging each sample using JEOL JSM 6700F field emission device with primary electron energy of 3 kV, and sputtering a layer of Pt on the sample before imaging to improve conductivity.
Example 12 comparison of bacteriostasis Properties Using Single Material and composite Material in dressing liquid
In order to study the antibacterial effect of single compound and composite material in the dressing liquid, the invention researches each compound by antibacterial experiments, wherein the first group is used as a blank control, the growth states of escherichia coli and staphylococcus aureus are good, and the second group is used for adding Na only according to the original basic condition of the formula in the embodiment 9 [EuW 10 O 36 ]·32H 2 O; in the third group of experiments, according to the original formula basic conditions in the embodiment, only AuNCs@GSH is added; in the fourth set of experiments, au-agncs@gsh was added as the original formulation base conditions were unchanged in the examples. In a fifth set of experiments Na was added according to the original recipe base conditions in the examples 9 [EuW 10 O 36 ]·32H 2 O and AuNCs@GSH, and Au-AgNCs@GSH is not added. In a sixth set of experiments Na was added according to the original recipe base conditions in the examples 9 [EuW 10 O 36 ]·32H 2 O and Au-AgNCs@GSH, auNCs@GSH was not added.
As can be seen from the colonies in FIG. 4, the bacterial viability was compared to the second by the first group of blank experimentsCompared with the blank control, the antibacterial material with Eu nano particles is found to have slightly reduced antibacterial effect on two bacteria compared with the number of bacteria in the blank control, no obvious difference is found, and only slight antibacterial effect is achieved. And counting the bacterial survival rate of a third group of parallel experiments, and finding that the antibacterial effect of the antibacterial material is reduced from the number of bacteria in a blank control, wherein the reduction of the two bacteria is 20% -40%. In the fourth group, the modified alloy nanoclusters Au-AgNCs@GSH are added, and the reduction of the two bacteria is between 50% and 60% compared with the number of bacteria in a blank control. Alloy nanoclusters AuNCs@GSH and Eu-containing nanoparticles Na before modification are added in a fifth group 9 [EuW 10 O 36 ]·32H 2 And O, counting the bacterial survival rate of parallel experiments, and finding that the antibacterial effect of the antibacterial material has a larger reduction than the number of bacteria in a blank control, wherein the reduction of the two bacteria is 60% -70%, but more bacterial colonies exist. The modified alloy nanocluster Au-AgNCs@GSH and Eu-containing nanoparticle Na are added in the sixth group 9 [EuW 10 O 36 ]·32H 2 O, counting the survival rate of the experimental bacteria, and finding out the pair of antibacterial materialsE.coliAndS.aureusthe two bacteria have good antibacterial effect onE.coliThe antibacterial rate of (2) reaches 100 percent, forS.aureusThe antibacterial rate of the composition reaches 99 percent. The comparison of the experiments shows that the dressing finally containing the multi-element compound has better bactericidal capability, and the antibacterial capability of the dressing is greatly improved compared with that of the dressing added with a single antibacterial compound and the antibacterial compound before modification.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.

Claims (6)

1. A rare earth metal-based dressing for wound surface sterilization, characterized in that: the dressing is prepared by dipping base cloth in dressing liquid; the base cloth is hydrophobic base cloth, and the warp yarn number is 75+/-35 per 100 mm; the number of weft yarns per 100 mm is 65+/-30; the dressing liquid is prepared from the following components: rare earth Eu-loaded nanoparticles: 4-8wt%; glycerol: 0.5-2wt%; butanediol: 0.5-2wt%; zinc gluconate: 1-6wt%; 0.1-0.5wt% of potassium persulfate; triethanolamine: 3-10wt%; phenoxyethanol: 1-2wt%; the balance of water.
2. A rare earth metal-based dressing according to claim 1, wherein: the rare earth Eu-loaded nano particles are prepared from raw materials containing Eu reagent, chloroauric acid, silver nitrate, glutathione and sodium citrate.
3. A rare earth metal-based dressing according to claim 2, wherein: the rare earth Eu-loaded nano particle contains Eu reagent, chloroauric acid, silver nitrate, glutathione and sodium citrate in a molar concentration ratio of 1: (8-9): (4-5): (30-32): (200-205).
4. A rare earth metal-based dressing according to claim 2, wherein: the Eu-containing reagent is Na x [EuW 10 O 36 ]•yH 2 O, where x is taken from 8, 9, 10 and y is taken from 30, 31, 32, 33, 34, 35.
5. A rare earth metal-based dressing according to claim 2, wherein: the Eu-containing reagent is Na 9 [EuW 10 O 36 ]·32H 2 O。
6. A method for preparing a rare earth metal-based dressing according to any one of claims 1 to 5, characterized in that: the method specifically comprises the following steps:
1) Preparation of glutathione-protected gold and silver nanoclusters
Sequentially adding silver nitrate, glutathione and sodium citrate into chloroauric acid solution, uniformly mixing, reacting at 100-120 ℃ for 2-3h, taking out, cooling to room temperature, collecting a crude product, adding ethanol into the crude product, uniformly mixing, centrifuging at 8000 rpm for not less than 30 min, removing supernatant, washing precipitate, and collecting to finally obtain glutathione-protected gold and silver nanocluster concentrate for later use;
2) Preparation of rare earth Eu-loaded nanoparticles
Adding Na into the purified glutathione-protected gold-silver nanocluster concentrated solution 9 [EuW 10 O 36 ]•32H 2 O, reacting the obtained mixed solution for 2-3 hours at 65-75 ℃ to obtain rare earth Eu-loaded nano particles, and refrigerating for later use;
3) Preparation of dressing liquid
Mixing rare earth Eu-loaded nano particles, glycerol, butanediol, zinc gluconate, potassium persulfate, triethanolamine, phenoxyethanol and water, and stirring at 35-45deg.C for 20-30 min to obtain a dressing liquid;
4) Preparation of rare earth metal-based dressing
Coating the dressing liquid on a base cloth, and drying at 55-70 ℃; then, the dried base cloth is coated with the dimethyl silicone oil, wherein the coating standard of the dimethyl silicone oil is 0.6-1g/100cm 2 The base cloth is sealed and packaged after being coated; finally, the base cloth is irradiated for 10 to 40 minutes with the irradiation intensity of 10 to 50kGy, and the final rare earth metal base dressing is obtained.
CN202310513553.6A 2023-05-09 2023-05-09 Rare earth metal-based dressing for wound surface sterilization and preparation method thereof Active CN116251223B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106962328A (en) * 2016-06-19 2017-07-21 王金明 A kind of preparation method of rare earth loaded antiseptic
CN108578753A (en) * 2018-03-13 2018-09-28 深圳市源兴医药股份有限公司 A kind of disinfectant dressing and preparation method thereof
CN110339079A (en) * 2019-07-03 2019-10-18 温州婧爵医疗科技有限公司 Composition comprising amide derivatives and its application in cosmetics

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106962328A (en) * 2016-06-19 2017-07-21 王金明 A kind of preparation method of rare earth loaded antiseptic
CN108578753A (en) * 2018-03-13 2018-09-28 深圳市源兴医药股份有限公司 A kind of disinfectant dressing and preparation method thereof
CN110339079A (en) * 2019-07-03 2019-10-18 温州婧爵医疗科技有限公司 Composition comprising amide derivatives and its application in cosmetics

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