CN117547607A - BaTiO 3 PDA-Cu nano material and preparation method thereof - Google Patents
BaTiO 3 PDA-Cu nano material and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims description 70
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 57
- 239000010949 copper Substances 0.000 claims description 50
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 44
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- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 23
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- 229910002113 barium titanate Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
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- 229960001412 pentobarbital Drugs 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K41/00—Medicinal preparations obtained by treating materials with wave energy or particle radiation ; Therapies using these preparations
- A61K41/0052—Thermotherapy; Hyperthermia; Magnetic induction; Induction heating therapy
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/34—Copper; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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Abstract
The invention provides BaTiO 3 PDA-Cu nano material and preparation method thereof, wherein PDA is wrapped on BaTiO 3 Can effectively reduce BaTiO on the surface of 3 At the same time, the simple substance Cu is inlaid on the surface of the shell-core structure, so that the prepared BaTiO 3 PDA-Cu nanomaterials possess the properties of three materials simultaneously.
Description
Technical Field
The invention relates to a nano material, in particular to a BaTiO 3 PDA-Cu nanomaterial and method of making the same.
Background
ROS play an important role as signal molecules in redox-dependent signaling pathways, and ROS are usually present in low concentrations and have important signaling and regulatory functions, and the main sources of intracellular ROS production include mitochondrial respiratory chain, NADPH oxidase, and endoplasmic reticulum, etc. There is growing evidence that ROS-induced oxidative stress is an important factor in the development of inflammation, ROS acting through direct injury and exacerbation of the inflammatory response, and also through direct stimulation of pro-inflammatory cytokine production, or through activation of the inflammatory body causing an inflammatory cascade amplification effect.
Barium titanate (BaTiO) 3 ) The ceramic material has ferroelectric property, good piezoelectric property and higher dielectric constant, can convert mechanical energy into electric energy, and is used for manufacturing high-performance dielectric materials in the fields of electronics and biological materials. Dopamine (DA) is a bioactive molecule, is often used as a multifunctional surface modifier, can be used for preparing a dopamine coating (PDA), has strong adhesion capability, and can form uniform, compact and controllable films on the surfaces of various materials. The dopamine coating can enhance the adhesiveness of the material, improve the surface performance, have good biocompatibility, and can reduce inflammatory reaction and cytotoxicity when in contact with organisms; the dopamine coating also has photo-thermal properties, since aromatic rings and phenolic groups in the molecular structure of dopamine can absorb light energy and convert it into heat energy. The PDA can absorb light rays in the wavelength ranges of visible light, near infrared light (NIR) and the like to generate a photo-thermal effect, the absorption capacity enables the dopamine coating to have potential value in photo-thermal treatment, photo-thermal conversion and other applications, the thermal conversion efficiency of the PDA in the photo-thermal conversion process is high, and the PDA can effectively convert light energy into heat energy.
Copper Cu is a transition metal element essential for human health, copper not only participates in activation of important enzymes in vivo energy metabolism processes, such as cytochrome C oxidase and superoxide dismutase, which participate in cellular respiratory chain and oxidative stress reaction to help produce energy, but also copper ions play a role of catalyst in various enzymes, participate in a number of important biochemical reactions, such as copper zinc superoxide dismutase, copper iron blue protein, dopamine beta monooxygenase, and the like. Bacterial Infection Microenvironment (IME) was demonstrated to have a low pH (4.5-6.5) environment and high levels of H202, unlike normal tissue. Thus, fenton-like reactions triggered by Cu (II)/Cu (I) redox cycles can increase the yield of hydroxyl radicals at the site of infection and achieve powerful antimicrobial functions. The research shows that copper is an important factor for promoting wound healing, can not only be used for strong antibacterial action, but also promote the expression of growth factors such as keratin, collagen, angiogenesis, vascular endothelial growth and the like.
The search for materials capable of absorbing Near Infrared (NIR) light to generate Reactive Oxygen Species (ROS) has significant research and application value, and near infrared induced release photothermal therapy Near Infrared (NIR) light-induced photothermal therapy (PTT) has received extensive attention in anti-infective therapy because of its low aggressiveness and low side effects in order to avoid excessive release of metal ions from nanomaterials to normal tissues. The metal nanomaterial with piezoelectric properties has wide application prospects in various fields, such as energy collection and conversion, sensors, energy storage devices, biomedical fields and the like. In recent years, advances in material synthesis and engineering have provided new opportunities for developing piezoelectric materials with excellent biocompatibility and piezoelectric properties. BaTiO 3 Has good piezoelectric properties, but in the previous study we found that BaTiO 3 Has certain cytotoxicity, small particle size and easy agglomeration, and limits the application of the composition in ultrasonic-mediated disease treatment.
Disclosure of Invention
The invention aims to provide BaTiO 3 Preparation method of PDA-Cu nano material, wrapping PDA in BaTiO 3 Can effectively reduce BaTiO on the surface of 3 At the same time, the simple substance Cu is inlaid on the surface of the shell-core structure, so that the prepared BaTiO 3 PDA-Cu nanomaterials possess the properties of three materials simultaneously.
In order to solve the technical problems, the technical scheme of the invention is as follows:
BaTiO 3 -a method for preparing PDA-Cu nanomaterial comprising the steps of:
s1, dissolving butyl titanate in isopropanol, dropwise adding glacial acetic acid at room temperature, and stirring for 0.5-2h to obtain a transparent titanic acyl compound solution;
s2, dissolving barium acetate in an acetic acid solution to obtain a barium acetate solution, dropwise adding the barium acetate solution into the titanic acyl compound solution obtained in the step S1, stirring for 0.5-2h, and then regulating the pH value to 3-5 by glacial acetic acid to obtain a gel;
s3, aging the gel obtained in the step S2 for 24 hours at room temperature, mashing, drying for 12 hours at 110-130 ℃ in a vacuum drying oven, taking out, grinding into gel powder, calcining the gel powder for 12-24 hours at 700-900 ℃ in a resistance furnace, taking out, cooling to room temperature, and grinding to obtain BaTiO 3 A powder;
s4, the BaTiO obtained in the step S3 is processed 3 Adding the powder into ultrapure water, and performing ultrasonic vibration for 3-5min to obtain BaTiO 3 Adding ammonia water and absolute ethanol into the suspension to obtain a suspension 3 Stirring the suspension for 25-35min to obtain a first mixed solution;
s5, dissolving dopamine hydrochloride in ultrapure water to obtain a dopamine solution, dripping the dopamine solution into the first mixed solution obtained in the step S4, and stirring for 20-24 hours to obtain a second mixed solution;
s6, dissolving copper chloride in ultrapure water to obtain a copper chloride solution, dropwise adding the copper chloride solution into the mixed solution II obtained in the step S5, and stirring for 8-12h to obtain a mixed solution III;
s7, dissolving ascorbic acid in ultrapure water to obtain an ascorbic acid solution, dropwise adding the ascorbic acid solution into the mixed solution III obtained in the step S6, stirring for 8-12h, centrifuging for 10min, discarding supernatant, resuspending the precipitate, centrifuging for 3 times by the same method to obtain a precipitate, and vacuum drying the precipitate at 60 ℃ to constant weight to obtain BaTiO 3 PDA-Cu nanomaterial.
Further, in the step S1, the molar ratio of the butyl titanate to the isopropanol to the glacial acetic acid is 1:6:3.
Further, in the step S2, the mass concentration of the acetic acid solution is 40%, the ratio of the barium acetate to the acetic acid solution is 3g to 10mL, and the ratio of the barium acetate to the butyl titanate is 3g to 0.1mol.
Further, in the step S4 of the present invention, the mass concentration of the ammonia water is 20%, and the BaTiO powder 3 The ratio of the ultrapure water, the ammonia water and the absolute ethyl alcohol is 40 mg:18 mL:150 mu L:7-9 mL.
Further, in the step S5 of the invention, the proportion of the dopamine hydrochloride to the ultrapure water is 100 mg/1 mL, and the proportion of the dopamine hydrochloride to the BaTiO is 100 mg/1 mL 3 The mass ratio of the powder is 25:2.
Further, in the step S6, the ratio of the copper chloride to the ultrapure water is 10mg to 1mL, and the mass ratio of the copper chloride to the dopamine hydrochloride is 1 to 10.
Further, in the step S7, the ratio of the ascorbic acid to the ultrapure water is 10 mg: lmL, and the mass ratio of the ascorbic acid to the dopamine hydrochloride is 1:10.
Further, in the step S7 of the invention, the speed of each centrifugation is 4000r/min.
Another technical problem to be solved by the invention is to provide BaTiO prepared by the preparation method 3 PDA-Cu nanomaterial.
Compared with the prior art, the invention has the following beneficial effects:
1) BaTiO according to the invention 3 PDA-Cu nano material is made of BaTiO 3 3 and dopamine hydrochloride, and copper chloride (shown in figure 1), wherein dopamine is adhered to and wrapped in BaTiO under alkaline condition 3 Can effectively reduce BaTiO on the surface of 3 At the same time, the simple substance Cu is inlaid on the surface of the shell-core structure to prepare the BaTiO 3 PDA-Cu nano material is provided with BaTiO at the same time 3 PDA, nano Cu simple substance.
2) The two steps of reaction of the invention have longer time, and the reaction is more controllable and safer.
3) The invention utilizes BaTiO with strong piezoelectric property 3 And Gao Guangre, and combined with metal Cu to obtain the composite nano material with strong and broad-spectrum antibacterial property.
4) BaTiO according to the invention 3 PDA-Cu nanomaterials on the one hand allow phototherapy, promote blood circulation and eliminate diseases by increasing local temperaturePiezoelectric therapy, on the other hand, can be implemented to stimulate cell growth and repair by creating potential changes.
5) BaTiO according to the invention 3 The PDA-Cu nanomaterial enables non-invasive treatment by photothermal irradiation and slight ultrasound pressure application, which reduces the risk of secondary injury and infection of the wound surface and improves the safety and comfort of treatment compared to traditional debridement and antibiotic treatment methods.
6) BaTiO according to the invention 3 The PDA-Cu nanometer material can also carry out customized treatment according to specific conditions, and personalized treatment is carried out according to different infectious wound conditions by adjusting parameters such as power and time of laser irradiation, applied pressure force, duration and the like, so that the pertinence and the effect of treatment are improved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this application, illustrate and do not limit the invention, and together with the description serve to explain the principle of the invention:
FIG. 1 is a schematic diagram of the synthesis of the present invention;
FIG. 2 is a graph showing cytotoxicity test results of example 1 and comparative example of the present invention;
FIG. 3 is a graph showing the results of in vitro bacteriostasis experiments in example 1 of the present invention;
FIG. 4 is a schematic diagram of a skin model according to example 1 of the present invention;
fig. 5 is a skin model simulation of example 1 of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples, wherein the exemplary embodiments and descriptions of the present invention are provided for the purpose of illustration and are not intended to be limiting.
Example 1
The BaTiO is prepared according to the following steps 3 PDA-Cu nanomaterial:
s1, dissolving butyl titanate in isopropanol, dropwise adding glacial acetic acid at room temperature, and stirring for 0.5h to obtain a transparent titanic acyl compound solution, wherein the molar ratio of the butyl titanate to the isopropanol to the glacial acetic acid is 1:6:3;
s2, dissolving barium acetate in acetic acid solution with the mass concentration of 40% according to the proportion of 3g to 10mL to obtain barium acetate solution, dropwise adding the barium acetate solution into the titanic acyl compound solution obtained in the step S1, wherein the proportion of barium acetate to butyl titanate is 3g to 0.1mol, stirring for 0.5h, and then regulating the pH value to 3 by glacial acetic acid to obtain gel;
s3, aging the gel obtained in the step S2 for 24 hours at room temperature, mashing, drying for 12 hours at 120 ℃ in a vacuum drying oven, taking out, grinding into gel powder, calcining the gel powder in a resistance furnace for 12 hours at 800 ℃, taking out, cooling to room temperature, and grinding to obtain BaTiO 3 A powder;
s4, the BaTiO obtained in the step S3 is processed 3 Adding the powder into ultrapure water, and performing ultrasonic vibration for 5min to obtain BaTiO 3 Adding ammonia water and absolute ethanol with mass concentration of 20% into the suspension, stirring for 30min to obtain mixed solution I, baTiO 3 The ratio of the powder to the ultrapure water to the ammonia water to the absolute ethanol is 40mg to 18mL to 150 mu L to 8mL;
s5, dissolving dopamine hydrochloride into ultrapure water according to the proportion of 100mg to 1mL to obtain a dopamine solution, dripping the dopamine solution into the mixed solution I obtained in the step S4, and adding dopamine hydrochloride and BaTiO into the mixed solution I 3 The mass ratio of the powder is 25:2, and stirring is carried out for 24 hours to obtain a mixed solution II;
s6, dissolving copper chloride into ultrapure water according to the proportion of 10mg to 1mL to obtain a copper chloride solution, dropwise adding the copper chloride solution into the mixed solution II obtained in the step S5, wherein the mass ratio of the copper chloride to the dopamine hydrochloride is 1 to 10, and stirring for 8 hours to obtain a mixed solution III;
s7, dissolving ascorbic acid in ultrapure water according to the proportion of 10mg to 1mL to obtain an ascorbic acid solution, dropwise adding the ascorbic acid solution into the mixed solution III obtained in the step S6, wherein the mass ratio of the ascorbic acid to the dopamine hydrochloride is 1 to 10, centrifuging for 10min at the speed of 4000r/min after stirring for 12h, discarding the supernatant, re-suspending the precipitate, centrifuging for 3 times by the same method to obtain a precipitate, and vacuum drying the precipitate at 60 ℃ to constant weight to obtain BaTiO 3 PDA-Cu nanomaterial.
Example 2
The BaTiO is prepared according to the following steps 3 PDA-Cu nanomaterial:
s1, dissolving butyl titanate in isopropanol, dropwise adding glacial acetic acid at room temperature, and stirring for 1h to obtain a transparent titanic acyl compound solution, wherein the molar ratio of the butyl titanate to the isopropanol to the glacial acetic acid is 1:6:3;
s2, dissolving barium acetate in acetic acid solution with the mass concentration of 40% according to the proportion of 3g to 10mL to obtain barium acetate solution, dropwise adding the barium acetate solution into the titanic acyl compound solution obtained in the step S1, wherein the proportion of barium acetate to butyl titanate is 3g to 0.1mol, stirring for 1h, and then regulating the pH value to 4 by glacial acetic acid to obtain gel;
s3, aging the gel obtained in the step S2 for 24 hours at room temperature, mashing, drying for 12 hours at 110 ℃ in a vacuum drying oven, taking out, grinding into gel powder, calcining the gel powder in a resistance furnace for 18 hours at 700 ℃, taking out, cooling to room temperature, and grinding to obtain BaTiO 3 A powder;
s4, the BaTiO obtained in the step S3 is processed 3 Adding the powder into ultrapure water, and performing ultrasonic vibration for 4min to obtain BaTiO 3 Adding ammonia water and absolute ethanol with mass concentration of 20% into the suspension, stirring for 25min to obtain mixed solution I, baTiO 3 The ratio of the powder to the ultrapure water to the ammonia water to the absolute ethanol is 40mg to 18mL to 150 mu L to 7mL;
s5, dissolving dopamine hydrochloride into ultrapure water according to the proportion of 100mg to 1mL to obtain a dopamine solution, dripping the dopamine solution into the mixed solution I obtained in the step S4, and adding dopamine hydrochloride and BaTiO into the mixed solution I 3 The mass ratio of the powder is 25:2, and stirring is carried out for 21h to obtain a mixed solution II;
s6, dissolving copper chloride into ultrapure water according to the proportion of 10mg to 1mL to obtain a copper chloride solution, dropwise adding the copper chloride solution into the mixed solution II obtained in the step S5, wherein the mass ratio of the copper chloride to the dopamine hydrochloride is 1 to 10, and stirring for 10 hours to obtain a mixed solution III;
s7, dissolving ascorbic acid in ultrapure water according to the proportion of 10mg to 1mL to obtain an ascorbic acid solution, dropwise adding the ascorbic acid solution into the mixed solution III obtained in the step S6, stirring, wherein the mass ratio of the ascorbic acid to the dopamine hydrochloride is 1 to 10Centrifuging at 4000r/min for 10 hr, removing supernatant, re-suspending the precipitate, centrifuging for 3 times to obtain precipitate, and vacuum drying at 60deg.C to constant weight to obtain BaTiO 3 PDA-Cu nanomaterial.
Example 3
The BaTiO is prepared according to the following steps 3 PDA-Cu nanomaterial:
s1, dissolving butyl titanate in isopropanol, dropwise adding glacial acetic acid at room temperature, and stirring for 2 hours to obtain a transparent titanic acyl compound solution, wherein the molar ratio of the butyl titanate to the isopropanol to the glacial acetic acid is 1:6:3;
s2, dissolving barium acetate in acetic acid solution with the mass concentration of 40% according to the proportion of 3g to 10mL to obtain barium acetate solution, dropwise adding the barium acetate solution into the titanic acyl compound solution obtained in the step S1, wherein the proportion of barium acetate to butyl titanate is 3g to 0.1mol, stirring for 2h, and then regulating the pH value to 5 by glacial acetic acid to obtain gel;
s3, aging the gel obtained in the step S2 for 24 hours at room temperature, mashing, drying for 12 hours at 130 ℃ in a vacuum drying oven, taking out, grinding into gel powder, calcining the gel powder for 24 hours at 900 ℃ in a resistance furnace, taking out, cooling to room temperature, and grinding to obtain BaTiO 3 A powder;
s4, the BaTiO obtained in the step S3 is processed 3 Adding the powder into ultrapure water, and performing ultrasonic vibration for 3min to obtain BaTiO 3 Adding ammonia water and absolute ethanol with mass concentration of 20% into the suspension, stirring for 35min to obtain mixed solution I, baTiO 3 The ratio of the powder to the ultrapure water to the ammonia water to the absolute ethanol is 40mg to 18mL to 150 mu L to 9mL;
s5, dissolving dopamine hydrochloride into ultrapure water according to the proportion of 100mg to 1mL to obtain a dopamine solution, dripping the dopamine solution into the mixed solution I obtained in the step S4, and adding dopamine hydrochloride and BaTiO into the mixed solution I 3 The mass ratio of the powder is 25:2, and stirring is carried out for 20 hours to obtain a mixed solution II;
s6, dissolving copper chloride into ultrapure water according to the proportion of 10mg to 1mL to obtain a copper chloride solution, dropwise adding the copper chloride solution into the mixed solution II obtained in the step S5, wherein the mass ratio of the copper chloride to the dopamine hydrochloride is 1 to 10, and stirring for 12 hours to obtain a mixed solution III;
s7, dissolving ascorbic acid in ultrapure water according to the proportion of 10mg to 1mL to obtain an ascorbic acid solution, dropwise adding the ascorbic acid solution into the mixed solution III obtained in the step S6, wherein the mass ratio of the ascorbic acid to the dopamine hydrochloride is 1 to 10, centrifuging for 10min at the speed of 4000r/min after stirring for 8h, discarding the supernatant, re-suspending the precipitate, centrifuging for 3 times by the same method to obtain a precipitate, and vacuum drying the precipitate at 60 ℃ to constant weight to obtain BaTiO 3 PDA-Cu nanomaterial.
Comparative example: the difference from example 1 is that the process does not include step S4-7, and a Cu-free BaTiO film not covered with PDA is produced 3 And (3) nanoparticles.
Experimental example one: cytotoxicity test
The test method is CCK 8 method: the cells were inoculated into 96-well plates at 5 thousand L929 cells per well, and after 24 hours the cells were attached, and the medium was changed to BaTiO prepared in example 1 having different concentrations (12.5. Mu.g/mL, 25. Mu.g/mL, 50. Mu.g/mL, 75. Mu.g/mL, 100. Mu.g/mL, 125. Mu.g/mL, 200. Mu.g/mL) 3 PDA-Cu nanomaterial and BaTiO prepared by comparative example 3 Culture medium for nanoparticles was continued for 24 hours. After 24 hours the medium was changed to normal medium and most of the material was washed out with PBS at the time of the change. Adding CCK 8 reagent according to the instruction steps, incubating for 1 hour at 37 ℃, absorbing supernatant to a 96-well plate after incubation, measuring the absorbance at 450nm by using an enzyme-labeled instrument, avoiding violently shaking the well plate in the whole operation process, preventing the residual materials from being sucked out and affecting the measurement of absorbance, wherein the test result is shown in figure 2, and the BaTiO prepared in the embodiment 1 of the invention is shown in figure 2 3 The cytotoxicity of the PDA-Cu nanomaterial is lower than that of BaTiO prepared in the comparative example 3 And (3) nanoparticles.
Experimental example two: in vitro bacteriostasis experiment
Dispersing Escherichia coli and Staphylococcus aureus in sterilized physiological saline (1×10) 6 CFU/mL), 100. Mu.L of the bacterial liquid was uniformly spread on a solid LB medium by a spreading method, the medium was equally divided into four regions, and BaTiO prepared in example 1 was added 3 -PDA-Cu nanomaterial solution impregnated drugSensitive paper sheet and BaTiO prepared in comparative example 3 One drug sensitive paper sheet soaked by nanoparticle solution, and treating BaTiO under photo-thermal-ultrasonic condition 3 -PDA-Cu solution impregnated and penicillin impregnated sheets of drug sensitive paper, one each. Two dishes were placed in an incubator at 37℃for 12 hours, and colonies of Escherichia coli and Staphylococcus aureus were observed and photographed, as shown in FIG. 3, and as can be seen from FIG. 3, baTiO was treated under photothermal-ultrasonic conditions 3 The PDA-Cu solution infiltration group and the penicillin infiltration group can obviously inhibit the bacterial growth, and have similar effects and are simple with BaTiO 3 The PDA-Cu solution infiltration group also has weaker inhibition effect, while the drug sensitive paper sheet infiltrated by the comparative example has no inhibition effect on bacterial growth, which shows that the BaTiO prepared by the invention 3 The PDA-Cu nano material as an antibacterial agent shows the antibacterial activity of broad-spectrum antibiotics like penicillin and the like, and can avoid the problem of drug resistance of the antibiotics.
Experimental example three:
6 SD rats 180-220g were randomly and equally divided into 3 groups. The anesthetized rats were intraperitoneally injected with about 0.3mL of 2.5% sodium pentobarbital, the back hair of the rats was shaved off with an electric razor, and the back hair was thoroughly removed with a depilatory cream. Skin defect of about 2cm in diameter was peeled off from the back of rat with a scalpel, and a wound containing Staphylococcus aureus (1X 10) was coated with gauze at the defect site 6 CFU/mL), escherichia coli (1X 10) 6 CFU/mL) and the wound infection model was completed.
After wound dressing, wounds were covered on 3 groups of rats: (1) physiological saline; (2) BaTiO prepared in example 1 3 -PDA-Cu nanomaterial solution; (3) BaTiO prepared in example 1 3 PDA-Cu nanomaterial solution and is subjected to photothermal and ultrasound treatment. Rats were kept in SPF-class laboratories at 20-25℃ under 12 hours of incandescent light and 12 hours of darkness each day, the rats were allowed to freely move in cages, eat and drink water, and wound healing was observed for each group of rats after 7 days.
As can be seen from FIG. 4, the normal saline-treated wound did not heal significantly, the wound had purulent exudates, hemorrhagic fluids oozed, and the woundThe mouth area was not significantly reduced and malodorous smell was emitted. BaTiO prepared in example 1 alone 3 The wound covered by the PDA-Cu nanomaterial solution was contracted and the wound surface was slightly scabbed. BaTiO prepared from example 1 3 PDA-Cu nanomaterial solution covered, photo-thermo-ultrasonic treatment group wound has no purulent liquid, wound edge has red swelling, but no bloody exudate and no malodor.
As can be seen from FIG. 4, which is a simulation diagram of wound healing model, baTiO prepared in example 1 3 The wound area covered by the PDA-Cu nano material solution is reduced, and meanwhile, the BaTiO for photo-thermal ultrasonic treatment is added 3 The wound area covered by the PDA-Cu nano material solution is more obviously reduced, which shows that the BaTiO prepared by the invention 3 The PDA-Cu nano material has good photo-thermal and piezoelectric properties, and can exert excellent antibacterial property and wound healing promoting property.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (9)
1. BaTiO 3 The preparation method of the PDA-Cu nanometer material is characterized in that: the method comprises the following steps:
s1, dissolving butyl titanate in isopropanol, dropwise adding glacial acetic acid at room temperature, and stirring for 0.5-2h to obtain a transparent titanic acyl compound solution;
s2, dissolving barium acetate in an acetic acid solution to obtain a barium acetate solution, dropwise adding the barium acetate solution into the titanic acyl compound solution obtained in the step S1, stirring for 0.5-2h, and then regulating the pH value to 3-5 by glacial acetic acid to obtain a gel;
s3, aging the gel obtained in the step S2 for 24 hours at room temperature, mashing, drying for 12 hours at 110-130 ℃ in a vacuum drying oven, taking out, grinding into gel powder, and obtaining the gel powderCalcining in a resistance furnace at 700-900 deg.C for 12-24 hr, taking out, cooling to room temperature, grinding to obtain BaTiO 3 A powder;
s4, the BaTiO obtained in the step S3 is processed 3 Adding the powder into ultrapure water, and performing ultrasonic vibration for 3-5min to obtain BaTiO 3 Adding ammonia water and absolute ethanol into the suspension to obtain a suspension 3 Stirring the suspension for 25-35min to obtain a first mixed solution;
s5, dissolving dopamine hydrochloride in ultrapure water to obtain a dopamine solution, dripping the dopamine solution into the first mixed solution obtained in the step S4, and stirring for 20-24 hours to obtain a second mixed solution;
s6, dissolving copper chloride in ultrapure water to obtain a copper chloride solution, dropwise adding the copper chloride solution into the mixed solution II obtained in the step S5, and stirring for 8-12h to obtain a mixed solution III;
s7, dissolving ascorbic acid in ultrapure water to obtain an ascorbic acid solution, dropwise adding the ascorbic acid solution into the mixed solution III obtained in the step S6, stirring for 8-12h, centrifuging for 10min, discarding supernatant, resuspending the precipitate, centrifuging for 3 times by the same method to obtain a precipitate, and vacuum drying the precipitate at 60 ℃ to constant weight to obtain BaTiO 3 PDA-Cu nanomaterial.
2. A BaTiO according to claim 1 3 The preparation method of the PDA-Cu nanometer material is characterized in that: in the step S1, the molar ratio of the butyl titanate to the isopropanol to the glacial acetic acid is 1:6:3.
3. A BaTiO according to claim 1 3 The preparation method of the PDA-Cu nanometer material is characterized in that: in the step S2, the mass concentration of the acetic acid solution is 40%, the ratio of the barium acetate to the acetic acid solution is 3g to 10mL, and the ratio of the barium acetate to the butyl titanate is 3g to 0.1mol.
4. A BaTiO according to claim 1 3 The preparation method of the PDA-Cu nanometer material is characterized in that: in the step S4, the mass concentration of the ammonia water is 20%, and the mass concentration of BaTiO is 3 The ratio of the powder, the ultrapure water, the ammonia water and the absolute ethanol is 40mg∶18mL∶150μL∶(7-9)mL。
5. A BaTiO according to claim 1 3 The preparation method of the PDA-Cu nanometer material is characterized in that: in the step S5, the proportion of the dopamine hydrochloride to the ultrapure water is 100mg to 1mL, and the proportion of the dopamine hydrochloride to the BaTiO is 100mg to 1mL 3 The mass ratio of the powder is 25:2.
6. A BaTiO according to claim 1 3 The preparation method of the PDA-Cu nanometer material is characterized in that: in the step S6, the ratio of the copper chloride to the ultrapure water is 10mg to 1mL, and the mass ratio of the copper chloride to the dopamine hydrochloride is 1 to 10.
7. A BaTiO according to claim 1 3 The preparation method of the PDA-Cu nanometer material is characterized in that: in the step S7, the ratio of the ascorbic acid to the ultrapure water is 10mg to 1mL, and the mass ratio of the ascorbic acid to the dopamine hydrochloride is 1 to 10.
8. A BaTiO according to claim 1 3 The preparation method of the PDA-Cu nanometer material is characterized in that: in the step S7, the speed of each centrifugation is 4000r/min.
9. BaTiO prepared by the preparation method according to claims 1 to 8 3 PDA-Cu nanomaterial.
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