CN112209445B - Preparation method and application of molybdenum trioxide nanodot antibacterial material - Google Patents
Preparation method and application of molybdenum trioxide nanodot antibacterial material Download PDFInfo
- Publication number
- CN112209445B CN112209445B CN202011102429.3A CN202011102429A CN112209445B CN 112209445 B CN112209445 B CN 112209445B CN 202011102429 A CN202011102429 A CN 202011102429A CN 112209445 B CN112209445 B CN 112209445B
- Authority
- CN
- China
- Prior art keywords
- molybdenum trioxide
- nanodots
- molybdenum
- preparation
- nanodot
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 title claims abstract description 154
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 title claims abstract description 24
- 239000002096 quantum dot Substances 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- ZSSVQAGPXAAOPV-UHFFFAOYSA-K molybdenum trichloride Chemical compound Cl[Mo](Cl)Cl ZSSVQAGPXAAOPV-UHFFFAOYSA-K 0.000 claims abstract description 11
- 238000010521 absorption reaction Methods 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 15
- 230000000694 effects Effects 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 12
- 239000006228 supernatant Substances 0.000 claims description 12
- 206010052428 Wound Diseases 0.000 claims description 9
- 208000027418 Wounds and injury Diseases 0.000 claims description 9
- 102000004190 Enzymes Human genes 0.000 claims description 8
- 108090000790 Enzymes Proteins 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 230000003385 bacteriostatic effect Effects 0.000 claims description 5
- 230000007547 defect Effects 0.000 claims description 5
- 241001052560 Thallis Species 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000001931 thermography Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 2
- 229910000476 molybdenum oxide Inorganic materials 0.000 abstract description 14
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 abstract description 14
- 239000002086 nanomaterial Substances 0.000 abstract description 11
- 239000000843 powder Substances 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 239000002243 precursor Substances 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 230000001954 sterilising effect Effects 0.000 abstract description 2
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 2
- 241000894006 Bacteria Species 0.000 description 13
- 238000002474 experimental method Methods 0.000 description 9
- 241000699666 Mus <mouse, genus> Species 0.000 description 8
- 102000003992 Peroxidases Human genes 0.000 description 7
- 239000003814 drug Substances 0.000 description 7
- 238000003384 imaging method Methods 0.000 description 7
- 108040007629 peroxidase activity proteins Proteins 0.000 description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 6
- 229940079593 drug Drugs 0.000 description 6
- 241000699670 Mus sp. Species 0.000 description 5
- 239000003242 anti bacterial agent Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000002609 medium Substances 0.000 description 5
- 239000003642 reactive oxygen metabolite Substances 0.000 description 5
- 230000001580 bacterial effect Effects 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- 238000007626 photothermal therapy Methods 0.000 description 4
- 230000003115 biocidal effect Effects 0.000 description 3
- 238000000338 in vitro Methods 0.000 description 3
- 238000001727 in vivo Methods 0.000 description 3
- 229910052750 molybdenum Inorganic materials 0.000 description 3
- 239000011733 molybdenum Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 239000012221 photothermal agent Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000002560 therapeutic procedure Methods 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- 238000002965 ELISA Methods 0.000 description 2
- 238000004435 EPR spectroscopy Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 241000191967 Staphylococcus aureus Species 0.000 description 2
- 230000002924 anti-infective effect Effects 0.000 description 2
- 208000022362 bacterial infectious disease Diseases 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 210000002216 heart Anatomy 0.000 description 2
- -1 hydroxyl free radical Chemical class 0.000 description 2
- 210000003734 kidney Anatomy 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 210000004072 lung Anatomy 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 2
- 238000002428 photodynamic therapy Methods 0.000 description 2
- 239000003504 photosensitizing agent Substances 0.000 description 2
- 210000000952 spleen Anatomy 0.000 description 2
- 230000007480 spreading Effects 0.000 description 2
- 238000003892 spreading Methods 0.000 description 2
- 108091023020 Aldehyde Oxidase Proteins 0.000 description 1
- 102100036826 Aldehyde oxidase Human genes 0.000 description 1
- 208000035143 Bacterial infection Diseases 0.000 description 1
- 239000006144 Dulbecco’s modified Eagle's medium Substances 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 208000000461 Esophageal Neoplasms Diseases 0.000 description 1
- 241000124008 Mammalia Species 0.000 description 1
- RJQXTJLFIWVMTO-TYNCELHUSA-N Methicillin Chemical compound COC1=CC=CC(OC)=C1C(=O)N[C@@H]1C(=O)N2[C@@H](C(O)=O)C(C)(C)S[C@@H]21 RJQXTJLFIWVMTO-TYNCELHUSA-N 0.000 description 1
- 206010030155 Oesophageal carcinoma Diseases 0.000 description 1
- 108010027912 Sulfite Oxidase Proteins 0.000 description 1
- 102000043440 Sulfite oxidase Human genes 0.000 description 1
- 206010048038 Wound infection Diseases 0.000 description 1
- 102100033220 Xanthine oxidase Human genes 0.000 description 1
- 108010093894 Xanthine oxidase Proteins 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000003178 anti-diabetic effect Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940041514 candida albicans extract Drugs 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 231100000135 cytotoxicity Toxicity 0.000 description 1
- 230000003013 cytotoxicity Effects 0.000 description 1
- 231100000263 cytotoxicity test Toxicity 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000003412 degenerative effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000027734 detection of oxygen Effects 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 230000000378 dietary effect Effects 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 201000004101 esophageal cancer Diseases 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 239000012678 infectious agent Substances 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229960003085 meticillin Drugs 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000007777 multifunctional material Substances 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000002186 photoactivation Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 231100000444 skin lesion Toxicity 0.000 description 1
- 206010040882 skin lesion Diseases 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229940124597 therapeutic agent Drugs 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 239000012137 tryptone Substances 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000012138 yeast extract Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- 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
-
- 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
- A61K41/0057—Photodynamic therapy with a photosensitizer, i.e. agent able to produce reactive oxygen species upon exposure to light or radiation, e.g. UV or visible light; photocleavage of nucleic acids with an agent
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K49/00—Preparations for testing in vivo
- A61K49/001—Preparation for luminescence or biological staining
- A61K49/0013—Luminescence
- A61K49/0017—Fluorescence in vivo
- A61K49/0019—Fluorescence in vivo characterised by the fluorescent group, e.g. oligomeric, polymeric or dendritic molecules
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
- A61P17/02—Drugs for dermatological disorders for treating wounds, ulcers, burns, scars, keloids, or the like
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention belongs to the field of nano-material preparation and performance detection and sterilization application, and relates to a preparation method and application of a molybdenum trioxide nanodot antibacterial material, wherein the molybdenum trioxide nanodots are prepared by a hydrothermal method from bottom to top, so that the molybdenum oxide nano-material is prepared by using molybdenum trichloride powder as a precursor in a one-step method, the method is simple and convenient, and is pollution-free, and the prepared molybdenum trioxide nanodots contain oxygen vacancies and have excellent infrared absorption performance, photo-thermal conversion performance and antibacterial performance; the preparation method is simple, the preparation equipment is easy to obtain, the preparation process is simple, the antibacterial effect is good and harmless to human bodies, the whole process is green and pollution-free, the application environment is friendly, and the market prospect is wide.
Description
The technical field is as follows:
the invention belongs to the field of nano material preparation and performance detection and sterilization application, and relates to a preparation method and application of a molybdenum trioxide nanodot antibacterial material.
Background art:
in recent years, bacterial infectious diseases are spreading worldwide. Currently, one of the biggest tasks is to control the spread of infectious agents. Antibiotics are commonly used antibacterial agents, the abuse of which leads to the emergence of a large number of resistant bacteria, H 2 O 2 Is widely used as an antibacterial agent for bacterial infections, and interestingly, H 2 O 2 Can be converted into hydroxyl free radical by functional nanoparticles with peroxidase property, and has great harm to bacteria, but high concentration of H 2 O 2 Is also harmful to living organisms. In order to overcome the above-mentioned drawbacks, it is urgently required to develop an antibacterial material having high efficiency in a simple and low-cost manner. Inspired by natural enzymes, people catalyze harmful Reactive Oxygen Species (ROS) produced by nanoenzymesTo destroy bacteria, nanoenzymes are generally easier to prepare and stable than the high cost of unstable native enzymes. These characteristics are beneficial to the application of nano enzyme in antibiosis. Now, some inorganic nanomaterials, such as graphene quantum dots, fe, have been reported 3 O 4 Nanoparticles and CeO 2 The nanoparticles can simulate the properties of natural peroxidase, such as H 2 O 2 Converting into hydroxyl free radical to kill bacteria.
Today, many challenges still remain in the development of antibacterial nanoenzymes, and among various anti-infective therapies, photoactivation therapies including photothermal therapy (PTT) have attracted extensive attention due to their non-invasiveness and low side effects. In addition, the antibacterial mechanism of photothermal is different from traditional antibiotic treatment, and photothermal therapy utilizes local light-induced high temperature to cause bacterial degenerative death. Photothermal therapy using Near Infrared (NIR) photothermal agents is almost free of working distance or micro-environment limitations, which is a viable approach. Therefore, NIR light-activated photothermal agents are considered as candidates for anti-infective therapy. At the same time, besides, photodynamic therapy (PDT) is considered as a promising alternative to antibiotic resistant biofilms and bacteria. The bacterium can be substituted by OH, and 1 O 2 ，O 2- and Reactive Oxygen Species (ROS) killing. In general, photosensitizers (PS) generate ROS only in the presence of light and exhibit antimicrobial properties. Thus, photodynamic therapy is controllable compared to other antibacterial agents.
Currently, molybdenum oxide material has attracted much attention worldwide as a new transition metal oxide due to its wide use. Molybdenum oxide has many excellent properties due to its unique crystal structure, and is widely used in reagents for spectroscopic analysis. Molybdenum is an essential trace element in mammals and humans, and is a cofactor for various enzymes such as xanthine oxidase, aldehyde oxidase and sulfite oxidase. Dietary molybdenum deficiency leads to an increased incidence of esophageal cancer. Molybdenum (VI) complexes are effective antidiabetics. Recently, some new functions of nano molybdenum oxide have been gradually explored, especially in the field of biomedical applications. As a multifunctional materialThe molybdenum oxide nano material has high photo-thermal conversion efficiency in a Near Infrared (NIR) region. And then used as a degradable photothermal agent and drug carrier. In addition, due to different valence states and forms of the molybdenum oxide nano material, the molybdenum trioxide nanodots (MoO) 3-x NDs) belong to a class of zero-dimensional nanodots (0D-NDs) with smaller size and abundant surface defects, making them more catalytically active than their bulk form.
Molybdenum oxide nanodots are generally prepared in the existing preparation mode by taking molybdenum disulfide or molybdenum powder as a molybdenum precursor and synthesizing the molybdenum disulfide or molybdenum powder in the presence of hydrogen peroxide or ethanol. The synthesis process has many safety hazards and the removal of strong oxidants complicates the preparation process. Compared with the method, the solvothermal method has the advantages that the preparation process is extremely simple and is most widely applied, the prior top-down solvothermal stripping technology generally needs pre-treatment steps such as ultrasonic crushing of a large molybdenum oxide raw material, the steps are complicated and time-consuming, and the material conversion rate and the yield are relatively low. Therefore, in order to further research the application and development of the molybdenum oxide nano material, a simple, easy and efficient preparation method of the molybdenum oxide nano structure is needed, and if the molybdenum oxide nano material with multiple valence states can be prepared by a one-step method, the preparation and research efficiency of the molybdenum oxide nano material can be greatly improved, but no research report is found at present. Therefore, the invention seeks to design and provide a method for preparing the molybdenum oxide nanodots by a one-step method, which is simple in steps, green and pollution-free.
The invention content is as follows:
the invention aims to overcome the defects in the prior art and provides a preparation method and application of a molybdenum trioxide nanodot antibacterial material.
In order to achieve the purpose, the preparation method of the molybdenum trioxide nanodot antibacterial material comprises the following specific process steps:
(1) Preparing a molybdenum trichloride aqueous solution with the mass concentration of 0.005g/mL-0.006g/mL, fully stirring to uniformly disperse the molybdenum trichloride aqueous solution, and putting the molybdenum trichloride aqueous solution into a reaction kettle;
(2) Putting the reaction kettle into a blast drier, and heating and reacting for 10 hours at 200 ℃;
(3) Taking out the reacted sample, centrifuging at 12000rpm/min for 9-11 minutes, removing the precipitate, collecting the supernatant, centrifuging the supernatant at 12000rpm/min for 9-11 minutes, removing the precipitate, collecting the supernatant again, repeating the steps of centrifuging, removing the precipitate and collecting the supernatant for several times until no precipitate appears in the centrifuged solution, obtaining the colorless dispersed molybdenum trioxide nanodot solution, and completing the preparation of the molybdenum trioxide nanodot antibacterial material.
The molybdenum trioxide nanodots related by the invention have uniform particle size of less than 10nm, average particle size of 3.07 +/-0.45 nm and thickness of 1.43 +/-0.08 nm, and good dispersibility.
The molybdenum trioxide nanodots provided by the invention contain oxygen vacancies, have more surface oxygen defects, have more active sites, and can better utilize the property of the nanoenzyme to inhibit and kill drug-resistant bacteria in wounds.
The molybdenum trioxide nanodots provided by the invention have wide absorption range from visible light to near infrared wavelength of 300-1000nm, and have excellent infrared absorption performance.
The molybdenum trioxide nanodots can well convert light energy into heat energy under near-infrared irradiation, and just reach the optimal temperature of enzyme-like (peroxidase) activity, so that the enzyme activity state is optimal, a proper amount of active oxygen is generated, and the growth of thalli is inhibited; the light-heat conversion efficiency reaches 21.26 percent.
The invention also provides application of the molybdenum trioxide nanodots in a photothermal imaging material, and particularly relates to application of the molybdenum trioxide nanodots as the photothermal imaging material for photo-thermal imaging of a photo-thermal imaging instrument.
The invention also provides application of the molybdenum trioxide nanodots as a bacteriostatic material, in particular application of the molybdenum trioxide nanodots as the bacteriostatic material in treating wounds.
The molybdenum trioxide nanodot-based material is used as a multifunctional material, has peroxidase activity, high photothermal conversion efficiency and good photodynamic property in Near Infrared (NIR), and the photothermal effect after NIR irradiation just reaches the optimal temperature of the enzyme-like property, so that the enzyme-like activity reaches the optimal state. Therefore, the method for inhibiting bacteria by utilizing the near infrared absorption and the enzyme-like property of the molybdenum trioxide nanodots has very important significance and application prospect.
Compared with the prior art, the molybdenum trioxide nanodots have the advantages of high catalytic activity, long-term storage, high tolerance to severe environment, high stability, adjustable catalytic activity and the like; the molybdenum trioxide nanodots prepared by the hydrothermal method realize that the molybdenum oxide nanomaterial is prepared by using molybdenum trichloride powder as a precursor through one-step method, the method is simple and convenient, and is pollution-free, and the prepared molybdenum trioxide nanodots contain oxygen vacancies and have excellent infrared absorption performance, photo-thermal conversion performance and antibacterial performance; the preparation method is simple, the preparation equipment is easy to obtain, the preparation process is simple, the antibacterial effect is good and harmless to human bodies, the whole process is green and pollution-free, the application environment is friendly, and the market prospect is wide.
Description of the drawings:
fig. 1 is a schematic diagram of a bacteriostatic principle of the molybdenum trioxide nanodots.
Fig. 2 is a transmission electron microscope image and a size distribution diagram of the molybdenum trioxide nanodots prepared in example 1, where fig. 2A is the transmission electron microscope image and the high-resolution transmission electron microscope image, fig. 2B is the size distribution diagram, and fig. 2C is an atomic force transmission microscope image.
FIG. 3 is a schematic diagram of the detection of oxygen vacancy (A), near infrared absorption property (B) and peroxidase property (C) of the molybdenum trioxide nanodot of the present invention.
FIG. 4 is a medium diagram of in vitro bacteriostasis experiment of the molybdenum trioxide nanodot solution.
FIG. 5 is a photograph showing the results of in vivo bacteriostatic experiments on the molybdenum trioxide nanodots of example 5 according to the present invention.
FIG. 6 is a comparison graph of the results of the application experiment of the molybdenum trioxide nanodots of example 3 in the aspect of photothermal imaging.
Fig. 7 is a comparative image of a wound section of a mouse treated with molybdenum trioxide nanodots according to example 4 of the present invention.
Fig. 8 is a graph showing the cytotoxicity test results of the molybdenum trioxide nanodots according to example 4 of the present invention.
The specific implementation mode is as follows:
the present invention will be described in detail below with reference to specific embodiments and accompanying drawings.
Example 1:
the preparation method of the molybdenum trioxide nanodot antibacterial material comprises the following specific process steps:
(1) Accurately weighing 0.2 g of molybdenum trichloride powder by using an electronic balance, putting the molybdenum trichloride powder into a 50ml reaction kettle, adding 35 ml of ultrapure water, and fully stirring to uniformly disperse the molybdenum trichloride powder;
(2) Putting the reaction kettle into a blast drier, and heating and reacting for 10 hours at 200 ℃;
(3) And taking out the reacted sample, centrifuging at 12000rpm/min for 10min, removing the precipitate, collecting the supernatant, centrifuging the supernatant at 12000rpm/min for 10min, removing the precipitate, collecting the supernatant, repeating the steps of centrifuging, removing the precipitate and collecting the supernatant for several times until no precipitate appears in the solution after centrifuging, thus obtaining a colorless dispersion liquid of the molybdenum trioxide nanodots and completing the preparation of the molybdenum trioxide nanodot antibacterial material.
The molybdenum trioxide nanodots prepared by the embodiment have uniform particle size of less than 10nm, average particle size of 3.07 +/-0.45 nm and thickness of 1.43 +/-0.08 nm, and good dispersibility.
The prepared molybdenum trioxide nanodots were then subjected to Electron Paramagnetic Resonance (EPR) to further verify oxygen vacancies as it provided evidence for surface defects and electrons trapped in the sample being tested. As shown in fig. 3A, the molybdenum trioxide nanodot sample showed an EPR signal at g =2.001 due to electrons captured by oxygen vacancies, indicating that the molybdenum trioxide nanodots have better oxygen vacancies. Meanwhile, the nanodots have good near infrared absorption performance under near infrared light irradiation, the temperature reached during irradiation is the optimal temperature of the nanoenzyme (peroxidase), and the more oxygen vacancies, the better the enzyme activity, and the peroxidase can exert the best activity (fig. 3C).
Example 2:
this example relates to an experiment of applying molybdenum trioxide nanodots to in vitro bacteriostasis, in which the molybdenum trioxide nanodot solution prepared in example 1 was applied to an in vitro antibacterial experiment, a single colony of non-drug resistant and drug resistant bacteria on a solid LB medium was inoculated into 50mL of sterile liquid LB medium containing tryptone (0.5 g), yeast extract (0.25 g) and NaCl (0.5 g), and then the suspension of the drug resistant bacteria was cultured overnight at 37 ℃ at 180rpm/min on a rotary shaker. The bacteria were then diluted to 10 with sterile PBS 6 CFU/mL, mixing the obtained bacterial solution (100. Mu.L) with 300. Mu.L of a mass concentration of 90. Mu.g.mL -1 50 microliter of H with a molar concentration of 100 micromoles per liter 2 O 2 And 550. Mu.l of PBS buffer at 37 ℃ for 30 minutes, then sucking 50. Mu.l of the solution and spreading it on a solid medium uniformly, incubating the solid medium in an incubator at 37 ℃ for 12 hours, counting bacterial colonies by the CFU method, using PBS as a blank, and incubating the bacteria alone with H 2 O 2 Or molybdenum trioxide nanodots. The measurement results are shown in FIG. 4, and H is added simultaneously under the irradiation of infrared light 2 O 2 And molybdenum trioxide nanodots, the plate has only few bacterial colonies, the antibacterial rates to drug-resistant escherichia coli and staphylococcus aureus are 98.4% and 98%, respectively, and the results show that the molybdenum trioxide nanodots are under near-infrared light and H 2 O 2 Under the existing condition, the antibacterial agent has extremely strong antibacterial performance.
Example 3:
this example is an experiment of applying the molybdenum trioxide nanodots in photothermographic imaging, wherein the molybdenum trioxide nanodots prepared in example 1 are applied in effective photothermographic imaging, and the mass concentration is 300 microliters90μg·mL -1 The molybdenum trioxide nanodot solution is injected to the wound part of a mouse, the experimental result is shown in figure 6, and the imaging temperature of the mouse is 35 ℃ when the near infrared irradiation is not added; 2W/cm at a wavelength of 808nm 2 After the near infrared light is irradiated for 20 minutes, the imaging temperature of the mouse is 55 ℃, which shows that the molybdenum trioxide nanodots can effectively convert light energy into heat energy, and then a photothermal imager can clearly and accurately shoot the wound of the mouse.
This example illustrates that the molybdenum trioxide nanodots have good photo-thermal conversion efficiency, and the photo-thermal conversion efficiency is calculated by the photo-thermal conversion formula to be 21.26%.
Example 4:
this example is an experiment for applying molybdenum trioxide nanodots in biotoxicity testing, the cells for the experiment were mouse L929 cells, the cells were incubated with 7 mixed solutions of 100. Mu.L of molybdenum trioxide nanodot solutions at different concentrations (0. Mu.g/mL, 2.5. Mu.g/mL, 5. Mu.g/mL, 10. Mu.g/mL, 25. Mu.g/mL, 50. Mu.g/mL, 100. Mu.g/mL) and 150. Mu.L of DMEM solution for 24 hours, 10mL of MTT solution containing 5mg/mL was added, and the process was continued to 5 CO 2 2 And incubation for 4 hours at 37 ℃, finally, fully dissolving the crystals by 100 mu L of dimethyl sulfoxide, measuring the absorbance of each well at 490nm of an enzyme-linked immunosorbent assay (ELISA) detector, wherein the measurement result is shown in FIG. 8, the activity of the cells which are not incubated by the molybdenum trioxide nanodot solution is set to be 100%, and the results show that the activity of the cells can be maintained to be more than 99% after the cells are incubated by the molybdenum trioxide nanodot solutions with different concentrations (0 mu g/mL,2.5 mu g/mL,5 mu g/mL,10 mu g/mL,25 mu g/mL,50 mu g/mL and 100 mu g/mL).
In addition, the major organs (liver, heart, lung, spleen and kidney) of the mice were treated with PBS and molybdenum trioxide nanodots at mass concentrations of 100 μ g/mL and 200 μ g/mL, respectively, and as a result, as shown in fig. 7, no significant damage or tissue abnormality was observed in any of the liver, heart, lung, spleen and kidney, demonstrating that the prepared molybdenum trioxide nanodots have good biocompatibility and low cytotoxicity.
Example 5:
this example is a molybdenum trioxide nano-meterApplication of the dots to in vivo bacteriostasis, the molybdenum trioxide nanodot solution prepared in example 1 was applied to in vivo antibacterial experiments, and a mouse wound infection model was established by using male and female mixed mice (six weeks, 180-200g, total 32 SD mice). Circular skin lesions of about 1cm diameter were made on the backs of all mice, which were divided into 8 groups of 4 mice each after infection with MRSA (methicillin-resistant staphylococcus aureus). Each group received different therapeutic agents, PBS, H 2 O 2 Molybdenum trioxide nanodots, H 2 O 2 + molybdenum trioxide nanodots, PBS + NIR, H 2 O 2 + NIR, molybdenum trioxide nanodots + NIR, H 2 O 2 + molybdenum trioxide nanodots + NIR. Photographs of the wounds were collected every other day and the entire course of treatment was designated as 6 days. As can be seen from FIG. 5, H 2 O 2 The minimum wound treated by the molybdenum trioxide nanodots and the NIR group shows that the molybdenum trioxide nanodots have obvious antibacterial performance on various drug-resistant bacteria, so that the wound of the mouse can be quickly healed.
Claims (5)
1. A preparation method of a molybdenum trioxide nanodot antibacterial material is characterized by comprising the following specific process steps:
(1) Preparing a molybdenum trichloride aqueous solution with the mass concentration of 0.005g/mL-0.006g/mL, fully stirring to uniformly disperse the molybdenum trichloride aqueous solution, and putting the molybdenum trichloride aqueous solution into a reaction kettle;
(2) Putting the reaction kettle into a blast drier, and heating and reacting for 10 hours at 200 ℃;
(3) Taking out the reacted sample, centrifuging at 12000rpm/min for 9-11 minutes, removing the precipitate, collecting the supernatant, centrifuging the supernatant at 12000rpm/min for 9-11 minutes, removing the precipitate, collecting the supernatant again, repeating the steps of centrifuging, removing the precipitate and collecting the supernatant for several times until no precipitate appears in the centrifuged solution, obtaining a colorless dispersion liquid of the molybdenum trioxide nanodots, and completing the preparation of the molybdenum trioxide nanodot antibacterial material;
the molybdenum trioxide nanodots are uniform in particle size and smaller than 10nm, the average particle size is 3.07 +/-0.45 nm, the thickness is 1.43 +/-0.08 nm, and the molybdenum trioxide nanodots have good dispersibility.
2. The preparation method of the molybdenum trioxide nanodot antibacterial material as in claim 1, wherein the molybdenum trioxide nanodots contain oxygen vacancies and have more surface oxygen defects, so that the molybdenum trioxide nanodots have more active sites and can better utilize the property of the nanoenzyme to inhibit and kill thalli in wounds.
3. The method for preparing the molybdenum trioxide nanodot bacteriostatic material as claimed in claim 1, wherein the molybdenum trioxide nanodots have wide absorption from visible light to near infrared wavelength of 300-1000nm and excellent infrared absorption property.
4. The use of the molybdenum trioxide nanodots prepared by the preparation method as defined in claim 1 in photothermographic materials, wherein the molybdenum trioxide nanodots are used as photothermographic materials for photo-thermal imaging.
5. The application of the molybdenum trioxide nanodots prepared by the preparation method according to claim 1 as an antibacterial material, wherein the molybdenum trioxide nanodots are used in combination with an enzyme-like enzyme under near-infrared irradiation, so that light energy can be well converted into heat energy, the optimal temperature of the enzyme-like activity can be just reached, the enzyme activity state is optimal, a proper amount of active oxygen is generated, and the growth of thalli is inhibited; the light-heat conversion efficiency reaches 21.26 percent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011102429.3A CN112209445B (en) | 2020-10-15 | 2020-10-15 | Preparation method and application of molybdenum trioxide nanodot antibacterial material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011102429.3A CN112209445B (en) | 2020-10-15 | 2020-10-15 | Preparation method and application of molybdenum trioxide nanodot antibacterial material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112209445A CN112209445A (en) | 2021-01-12 |
| CN112209445B true CN112209445B (en) | 2023-03-24 |
Family
ID=74054235
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011102429.3A Active CN112209445B (en) | 2020-10-15 | 2020-10-15 | Preparation method and application of molybdenum trioxide nanodot antibacterial material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112209445B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2022546316A (en) * | 2019-08-29 | 2022-11-04 | クロー バイオテック ホールディングス， エルエルシー | antipathogen composition |
| CN112915204A (en) * | 2021-02-03 | 2021-06-08 | 青岛大学 | Anti-pseudomonas aeruginosa targeted bactericide and preparation method thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9643842B2 (en) * | 2011-03-14 | 2017-05-09 | Imra America, Inc. | Nanoarchitectured multi-component electrode materials and methods of making the same |
| KR101647001B1 (en) * | 2015-06-12 | 2016-08-10 | 경희대학교 산학협력단 | A method for preparing molybdenum oxide nanoparticles |
| CN110316757B (en) * | 2019-07-24 | 2021-08-24 | 青岛大学 | Preparation method and application of vanadium oxide |
-
2020
- 2020-10-15 CN CN202011102429.3A patent/CN112209445B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN112209445A (en) | 2021-01-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Yu et al. | Ag-Conjugated graphene quantum dots with blue light-enhanced singlet oxygen generation for ternary-mode highly-efficient antimicrobial therapy | |
| CN105948124B (en) | Nanometer molybdenum sulfide anti-biotic material and its synthetic method, application | |
| CN112209445B (en) | Preparation method and application of molybdenum trioxide nanodot antibacterial material | |
| CN113016823B (en) | Preparation method of photo-thermal antibacterial near-infrared bimetallic nanoparticles | |
| CN110496219B (en) | Synthesis method of novel ferrihydrite nano photosensitizer and application of novel ferrihydrite nano photosensitizer in anticancer and antibacterial | |
| CN111017996A (en) | Synthesis of MoO with double simulated enzyme activity3-XMethod for producing antimicrobial material | |
| CN113234436B (en) | Near-infrared carbon quantum dot/silicon dioxide composite material and preparation method and application thereof | |
| CN110101860B (en) | Bismuth-doped metal sulfide nanoflower and preparation method thereof | |
| Ali et al. | Graphdiyne–hemin-mediated catalytic system for wound disinfection and accelerated wound healing | |
| CN114191562B (en) | Preparation method and application of double-enzyme-activity antibacterial material | |
| Li et al. | Sugar-disguised bullets for combating multidrug-resistant bacteria infections based on an oxygen vacancy-engineered glucose-functionalized MoO3-x photo-coordinated bienzyme | |
| CN111097038A (en) | Vancomycin-modified molybdenum disulfide/gold nanoneedle composite material and preparation method thereof | |
| Shi et al. | Glutathione-depletion reinforced enzyme catalytic activity for photothermal assisted bacterial killing by hollow mesoporous CuO | |
| CN112274639B (en) | Fe2C @ Fe3O4 heterogeneous nano-particles, preparation method and application | |
| CN113042076B (en) | Catalase activity-simulated photocatalytic nanoenzyme, and preparation method and application thereof | |
| CN116395747A (en) | Manganese tetraoxide-silver sulfide Janus structure nanocomposite and preparation method thereof | |
| CN113387395B (en) | Efficient magnetic response catalytic medical nano-particle and preparation method and application thereof | |
| CN115475244B (en) | Metal organic framework nano-composite and preparation method and application thereof | |
| CN108904472A (en) | The modified photosensitizer nanocomposite of graphene and its application | |
| CN115463151B (en) | Nano-enzyme, preparation method and application thereof, and bacteriostat | |
| CN114711251B (en) | Titanium carbide-manganese sulfide composite antibacterial material, preparation method thereof and antibacterial method | |
| CN113546171A (en) | Phototherapy nano antibacterial material and preparation method and application thereof | |
| Anjum et al. | Synthesis of Gold Nanoparticles and Their Reduced Graphene Oxide Nanocomposites Through a Simplified Approach and Assessment of Their Bactericidal Potential | |
| CN114532333B (en) | Method for constructing attapulgite-zinc oxide nano composite antibacterial material by using liquorice extract | |
| CN113666641B (en) | Multifunctional bioactive glass ceramic nano material and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |