CN115364213A - Preparation method and application of ferric oxide-molybdenum disulfide-sodium dodecyl sulfate composite nano material - Google Patents
Preparation method and application of ferric oxide-molybdenum disulfide-sodium dodecyl sulfate composite nano material Download PDFInfo
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- CN115364213A CN115364213A CN202211006173.5A CN202211006173A CN115364213A CN 115364213 A CN115364213 A CN 115364213A CN 202211006173 A CN202211006173 A CN 202211006173A CN 115364213 A CN115364213 A CN 115364213A
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- ferric oxide
- molybdenum disulfide
- nano material
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- lauryl sodium
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- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 56
- 239000011733 molybdenum Substances 0.000 title claims abstract description 56
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 56
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 38
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 230000006698 induction Effects 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 14
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims abstract description 10
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000203 mixture Substances 0.000 claims abstract description 10
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 6
- 239000005708 Sodium hypochlorite Substances 0.000 claims abstract description 5
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 claims abstract description 5
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 5
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 4
- 241000894006 Bacteria Species 0.000 claims description 29
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 22
- 238000012360 testing method Methods 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 17
- 108090000623 proteins and genes Proteins 0.000 claims description 16
- 230000000694 effects Effects 0.000 claims description 15
- 239000011521 glass Substances 0.000 claims description 15
- 239000003814 drug Substances 0.000 claims description 14
- 229940079593 drug Drugs 0.000 claims description 14
- 238000012546 transfer Methods 0.000 claims description 14
- 230000005540 biological transmission Effects 0.000 claims description 12
- 239000001963 growth medium Substances 0.000 claims description 11
- 230000005764 inhibitory process Effects 0.000 claims description 11
- 229910052742 iron Inorganic materials 0.000 claims description 11
- 230000002401 inhibitory effect Effects 0.000 claims description 10
- 239000013612 plasmid Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 230000021615 conjugation Effects 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- 241000589517 Pseudomonas aeruginosa Species 0.000 claims description 6
- 239000003242 anti bacterial agent Substances 0.000 claims description 6
- 230000001580 bacterial effect Effects 0.000 claims description 6
- AIUDWMLXCFRVDR-UHFFFAOYSA-N dimethyl 2-(3-ethyl-3-methylpentyl)propanedioate Chemical compound CCC(C)(CC)CCC(C(=O)OC)C(=O)OC AIUDWMLXCFRVDR-UHFFFAOYSA-N 0.000 claims description 6
- 239000000725 suspension Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 241000588724 Escherichia coli Species 0.000 claims description 5
- 241000191967 Staphylococcus aureus Species 0.000 claims description 5
- 229940088710 antibiotic agent Drugs 0.000 claims description 5
- 238000012258 culturing Methods 0.000 claims description 5
- -1 iron trioxide-molybdenum disulfide-sodium dodecyl sulfate Chemical compound 0.000 claims description 5
- 238000009630 liquid culture Methods 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- 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 claims description 4
- 241001052560 Thallis Species 0.000 claims description 4
- 230000003385 bacteriostatic effect Effects 0.000 claims description 4
- 238000002474 experimental method Methods 0.000 claims description 4
- 239000002609 medium Substances 0.000 claims description 4
- 229960003085 meticillin Drugs 0.000 claims description 4
- RWVGQQGBQSJDQV-UHFFFAOYSA-M sodium;3-[[4-[(e)-[4-(4-ethoxyanilino)phenyl]-[4-[ethyl-[(3-sulfonatophenyl)methyl]azaniumylidene]-2-methylcyclohexa-2,5-dien-1-ylidene]methyl]-n-ethyl-3-methylanilino]methyl]benzenesulfonate Chemical compound [Na+].C1=CC(OCC)=CC=C1NC1=CC=C(C(=C2C(=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=2C(=CC(=CC=2)N(CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C)C=C1 RWVGQQGBQSJDQV-UHFFFAOYSA-M 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000012137 tryptone Substances 0.000 claims description 4
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000007865 diluting Methods 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 108010050327 trypticase-soy broth Proteins 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 230000001939 inductive effect Effects 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 3
- 235000015393 sodium molybdate Nutrition 0.000 abstract 1
- 239000011684 sodium molybdate Substances 0.000 abstract 1
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 abstract 1
- 239000000047 product Substances 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 7
- 238000000926 separation method Methods 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 206010059866 Drug resistance Diseases 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 206010048038 Wound infection Diseases 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
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- 238000002428 photodynamic therapy Methods 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 230000029663 wound healing Effects 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 238000004435 EPR spectroscopy Methods 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 210000002429 large intestine Anatomy 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
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- 239000011259 mixed solution Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
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- 239000002244 precipitate Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
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Abstract
The invention relates to a preparation method and application of a ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material, which comprises the following steps: (1) Uniformly stirring ferrous sulfate heptahydrate and a sodium hypochlorite solution; (2) transferring the mixture into a high-pressure reaction kettle for reaction; (3) Separating the product obtained by the reaction, washing and drying to obtain the ferric oxide nano material; (4) Dissolving ferric oxide, thioacetamide and sodium molybdate in pure water and stirring uniformly; (5) Transferring the mixture obtained by uniformly stirring into a high-pressure reaction kettle for reaction; (6) Separating the product obtained by the reaction, washing and drying to obtain the ferric oxide-molybdenum disulfide nano compound; (7) Mixing the product with sodium dodecyl sulfate in pure water, and then carrying out ultrasonic treatment; and (8) separating a product and drying. According to the invention, the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material has a good antibacterial effect under infrared induction.
Description
Technical Field
The invention relates to a preparation method and application of a ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material, in particular to an application technology of the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material in infrared induction bacteriostasis and drug-resistant gene propagation inhibition, belonging to the field of nano biology.
Background
Infections caused by drug-resistant bacteria pose a serious threat to public health, and therefore, development of novel antibacterial agents having various functions is required. In particular, nanomaterials are one of the promising candidates against the growing crisis of antibiotic resistance. Different iron trioxide-molybdenum disulfide-sodium lauryl sulfate nanocomposites were synthesized herein by coating sodium lauryl sulfate on iron trioxide-molybdenum disulfide. Photothermal research shows that the ferric oxide-molybdenum disulfide-sodium dodecyl sulfate has excellent and stable photothermal performance and can be used as an NIR-induced photothermal reagent. Has good disinfection capability to escherichia coli, methicillin-resistant staphylococcus aureus and pseudomonas aeruginosa and wound healing capability in vivo under near-infrared irradiation. According to the results of electron paramagnetic resonance and free radical capture experiments, a large amount of superoxide, hydroxyl free radicals, singlet oxygen and living cell active oxygen can be observed under near infrared irradiation.
In addition, its inhibitory effect on the spread of antibiotic resistance genes was investigated. As expected, ferric oxide-molybdenum disulfide-sodium lauryl sulfate can effectively and broadly block the transmission of plasmid-mediated resistance. In summary, our findings show that ferric oxide-molybdenum disulfide-sodium dodecyl sulfate may be a potential candidate for photothermal-photodynamic therapy and inhibition of drug resistance gene transmission.
Disclosure of Invention
The invention aims to provide a preparation method and application of a ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material aiming at the problems in the prior art, in particular to an application technology of the composite nano material in photothermal-photodynamic therapy and drug resistance gene propagation inhibition.
The purpose of the invention is realized as follows: a preparation method of a ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material is characterized by comprising the following steps:
(1) Weighing 1.0 to 1.2 grams of ferrous sulfate heptahydrate and 60ml of sodium hypochlorite solution, and uniformly stirring;
(2) Transferring the mixture uniformly stirred in the step (1) into a high-pressure reaction kettle, and reacting at 160-200 ℃;
(3) Separating the product obtained in the step (2), washing and drying to obtain the ferric oxide nano material;
(4) Respectively weighing 0.05 to 0.2 g of ferric oxide obtained in the step (3), 0.2 to 0.4 g of thioacetamide and 0.1 to 0.3 g of sodium molybdate dihydrate, dissolving in pure water, and stirring uniformly;
(5) Transferring the mixture obtained by uniformly stirring in the step (4) into a high-pressure reaction kettle, and reacting at the temperature of 170-200 ℃;
(6) Separating the product obtained by the reaction in the step (5), washing and drying to obtain the ferric oxide-molybdenum disulfide nano compound;
(7) Mixing the ferric oxide-molybdenum disulfide obtained in the step (6) and sodium dodecyl sulfate in pure water, and then carrying out ultrasonic treatment;
(8) And (5) separating the product obtained in the step (7), and drying to obtain the ferric oxide-molybdenum disulfide-lauryl sodium sulfate nano material.
In step (7), iron sesquioxide-molybdenum disulfide and sodium dodecyl sulfate are mixed in water and washed with ultrapure water and ethanol at least three times under ultrasound for 6 hours, and then dried at 60 ℃.
A ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material is used for infrared induced photothermal effect and a method for inhibiting bacteria, and the specific process is as follows:
a) Adding 0.6 mL of solution containing ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material into a test tube, and then irradiating by infrared, wherein the experimental result shows that: the ferric oxide-molybdenum disulfide-lauryl sodium sulfate has better thermal effect under the concentration of 120 ug/mL, the photothermal conversion efficiency is as high as 45.96 percent, and the photothermal conversion efficiency is almost unchanged in the process of repeated use;
b) Respectively culturing Escherichia coli, methicillin-resistant staphylococcus aureus and pseudomonas aeruginosa at 37 ℃ overnight by using a TSB liquid culture medium, respectively collecting thalli, washing for 2-3 times by using 0.03M PBS, and suspending by using the PBS to make the concentration of the thalli reach 10 6 CFU/mL; respectively putting 0.6 mL of the suspension of the 3 bacteria into a test tube, simultaneously adding the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material, carrying out induction irradiation for 5 minutes by using far-infrared light, and analyzing the inhibition effect of the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material on the bacteria under infrared induction by using a plate coating counting method.
In the step b), the far-red light induction time is 5 minutes, the photo-thermal conversion efficiency is 45.96 percent, the repeatability is good, and the bacteriostasis efficiency is high.
A method for inhibiting drug-resistant gene transmission by using a ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material comprises the following specific steps:
a) And preparation before experiment: a plurality of 15ml glass test tubes, a plurality of 5ml glass tubes, tryptone soy peptone liquid medium and 0.2 mol PBS are subjected to high-pressure steam sterilization at 121 ℃ for 15-20 minutes for later use;
b) And shaking the bacteria: taking two 15ml glass test tubes, respectively adding 10-12ml tryptone soy peptone liquid culture medium culture solution, respectively inoculating donor bacteria and acceptor bacteria, and culturing at 37 ℃ at 160r/min for 14 hours;
c) Collecting donor bacteria and acceptor bacteria in the step b), washing with PBS for 2-3 times to remove residual substances, wherein the residual substances comprise a culture medium and antibiotics, and diluting the bacteria to 5 x 10 by using PBS 8 CFU/mL;
d) Respectively taking 1.5ml of the bacterial suspension in the step c) and uniformly mixing in a 5ml glass test tube, respectively adding the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material into the 5ml glass test tube, and taking the component without the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite material as a reference;
e) The components are placed at 30 ℃ for joint culture, after the culture is finished, a certain volume of bacterial liquid is taken and coated on a screening culture medium, and then the bacterial liquid is inverted and cultured overnight; counting the colony number on each plate, calculating a conjugation transformant and a conjugation transfer frequency, and then analyzing the influence of different doses of the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material on the conjugation transfer of the drug-resistant gene.
The ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material has good inhibition effect on conjugative transfer transmission of wide host plasmids and narrow host plasmids.
Compared with the prior art, the invention has the following beneficial effects:
the mixture of the ferric oxide-molybdenum disulfide and the sodium dodecyl sulfate is subjected to ultrasonic treatment for 6 hours, so that the sodium dodecyl sulfate can be uniformly coated outside the ferric oxide-molybdenum disulfide.
The ferric oxide-molybdenum disulfide-lauryl sodium sulfate has excellent photo-thermal conversion efficiency and infrared induction bacteriostasis efficiency.
The ferric oxide-molybdenum disulfide-lauryl sodium sulfate not only has good inhibition effect on wide host plasmids, but also has good inhibition effect on conjugative transfer propagation of narrow host plasmids.
In summary, the invention relates to the application of a ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material in infrared induction bacteriostasis and inhibition of drug-resistant gene transmission. The method comprises the following steps: stirring ferrous sulfate heptahydrate and sodium hypochlorite solution in a magnetic stirrer for 1 hour, transferring the prepared solution into a polytetrafluoroethylene-lined high-pressure reaction kettle, continuously reacting for 8 hours at 200 ℃, centrifuging to collect a product, washing the product with ultrapure water and ethanol until the product is clean, and drying the product in vacuum for 8 hours at 60 ℃ to collect a brown product ferric oxide. In order to synthesize the ferric oxide-molybdenum disulfide composite material, ferric oxide, thioacetamide and sodium molybdate dihydrate are mixed into 60ml of ultrapure water and stirred uniformly. Subsequently, the mixed solution was transferred to a 100mL autoclave and reacted at 200 ℃ for 20 hours. After natural cooling to room temperature, the precipitate was collected by centrifugation, washed with ultrapure water and ethanol at least three times, and then vacuum-dried overnight at 60 ℃ to obtain a ferric oxide-molybdenum disulfide composite material. Adding ferric oxide-molybdenum disulfide into SDS solution, then carrying out ultrasonic treatment for 6 hours, washing and drying to obtain the ferric oxide-molybdenum disulfide-sodium dodecyl sulfate composite nano material.
Escherichia coli, staphylococcus aureus and pseudomonas aeruginosa are used as strains to test the bacteriostasis effect of the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material under infrared induction. The situation that the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material inhibits diffusion transfer of drug-resistant genes is tested by using a broad-spectrum host IncP type plasmid RP4-7 and a narrow-host IncF type plasmid F33: A-B-and IncX type plasmid IncX 4. The test results show that: the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material has good infrared induction bacteriostasis capability, is used for infrared induction bacteriostasis and inhibition of drug-resistant gene conjugation transfer, has the advantages of low cost, good performance, low biological toxicity and the like, and has good application prospect in treatment of water polluted by drug-resistant bacteria and the like and wound infection in the future.
The ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material has a good antibacterial effect under infrared induction; and has the function of inhibiting the transmission of drug-resistant genes under the condition of no induction.
Because of the harm of antibiotics, the use of antibiotics is limited or reduced in more and more fields at present, and the iron trioxide-molybdenum disulfide-sodium dodecyl sulfate composite nano material has the functions of inhibiting bacteria and promoting wound healing and also has the effect of preventing drug-resistant gene transmission, so that the iron trioxide-molybdenum disulfide-sodium dodecyl sulfate composite nano material has a wide application prospect in wound infection treatment or environmental disinfection.
Drawings
FIG. 1 is a transmission electron micrograph of iron sesquioxide @ molybdenum disulfide according to example 1 of the present invention;
FIG. 2 is a transmission electron microscope image of the iron sesquioxide-molybdenum disulfide-sodium dodecyl sulfate composite nanomaterial of example 1 of the present invention;
FIG. 3 shows the photothermal conversion efficiency of the iron sesquioxide-molybdenum disulfide-sodium lauryl sulfate composite nanomaterial of example 2 of the present invention;
fig. 4 shows the bacteriostatic effect of the iron sesquioxide-molybdenum disulfide-sodium dodecyl sulfate composite nanomaterial of example 2 of the present invention under infrared induction.
Fig. 5 shows the effect of the iron sesquioxide-molybdenum disulfide-sodium dodecyl sulfate composite nanomaterial of example 3 of the present invention on inhibiting the transmission of drug-resistant gene joining transfer.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. The preparation of the iron sesquioxide-molybdenum disulfide-sodium lauryl sulfate composite is further illustrated by the following specific examples.
Example 1:
weighing 1.11 g of ferrous sulfate heptahydrate and 60ml of sodium hypochlorite solution, and uniformly stirring;
will be provided withTransferring the mixture to a high-pressure reaction kettle, and reacting at 180 ℃;
respectively weighingDissolving 0.1 g of ferric oxide, 0.37 g of thioacetamide and 0.24 g of sodium molybdate dihydrate in pure water and uniformly stirring;
will be described in detailTransferring the mixture to a high-pressure reaction kettle, and reacting at 200 ℃;
separation stepWashing and drying the product to obtain the ferric oxide-molybdenum disulfide nano compound;
will be described in detailMixing the product with sodium dodecyl sulfate in pure water, and then carrying out ultrasonic treatment;
separation stepAnd drying the product to obtain the ferric oxide-molybdenum disulfide-lauryl sodium sulfate nano material.
FIG. 1 is a transmission electron micrograph of iron sesquioxide-molybdenum disulfide according to example 1 of the present invention; fig. 2 is a transmission electron microscope image of the iron sesquioxide-molybdenum disulfide-sodium dodecyl sulfate composite nanomaterial of example 1 of the present invention.
Example 2:
the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material obtained in the embodiment 1 is used for infrared induction photothermal effect and bacteriostatic effect thereof, and the specific process is as follows:
a) 0.6 mL of the nanomaterial-containing solution was added to the tube and then irradiated with infrared, and the experimental results showed that: the ferric oxide-molybdenum disulfide-lauryl sodium sulfate has better thermal effect under the concentration of 120 ug/mL, the photothermal conversion efficiency is as high as 45.96% (figure 3), and the photothermal conversion efficiency is almost unchanged in the process of repeated use;
b) Respectively culturing Escherichia coli, methicillin-resistant Staphylococcus aureus (MRSA) and Pseudomonas aeruginosa at 37 deg.C overnight with TSB liquid culture medium, respectively collecting thallus, washing with 0.03M PBS for 2-3 times, and suspending with PBS to obtain thallus concentration of 10 6 CFU/mL. 0.6 mL of the suspension of the 3 bacteria is added into a test tube, the nano material is added into the test tube, and then the test tube is induced and irradiated by 0.7W of far-infrared light for 5 minutes, and the experimental result shows that: ferric oxide-molybdenum disulfide-sodium dodecyl sulfate is used for treating large intestine, MRSA and copper under infrared inductionThe bactericidal efficiency of pseudomonas aeruginosa was 99.95%, 99.97% and 99.58%, respectively (fig. 4).
FIG. 3 shows the photothermal conversion efficiency of the iron sesquioxide-molybdenum disulfide-sodium dodecyl sulfate composite nanomaterial of example 2 of the present invention; fig. 4 shows the bacteriostatic effect of the ferric oxide-molybdenum disulfide-sodium dodecyl sulfate composite nanomaterial of example 2 under infrared induction.
Example 3:
the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material obtained in the example 1 is used for inhibiting the gene junction transfer performance, and the specific process is as follows:
a) Preparation before experiment: several 15ml glass test tubes and several 5ml glass tubes are used, and the whole is sterilized by high pressure steam at 121 ℃ for 15-20 minutes by using a 1.5ml centrifuge tube, trypticase soy peptone liquid medium and 0.2 mol PBS for standby.
b) Shaking the bacteria: two 15ml glass test tubes are taken, 10-12ml tryptone soy peptone liquid medium culture solution is respectively added, then donor bacteria and acceptor bacteria are respectively inoculated, and the culture is carried out for 14 hours at 37 ℃ and at 160 r/min.
c) Collecting donor bacteria and acceptor bacteria in the step b), washing with PBS for 2-3 times to remove residual culture medium and antibiotics, and diluting the bacteria with PBS to 5 × 10 8 CFU/mL;
d) Respectively taking 1.5ml of the bacterial suspension in c) into a 5ml glass test tube and uniformly mixing, respectively adding 100 mg/L of nano material into the glass test tube, and taking the component without the material as a reference;
e) The components are placed at 30 ℃ for joint culture, after the culture is finished, a certain volume of bacterial liquid is diluted by a centrifugal tube of 1.5ml and coated on a screening culture medium, and then the culture is carried out in an inverted mode overnight. The colony number on each plate is counted, and the joint transformant and the joint transfer frequency are calculated, and the results show that: fe 2 O 3 @MoS 2 The @ SDS (1)The fold inhibition of the junction transfer propagation is: 130-, 14-, 43-fold (FIG. 5).
Fig. 5 shows the effect of the iron sesquioxide-molybdenum disulfide-sodium dodecyl sulfate composite nanomaterial of example 3 of the present invention on inhibiting the transmission of drug-resistant gene joining transfer.
The above description is only a preferred embodiment of the present invention, and not intended to limit the scope of the present invention. In addition to the above examples, the present invention may have other embodiments, for example, the amount of the composite nanomaterial and the sampling and plating time may be appropriately enlarged. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention. Technical features of the present invention which are not described may be implemented by or using the prior art, and will not be described herein.
Claims (6)
1. A preparation method of a ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material is characterized by comprising the following steps:
(1) Weighing 1.0 to 1.2 grams of ferrous sulfate heptahydrate and 60ml of sodium hypochlorite solution, and uniformly stirring;
(2) Transferring the mixture obtained by uniformly stirring in the step (1) into a high-pressure reaction kettle, and reacting at 160-200 ℃;
(3) Separating the product obtained by the reaction in the step (2), washing and drying to obtain the ferric oxide nano material;
(4) Respectively weighing 0.05 to 0.2 g of ferric oxide obtained in the step (3), 0.2 to 0.4 g of thioacetamide and 0.1 to 0.3 g of sodium molybdate dihydrate, dissolving in pure water, and stirring uniformly;
(5) Transferring the mixture obtained by uniformly stirring in the step (4) into a high-pressure reaction kettle, and reacting at the temperature of 170-200 ℃;
(6) Separating the product obtained in the step (5), washing and drying to obtain the ferric oxide-molybdenum disulfide nano compound;
(7) Mixing the ferric oxide-molybdenum disulfide obtained in the step (6) and sodium dodecyl sulfate in pure water, and then carrying out ultrasonic treatment;
(8) And (5) separating the product obtained in the step (7), and drying to obtain the ferric oxide-molybdenum disulfide-lauryl sodium sulfate nano material.
2. The method of claim 1, wherein in the step (7), the iron sesquioxide-molybdenum disulfide-sodium dodecyl sulfate is mixed with sodium dodecyl sulfate in water, and the mixture is washed with ultrapure water and ethanol at least three times under ultrasound for 6 hours, and then dried at 60 ℃.
3. The method for infrared-induced photothermal effect and its bacteriostasis of the iron trioxide-molybdenum disulfide-sodium dodecyl sulfate composite nanomaterial of claim 1, wherein the specific process is as follows:
a) Adding 0.6 mL of solution containing ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material into a test tube, and then irradiating by infrared rays, wherein the experimental result shows that: the ferric oxide-molybdenum disulfide-lauryl sodium sulfate has better thermal effect under the concentration of 120 ug/mL, the photothermal conversion efficiency is as high as 45.96 percent, and the photothermal conversion efficiency is almost unchanged in the process of repeated use;
b) Respectively culturing Escherichia coli, methicillin-resistant staphylococcus aureus and pseudomonas aeruginosa at 37 ℃ overnight by using a TSB liquid culture medium, respectively collecting thalli, washing for 2-3 times by using 0.03M PBS, and suspending by using the PBS to make the concentration of the thalli reach 10 6 CFU/mL; respectively putting 0.6 mL of the suspension of the 3 bacteria into a test tube, simultaneously adding the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material, inducing and irradiating for 5 minutes by using far-infrared light, and analyzing the inhibition effect of the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material on the bacteria under infrared induction by using a plate coating counting method.
4. The method as claimed in claim 3, wherein in the step b), the far-red light induction time is 5 minutes, the photothermal conversion efficiency is 45.96%, the repeatability is good, and the bacteriostatic efficiency is high.
5. The method for inhibiting the transmission of drug-resistant genes by using the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material as claimed in claim 1, which is characterized by comprising the following specific steps:
a) And preparation before experiment: a plurality of 15ml glass test tubes, a plurality of 5ml glass tubes, a plurality of 1.5ml centrifuge tubes, a trypticase soy peptone liquid medium and 0.2 mol PBS are all sterilized by high pressure steam at 121 ℃ for 15-20 minutes for later use;
b) And shaking the bacteria: taking two 15ml glass test tubes, respectively adding 10-12ml tryptone soy peptone liquid culture medium culture solution, respectively inoculating donor bacteria and acceptor bacteria, and culturing at 37 ℃ at 160r/min for 14 hours;
c) Washing the donor bacteria and the acceptor bacteria in the step b) with PBS for 2-3 times to remove residual substances, wherein the residual substances comprise a culture medium and antibiotics, and diluting the bacteria to 5 x 10 by using PBS 8 CFU/mL;
d) Respectively taking 1.5ml of the bacterial suspension in the step c) and uniformly mixing in a 5ml glass test tube, respectively adding the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material into the 5ml glass test tube, and taking the component without the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite material as a reference;
e) The components are placed at 30 ℃ for joint culture, after the culture is finished, a certain volume of bacterium liquid is diluted by a centrifugal tube of 1.5ml and coated on a screening culture medium, and then the bacterium liquid is inverted and cultured overnight; counting the colony number on each plate, calculating a conjugation transformant and a conjugation transfer frequency, and then analyzing the influence of different doses of the ferric oxide-molybdenum disulfide-lauryl sodium sulfate composite nano material on the conjugation transfer of the drug-resistant gene.
6. The method of claim 5, wherein the ferric oxide-molybdenum disulfide-sodium dodecyl sulfate composite nanomaterial has a good inhibitory effect on conjugative transfer propagation of both broad host plasmids and narrow host plasmids.
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