Inorganic-organic hybrid Keggin type polyoxometallate compound as well as preparation method and antibacterial application thereof
A technology of polyoxometalates and organic hybridization, which is applied in organic chemistry, antibacterial drugs, organic active ingredients, etc., can solve the problems of instability of pure inorganic substances, limit cell penetration, etc., and achieve enhanced stability and Penetration ability, excellent antibacterial performance, strong stability effect
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[0034] Example 1
[0035] A method for preparing an inorganic-organic hybrid Keggin type polyoxometalate complex includes the following steps:
[0036] Co(NO 3 ) 2 ·6H 2 O (0.189 g, 1.3 mmol), Na 2 MoO 4 ·2H 2 O (0.48 g, 2.0 mmol), EDTMP (0.35 g, 0.8 mmol) and 2-acetylpyrazine thiosemicarbazone (0.097 g, 0.5 mmol) were added to 60 mL of water and methanol (volume ratio 2:1) In the mixed solvent, stir for 40 minutes until the dissolution is complete. Use dilute hydrochloric acid to adjust the pH value between 2.5 and 3.0, then transfer it to the reaction flask, put it in a polytetrafluoroethylene lining and keep it at 130°C for 3 days, and cool At room temperature, wash with water and dry to obtain black quadrilateral crystals, which are composites.
[0037] The above-mentioned inorganic-organic hybrid Keggin polyoxometalate belongs to the monoclinic crystal system, C2 / c Space group, its unit cell parameters are: a = 29.1829(13) Å, b = 16.5031(7) Å, c = 18.9095(9) Å, α = 90°, β ...
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[0046] Example 2
[0047] Evaluation method of antibacterial effect 1 Disc diffusion method:
[0048] With DMSO as the blank control group, the test was carried out on agar plates to study the antibacterial activity of the material. Before the test, the complex was diluted with DMSO in a gradient (1 mg / mL, 0.5 mg / mL, 0.25 mg / mL, 0.125 mg / mL, 0.0625 mg / mL, 0.03125 mg / mL...). All materials used in the testing process were autoclaved, and the nutrient agar plate (NA) was sterilized by ultraviolet radiation for 1 hour. Will 10 7 CFU / mL Staphylococcus aureus ( S. aureus ), Bacillus subtilis ( B. subtilis ) And 10 6 CFU / mL Escherichia coli ( E. coli ) And Agrobacterium tumefaciens ( A. tumefaciens ) Fresh bacteria solution was evenly spread on the nutrient agar (NA) plate, and then punched, the prepared complex was sucked into the agar plate wells, and then sealed, the culture was incubated at 37°C for 16 hours , Finally, measure the zone of inhibition (ZOI) of all samples, and rec...
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[0053] Example 3
[0054] Time killing experiment evaluation 2 colony forming unit (CFU) method:
[0055] The bactericidal ability of the compound was studied by the plate coating culture method. Serially dilute the E. coli and Staphylococcus aureus solution to 10 5 CFU / mL, and prepare a 1 mg / mL complex solution. Incubate the same volume of the inoculum solution and the complex solution for different times at 37°C. The bacterial solution without complexes is used as a control experiment. The mixed solution of the different culture time is evenly spread on the nutrient agar (NA) plate, each time The measurement was repeated three times and cultured in a 37°C constant temperature incubator for 16 hours. The experiment continued until almost no colonies were observed. The experimental results show as Picture 9 with 10 . Bacterial cell survival rate (%)= (number of colonies in the experimental group / number of colonies in the control group)×100%.
[0056] Picture 9 with Picture 1...
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