A carbon black adsorbed gallium nitrate antibacterial agent and its preparation method and application

Abstract

The invention discloses a carbon black adsorbed gallium nitrate antibacterial agent and a preparation method and application thereof, and relates to the technical field of antibacterial agents. The carbon black adsorbed gallium nitrate antibacterial agent is obtained by adding gallium nitrate and carbon black into water and mixing, then heating, filtering and drying. The carbon black adsorbed gallium nitrate antibacterial agent uses carbon black as a carrier to load gallium nitrate; the mass ratio of the gallium nitrate to the carbon black is 1:5-100. The preparation method of the invention is simple and easy to expand the scale of production. The carbon black adsorbed gallium nitrate antibacterial agent prepared by the invention has good antibacterial effects on Escherichia coli, Staphylococcus aureus and EM bacteria.

Description

Technical Field

[0001] The invention relates to the technical field of antibacterial agents, and in particular to a carbon black adsorbed gallium nitrate antibacterial agent and a preparation method and application thereof. Background Art

[0002] The continuous use of antibiotics has put great pressure on bacteria to survive. Only bacteria with drug-resistant mutant genes can survive, and the mutant genes will be transmitted between bacteria. At present, most pathogens have drug resistance problems, and the changes in drug resistance are accelerating. In addition, the drug resistance mechanisms of many pathogenic microorganisms are complex, making some antibiotics ineffective.

[0003] EM bacteria is a mixed bacteria, including photosynthetic bacteria, yeast and lactic acid bacteria, which can be used for food additives, soil improvement, sewage treatment, etc. However, excessive abuse of EM bacteria may cause the water to turn black and deteriorate, causing aquatic products to die of lack of oxygen; when treating soil, if EM bacteria are abused too much, the soil will also be damaged. At present, there are no reports on antibacterial agents that effectively inhibit EM bacteria.

[0004] Gallium nitrate is an inorganic antibacterial agent that can kill a wide range of bacteria, has a low incidence of drug resistance, and has stable chemical properties. However, the antibacterial properties of gallium nitrate need to be further improved. Summary of the invention

[0005] Based on the above content, the present invention provides a carbon black adsorbed gallium nitrate antibacterial agent and its preparation method and application, by loading gallium nitrate on carbon black to improve the antibacterial performance of gallium nitrate and at the same time play a sustained release effect.

[0006] To achieve the above object, the present invention provides the following solutions:

[0007] One of the technical solutions of the present invention is a carbon black adsorbed gallium nitrate antibacterial agent, in which carbon black is used as a carrier to load gallium nitrate; the mass ratio of the gallium nitrate to the carbon black is 1:5-100.

[0008] The second technical solution of the present invention is a method for preparing the above-mentioned carbon black adsorbed gallium nitrate antibacterial agent, comprising the following steps:

[0009] Gallium nitrate and carbon black are added into water and mixed evenly, and then heated, filtered and dried to obtain the carbon black adsorbed gallium nitrate antibacterial agent.

[0010] Furthermore, before being added to water, the carbon black is first soaked in acid, then washed to neutrality, and dried to remove moisture.

[0011] Furthermore, the mass volume ratio of the carbon black to the water is 50 mg:2-10 mL.

[0012] Furthermore, the mixing is specifically performed by vortexing for 5 minutes and then ultrasonicating for 10 minutes.

[0013] Furthermore, the heating is specifically heating at 50° C. for 3-5 hours.

[0014] Furthermore, the drying is specifically drying at 40-60° C. for 6-10 hours.

[0015] The third technical solution of the present invention is the use of the above-mentioned carbon black adsorbed gallium nitrate antibacterial agent in inhibiting Escherichia coli, Staphylococcus aureus and / or EM bacteria.

[0016] A fourth technical solution of the present invention is an EM bacteria antibacterial agent, comprising the above-mentioned carbon black adsorbed gallium nitrate antibacterial agent.

[0017] The present invention discloses the following technical effects:

[0018] The preparation method of the invention is simple and easy to expand scale production.

[0019] The carbon black adsorbed gallium nitrate antibacterial agent prepared by the invention has good antibacterial effects on Escherichia coli, Staphylococcus aureus and EM bacteria. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0021] Figure 1 The antibacterial agent prepared in Example 1 shows the anti-Escherichia coli effect by diffusion method; the left picture is the blank control group, and the right picture is the experimental group and the positive control group;

[0022] Figure 2 The antibacterial agent diffusion method prepared in Example 1 shows the anti-Staphylococcus aureus effect; the left picture is the blank control group, and the right picture is the experimental group and the positive control group;

[0023] Figure 3 The antimicrobial agent diffusion method prepared in Example 1 shows the anti-EM bacteria effect; the left picture is the blank control group, and the right picture is the experimental group and the positive control group;

[0024] Figure 4 The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Escherichia coli bacterial solution in the absorbance antibacterial experiment of the present invention at 0h; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0025] Figure 5The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Escherichia coli bacterial solution for 2 hours in the absorbance antibacterial experiment of the present invention; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0026] Figure 6 The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Escherichia coli bacterial solution for 4 hours in the absorbance antibacterial experiment of the present invention; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0027] Figure 7 The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Escherichia coli bacterial solution for 6 hours in the absorbance antibacterial experiment of the present invention; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0028] Figure 8 The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Escherichia coli bacterial solution in the absorbance antibacterial experiment of the present invention for 8 hours; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0029] Fig. 9 The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Escherichia coli bacterial solution in the absorbance antibacterial experiment of the present invention for 10 hours; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0030] Fig.10 The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Escherichia coli bacterial solution in the absorbance antibacterial experiment of the present invention for 24 hours; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0031] Fig.11 It is a growth curve diagram of the Escherichia coli liquid of the present invention under different concentrations of the antibacterial agent (prepared in Example 1);

[0032] Fig.12 The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Staphylococcus aureus bacterial solution in the absorbance antibacterial experiment of the present invention for 0h; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0033] Fig.13 The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Staphylococcus aureus bacterial solution for 2 hours in the absorbance antibacterial experiment of the present invention; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0034] Fig.14 The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Staphylococcus aureus bacterial solution for 4 hours in the absorbance antibacterial experiment of the present invention; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0035] Fig.15The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Staphylococcus aureus bacterial solution for 6 hours in the absorbance antibacterial experiment of the present invention; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0036] Fig.16 The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Staphylococcus aureus bacterial solution in the absorbance antibacterial experiment of the present invention for 8 hours; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0037] Fig.17 The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Staphylococcus aureus bacterial solution in the absorbance antibacterial experiment of the present invention for 10 hours; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0038] Fig.18 The graph is a graph showing the experimental results of adding the antibacterial agent prepared in Example 1 to the Staphylococcus aureus bacterial solution for 24 hours in the absorbance antibacterial experiment of the present invention; wherein the left graph is the bacterial solution plus the antibacterial agent, and the right graph is only the antibacterial agent;

[0039] Fig.19 It is a growth curve diagram of the Staphylococcus aureus bacterial liquid of the present invention under different concentrations of the antibacterial agent (prepared in Example 1);

[0040] Fig. 20 This is the full XPS spectrum of the antibacterial agent prepared in Example 1;

[0041] Fig.21 This is the Ga 3d XPS spectrum of the antibacterial agent prepared in Example 1. DETAILED DESCRIPTION

[0042] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as limiting the present invention, but should be understood as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0043] It should be understood that the terms described in the present invention are only for describing special embodiments and are not intended to limit the present invention. In addition, for the numerical range in the present invention, it should be understood that each intermediate value between the upper and lower limits of the scope is also specifically disclosed. Each smaller range between the intermediate value in any stated value or stated range and any other stated value or intermediate value in the described range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded in the scope.

[0044] Unless otherwise indicated, all technical and scientific terms used herein have the same meanings as those generally understood by those skilled in the art. Although the present invention describes only preferred methods and materials, any methods and materials similar or equivalent to those described herein may also be used in the implementation or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and / or materials associated with the documents. In the event of a conflict with any incorporated document, the content of this specification shall prevail.

[0045] It will be apparent to those skilled in the art that various modifications and variations may be made to the specific embodiments of the present invention description without departing from the scope or spirit of the present invention. Other embodiments derived from the present invention description will be apparent to the skilled artisan. The present invention description and examples are exemplary only.

[0046] The words “include,” “including,” “have,” “contain,” etc. used in this document are open-ended terms, meaning including but not limited to.

[0047] Unless otherwise specified, the "%" in the present invention is based on mass percentage.

[0048] The gallium nitrate used in the embodiment of the present invention is prepared by the following steps:

[0049] (1) First, add 1.88 g of solid gallium oxide to a three-necked flask, which is equipped with a reflux condenser and a thermometer. Then add 10.8 mL of concentrated hydrochloric acid to a 50 mL beaker, add 3.6 mL of concentrated nitric acid, stir for two minutes, pour the prepared mixed solution into the three-necked flask, place it in a water bath thermostatic magnetic stirring device, then add distilled water, and heat it in a water bath pot, adjust the temperature to 90 ° C, and heat for 3 hours until a transparent solution is formed.

[0050] (2) Cool the transparent solution to 20°C, slowly drip ammonia water into the transparent solution, and the transparent solution will slowly become turbid until gallium hydroxide precipitation is observed. Filter through a Buchner funnel and a vacuum pump to obtain a gallium hydroxide precipitate, and slowly wash the gallium hydroxide precipitate with deionized water until the pH value of the final washing water is neutral. Put all the gallium hydroxide precipitates into a beaker, add water first and then nitric acid in sequence, pour the mixed solution into a water bath thermostatic magnetic stirring device, heat the temperature to 50°C, dissolve all the gallium hydroxide precipitates, and prepare a gallium nitrate solution.

[0051] (3) The gallium nitrate solution was subjected to reduced pressure distillation for 12 hours at a system pressure of 0.09 MPa and a temperature of 60° C. The transparent viscous liquid was then placed in a drying oven at 60° C. and dried at normal pressure for 24 hours to obtain white gallium nitrate powder.

[0052] Gallium nitrate powder obtained by other preparation methods or purchased can also achieve the technical effects of the present invention.

[0053] The carbon black used in the embodiments of the present invention is treated as follows before use: first, it is washed by soaking in dilute nitric acid, and then washed with tap water and distilled water until the carbon black is neutral. If it is neutral, it means that the nitric acid on the surface of the carbon black has been washed away. The carbon black is placed in an oven for heating and drying to remove moisture for use.

[0054] Example 1

[0055] Weigh 6 mg of gallium nitrate and 50 mg of carbon black respectively, measure 10 mL of distilled water, add them together into a 20 mL small white bottle, use a mixer to vortex for 5 minutes, use an ultrasonic cleaner to ultrasonicate for 10 minutes, and mix the solution thoroughly. Pour the mixed solution into a water bath constant temperature magnetic stirring device, adjust the temperature to 50°C and stir for 4 hours (3-5 hours is equivalent to 4 hours in terms of technical effect). Filter the mixed solution again to obtain a black solid with carbon black adsorbing gallium nitrate. Place it in a drying oven at 50°C (40-60°C is equivalent to 50°C in terms of technical effect) and dry it for 7 hours (6-10 hours is equivalent to 7 hours in terms of technical effect) to obtain a powdered carbon black adsorbed gallium nitrate antibacterial agent (abbreviated as: antibacterial agent).

[0056] The performance of the carbon black prepared in Example 1 in adsorbing gallium nitrate antibacterial agent was verified as follows:

[0057] 1. Antibacterial test

[0058] 1.1 Bacterial culture

[0059] (1) Preparation of culture medium:

[0060] LB liquid culture medium: According to the standard formula of nutrient broth, pour an appropriate amount of nutrient broth powder into a round-mouth conical bottle, pour an appropriate amount of deionized water into the round-mouth conical bottle, heat and stir to fully dissolve, then seal it with kraft paper and rope, sterilize it at 121°C, and it is ready for use.

[0061] LB solid culture medium: According to the standard formula of nutrient agar, pour an appropriate amount of nutrient agar powder into a round-mouth conical bottle, then add deionized water to dissolve it completely, then seal it with kraft paper and rope, and sterilize it at 121°C for use.

[0062] PDA solid culture medium: According to the standard formula, add an appropriate amount of PDA powder into a round-mouth conical flask, then add an appropriate amount of deionized water, heat and stir to fully dissolve, seal it with a kraft paper box rope, and sterilize it at 121°C for use.

[0063] (2) Utensils and reagents used in antibacterial experiments:

[0064] Place the utensils and reagents required for the antibacterial experiment: LB solid culture medium, LB liquid culture medium, disposable plastic culture dish, triangular glass applicator, pipette tip, 0.85% sodium chloride solution, deionized water, test tube, tweezers, etc. in a high pressure sterilizer at 121°C and take them out after 20 minutes.

[0065] (3) Activation of bacteria:

[0066] Add an appropriate amount of culture medium into a round-mouth conical flask, burn and disinfect the inoculation loop and then cool it. After cooling, use the inoculation loop to pick out the cultured Escherichia coli, Staphylococcus aureus and EM bacteria and put them into the culture medium. Then put the round-mouth conical flask into a constant temperature shaking incubator. The temperature needs to be 37°C and the time needs to be 18-24 hours. If the color of the culture medium gradually becomes turbid, it means that the Escherichia coli, Staphylococcus aureus and EM bacteria have been activated.

[0067] (4) Inoculation and subculture of bacterial strains:

[0068] Add culture agar to the culture plate, and after the agar solidifies, divide the bottom of the culture dish into areas 1, 2, and 3. Disinfect the inoculation loop first, then use the inoculation loop to pick up the active E. coli liquid, first quickly and continuously streak in area 1 of the solid culture medium, then burn and cool the inoculation loop, then streak in area 2, and finally streak in area 3. After streaking, place the disposable culture dish in a bacterial incubator, set the temperature to 37°C, and culture for 18-24 hours. If multiple single colonies appear in area 3 of the solid culture medium, it means that it meets the requirements and is frozen and stored as the first generation of bacteria. Use the same method to culture the second and third generations of bacteria. The subculture method of Staphylococcus aureus, EM bacteria and E. coli is the same.

[0069] 1.2 Diffusion method experiment

[0070] (1) Experimental strains

[0071] Escherichia coli, Staphylococcus aureus and EM bacteria were selected as research objects.

[0072] (2) Utensils and reagents

[0073] Disposable plastic culture dishes, Oxford cups, test tubes, tweezers, inoculation loops, 0.85% sodium chloride solution, LB solid culture medium, 0.1wt% carbon black adsorbed gallium nitrate antibacterial agent solution, 0.1% penicillin.

[0074] (3) Experimental procedures

[0075] Use 1mL 0.85% sodium chloride solution to elute the third generation E. coli colonies adsorbed on the culture dish and mix thoroughly. Pour 10uL of the bacterial mixture into the first test tube (containing 9.99mL 0.85% sodium chloride solution) and mix them; take 100uL of the mixed bacteria from the first test tube and pour it into the second test tube (containing 9.9mL 0.85% sodium chloride solution) and mix them; take 100uL of the mixed liquid from the third test tube and add it to the third one (containing 9.9mL 0.85% sodium chloride solution) and mix them. The liquid in the third test tube is used for absorbance experiments. Pipette 200uL of bacterial solution from the third test tube and add it to the culture plate. Then put two Oxford cups into the culture plate, and then drop 0.1% carbon black adsorbed gallium nitrate solution (experimental group) and 0.1% penicillin (positive control group) into different Oxford cups. Be careful during the dropping process to avoid dropping the antibacterial solution into the position outside the Oxford cup, which will affect the experimental results. Place the culture dish in a 37℃ culture environment for 24 hours. Observe and record the transparent antibacterial zone generated around the Oxford cup to determine whether the antibacterial agent has an antibacterial effect. At the same time, set up a blank control group. The same method was used to conduct diffusion experiments on Staphylococcus aureus and EM bacteria.

[0076] 1.3 Absorbance antibacterial test

[0077] (1) Take 0.85% sodium chloride solution and inject it onto the plate with the third generation Escherichia coli cultured. Wash off a colony and put it into a sterilized test tube. Then add an appropriate amount of 0.85% sodium chloride solution and mix well. Put a small amount of bacterial solution into a colorimetric dish and measure it with a UV spectrometer. If the absorbance value of the bacterial solution is 0.3-0.5, it meets the requirements for the absorbance experiment.

[0078] (2) Add a certain amount of nutrient broth to twelve test tubes and number them: blank solution, Z1, A1, A2, A3, A4, A5, B1, B2, B3, B4, B5. The blank solution test tube contains only nutrient broth, the Z1 test tube contains a small amount of E. coli liquid, and the A1, A2, A3, A4, and A5 test tubes contain different concentrations of antimicrobial agents (the concentration of antimicrobial agents: 200 μL, 10%, 20%, 30%, 40%, and 50% of antimicrobial agents are added to each tube, so that the total volume of each tube is 6.5 mL) and a small amount of E. coli liquid (the amount of liquid added is 200 μL per tube, and the concentration is 0.4×10 8Bacteria / mL,); B1, B2, B3, B4, B5 represent tubes containing only different concentrations of antimicrobial agents (the concentrations of antimicrobial agents are added with 200 μL, 10%, 20%, 30%, 40%, 50%, respectively, so that the total volume of each tube is 6.5 mL). Put all the test tubes into the bacterial incubator, and measure the absorbance of each test tube with a UV spectrometer every 2 hours. The absorbance method against Staphylococcus aureus is the same as that for Escherichia coli.

[0079] 2. Results

[0080] 2.1 Figure 1 , Figure 2 , Figure 3 These are diffusion experiments on Escherichia coli, Staphylococcus aureus, and EM bacteria, respectively. The Oxford cup used has an inner diameter of 6 mm and an outer diameter of 7.8 mm. Figure 1 It can be seen that in the anti-E. coli experiment, the diameter of the antibacterial zone produced by 0.1% carbon black adsorbed gallium nitrate antibacterial agent solution is 20mm, and the diameter of the antibacterial zone produced by 0.1% penicillin is 23.6mm. Figure 2 It can be seen that in the anti-Staphylococcus aureus experiment, the diameter of the inhibition zone produced by 0.1% carbon black adsorbed gallium nitrate solution is 19.1mm, and the diameter of the inhibition zone produced by 0.1% penicillin is 22.5mm. Figure 3 It can be seen that in the anti-EM bacteria experiment, the diameter of the inhibition zone produced by 0.1% carbon black adsorbed gallium nitrate solution is 30.1mm, and 0.1% penicillin has no obvious inhibition zone, and the inhibition zone is almost 0. The results show that the carbon black adsorbed gallium nitrate antibacterial agent does have a good killing effect on Escherichia coli, Staphylococcus aureus, and EM bacteria, and the effect against EM bacteria is more significant than that against Escherichia coli and Staphylococcus aureus.

[0081] 2.2 Figure 4-Figure 10 They are respectively the experimental result graphs of the Escherichia coli bacterial solution in the absorbance antibacterial experiment at 0h, 2h, 4h, 6h, 8h, 10h and 24h after the carbon black adsorbed gallium nitrate antibacterial agent prepared in Example 1 was added, and Table 1 is the absorbance value of the Escherichia coli bacterial solution at 600nm.

[0082] Table 1 Absorbance of Escherichia coli culture at 600nm

[0083] Measuring time Z-Blank Solution A1-B1 A2-B2 A3-B3 A4-B4 A5-B5 0h 0.0407 0.0405 0.0406 0.0407 0.0404 0.0405 2h 0.0421 0.0418 0.0394 0.0393 0.0388 0.0391 4h 0.0438 0.0414 0.0389 0.0376 0.0371 0.0372 6h 0.0452 0.0394 0.0396 0.0334 0.0291 0.0327 8h 0.0502 0.0370 0.0367 0.0285 0.0322 0.0278 10h 0.0529 0.0360 0.0333 0.0243 0.0212 0.0240 24h 0.0997 0.0667 0.0559 0.0395 0.0298 0.0308

[0084] According to the data in Table 1, the growth of Escherichia coli in carbon black adsorbed gallium nitrate antibacterial agent solutions of different concentrations is reflected. Based on this table, a curve diagram of the antibacterial agent dosage and bacterial growth is drawn (see Fig.11 ). Fig.11This is a growth curve of E. coli liquid under different concentrations of carbon black adsorbed gallium nitrate antibacterial agent. There is only E. coli in Z-blank liquid. From A1-B1 to A5-B5, it can be seen that the concentration of the antibacterial agent is increasing. The overall absorbance of these five curves is smaller than the absorbance of the Z-blank curve within 0-24h, indicating that carbon black adsorbed gallium nitrate does have bactericidal ability. And the absorbance of the five curves from A1-B1 to A5-B5 begins to rise when the sterilization time is 10h, indicating that the best antibacterial time of the antibacterial agent is about 10h.

[0085] 2.3 Figure 12-Figure 18 They are respectively the experimental result graphs of 0h, 2h, 4h, 6h, 8h, 10h and 24h after the carbon black adsorbed gallium nitrate antibacterial agent prepared in Example 1 was added to the Staphylococcus aureus solution in the absorbance antibacterial experiment, and Table 2 is the absorbance value of the Staphylococcus aureus solution at 600nm.

[0086] Table 2 Absorbance of Staphylococcus aureus at 600 nm

[0087] time Z-Blank Solution C1-D1 C2-D2 C3-D3 C4-D4 C5-D5 0h 0.0375 0.0371 0.0378 0.0369 0.0368 0.0372 2h 0.0364 0.0333 0.0374 0.0359 0.0348 0.0355 4h 0.0379 0.0292 0.0321 0.0240 0.0189 0.0230 6h 0.0460 0.0261 0.0304 0.0167 0.0132 0.0155 8h 0.0556 0.0151 0.0241 0.0118 0.0102 0.0104 10h 0.0628 0.0279 0.0360 0.0223 0.0156 0.0210 24h 0.0910 0.0567 0.0632 0.0577 0.0424 0.0378

[0088] The data in Table 2 reflect the growth of Staphylococcus aureus in different concentrations of carbon black adsorbed gallium nitrate antibacterial agent solutions. Based on this table, a curve of antibacterial agent dosage and bacterial growth was drawn (see Fig.19 ). Fig.19 This is a graph of the growth of Staphylococcus aureus under different concentrations of antimicrobial agents. There is only Staphylococcus aureus in the Z-blank solution. From A1-B1 to A5-B5, it can be seen that the concentration of the antimicrobial agent is increasing. Within 0-24h, the absorbance of these five curves is smaller than that of the Z-blank curve, indicating that carbon black adsorbed gallium nitrate does have bactericidal ability. And the absorbance of the five curves from A1-B1 to A5-B5 all began to rise when the sterilization time was 18h, indicating that the optimal antibacterial time of the antibacterial agent is about 8h (the above-mentioned Escherichia coli and Staphylococcus aureus experiments were carried out without using a shaking table. When a shaking table was used for the antibacterial experiment of Staphylococcus aureus, the antibacterial effect of the antibacterial agent prepared in Example 1 of the present invention was equivalent to the antibacterial effect of the above-mentioned experiment without using a shaking table. After the antibacterial experiment was carried out for 8h, all the bacteria died. The shaking table antibacterial experiment was continued, and it was found that the antibacterial time of the antibacterial agent prepared in Example 1 of the present invention can reach 180d. This is because gallium nitrate is confined in the ultrafine nanopores of carbon black, and the gallium nitrate in the carbon black is a nanostructure. This nanostructure improves the antibacterial performance of gallium nitrate, and the gallium nitrate in the carbon black is continuously and slowly released, which prolongs the antibacterial time of the antibacterial agent).

[0089] 2.4 In order to study the valence state of gallium ions adsorbed in carbon black, XPS analysis was performed on the carbon black adsorbed gallium nitrate antibacterial agent (sample) prepared in Example 1 (in order to accurately obtain the valence state of gallium ions in the sample, the sample corresponding to this spectrum was directly dried after synthesis, and the XPS test was performed directly after the sample was dried, without being stored for too long before the test). The Thermo Fisher Scientific K-Alpha X-ray photoelectron spectrometer was used to analyze the sample valence state, and the X-ray source used was Al KAlpha.

[0090] like Fig. 20 As shown in the figure, there are five obvious peaks at binding energies of 1118.08eV, 532.08eV, 425.08eV, 284eV, and 20.08eV, respectively. These five peaks are attributed to Cl 1s, O 1s, N 1s, C 1s, and Ga 3d, respectively, indicating that carbon black adsorbed gallium nitrate contains elements such as Cl, O, N, C, and Ga.

[0091] like Fig.21 As shown in the figure, there is only one obvious peak at a binding energy of 20.08 eV. According to the NIST X-ray Photoelectron Spectroscopy Database, the binding energy corresponding to the 3d orbital of gallium ions in gallium oxide compounds is 20.8 eV. Based on this, it is inferred that carbon black adsorbs trivalent gallium ions.

[0092] In the anti-EM bacteria experiment, the diameter of the antibacterial zone produced by the 0.1% carbon black adsorbed gallium nitrate antibacterial agent solution prepared in Example 1 was 28 mm, and there was no obvious antibacterial zone for 0.1% penicillin. The results show that the carbon black adsorbed gallium nitrate antibacterial agent prepared in Example 1 does have a good killing effect on Escherichia coli, Staphylococcus aureus, and EM bacteria, and the effect of anti-EM bacteria is more significant than that of anti-Escherichia coli and Staphylococcus aureus (when the antibacterial effect of the antibacterial agent prepared in Example 1 of the present invention is equivalent to the antibacterial effect of the above-mentioned antibacterial effect without the shaking table experiment, and the shaking table antibacterial experiment is continuously carried out, and it is found that the antibacterial time of the antibacterial agent prepared in Example 1 of the present invention on EM bacteria can reach more than 180 days).

[0093] Example 2

[0094] Gallium nitrate as an antimicrobial agent.

[0095] Results: In the anti-EM bacteria experiment, the diameter of the antibacterial zone produced by the 0.1% antibacterial agent solution prepared in this example was 1.9 mm. The same shaking table antibacterial experiment as in Example 1 was carried out. The results showed that the antibacterial time could only last for 8 hours, which was much shorter than the antibacterial time of more than 180 days of the carbon black adsorbed gallium nitrate antibacterial agent prepared in Example 1.

[0096] The embodiments described above are only descriptions of the preferred modes of the present invention, and are not intended to limit the scope of the present invention. Without departing from the design spirit of the present invention, various modifications and improvements made to the technical solutions of the present invention by ordinary technicians in this field should all fall within the protection scope determined by the claims of the present invention.

Claims

1. An EM bacteria antibacterial agent, characterized in that: It contains carbon black adsorbed gallium nitrate antimicrobial agent; The carbon black adsorbed gallium nitrate antibacterial agent uses carbon black as a carrier to load gallium nitrate; the mass ratio of the gallium nitrate to the carbon black is 1:5-100; The method for preparing the carbon black adsorbed gallium nitrate antibacterial agent comprises the following steps: Gallium nitrate and carbon black are added into water and mixed, and then heated, filtered and dried to obtain the carbon black adsorbed gallium nitrate antibacterial agent; Before adding the carbon black to water, it is first soaked in acid, then washed to neutrality, and the water is dried; The mass volume ratio of the carbon black to the water is 50 mg: 2-10 mL; The heating is specifically heating at 50° C. for 3-5 hours.

2. The EM bacteria antibacterial agent according to claim 1, characterized in that: The mixing specifically includes vortexing for 5 minutes and then ultrasonicating for 10 minutes.

3. The EM bacteria antibacterial agent according to claim 1, characterized in that: The drying is specifically performed at 40-60° C. for 6-10 hours.

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