CN114177198A - Nano-gold antibacterial agent and preparation method and application thereof - Google Patents

Nano-gold antibacterial agent and preparation method and application thereof Download PDF

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CN114177198A
CN114177198A CN202111277161.1A CN202111277161A CN114177198A CN 114177198 A CN114177198 A CN 114177198A CN 202111277161 A CN202111277161 A CN 202111277161A CN 114177198 A CN114177198 A CN 114177198A
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郑文富
冯超
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GBA National Institute for Nanotechnology Innovation
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Abstract

The invention discloses a nanogold antibacterial agent, and a preparation method and application thereof, and belongs to the technical field of antibacterial materials. The preparation method of the nano gold antibacterial agent comprises the following steps: s1, mixing a chloroauric acid solution with a sodium citrate solution and/or a sodium borohydride solution to obtain a mixed solution A; s2, continuously adding ethanol or ethylene glycol solution into the mixed solution A to obtain a mixed solution B; s3, adding a cationic surfactant into the mixed solution B to obtain a mixed solution C; and S4, adding a sulfydryl micromolecule reagent into the mixed solution C, and reacting in an inert gas atmosphere to obtain the nanogold antibacterial agent. The nano-gold antibacterial agent with excellent antibacterial effect is prepared by combining a specific cationic surfactant with a sulfhydryl micromolecule reagent for modification, has excellent antibacterial effect on gram-positive bacteria and gram-negative bacteria, and is effectively used for object surface bacteriostasis, treatment of burns, scalds, various wound infections and other applications.

Description

Nano-gold antibacterial agent and preparation method and application thereof
Technical Field
The invention relates to the technical field of antibacterial materials, and particularly relates to a nanogold antibacterial agent and a preparation method and application thereof.
Background
With the widespread use of antibacterial drugs, the treatment of infectious diseases faces new challenges, and bacteria develop resistance to antibiotics. The problem of bacterial resistance is exacerbated by the continued use of antibiotics. On one hand, the drug-resistant bacteria can cause various antibiotic drugs to lose the treatment effect, and the growth and the reproduction process of the bacteria are difficult to control; on the other hand, the health of human body is seriously harmed, and even the living environment of human is threatened. In recent years, reports have shown that overuse and abuse of antibiotics has led to an increasing trend of bacterial resistance. Multiple-resistant and widely resistant strains have seriously threatened effective treatment of clinical antibacterial drugs. Bacterial resistance to antibiotics has become a serious global problem. Therefore, it is of great importance to develop a drug which can effectively inhibit drug-resistant bacteria and is used for replacing and relieving the crisis of antibiotics.
CN110292652A discloses a gold nanoparticle activated by mercaptophenylboronic acid, a preparation method and an application thereof, wherein the gold nanoparticle activated by the mercaptophenylboronic acid has a certain antibacterial effect on sensitive strains and multi-drug resistant strains of gram-positive bacteria, but the antibacterial effect is poor, the gold nanoparticle can only aim at the gram-positive bacteria, and the antibacterial effect on the gram-negative bacteria is poor.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings that the existing gold nano antibacterial agent has poor antibacterial effect and cannot simultaneously have antibacterial effect on gram-positive bacteria and gram-negative bacteria, and provides a preparation method of a nano gold antibacterial agent.
Another object of the present invention is to provide a nanogold antibacterial agent.
The invention also aims to provide application of the nano-gold antibacterial agent in preparation of the surface antibacterial agent.
The above purpose of the invention is realized by the following technical scheme:
compared with the prior art, the invention has the beneficial effects that:
a preparation method of a nanogold antibacterial agent comprises the following steps:
s1, mixing a chloroauric acid solution with a sodium citrate solution and/or a sodium borohydride solution to obtain a mixed solution A;
s2, continuously adding ethanol or ethylene glycol solution into the mixed solution A to obtain a mixed solution B;
s3, adding a cationic surfactant into the mixed solution B to obtain a mixed solution C;
s4, adding a sulfydryl micromolecule reagent into the mixed solution C, reacting in an inert gas atmosphere to obtain a nanogold antibacterial agent,
wherein the addition volume of the cationic surfactant in the S3 is 0.2-3.0% of the volume of the mixed solution B;
the adding amount of the sulfydryl small molecular reagent in the S4 is 0.2-2.5% of the volume of the mixed solution C, the reaction temperature is 2-60 ℃, and the reaction time is 2-10 hours.
Among them, it should be noted that:
in the preparation method of the nano-gold antibacterial agent, the steps from S3 to S3 are to form stable nano-gold particles and control the particle size of the nano-gold antibacterial agent to be 3-30 nm, and finally, a sulfydryl small molecule reagent is added to modify the nano-gold particles through the step of S4, so that the nano-gold particles are modified, and the antibacterial performance is improved. If the sulfydryl micromolecule reagent and other reaction reagents are added together, the complexity of a reaction system is increased, on one hand, the nano-gold particles with stable size cannot be formed, on the other hand, the effectiveness of the sulfydryl micromolecule modified nano-gold particles is also reduced, and therefore the antibacterial performance is not favorably improved.
The surfactant is a cationic surfactant, and compared with a non-ionic surfactant and an anionic surfactant, the cationic surfactant can be selected to effectively improve the surface tension of a system, enhance the probability of modifying the gold nanoparticles by the sulfydryl small molecule reagent and improve the overall antibacterial performance.
The addition amount of the sulfydryl small molecular reagent not only needs to consider the modification antibacterial effect, but also needs to consider the stability of the whole system, and excessive or too little addition amount of the sulfydryl small molecular reagent can influence the stability of the system, influence the reaction effect and is not beneficial to improving the antibacterial effect of the nanogold antibacterial agent.
Preferably, the reaction temperature in S4 is 2-10 ℃, and the reaction time is 2-8 h.
Preferably, the cationic surfactant is one or two of dimethyl diallyl ammonium chloride, stearamidopropyl dimethylamine, benzyl triethyl ammonium chloride, hexadecyl trimethyl ammonium bromide, octadecyl dimethyl benzyl ammonium chloride, behenamidopropyl dimethylamine and hydroxyethyl lauryl dimethyl ammonium chloride.
The cationic surfactant is more suitable for the reaction system of the invention and is more favorable for maintaining the uniform stability of the reaction system.
In the first production method, preferably, the chloroauric acid solution is mixed with the sodium borohydride solution in S1 to obtain a mixed solution a,
the mercapto small molecule reagent added in S4 is one or more of 4-mercaptobenzoic acid, 4- (methylthio) benzoic acid, 3-mercapto-2-pentanone, 2-mercaptonicotinic acid and 3-mercaptopropionic acid.
Among them, it should be noted that:
the mass concentration of the chloroauric acid solution in the S1 may be preferably 10 to 35%, and more preferably 15 to 25%.
In order to control the generation of the nano gold particles and improve the size controllability of the nano gold particles, the mass concentration of the sodium borohydride reducing agent can be preferably 2-12%, and further preferably 2-8%.
The dosage of the ethanol or the ethylene glycol in the S2 is preferably 6-20% of the total volume fraction of the solution, and more preferably 6-12%.
And in the step S4, the reaction is carried out in an inert gas atmosphere, the inert gas can be nitrogen, the nitrogen speed is 35mL/min, the stirring reaction is carried out, the stirring speed is controlled to be 50-300 rpm/min, and the stirring speed is further preferably 50-200 rpm/min.
The nitrogen protection is to ensure the stability of the reaction system and prevent oxygen from influencing the reaction. The uniformity of the reaction system can be ensured by controlling the specific stirring speed.
Preferably, the cationic surfactant is one or two of dimethyl diallyl ammonium chloride, stearamidopropyl dimethylamine, benzyl triethyl ammonium chloride and hexadecyl trimethyl ammonium bromide.
Preferably, the volume of the cationic surfactant added is 0.6-2.2% of the volume of the mixed solution B.
Further preferably, the addition amount of the thiol small molecule reagent in the S4 is 0.4-1.5% of the volume of the mixed solution C.
In a specific embodiment, the addition amount of the thiol small molecule reagent in S4 may be 0.4% of the volume of the mixed solution C;
or the adding amount of the sulfydryl small molecular reagent in the S4 is 0.8 percent of the volume of the mixed solution C;
or the adding amount of the sulfydryl small molecular reagent in the S4 is 1.2 percent of the volume of the mixed solution C;
or the adding amount of the sulfydryl small molecule reagent in S4 is 1.5 percent of the volume of the mixed solution C.
In the second preparation method, preferably, the chloroauric acid solution is mixed with the sodium citrate and sodium borohydride solution in S1 to obtain a mixed solution a,
the sulfhydryl micromolecule reagent added in S4 is one or more of 6-hexanedithiol, 1, 2-butanedithiol, 4-mercaptophenylboronic acid, 3-mercaptopropionic acid and dithiothreitol.
Among them, it should be noted that:
in S1, the chloroauric acid solution, the sodium citrate solution and the sodium borohydride solution are mixed to obtain a mixed solution A, and the specific operation is as follows:
mixing the chloroauric acid solution and the sodium citrate solution to obtain a mixed solution, carrying out ice bath, introducing inert gas (such as nitrogen), adding the sodium borohydride solution, and mixing to obtain a mixed solution A.
The mass concentration of the chloroauric acid solution can be preferably 1-20%, the further preferable concentration is 5-10%, the mass concentration of the sodium citrate solution can be preferably 1-30%, the further preferable concentration is 5-15%, and the volume ratio of the chloroauric acid solution to the sodium citrate solution can be preferably 5-10: 1.
in order to better reduce gold to form gold nanoparticles and improve the size controllability of the gold nanoparticles, the mass concentration of the sodium borohydride reducing agent can be preferably 10-25%, and further preferably 8-16%.
The dosage of the ethanol or the ethylene glycol in the S2 is preferably 5-30% of the total volume fraction of the solution, and more preferably 8-15%.
And in the S4, the reaction is carried out in an inert gas atmosphere, the inert gas can be nitrogen, the nitrogen speed is 30mL/min, the stirring reaction is carried out, the stirring speed is controlled to be 80-1000 rpm/min, and the stirring speed is further preferably 100-300 rpm/min.
The nitrogen protection is to ensure the stability of the reaction system and prevent oxygen from influencing the reaction. The uniformity of the reaction system can be ensured by controlling the specific stirring speed.
Further preferably, the mercapto small molecule reagent added in S4 is 4-mercaptophenylboronic acid and 3-mercaptopropionic acid.
Further preferably, the addition amount of the thiol small molecule reagent in the S4 is 0.2-1.2% of the volume of the mixed solution C.
In a specific embodiment, the adding amount of the sulfydryl small molecule reagent in the S4 is 0.2% of the volume of the mixed solution C;
or the adding amount of the sulfydryl small molecular reagent in the S4 is 0.5 percent of the volume of the mixed solution C;
or the adding amount of the sulfydryl small molecular reagent in the S4 is 0.7 percent of the volume of the mixed solution C;
or the adding amount of the sulfydryl small molecular reagent in the S4 is 0.9 percent of the volume of the mixed solution C;
or the adding amount of the sulfydryl small molecule reagent in S4 is 1.2 percent of the volume of the mixed solution C.
Preferably, the cationic surfactant is one or two of octadecyl dimethyl benzyl ammonium chloride, hexadecyl trimethyl ammonium bromide, behenamidopropyl dimethylamine and hydroxyethyl lauryl dimethyl ammonium chloride, and further preferably one or two of hydroxyethyl lauryl dimethyl ammonium chloride and hexadecyl trimethyl ammonium bromide.
Preferably, the volume of the cationic surfactant added is 0.5-1.6% of the volume of the mixed solution B.
The nano-gold antibacterial agent prepared by the preparation method of the nano-gold antibacterial agent is also within the protection range of the invention, and the particle size of the nano-gold antibacterial agent is 3-30 nm.
The grain size of the nano gold antibacterial agent is controlled to ensure that the nano gold has stable antibacterial performance, and the antibacterial performance is adversely affected when the grain size of the nano gold antibacterial agent is too large or too small.
Preferably, the particle size of the nano-gold antibacterial agent prepared by the first preparation method is 3-20 nm, and preferably 10-15 nm.
Preferably, the particle size of the nano-gold antibacterial agent prepared by the second preparation method is 5-10 nm.
The invention also specifically protects the application of the nano-gold antibacterial agent in preparing the surface antibacterial agent.
The nanogold antibacterial agent disclosed by the invention not only can be used for preparing a nanogold antibacterial agent with a good antibacterial effect only on gram-positive bacteria such as staphylococcus aureus, but also can be used for preparing a nanogold antibacterial agent with an excellent antibacterial effect on gram-positive bacteria and gram-negative bacteria such as staphylococcus aureus and escherichia coli, can be widely applied to preparing a surface antibacterial agent, can be applied to antibacterial drug treatment of specific bacteria groups, and can also be applied to preparing antibacterial preparations for treating burns, scalds, various wound infections and the like.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a preparation method of a nanogold antibacterial agent, which is characterized in that sodium citrate and sodium borohydride are used as a reducing agent and a control agent, and a specific cationic surfactant is combined with a sulfydryl micromolecule reagent for modification to prepare the nanogold antibacterial agent with excellent antibacterial effect, and the preparation process is simple.
The nanogold antibacterial agent disclosed by the invention not only has an excellent antibacterial effect on gram-positive bacteria, but also has an excellent antibacterial effect on gram-positive bacteria and gram-negative bacteria, performs selective narrow-spectrum or broad-spectrum antibacterial, and can be effectively applied to object surface bacteriostasis and treatment of burns, scalds, various wound infections and the like.
Drawings
FIG. 1 is a transmission electron microscope photograph of the nanogold antibacterial agent of example 1.
Fig. 2 is a transmission electron microscope image of the nanogold antibacterial agent of example 2.
FIG. 3 is a transmission electron microscope image of the nanogold antimicrobial of example 3.
Fig. 4 is a transmission electron microscope image of the nanogold antibacterial agent of example 4.
Fig. 5 is a transmission electron microscope image of the nanogold antibacterial agent of example 5.
Fig. 6 is a transmission electron microscope image of the nanogold antibacterial agent of example 6.
Fig. 7 is a transmission electron microscope image of the nanogold antibacterial agent of example 7.
Fig. 8 is a transmission electron microscope image of the nanogold antibacterial agent of example 8.
Fig. 9 is a transmission electron microscope photograph of the nanogold antibacterial agent of example 9.
Detailed Description
The present invention will be further described with reference to specific embodiments, but the present invention is not limited to the examples in any way. The starting reagents employed in the examples of the present invention are, unless otherwise specified, those that are conventionally purchased.
Example 1
A preparation method of a nanogold antibacterial agent comprises the following steps:
s1, adding a 2% sodium borohydride solution into a chloroauric acid solution with the mass concentration of 12% to obtain a mixed solution A, and introducing nitrogen;
s2, continuously adding an ethylene glycol solution with the volume fraction of 6% into the mixed solution A to obtain a mixed solution B;
s3, adding 0.6% of dimethyl diallyl ammonium chloride with the total volume fraction of the solution into the mixed solution B to obtain a mixed solution C;
s4, adding 0.4% of 4-mercaptobenzoic acid in the total volume fraction of the solution into the mixed solution C, and reacting for 3 hours at the reaction temperature of 2 ℃, the stirring speed of 50rpm/min and the nitrogen speed of 35mL/min in a nitrogen atmosphere to obtain the nanogold antibacterial agent.
Example 2
A preparation method of a nanogold antibacterial agent comprises the following steps:
s1, adding a sodium borohydride solution with the mass concentration of 4% into a chloroauric acid solution with the mass concentration of 15% to obtain a mixed solution A, and introducing nitrogen;
s2, continuously adding an ethylene glycol solution with the volume fraction of 8% into the mixed solution A to obtain a mixed solution B;
s3, adding 1.2% of dimethyldiallylammonium chloride in the mixed solution B according to the total volume fraction of the solution to obtain a mixed solution C;
s4, adding 1.5% of 3-mercapto-2-pentanone in the total volume fraction of the solution into the mixed solution C, and reacting for 5 hours at the reaction temperature of 4 ℃, the stirring speed of 100rpm/min and the nitrogen speed of 35mL/min in a nitrogen atmosphere to obtain the nanogold antibacterial agent.
Example 3
A preparation method of a nanogold antibacterial agent comprises the following steps:
s1, adding a sodium borohydride solution with the mass concentration of 6% into a chloroauric acid solution with the mass concentration of 20% to obtain a mixed solution A, and introducing nitrogen;
s2, continuously adding an ethylene glycol solution with the volume fraction of 10% into the mixed solution A to obtain a mixed solution B;
s3, adding 1.7% of hexadecyl trimethyl ammonium bromide with the total volume fraction of the solution into the mixed solution B to obtain a mixed solution C;
s4, adding 1.2% of 3-mercaptopropionic acid of the total volume fraction of the solution into the mixed solution C, and reacting for 6 hours at the reaction temperature of 8 ℃, the stirring speed of 200rpm/min and the nitrogen speed of 35mL/min in a nitrogen atmosphere to obtain the nanogold antibacterial agent.
Example 4
A preparation method of a nanogold antibacterial agent comprises the following steps:
s1, adding a sodium borohydride solution with the mass concentration of 8% into a chloroauric acid solution with the mass concentration of 25% to obtain a mixed solution A, and introducing nitrogen;
s2, continuously adding an ethylene glycol solution with the volume fraction of 12% into the mixed solution A to obtain a mixed solution B;
s3, adding 2.2% of methyldiallylammonium chloride in the total volume fraction of the solution into the mixed solution B to obtain a mixed solution C;
s4, adding 0.8 percent of 2-mercaptonicotinic acid of the total volume fraction of the solution into the mixed solution C, and reacting for 8 hours at the reaction temperature of 10 ℃, the stirring speed of 200rpm/min and the nitrogen speed of 35mL/min in the nitrogen atmosphere to obtain the nanogold antibacterial agent.
Example 5
A preparation method of a nanogold antibacterial agent comprises the following steps:
s1, mixing a chloroauric acid solution with the mass concentration of 5% and a sodium citrate solution with the mass concentration of 5% according to the volume ratio of 5:1, carrying out ice bath, introducing nitrogen, and then adding a sodium borohydride solution with the mass concentration of 8% to obtain a mixed solution A;
s2, continuously adding an ethylene glycol solution with the volume fraction of 8% into the mixed solution A to obtain a mixed solution B;
s3, adding 0.5% of hexadecyl trimethyl ammonium bromide with the total volume fraction of the solution into the mixed solution B to obtain a mixed solution C;
s4, adding 0.2% of 1, 6-hexanedithiol of the total volume fraction of the solution into the mixed solution C, and reacting for 2 hours at the reaction temperature of 10 ℃, the stirring speed of 100rpm/min and the nitrogen speed of 30mL/min in a nitrogen atmosphere to obtain the nanogold antibacterial agent.
Example 6
A preparation method of a nanogold antibacterial agent comprises the following steps:
s1, mixing a chloroauric acid solution with the mass concentration of 7% and a sodium citrate solution with the mass concentration of 9% according to the volume ratio of 7:1, carrying out ice bath, introducing nitrogen, and then adding a sodium borohydride solution with the mass concentration of 10% to obtain a mixed solution A;
s2, continuously adding an ethylene glycol solution with the volume fraction of 10% into the mixed solution A to obtain a mixed solution B;
s3, adding 0.8 percent of hydroxyethyl lauryl dimethyl ammonium chloride in the mixed solution B according to the total volume fraction to obtain a mixed solution C;
s4, adding 0.5 percent of 4-mercaptophenylboronic acid of the total volume fraction of the solution into the mixed solution C, and reacting for 3 hours at the reaction temperature of 15 ℃, the stirring speed of 150rpm/min and the nitrogen speed of 30mL/min in a nitrogen atmosphere to obtain the nanogold antibacterial agent.
Example 7
A preparation method of a nanogold antibacterial agent comprises the following steps:
s1, mixing a chloroauric acid solution with the mass concentration of 9% and a sodium citrate solution with the mass concentration of 12% according to the volume ratio of 9:1, carrying out ice bath, introducing nitrogen, and then adding a sodium borohydride solution with the mass concentration of 14% to obtain a mixed solution A;
s2, continuously adding an ethylene glycol solution with the volume fraction of 10% into the mixed solution A to obtain a mixed solution B;
s3, adding 1.2% of hydroxyethyl lauryl dimethyl ammonium chloride with the total volume fraction of the solution into the mixed solution B to obtain a mixed solution C;
s4, adding 0.7 percent of dithiothreitol of the total volume fraction of the solution into the mixed solution C, and reacting for 4 hours at the reaction temperature of 20 ℃ and the stirring speed of 200rpm/min and the nitrogen speed of 30mL/min in the nitrogen atmosphere to obtain the nano-gold antibacterial agent.
Example 8
A preparation method of a nanogold antibacterial agent comprises the following steps:
s1, mixing a chloroauric acid solution with the mass concentration of 10% and a sodium citrate solution with the mass concentration of 15% according to the volume ratio of 10:1, carrying out ice bath, introducing nitrogen, and then adding a sodium borohydride solution with the mass concentration of 16% to obtain a mixed solution A;
s2, continuously adding an ethylene glycol solution with the volume fraction of 13% into the mixed solution A to obtain a mixed solution B;
s3, adding 1.4% of hexadecyl trimethyl ammonium bromide with the total volume fraction of the solution into the mixed solution B to obtain a mixed solution C;
s4, adding 1, 2-butanedithiol with the total volume fraction of 1.2% of the solution into the mixed solution C, and reacting for 6 hours at the reaction temperature of 30 ℃, the stirring speed of 300rpm/min and the nitrogen speed of 30mL/min in a nitrogen atmosphere to obtain the nanogold antibacterial agent.
Example 9
A preparation method of a nanogold antibacterial agent comprises the following steps:
s1, mixing a chloroauric acid solution with the mass concentration of 6% and a sodium citrate solution with the mass concentration of 10% according to the volume ratio of 9:1, carrying out ice bath, introducing nitrogen, and then adding a sodium borohydride solution with the mass concentration of 12% to obtain a mixed solution A;
s2, continuously adding an ethylene glycol solution with the volume fraction of 10% into the mixed solution A to obtain a mixed solution B;
s3, adding 1.6 percent of hexadecyl trimethyl ammonium bromide with the total volume fraction of the solution into the mixed solution B to obtain a mixed solution C;
s4, adding 0.9% dithiothreitol of the total volume fraction of the solution into the mixed solution C, and reacting for 3 hours at the reaction temperature of 25 ℃ and the stirring speed of 400rpm/min and the nitrogen speed of 30mL/min in a nitrogen atmosphere to obtain the nano-gold antibacterial agent.
Comparative example 1
A preparation method of a nanogold antibacterial agent comprises the following steps:
s1, adding a sodium borohydride solution with the mass concentration of 8% into a chloroauric acid solution with the mass concentration of 25% to obtain a mixed solution A, and introducing nitrogen;
s2, continuously adding an ethylene glycol solution with the volume fraction of 12% into the mixed solution A to obtain a mixed solution B;
s3, adding 2.2% of non-cationic surfactant ammonium chloride with the total volume fraction of the solution into the mixed solution B to obtain a mixed solution C;
s4, adding 1.5 percent of 2-mercaptonicotinic acid of the total volume fraction of the solution into the mixed solution C, and reacting for 8 hours at the reaction temperature of 8 ℃, the stirring speed of 200rpm/min and the nitrogen speed of 35mL/min in a nitrogen atmosphere to obtain the nanogold antibacterial agent.
Comparative example 2
A preparation method of a nanogold antibacterial agent comprises the following steps:
s1, mixing a chloroauric acid solution with the mass concentration of 6% and a sodium citrate solution with the mass concentration of 10% according to the volume ratio of 9:1, carrying out ice bath, introducing nitrogen, and then adding a sodium borohydride solution with the mass concentration of 12% to obtain a mixed solution A;
s2, continuously adding an ethylene glycol solution with the volume fraction of 10% into the mixed solution A to obtain a mixed solution B;
s3, adding 1.6 percent of non-cationic surfactant polyvinylpyrrolidone with the total volume fraction of the solution into the mixed solution B to obtain a mixed solution C;
s4, adding 0.5 percent of dithiothreitol of the total volume fraction of the solution into the mixed solution C, and reacting for 3 hours at the reaction temperature of 25 ℃ and the stirring speed of 400rpm/min and the nitrogen speed of 30mL/min in the nitrogen atmosphere to obtain the nano-gold antibacterial agent.
Result detection
(1) Morphology particle size detection
The shapes and the particle diameters of the nanogold antibacterial agents prepared in the examples 1 to 9 are detected by a transmission electron microscope, and the detection results are shown in figures 1 to 9:
fig. 1 is a transmission electron microscope photograph of the nano-gold antibacterial agent of example 1, and it can be seen from the experimental results shown in fig. 1 that the nano-gold of example 1 has a particle size of 3 to 12nm and is spherical.
Fig. 2 is a transmission electron microscope photograph of the nano-gold antibacterial agent of example 2, and it can be understood from the experimental results shown in fig. 2 that the nano-gold of example 2 has a particle size of 5 to 15nm and is spherical.
Fig. 3 is a transmission electron microscope photograph of the nano-gold antibacterial agent of example 3, and from the experimental results shown in fig. 3, it can be seen that the nano-gold of example 3 has a particle size of 6 to 18nm and is spherical.
Fig. 4 is a transmission electron microscope image of the nano-gold antibacterial agent of example 4, and from the experimental results shown in fig. 4, it can be seen that the nano-gold of example 4 has a particle size of 5-20nm and is spherical.
Fig. 5 is a transmission electron microscope photograph of the nano-gold antibacterial agent of example 5, and from the experimental results shown in fig. 5, it can be seen that the nano-gold of example 5 has a particle size of 5 to 10nm and is spherical.
Fig. 6 is a transmission electron microscope photograph of the nano-gold antibacterial agent of example 6, and from the experimental results shown in fig. 6, it can be seen that the nano-gold of example 6 has a particle size of 3 to 10nm and is spherical.
Fig. 7 is a transmission electron microscope photograph of the nano-gold antibacterial agent of example 7, and from the experimental results shown in fig. 7, it can be seen that the nano-gold of example 7 has a particle size of 5 to 10nm and is spherical.
Fig. 8 is a transmission electron microscope photograph of the nano-gold antibacterial agent of example 8, and from the experimental results shown in fig. 8, it can be seen that the nano-gold of example 8 has a particle size of 5 to 12nm and is spherical.
Fig. 9 is a transmission electron microscope photograph of the nano-gold antibacterial agent of example 9, and from the experimental results shown in fig. 9, it can be seen that the nano-gold of example 9 has a particle size of 5 to 11nm and is spherical.
(2) Detection of antibacterial Properties
Mixing and dissolving nanogold with different concentrations in nutrient broth by adopting an agar dilution method, then inoculating bacteria, and determining the minimum Concentration of the anti (bacteriostatic) bacterial agent for inhibiting the growth of the tested bacteria, namely the minimum bacteriostatic Concentration (MIC) according to the growth or not of the bacteria.
Test strains: staphylococcus aureus ATCC 6538, Escherichia coli 8099 or ATCC 11229.
The test steps are as follows:
(1) the nanogold solution was diluted in distilled water in a double series to test solutions of different concentrations, and 2.5mL of each dilution of the test solution was added to a test tube containing 2.5mL of double-strength nutrient broth.
(3) Taking 0.1mL of the mixture with the bacterial content of about 108The cfu/m L bacterial suspension was inoculated into a test tube of nutrient broth containing nanogold as a test group sample.
(4) Test tubes of nutrient broth without nanogold were inoculated in the same manner as positive control samples.
(5) 2 tubes containing the nutrient broth were used as negative control samples.
(6) And placing the test group sample, the positive control group sample and the negative control group sample in an incubator at 37 ℃, culturing for 48h, and observing the result.
(7) The test bacterial suspension should be subjected to viable bacteria culture counting, and the action concentration should be 5 × 105CFU/mL～5×106CFU/mL。
And (4) judging a result: when the positive control tube has bacteria growth (turbidity) and the negative control tube has bacteria growth (transparency), the active concentration of the test bacterial suspension is 5X 105CFU/mL～5×106And in CFUmL, the concentration of the nanogold corresponding to the highest dilution for sterile growth of the test group is the MIC of the sample to the tested bacteria.
The specific test results are shown in the following tables 1 and 2.
TABLE 1 MIC values (minimum inhibitory concentration) of Staphylococcus aureus of samples of examples 1 to 4 and comparative example 1
Figure BDA0003329866750000111
Figure BDA0003329866750000121
As can be seen from Table 1, the nanogold antibacterial agent has good antibacterial effect on Staphylococcus aureus, the MIC value can reach below 30ppm, while the MIC value of the comparative example is above 300ppm, the antibacterial effect difference is obvious, and obviously, the antibacterial effect of the nanogold antibacterial agent on Staphylococcus aureus cannot be reached.
TABLE 2 MIC values (minimum inhibitory concentration) of Staphylococcus aureus of examples 5 to 9 and comparative example 2
Serial number Escherichia coli (MIC)/ppm Staphylococcus aureus (MIC)/ppm
Example 5 30 15
Example 6 20 10
Example 7 2 1
Example 8 20 10
Example 9 10 5
Comparative example 2 >300 >300
The experimental results in table 2 also show that the nanogold antibacterial agent of the invention has good antibacterial effects on staphylococcus aureus and escherichia coli, the MIC values can reach below 30ppm, the MIC values of the comparative examples are above 300ppm, the antibacterial effect difference is significant, and obviously the antibacterial effect of the nanogold antibacterial agent of the invention cannot be reached.
The staphylococcus aureus is a representative of gram-positive bacteria, the escherichia coli is a representative of gram-negative bacteria, and the nanogold antibacterial agent disclosed by the invention has good antibacterial effects on the staphylococcus aureus and the escherichia coli, so that the nanogold antibacterial agent has broad-spectrum antibacterial property.
Therefore, the preparation method of the nanogold antibacterial agent can be used for preparing one antibacterial agent only having an antibacterial effect on gram-positive bacteria and preparing the other antibacterial agent having an antibacterial effect on both gram-positive bacteria and gram-negative bacteria.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.

Claims (10)

1. A preparation method of a nano-gold antibacterial agent is characterized by comprising the following steps:
s1, mixing a chloroauric acid solution with a sodium citrate solution and/or a sodium borohydride solution to obtain a mixed solution A;
s2, continuously adding ethanol or ethylene glycol solution into the mixed solution A to obtain a mixed solution B;
s3, adding a cationic surfactant into the mixed solution B to obtain a mixed solution C;
s4, adding a sulfydryl micromolecule reagent into the mixed solution C, reacting in an inert gas atmosphere to obtain a nanogold antibacterial agent,
wherein the addition volume of the cationic surfactant in the S3 is 0.2-3.0% of the volume of the mixed solution B;
the adding amount of the sulfydryl small molecular reagent in the S4 is 0.2-2.5% of the volume of the mixed solution C, the reaction temperature is 2-60 ℃, and the reaction time is 2-10 hours.
2. The method for preparing a nanogold antibacterial agent according to claim 1, wherein the reaction temperature in S4 is 2-10 ℃ and the reaction time is 2-8 hours.
3. The method for preparing the nanogold antibacterial agent according to claim 1, wherein the cationic surfactant is one or two of dimethyldiallylammonium chloride, stearamidopropyl dimethylamine, benzyltriethylammonium chloride, hexadecyltrimethylammonium bromide, octadecyldimethylbenzylammonium chloride, behenamidopropyl dimethylamine, and hydroxyethyl lauryl dimethylammonium chloride.
4. The method of preparing nano-gold antibacterial agent according to claim 1, wherein, in S1, chloroauric acid solution is mixed with sodium borohydride solution to obtain mixed solution A,
the mercapto small molecule reagent added in S4 is one or more of 4-mercaptobenzoic acid, 4- (methylthio) benzoic acid, 3-mercapto-2-pentanone, 2-mercaptonicotinic acid and 3-mercaptopropionic acid.
5. The method for preparing the nanogold antibacterial agent according to claim 4, wherein the addition amount of the thiol small-molecule reagent in S4 is 0.4-1.5% of the volume of the mixed solution C.
6. The method of preparing nano-gold antibacterial agent according to claim 1, wherein, in S1, chloroauric acid solution is mixed with sodium citrate and sodium borohydride solution to obtain mixed solution A,
the sulfhydryl micromolecule reagent added in S4 is one or more of 6-hexanedithiol, 1, 2-butanedithiol, 4-mercaptophenylboronic acid, 3-mercaptopropionic acid and dithiothreitol.
7. The method for preparing nano-gold antibacterial agent according to claim 6, wherein the mercapto small molecule reagent added in S4 is 4-mercaptophenylboronic acid and 3-mercaptopropionic acid.
8. The method for preparing the nanogold antibacterial agent according to claim 6, wherein the addition amount of the thiol small-molecule reagent in S4 is 0.2-1.2% of the volume of the mixed solution C.
9. The nanogold antibacterial agent prepared by the preparation method of the nanogold antibacterial agent according to any one of claims 1 to 8 is characterized in that the particle size of the nanogold antibacterial agent is 3 to 30 nm.
10. Use of the nanogold antibacterial agent of claim 9 in the preparation of a surface bacteriostatic agent.
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