CN112296352B - Preparation method for quickly etching gold and silver nanocages by using sodium citrate in cooperation with hydrogen peroxide - Google Patents
Preparation method for quickly etching gold and silver nanocages by using sodium citrate in cooperation with hydrogen peroxide Download PDFInfo
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Abstract
The invention discloses a preparation method for quickly etching gold and silver nanocages by using sodium citrate in cooperation with hydrogen peroxide, which comprises the following steps: (1) preparing a gold and silver nanocage: taking a polyvinylpyrrolidone aqueous solution, adding a silver nano cubic solution in a water bath environment, stirring, dropwise adding a chloroauric acid aqueous solution, stopping dropwise adding when the solution becomes purple, cooling a reaction liquid to room temperature, adding excessive sodium chloride, fully stirring, collecting a supernatant, washing with an ethanol aqueous solution, and fixing the volume of the supernatant with ethanol ultrapure water; (2) preparing an antibacterial gold and silver nano material: and (2) adding the gold and silver nanocages prepared in the step (1) into a sodium citrate solution, uniformly mixing, and then adding hydrogen peroxide. Under the action of sodium citrate, polyvinylpyrrolidone molecules on the surfaces of the gold and silver nanocages can be replaced, and then hydrogen peroxide is introduced, the high-load silver particles in the gold and silver nanocages can be quickly released, so that a remarkable sterilization effect is shown.
Description
Technical Field
The invention relates to a preparation method of an antibacterial nano material, in particular to a preparation method for quickly etching a gold and silver nano cage by using sodium citrate in cooperation with hydrogen peroxide.
Background
The gold and silver nanocages as a good nano-carrier are widely applied to various fields, particularly in cancer treatment and infection treatment. The gold nano-particles can be stabilized by coating the surfaces of the silver nano-particles with a layer of gold material, however, the release of silver ions is inhibited, and the sterilization effect is reduced.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to provide a preparation method for quickly etching a gold and silver nanocage by using sodium citrate and hydrogen peroxide, which can promote quick release of silver ions and enhance the sterilization effect.
The technical scheme is as follows: the invention provides a preparation method for quickly etching gold and silver nanocages by using sodium citrate in cooperation with hydrogen peroxide, which comprises the following steps:
(1) preparing a gold and silver nanocage: taking a polyvinylpyrrolidone aqueous solution, adding a silver nano cubic solution in a water bath environment, stirring, dropwise adding a chloroauric acid aqueous solution, stopping dropwise adding when the solution becomes purple, cooling a reaction liquid to room temperature, adding excessive sodium chloride, fully stirring, collecting a supernatant, washing with an ethanol aqueous solution, and performing constant volume on the supernatant by using ethanol ultrapure water;
(2) preparing an antibacterial gold and silver nano material: and (2) adding the gold and silver nanocages prepared in the step (1) into a sodium citrate solution, uniformly mixing, and then adding hydrogen peroxide.
Further, the preparation method of the silver nano cube comprises the following steps:
(1) respectively dissolving silver nitrate, sodium hydrosulfide and polyvinylpyrrolidone in ethylene glycol, and freezing the silver nitrate solution and the sodium hydrosulfide solution for later use after the dissolution is finished;
(2) heating the ethylene glycol solution, stirring, introducing nitrogen, sequentially adding the polyvinylpyrrolidone solution and the sodium hydrosulfide solution, stopping introducing the nitrogen, adding the silver acid solution, continuing heating and stirring, cooling when the color of the solution is changed from wine red to yellow green, and stopping reaction;
(3) mixing the obtained product with acetone of the same volume, centrifuging, removing supernatant, washing with ethanol water solution, ultrasonic dissolving for precipitation, metering volume, packaging, and keeping away from light.
Further, the grain size of the silver nanocages in the step (1) is 30-100nm, and the ultraviolet and visible light absorption peak is 480-550 nm.
Further, the air conditioner is provided with a fan,the concentration of the silver nanocages in the step (2) is 5-100 mug mL-1。
Further, the concentration of the gold and silver nanocages is 32 mug mL-1。
Further, the concentration of the sodium citrate solution in the step (2) is 100-1000 mM.
Further, the concentration of the sodium citrate solution is 500 mM.
Further, the concentration of hydrogen peroxide in the step (2) is 10-100 mM.
Further, the concentration of the hydrogen peroxide is 100 mM.
Has the advantages that: the gold-silver nano material particles formed by coating the gold layer on the surfaces of the silver nano cubic blocks have good stability and are convenient to store for a long time. Under the action of sodium citrate, polyvinylpyrrolidone molecules on the surfaces of the gold and silver nanocages can be replaced, and then hydrogen peroxide is introduced, the high-load silver particles in the gold and silver nanocages can be quickly released, so that a remarkable sterilization effect is shown.
Drawings
FIG. 1 shows the silver release measured after processing a gold and silver nanocage for 2h by different strategies;
FIG. 2 is an evaluation of the bacteriostatic effect of the gold and silver nanocages etched by the sodium citrate in cooperation with the hydrogen peroxide on Escherichia coli and Staphylococcus aureus.
Detailed Description
Silver nitrate, ethylene glycol, sodium hydrosulfide, sodium citrate, hydrogen peroxide, polyvinylpyrrolidone (Kr ═ 40000) used in this example were purchased from aladdin corporation, chloroauric acid and other reagents were purchased from chemical reagents ltd, a pharmaceutical group of shanghai, and deionized water was manufactured by Milli-Q integrated pure water system of milliore corporation.
Example 1: the preparation method of the material comprises the following steps:
(1) preparing a template silver nano cube of a gold and silver nano cage: 0.192g of silver nitrate, 0.11g of sodium hydrosulfide and 0.1g of polyvinylpyrrolidone were weighed out and dissolved in 4mL of ethylene glycol, 5mL of ethylene glycol and 5mL of ethylene glycol, respectively. After the dissolution is finished, immediately putting the silver nitrate solution and the sodium hydrosulfide solution into a temperature of minus 20 ℃ for freezingAnd (5) a little for half an hour for standby. Heating the ethylene glycol solution to 150 deg.C in an oil bath, introducing nitrogen gas (100mL min) while heating-1) While stirring with magneton at 1000 rpm-1After 30min, 2.5mL of polyvinylpyrrolidone solution and 120ul of sodium hydrosulfide solution were added successively. And continuously heating and stirring. After 30min, the nitrogen valve was closed, the nitrogen-filled catheter was pulled out, and 850ul of silver nitrate solution was slowly added. And (3) continuing heating and stirring, immediately putting the whole reaction flask into a beaker filled with tap water to cool when the color of the solution is observed to change from wine red to yellow green, and stopping the reaction. Cooling to room temperature, mixing the obtained silver nano cubic block with acetone of equal volume, and cooling at room temperature for 6000r min-1And centrifuging for 30min at the rotating speed of (1). Discarding supernatant, adding 20mL ethanol water solution with volume ratio of 1: 1, ultrasonic treating to dissolve precipitate completely, and repeating at 8000r min-1Centrifuge for 30 min. Thus, the solution was repeatedly washed with an ethanol aqueous solution 3 times, and finally the volume of the solution was adjusted to 6mL with ethanol ultrapure water, and the solution was dispensed into 6 tubes of 2mL EP, each tube containing 1mL, and kept at 4 ℃ in the dark for use.
(2) Preparing a gold and silver nanocage: 0.1g of polyvinylpyrrolidone was weighed out and dissolved in 50mL of ultrapure water. Taking 10mL of polyvinylpyrrolidone water solution under the water bath environment of 80 ℃, adding 1mL of prepared silver nano cubic block solution, and stirring by using magnetons at the same time, wherein the rotating speed is 8000r min-1. Slowly dropwise adding 1mM chloroauric acid aqueous solution into the mixture at the dropping speed of 0.3mL-1. When the solution is observed to be purple, the dripping is stopped. And (3) placing the reaction device in a normal-temperature water bath, cooling to room temperature, adding excessive sodium chloride, fully stirring, removing insoluble substances, and collecting supernatant. Washing for three times by the same washing method as the above (1), and finally fixing the volume to 1mL, and keeping away from light at 4 ℃ for later use.
Example 2: sodium citrate induced hydrogen peroxide rapid etching gold and silver nano cage to release silver ions
Sodium citrate solution with concentration of 0.5M and 100mM hydrogen peroxide solution are prepared by using ultrapure water as a solvent for standby. The gold and silver nanocages were diluted with deionized water to 32. mu.g/mL. Mixing the three materials according to the volume ratio of 1: 2. And then separating the mixed solution for 2 hours by using an ultrafiltration tube with the molecular weight cutoff of 10kDa, centrifuging at the speed of 5000 rpm for 5 minutes, and taking the lower layer part by using an inductively coupled plasma mass spectrometry to measure the content of silver in the lower layer part. As can be seen from the figure, neither pure hydrogen peroxide nor sodium citrate can promote the rapid release of silver ions, a small amount of citric acid is doped in the sodium citrate to also hinder the release of the silver ions, and the silver ions can be rapidly released only by the simultaneous action of the sodium citrate and the hydrogen peroxide.
Example 3: silver release condition measured after processing gold and silver nanocages for 2h by different strategies
Mixing gold and silver nanocages with different substances respectively, testing the silver release condition, and grouping (including adding sequence) as follows:
1, a gold and silver nano cage; 2, adding hydrogen peroxide into the gold and silver nanocages; 3, adding citric acid into the gold and silver nano cage; 4, gold and silver nanocages and sodium citrate; 5, gold and silver nanocages, hydrogen peroxide and sodium citrate; 6 gold and silver nanocages, hydrogen peroxide and sodium citrate (34: 1); 7, gold and silver nanocages, hydrogen peroxide and sodium citrate (6: 1); 8, gold and silver nanocages, hydrogen peroxide and citric acid; 9 gold and silver nanocages, hydrogen peroxide and sodium hydroxide; 10 gold and silver nanocages, sodium citrate and hydrogen peroxide.
From the results of the graphs, the concentration of the silver ions released by the nanocages composed of the gold and silver nanocages, hydrogen peroxide and sodium citrate is generally higher than that released by other groups, wherein the concentration of the silver ions released by 5 groups is the highest.
Example 4: evaluation of bacteriostatic effect of sodium citrate induced hydrogen peroxide on drug-resistant staphylococcus aureus by quickly etching gold and silver nanocages with silver ions released by hydrogen peroxide
The gold and silver nanocages, the sodium citrate and the hydrogen peroxide which are in the same proportion in the embodiment 2 are mixed with the drug-resistant staphylococcus aureus. Wherein the concentration of the gold and silver nanocages is 40 mug/mL, the volume is 25 mug L, the concentration of sodium citrate is 0.5M, the volume is 25 mug L, the concentration of hydrogen peroxide is 100mM, the volume is 25uL, and the OD of bacteria liquid is6000.4, volume 25 μ L. In 6h, 10uL of the mixed solution was added dropwise to 90uL of the bacterial culture solution. After 12 hours, OD was measured by a microplate reader600The antibacterial effect is presumed. As can be seen from fig. 2, only hydrogen peroxide was added to the other control group 1; 2 adding sodium citrate only; 3, only adding a gold and silver nanocage; 4, adding hydrogen peroxide and sodium citrate; 5 adding hydrogen peroxide anda gold and silver nanocage; 6 adding gold and silver nanocages and sodium citrate; 7 adding gold and silver nanocages, sodium citrate and hydrogen peroxide; 8 blank control), the sodium citrate and the hydrogen peroxide can synergistically enhance the sterilization effect of the gold and silver nanocages.
Claims (9)
1. A preparation method for quickly etching gold and silver nanocages by using sodium citrate in cooperation with hydrogen peroxide is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a gold and silver nanocage: taking a polyvinylpyrrolidone aqueous solution, adding a silver nano cubic solution in a water bath environment, stirring, dropwise adding a chloroauric acid aqueous solution, stopping dropwise adding when the solution becomes purple, cooling a reaction liquid to room temperature, adding excessive sodium chloride, fully stirring, collecting a supernatant, washing with an ethanol aqueous solution, and fixing the volume of the supernatant with ethanol ultrapure water;
(2) preparing an antibacterial gold and silver nano material: adding the gold and silver nanocages prepared in the step (1) into a sodium citrate solution, uniformly mixing, and then adding hydrogen peroxide;
the concentration of the hydrogen peroxide in the step (2) is 10-100 mM.
2. The preparation method of the sodium citrate and hydrogen peroxide cooperated for rapidly etching the gold and silver nanocages according to claim 1 is characterized in that: the preparation method of the silver nano cube comprises the following steps:
(1) respectively dissolving silver nitrate, sodium hydrosulfide and polyvinylpyrrolidone in ethylene glycol, and freezing the silver nitrate solution and the sodium hydrosulfide solution for later use after the dissolution is finished;
(2) heating the ethylene glycol solution, stirring, introducing nitrogen, sequentially adding the polyvinylpyrrolidone solution and the sodium hydrosulfide solution, stopping introducing the nitrogen, adding the silver acid solution, continuing heating and stirring, cooling when the color of the solution is changed from wine red to yellow green, and stopping reaction;
(3) mixing the obtained product with acetone with the same volume, centrifuging, discarding supernatant, adding ethanol water solution for washing, ultrasonically dissolving precipitate, fixing volume, packaging, and keeping away from light for use.
3. The preparation method of the sodium citrate and hydrogen peroxide cooperated for rapidly etching the gold and silver nanocages according to claim 1 is characterized in that: the grain diameter of the silver nanocages in the step (1) is 30-100nm, and the ultraviolet visible light absorption peak is 480-550 nm.
4. The preparation method of the sodium citrate and hydrogen peroxide cooperated for rapidly etching the gold and silver nanocages according to claim 1 is characterized in that: the concentration of the silver nanocages in the step (2) is 5-100 mug mL-1。
5. The preparation method of the sodium citrate cooperated with hydrogen peroxide for rapidly etching the gold and silver nanocages according to claim 4 is characterized in that: the concentration of the gold and silver nanocages is 32 mug mL-1。
6. The preparation method of the sodium citrate and hydrogen peroxide cooperated for rapidly etching the gold and silver nanocages according to claim 1 is characterized in that: the concentration of the sodium citrate solution in the step (2) is 100-1000 mM.
7. The preparation method of the sodium citrate and hydrogen peroxide cooperated for rapidly etching the gold and silver nanocages according to claim 6 is characterized in that: the concentration of the sodium citrate solution is 500 mM.
8. The preparation method of the sodium citrate and hydrogen peroxide cooperated for rapidly etching the gold and silver nanocages according to claim 1 is characterized in that: the concentration of the hydrogen peroxide is 100 mM.
9. The preparation method of the sodium citrate and hydrogen peroxide cooperated for rapidly etching the gold and silver nanocages according to claim 1 is characterized in that: the bacteria are Escherichia coli or Staphylococcus aureus.
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| KR101722992B1 (en) * | 2015-05-18 | 2017-04-04 | 국방과학연구소 | Gold nanofluids, silver nanofluids and production methods thereof |
| CN106563812B (en) * | 2016-10-26 | 2018-04-24 | 东南大学 | A kind of method of light triggering synthesizing superfine nano silver wire in aqueous solution |
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| CN110693904B (en) * | 2019-10-28 | 2021-06-25 | 东南大学 | Preparation method of cysteamine cooperated gold and silver nano material |
| CN111748608B (en) * | 2020-05-25 | 2023-01-31 | 南京邮电大学 | Nano cage probe, application thereof and nucleic acid detection method |
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