CN105817642A - Au/Ag core shell nanomaterial with efficient antibacterial property and preparation method of Au/Ag core shell nanomaterial - Google Patents
Au/Ag core shell nanomaterial with efficient antibacterial property and preparation method of Au/Ag core shell nanomaterial Download PDFInfo
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- CN105817642A CN105817642A CN201610244061.1A CN201610244061A CN105817642A CN 105817642 A CN105817642 A CN 105817642A CN 201610244061 A CN201610244061 A CN 201610244061A CN 105817642 A CN105817642 A CN 105817642A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
Abstract
The invention discloses an Au/Ag core shell nanomaterial with efficient antibacterial property and a preparation method of the Au/Ag core shell nanomaterial, and belongs to the technical field of nanomaterials. The method comprises the following steps: preparing an Au/Ag core shell nanomaterial which takes gold nanoparticles as cores and takes silver nanoparticles as shells by utilizing a nano-silver in-situ growth method; modifying sodium dodecyl sulfate on the surface of the nanomaterial; and preparing to obtain the Au/Ag core shell nanomaterial with the high antibacterial property. Compared with pure gold nanoparticles and silver nanoparticles, the Au/Ag core shell nanomaterial has the advantages that (1) high sterilizing effect on gram-negative bacteria and gram-positive bacteria can be achieved by small concentration only, and the Au/Ag core shell nanomaterial has the broad-spectrum sterilization property; (2) through modification of the sodium dodecyl sulfate, the antibacterial property of the nanomaterial can be improved effectively, and toxicity of the nanomaterial is reduced; and (3) the Au/Ag core shell nanomaterial is good in dispersibility and stable in chemical property, and can be stored for a long time. The nanomaterial has quite wide application prospect.
Description
Technical field
The present invention relates to a kind of Au/Ag core-shell nano material with Efficient antibacterial performance and preparation method thereof, belong to technical field of nano material.
Background technology
Silver nano-grain is the noble metal nanometer material being most widely used at present, owing to having higher surface activity, surface catalysis performance and conductance hot property etc., silver nano-grain is made to be easily absorbing at antimicrobial surface, utilize the silver ion destruction to protein, DNA etc., thus effectively kill the pathogenic microorganism such as antibacterial, fungus, mycoplasma, efficiently and be not likely to produce drug resistance.Due to the antibacterial activity of its wide spectrum, nanometer silver is used widely in daily life and medical and health.But, studies have found that nanometer silver has certain toxicity to mammal at present, nanometer silver is directly entered the organ such as blood and liver by digestive tract after being absorbed, and accumulate in its hetero-organization and organ, when reach a certain amount of after, human body can be produced the toxic reaction such as liver toxicity, nephrotoxicity, neurotoxicity.Therefore, how to obtain green, silver system nontoxic, efficient antibacterial has become the hot issue studied at present.
Summary of the invention
The present invention be directed to the defect that prior art exists, a kind of Au/Ag core-shell nano material with Efficient antibacterial performance and preparation method thereof is provided, the metal material that two kinds different can be incorporated into one on the whole by this material, while having core and shell bi-material advantage concurrently, can the Nomenclature Composition and Structure of Complexes to core Yu shell be controlled obtaining unprecedented physics and chemical property as required.It addition, by core-shell nano material surface modification activities material, the biocidal property of nano material can not only be effectively improved, the biocompatibility of nano material can be improved simultaneously, be substantially reduced the toxicity of nano material.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of Au/Ag core-shell nano material with Efficient antibacterial performance, this material is to be prepared via a method which to obtain:
1) react after gold nano grain solution being mixed with polyvinylpyrrolidonesolution solution, ascorbic acid solution, silver nitrate solution, prepare Au/Ag core shell nanoparticles solution；
2) by step 1) the Au/Ag core shell nanoparticles solution prepared and dodecyl sodium sulfate hybrid reaction, obtain the Au/Ag core-shell nano antibacterial material of SDS functionalization.
The step 1 of technical solution of the present invention) in the particle diameter of gold nano grain be 5～15nm；In the solution of gold nano grain, nanometer gold molar concentration is 5-20nmol/L.
The step 1 of technical solution of the present invention) in the content of PVP be 0.2～1%；The content of ascorbic acid is 100～400mmol/L；The content of silver nitrate is 0.1～0.4mmol/L；Gold nano grain solution is 5～10:2～6:1～3:0.5～2.5 with polyvinylpyrrolidonesolution solution, ascorbic acid solution, the volume ratio of silver nitrate solution.
The step 1 of technical solution of the present invention) in mixing after room temperature lucifuge concussion reaction 2～4h.
The step 2 of technical solution of the present invention) in the volume mass ratio of Au/Ag core shell nanoparticles solution and dodecyl sodium sulfate be 100～500 μ L:1～5mg.
A kind of Au/Ag core-shell nano material preparation method with Efficient antibacterial performance, the method comprises the following steps:
1) react after gold nano grain solution being mixed with polyvinylpyrrolidonesolution solution, ascorbic acid solution, silver nitrate solution, prepare Au/Ag core shell nanoparticles solution；
2) by step 1) the Au/Ag core shell nanoparticles solution prepared and dodecyl sodium sulfate hybrid reaction, obtain the Au/Ag core-shell nano antibacterial material of SDS functionalization.
The step 1 of technical solution of the present invention) in the particle diameter of gold nano grain be 5～15nm；In the solution of gold nano grain, nanometer gold molar concentration is 5-20nmol/L.
The step 1 of technical solution of the present invention) in the content of PVP be 0.2～1%；The content of ascorbic acid is 100～400mmol/L；The content of silver nitrate is 0.1～0.4mmol/L；Gold nano grain solution and polyvinylpyrrolidonesolution solution, ascorbic acid solution, the volume ratio 5～10:2～6:1～3:0.5～2.5 of silver nitrate solution.
The step 1 of technical solution of the present invention) in mixed liquor room temperature lucifuge concussion reaction 2-4h.
The step 2 of technical solution of the present invention) in the volume mass ratio of Au/Ag core shell nanoparticles solution and dodecyl sodium sulfate be 100～500 μ L:1～5mg.
Beneficial effects of the present invention:
(1) nano material only needing a small amount of concentration can produce strong bactericidal effect to gram negative bacteria and gram positive bacteria, has broad-spectrum sterilization.
(2) by Surface-modification of Nanoparticles anion surfactant SDS, it is effectively increased the biocidal property of nano material, is substantially reduced its toxicity；
(3) good dispersion, stable chemical nature, effectively prevent oxidation and the reunion of nanometer silver, can preserve for a long time.
(4) reaction condition gentleness, reagent environmental protection, simple to operate, it is easy to controls.
Accompanying drawing explanation
Fig. 1 is the TEM photo of the Au/Ag nano-particle that embodiment 1 prepares.
Fig. 2 is embodiment 1～3 and the cytotoxicity test result figure of comparative example 1～4.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described, but protection scope of the present invention is not limited to this:
In the embodiment of the present invention, the particle diameter of gold nano grain is 8～12nm.
Embodiment 1
(1) preparation of Au/Ag core shell nanoparticles
It is 5nmol/L gold nano grain solution and the PVP solution of 100 μ L0.2% by 250 μ L concentration, the ascorbic acid solution of 50 μ L0.1mol/L, after mix homogeneously, add the AgNO of 35 μ L0.1mmol/L3Solution, under room temperature, lucifuge concussion reaction 2h, prepares Au/Ag core shell nanoparticles solution；
(2) SDS is modified on Au/Ag core shell nanoparticles surface
Take Au/Ag core shell nanoparticles solution 500 μ L prepared by step (1) in 1mL centrifuge tube, be added thereto to 1mg dodecyl sodium sulfate, room temperature reaction 1h, prepare the Au/Ag core shell nanoparticles of SDS functionalization.
Embodiment 2
(1) preparation of Au/Ag core shell nanoparticles
It is 10nmol/L gold nano grain solution and the PVP solution of 200 μ L0.5% by 350 μ L concentration, the ascorbic acid solution of 100 μ L0.2mol/L, after mix homogeneously, add the AgNO of 70 μ L0.2mmol/L3Solution, under room temperature, lucifuge concussion reaction 2h, prepares Au/Ag core shell nanoparticles solution；
(2) SDS is modified on Au/Ag core shell nanoparticles surface
Take Au/Ag core shell nanoparticles solution 300 μ L prepared by step (1) in 1mL centrifuge tube, be added thereto to 3mg dodecyl sodium sulfate, room temperature reaction 1h, prepare the Au/Ag core shell nanoparticles of SDS functionalization.
Embodiment 3
(1) preparation of Au/Ag core shell nanoparticles
It is 20nmol/L gold nano grain solution and the PVP solution of 300 μ L1% by 500 μ L concentration, the ascorbic acid solution of 150 μ L0.4mol/L, after mix homogeneously, add the AgNO of 125 μ L0.4mmol/L3Solution, under room temperature, lucifuge concussion reaction 2h, prepares Au/Ag core shell nanoparticles solution；
(2) SDS is modified on Au/Ag core shell nanoparticles surface
Take Au/Ag core shell nanoparticles solution 100 μ L prepared by step (1) in 1mL centrifuge tube, be added thereto to 5mg dodecyl sodium sulfate, room temperature reaction 1h, prepare the Au/Ag core shell nanoparticles of SDS functionalization.
Comparative example 1
The synthesis of Au nano-particle: conical flask A taking a cleaning is sequentially added into the chlorauric acid solution of 79mL ultra-pure water and 1mL1%.Separately take conical flask B and be sequentially added into 15.8mL ultra-pure water, the citric acid three sodium solution of 4mL1%, the tannic acid solution of 0.1mL1%, the K of 0.1mL25mmol/L2CO3.A, B solution being positioned over 60 DEG C of heating in water bath 30min, is then quickly adding in A liquid by B liquid, and quickly stirs, 60 DEG C are continued heating 30min, until after solution colour becomes claret, stopping heating, being cooled to room temperature.
Comparative example 2
The synthesis of Ag nano-particle: the conical flask taking a cleaning is placed in ice bath, is sequentially added into 20mL ultra-pure water, the polyvinylpyrrolidone of 5mL1% and 0.6mL0.01mol/L sodium borohydride aqueous solution.Then, the aqueous povidone solution of 5mL1% and the silver nitrate aqueous solution of 5mL0.1% is filled respectively with the needle tubing of two 50mL, two both sides being fixed on miniflow syringe pump by all means, two kinds of solution are joined in the conical flask in ice bath with the speed of 30mL/h simultaneously, add until reaction terminates while stirring, solution becomes buff from colourless, reactant is placed in 80 DEG C of reaction 2h and removes unreacted sodium borohydride, and last solution becomes glassy yellow.
Comparative example 3
(1) preparation of Au/Ag core shell nanoparticles
It is 20nmol/L gold nano grain solution and the PVP solution of 300 μ L1% by 250 μ L concentration, the ascorbic acid solution of 150 μ L0.4mol/L, after mix homogeneously, add the AgNO of 125 μ L0.4mmol/L3Solution, under room temperature, lucifuge concussion reaction 2h, prepares Au/Ag core shell nanoparticles solution, is centrifuged and removes supernatant, obtains Au/Ag core shell nanoparticles.
Comparative example 4
(1) preparation of Au/Ag core shell nanoparticles
It is 20nmol/L gold nano grain solution and the PVP solution of 300 μ L1% by 500 μ L concentration, the ascorbic acid solution of 150 μ L0.4mol/L, after mix homogeneously, add the AgNO of 125 μ L0.4mmol/L3Solution, under room temperature, lucifuge concussion reaction 2h, prepares Au/Ag core shell nanoparticles solution；
(2) SH-PEG is modified on Au/Ag core shell nanoparticles surface
Take Au/Ag core shell nanoparticles solution 100 μ L prepared by step (1) in 1mL centrifuge tube, it is added thereto to 5mg sulfydryl-Polyethylene Glycol (SH PEG, molecular weight 1000), room temperature reaction 1h, prepare the Au/Ag core shell nanoparticles of SH-PEG functionalization.
Blank group
With normal saline for blank group.
Performance detects:
The Au/Ag core-shell nano material of preparation is carried out structure and performance test, specific as follows:
(1) transmission electron microscope (TEM) test
The TEM photo of the Au/Ag nano-particle that embodiment 1 prepares is as shown in Figure 1.It can be seen that Au/Ag nano-particle presents obvious two-layer core shell structure, it is internal is gold nano core, and particle diameter is at about 10nm, and outer wrap one layer is silver shell, and its thickness is 2-4nm.Core shell nanoparticles is evenly distributed, and defines the spherical of rule, and its mean diameter is at about 15nm.
(2) bacteriostasis property test:
Using staphylococcus aureus and escherichia coli as representative, measure Au/Ag core-shell nano material to gram positive bacteria and the bacteriostasis property of negative bacterium, embodiment 1～3, blank group and comparative example 1～4 take same volume, after being mixed 6h with bacterial solution respectively, by contrasting the change of bacteria colony count, evaluate the bacteriostasis property of Au/Ag nano material.
Before sterilization processing, the clump count of antibacterial is 7.0 ± 0.15log.
After embodiment 1～3, blank group and comparative example 1～4 are mixed with bacterial solution, it is as shown in the table for bacteria colony count reduced value.
Table 1 S. aureus colonies number reduced value
As can be seen from Table 1, the clump count reduced value of (embodiment 1～3) staphylococcus aureus that Au/Ag core-shell nano material processes is far longer than blank group, simple gold, silver nano-particle group (comparative example 1,2), Au/Ag core shell nanoparticles group (comparative example 3) and Au/Ag core shell nanoparticles and modifies SH-PEG group (comparative example 4), and fungistatic effect is obvious.This main with Au in nano material and the concentration ratio of silver-colored Ag and nano material relevant with the synergic remove of SDS.
Table 2 E. coli clones number reduced value
| Group | Clump count reduced value (log) |
| Embodiment 1 | 6.31±0.84 |
| Embodiment 2 | 6.73±0.95 |
| Embodiment 3 | 6.55±0.64 |
| Comparative example 1 | 1.24±1.04 |
| Comparative example 2 | 3.52±0.92 |
| Comparative example 3 | 3.21±0.85 |
| Comparative example 4 | 2.48±0.75 |
| Blank group | 0 |
As can be seen from Table 2, (embodiment 1～3) colibacillary clump count reduced value that Au/Ag core-shell nano material processes is far longer than blank group, simple gold, silver nano-particle group (comparative example 1,2), Au/Ag core shell nanoparticles group (comparative example 3) and Au/Ag core shell nanoparticles and modifies SH-PEG group (comparative example 4), and fungistatic effect is obvious.
3) cytotoxicity test
Use tetramethyl azo azoles salt (MTT) colorimetry, measure the cytotoxicity of Au/Ag core-shell nano material.Embodiment 1～3 and the material of comparative example 1～4 take same volume, mix with Hela cell suspending liquid respectively, 2.5%CO2, hatch 24h under the conditions of 37 DEG C, add MTT dyeing liquor, continue to cultivate 4h.Being taken out by cell, reject culture fluid, add dimethyl sulfoxide, under room temperature, lucifuge is vibrated 15min gently.The absorption value at solution 570nm is measured with enzyme-linked immunosorbent assay instrument.
Figure it is seen that embodiment 1～3 and comparative example 1 and 4 demonstrate less cytotoxicity, and the cytotoxicity that comparative example 2 and 3 display is bigger.
By the above results it can be seen that Au/Ag core shell nanoparticles prepared by this method is a kind of efficient wide-spectrum bactericide, it is only necessary to a small amount of concentration, gram negative bacteria and gram positive bacteria can be produced strong bactericidal effect.Additionally, nanometer Ag in view of high concentration can produce bigger toxicity to mammal, Au/Ag nano-particle prepared by this method, under same concentrations of nanoparticles, the content of its silver ion is well below the content of silver ion in pure nano-Ag particles, it is substantially reduced its bio-toxicity, is a kind of novel green, efficient silver system antibacterial, is with a wide range of applications.
Claims (10)
1. there is an Au/Ag core-shell nano material for Efficient antibacterial performance, it is characterized in that: this material is to be prepared via a method which to obtain:
1) react after gold nano grain solution being mixed with polyvinylpyrrolidonesolution solution, ascorbic acid solution, silver nitrate solution, prepare Au/Ag core shell nanoparticles solution；
2) by step 1) the Au/Ag core shell nanoparticles solution prepared and dodecyl sodium sulfate hybrid reaction, obtain the Au/Ag core-shell nano antibacterial material of SDS functionalization.
The Au/Ag core-shell nano material with Efficient antibacterial performance the most according to claim 1, it is characterised in that: step 1) in the particle diameter of gold nano grain be 5～15nm；In the solution of gold nano grain, nanometer gold molar concentration is 5-20nmol/L.
The Au/Ag core-shell nano material with Efficient antibacterial performance the most according to claim 1, it is characterised in that: step 1) in the content of PVP be 0.2～1%；The content of ascorbic acid is 100～400mmol/L；The content of silver nitrate is 0.1～0.4mmol/L；Gold nano grain solution is 5～10:2～6:1～3:0.5～2.5 with polyvinylpyrrolidonesolution solution, ascorbic acid solution, the volume ratio of silver nitrate solution.
The Au/Ag core-shell nano material with Efficient antibacterial performance the most according to claim 1, it is characterised in that: step 1) in mixing after room temperature lucifuge concussion reaction 2～4h.
The Au/Ag core-shell nano material with Efficient antibacterial performance the most according to claim 1, it is characterised in that: step 2) in the volume mass ratio of Au/Ag core shell nanoparticles solution and dodecyl sodium sulfate be 100～500 μ L:1～5mg.
6. there is an Au/Ag core-shell nano material preparation method for Efficient antibacterial performance, it is characterized in that: the method comprises the following steps:
1) react after gold nano grain solution being mixed with polyvinylpyrrolidonesolution solution, ascorbic acid solution, silver nitrate solution, prepare Au/Ag core shell nanoparticles solution；
2) by step 1) the Au/Ag core shell nanoparticles solution prepared and dodecyl sodium sulfate hybrid reaction, obtain the Au/Ag core-shell nano antibacterial material of SDS functionalization.
The Au/Ag core-shell nano material preparation method with Efficient antibacterial performance the most according to claim 6, it is characterised in that: step 1) in the particle diameter of gold nano grain be 5～15nm；In the solution of gold nano grain, nanometer gold molar concentration is 5-20nmol/L.
The Au/Ag core-shell nano material preparation method with Efficient antibacterial performance the most according to claim 6, it is characterised in that: step 1) in the content of PVP be 0.2～1%；The content of ascorbic acid is 100～400mmol/L；The content of silver nitrate is 0.1～0.4mmol/L；Gold nano grain solution and polyvinylpyrrolidonesolution solution, ascorbic acid solution, the volume ratio 5～10:2～6:1～3:0.5～2.5 of silver nitrate solution.
The Au/Ag core-shell nano material preparation method with Efficient antibacterial performance the most according to claim 6, it is characterised in that: step 1) in mixed liquor room temperature lucifuge concussion reaction 2-4h.
The Au/Ag core-shell nano material preparation method with Efficient antibacterial performance the most according to claim 6, it is characterised in that: step 2) in the volume mass ratio of Au/Ag core shell nanoparticles solution and dodecyl sodium sulfate be 100～500 μ L:1～5mg.
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| CN107347913A (en) * | 2017-06-14 | 2017-11-17 | 南阳师范学院 | The preparation method of paper substrate two dimension Au@Ag core-shell nano compound disinfectants |
| CN109387500A (en) * | 2018-09-29 | 2019-02-26 | 南京农业大学 | A method of Escherichia coli are detected based on magnetic graphene oxide compound Venus@gold-silver alloy nano particle |
| CN114082973A (en) * | 2021-10-22 | 2022-02-25 | 北京航空航天大学 | Ag shell thickness control method of Au @ Ag nano core-shell material and application thereof |
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