CN106077674B - A kind of silver nano-grain colloidal solution with efficient sterilizing performance - Google Patents
A kind of silver nano-grain colloidal solution with efficient sterilizing performance Download PDFInfo
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- CN106077674B CN106077674B CN201610443315.2A CN201610443315A CN106077674B CN 106077674 B CN106077674 B CN 106077674B CN 201610443315 A CN201610443315 A CN 201610443315A CN 106077674 B CN106077674 B CN 106077674B
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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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K33/00—Medicinal preparations containing inorganic active ingredients
- A61K33/24—Heavy metals; Compounds thereof
- A61K33/38—Silver; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/08—Solutions
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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
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0545—Dispersions or suspensions of nanosized particles
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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
A kind of application the invention discloses silver nano-grain colloidal solution with efficient sterilizing performance as the germ killing drugs for preparing Human Lung fibroblast, preparation method includes: to carry out liquid laser corrode to the elemental silver target being soaked in deionized water using pulse laser, burn-out time is 10~60 minutes, so that the evenly dispersed silver nano-grain colloidal solution with efficient sterilizing performance be made.The present invention not only has many advantages, such as that size is extra small, surface is pure, is uniformly dispersed, stability is good, pure free from admixture, and can efficient sterilizing, to human normal cell's nonhazardous.
Description
Technical field
The present invention relates to silver nano-grain preparation technical field more particularly to a kind of silver nanoparticles with efficient sterilizing performance
Particle colloid solution.
Background technique
The surface atom of silver nano-grain is " Jie's state " between solid and molecule, and the silver that these are in " Jie's state " is former
Son has very high activity and very strong antibacterial ability, can kill the pathogenic microorganisms such as virus, bacterium, mycoplasma, Chlamydia,
Therefore silver nano-grain has the antibacterial characteristics such as potent, quick, lasting, wide spectrum, is a kind of inorganic antibacterial material being concerned.
Currently, the synthetic method of silver nano-grain can be divided into two class of chemical method and physical method: chemical method mainly includes also
Former agent reduction method, electrochemical reduction method and photoreduction met hod etc., and physical method mainly includes that mechanical milling method, vacuum vapour deposition, vacuum are splashed
Penetrate hair and plasma sputtering method etc..Physical method be all can obtain pure silver nano-grain directly using elemental silver as raw material, but
It is that physical method in the prior art has the shortcomings that device therefor valuableness, low output, synthesis poor controllability；Chemical method has cost
The advantages that silver nano-grain colloidal stability low, that yield is high, controllability is strong, prepared is good, but chemistry in the prior art
Method inevitably introduces impurity in the synthesis process, it is difficult to obtain pure silver nano-grain.
Summary of the invention
For above-mentioned shortcoming in the prior art, the present invention provides a kind of silver nanoparticles with efficient sterilizing performance
Particle colloid solution, not only has many advantages, such as that size is extra small, surface is pure, is uniformly dispersed, stability is good, pure free from admixture, and
And can efficient sterilizing, to human normal cell's nonhazardous.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of silver nano-grain colloidal solution with efficient sterilizing performance, preparation method includes: using pulse laser
Liquid laser corrode is carried out to the elemental silver target being soaked in deionized water, burn-out time is 10~60 minutes, to be made
The evenly dispersed silver nano-grain colloidal solution with efficient sterilizing performance.
Preferably, the wavelength of the pulse laser is 1064nm, 532nm or 355nm.
Preferably, the energy of the pulse laser is 30~150mJ/pulse.
Preferably, the granularity of the silver nano-grain is 1~50nm.
Silver nano-grain colloidal solution as described in the above technical scheme is used for efficient sterilizing field.
Silver nano-grain colloidal solution as described in the above technical scheme is used for efficient sterilizing related with human body field.
Silver nano-grain colloidal solution as described in the above technical scheme is used for Candida albicans, Escherichia coli or golden yellow
At least one in color staphylococcus is sterilized.
As seen from the above technical solution provided by the invention, the silver provided by the present invention with efficient sterilizing performance
Nanoparticle colloid solution is to carry out liquid laser corrode to the elemental silver target being soaked in deionized water using pulse laser
Made of one step, it is not added with any surfactant and stabilizer, therefore silver nano-grain surface is pure, active height, and should
Any other impurity is free of in addition to water molecule and silver in silver nano-grain colloidal solution.Simultaneously as silver nano-grain surface band
There is a charge, therefore the silver nano-grain colloidal solution also has many advantages, such as to be uniformly dispersed, stability is good.In liquid laser corrode mistake
Cheng Zhong can make to be made by adjusting one or several in the wavelength of pulse laser, the energy of pulse laser or burn-out time
The granularity of silver nano-grain change between 1~50nm.The present invention not only have size is extra small, surface is pure, be uniformly dispersed,
The advantages that stability is good, pure free from admixture, and can efficient sterilizing, to human normal cell's nonhazardous, therefore the silver nanoparticle
Particle colloid solution can be used for efficient sterilizing field, be particularly suitable for efficient sterilization related with human body field.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill in field, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
Fig. 1 is the transmission electron microscope photo of silver nano-grain colloidal solution obtained by the embodiment of the present invention 1.
Fig. 2 is the uv-visible absorption spectroscopy figure of silver nano-grain colloidal solution obtained by the embodiment of the present invention 1.
Fig. 3 is silver nano-grain colloidal solution obtained by the embodiment of the present invention 1 respectively to staphylococcus aureus, large intestine
The bactericidal effect figure that bacillus and Candida albicans are sterilized.
Fig. 4 is the silver of silver nano-grain colloidal solution obtained by the embodiment of the present invention 1 and conventional chemical reduction synthesis
Nanoparticle colloid solution carries out the toxicity test to Human Lung fibroblast, the comparison of the cell viability obtained from respectively
Figure.
Specific embodiment
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
The embodiment of invention, those of ordinary skill in the art's every other implementation obtained under that premise of not paying creative labor
Example, belongs to protection scope of the present invention.
The silver nano-grain colloidal solution provided by the present invention with efficient sterilizing performance is described in detail below.
A kind of silver nano-grain colloidal solution with efficient sterilizing performance, preparation method includes: using pulse laser
Liquid laser corrode is carried out to the elemental silver target being soaked in deionized water, burn-out time is 10~60 minutes, to be made
The evenly dispersed silver nano-grain colloidal solution with efficient sterilizing performance.
Wherein, the wavelength of pulse laser is 1064nm, 532nm or 355nm, and the energy of pulse laser is 30~150mJ/
pulse.By adjusting one or several in the wavelength of pulse laser, the energy of pulse laser or burn-out time, can make to make
The granularity of the silver nano-grain obtained changes between 1~50nm.
Specifically, the silver nano-grain colloidal solution provided by the present invention with efficient sterilizing performance is swashed using liquid phase
Made of one step of light corrode, it is not added with any surfactant and stabilizer, therefore silver nano-grain surface is pure, active height,
And any other impurity is free of in addition to water molecule and silver in the silver nano-grain colloidal solution.Simultaneously as silver nanoparticle
Grain surface has charge, therefore the silver nano-grain colloidal solution also has many advantages, such as to be uniformly dispersed, stability is good.In liquid phase
During laser ablation, by adjusting one or several in the wavelength of pulse laser, the energy of pulse laser or burn-out time,
The granularity of silver nano-grain obtained can be made to change between 1~50nm.In addition, the present invention not only has, size is extra small, table
Face is pure, is uniformly dispersed, the advantages that stability is good, pure free from admixture, and can efficient sterilizing, it is nontoxic to human normal cell
Evil, therefore the silver nano-grain colloidal solution can be used for efficient sterilizing field, be particularly suitable for efficient sterilizing related with human body
Disinfection field, such as: the silver nano-grain colloidal solution can be used for Candida albicans, Escherichia coli or Staphylococcus aureus
At least one in bacterium is sterilized.
In order to more clearly from show technical solution provided by the present invention and generated technical effect, below with tool
The silver nano-grain colloidal solution provided by the present invention with efficient sterilizing performance is described in detail in body embodiment.
Embodiment 1
A kind of silver nano-grain colloidal solution with efficient sterilizing performance, preparation method are as follows: use wavelength for
It is molten that 532nm, the pulse laser that energy is 100mJ/pulse carry out liquid laser to the elemental silver target being soaked in deionized water
Erosion, focal beam spot diameter are 1mm, and burn-out time is 30 minutes, so that the evenly dispersed silver with efficient sterilizing performance be made
Nanoparticle colloid solution.
Specifically, silver nano-grain colloidal solution obtained by the embodiment of the present invention 1 is detected, result is as follows:
(1) silver nano-grain colloidal solution obtained by the embodiment of the present invention 1 is in yellowish-brown, and pure free from admixture, pH value is
6.0, colloidal stability is 1 week at normal temperature, and silver nano-grain content is 25 μ g/mL, and the granularity of silver nano-grain is 1~2nm.
The minimum inhibitory concentration of the silver nano-grain colloidal solution is 1 μ g/mL, it is proposed that using concentration is 5 μ g/mL.
(2) silver nano-grain colloidal solution obtained by the embodiment of the present invention 1 is seen using transmission electron microscope
Shooting is examined, to obtain transmission electron microscope photo as shown in Figure 1.As seen from Figure 1: the silver nano-grain colloid is molten
In liquid, the even size distribution of silver nano-grain；Known to further progress granularmetric analysis: in the silver nano-grain colloidal solution
In, the size of silver nano-grain is distributed as 1~2nm, and this super-small, surface be clean, finely dispersed silver nano-grain is
It can not be obtained by existing chemical reduction method.
(3) extinction experiment is carried out to silver nano-grain colloidal solution obtained by the embodiment of the present invention 1, to obtain such as figure
Uv-visible absorption spectroscopy figure shown in 2.As seen from Figure 2: the silver nano-grain colloidal solution occurs at 397nm
The plasma resonance of typical silver nano-grain (surface plasma resonance, SPR) optical absorption peak.
(4) silver nano-grain colloidal solution obtained by the embodiment of the present invention 1 is diluted to silver nano-grain content difference
For three kinds of silver nano-grain colloidal solution of 1.0 μ g/mL, 5.0 μ g/mL and 10.0 μ g/mL, and use these three silver nano-grains
Colloidal solution carries out sterilization experiment to staphylococcus aureus, Escherichia coli and Candida albicans respectively, to obtain such as Fig. 3 institute
The bactericidal effect figure shown.Wherein, Fig. 3 a is the staphylococcus aureus training for being separately added into these three silver nano-grain colloidal solution
The relational graph of light absorption value and incubation time of the nutrient solution at 600nm；Fig. 3 b is molten to be separately added into these three silver nano-grain colloids
The relational graph of light absorption value and incubation time of the E. coli broth of liquid at 600nm；Fig. 3 c is to be separately added into these three silver
The relational graph of light absorption value and incubation time of the Candida albicans bacteria culture fluid of nanoparticle colloid solution at 600nm；Fig. 3 d is
It is separately added into bacterial population of the staphylococcus aureus culture solution of these three silver nano-grain colloidal solution after culture four hours
Mesh statistical chart；Fig. 3 e is to be separately added into the E. coli broth of these three silver nano-grain colloidal solution after culture four hours
Number of bacteria statistical chart；Fig. 3 f is to be separately added into the Candida albicans bacteria culture fluids of these three silver nano-grain colloidal solution training
Number of bacteria statistical chart after supporting four hours.By Fig. 3 a, 3b and 3c it can be seen that with incubation time extension, three kinds of bacteriums
The light absorption value of culture solution gradually decreases, this show silver nano-grain colloidal solution obtained by the embodiment of the present invention 1 to this three
Kind bacterium has killing effect；And under identical incubation time, the concentration of the silver nano-grain colloidal solution is higher, kills
Bacterium efficiency is higher.By Fig. 3 d, 3e and 3f it can be seen that when silver nano-grain content is 5.0 μ g/mL, 1 institute of the embodiment of the present invention
Silver nano-grain colloidal solution obtained is respectively to the sterilizing rate of staphylococcus aureus, Candida albicans, Escherichia coli
96%, 92%, 100%, this shows that silver nano-grain colloidal solution obtained by the embodiment of the present invention 1 also has in very low concentrations
There is extremely strong sterilizing ability.
(5) using silver nano-grain colloidal solution obtained by the embodiment of the present invention 1 as sample A, and also by traditional chemical
As sample B, sample A is then diluted to silver nano-grain content is respectively the silver nano-grain colloidal solution of former method synthesis
Four kinds of colloidal solution of 2.5 μ g/mL, 5.0 μ g/mL, 10.0 μ g/mL and 20.0 μ g/mL, are also diluted to silver nanoparticle for sample B
Grain content is respectively four kinds of colloidal solution of 2.5 μ g/mL, 5.0 μ g/mL, 10.0 μ g/mL and 20.0 μ g/mL.Sample is respectively adopted
Four kinds of colloidal solution after four kinds of colloidal solution and sample B dilution after A dilution carry out the toxicity to Human Lung fibroblast
Experiment, to obtain cell viability comparison diagram as shown in Figure 4.As seen from Figure 4: sample B is to Human Lung fibroblast
With certain toxicity, and the bigger toxicity of silver nano-grain concentration is stronger；And sample A to Human Lung fibroblast not only
There is no toxic action, play the role of promoting its vigor instead, and with the increase of silver nano-grain concentration, cell viability first by
It is cumulative it is big after be gradually reduced；When the silver nano-grain concentration of sample A is 10 μ g/mL, cell viability reaches maximum value (i.e.
130%)；Therefore compared with the silver nano-grain colloidal solution of conventional chemical reduction synthesis, silver nanoparticle obtained by the present invention
Particle colloid solution is very suitable for the fields such as sterilizing relevant to human body to human normal cell's nonhazardous.
To sum up, the embodiment of the present invention not only has that size is extra small, surface is pure, be uniformly dispersed, stability is good, pure
The advantages that free from admixture, and can efficient sterilizing, to human normal cell's nonhazardous.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (1)
1. a kind of silver nano-grain colloidal solution with efficient sterilizing performance is as the sterilization for preparing Human Lung fibroblast
The application of drug, which is characterized in that preparation method includes: using pulse laser to the elemental silver target being soaked in deionized water
Material carries out liquid laser corrode, and focal beam spot diameter is 1mm, and burn-out time is 30 minutes, so that being made evenly dispersed has
The silver nano-grain colloidal solution of efficient sterilizing performance；
Wherein, the wavelength of the pulse laser is 532nm；The energy of the pulse laser is 100mJ/pulse；The silver
The granularity of silver nano-grain is 1~2nm in nanoparticle colloid solution；
Wherein silver nano-grain concentration is 10 μ g/mL.
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| ES2292375B1 (en) * | 2007-08-28 | 2009-09-14 | Universitat De Valencia, Estudi General | METHOD INTENDED FOR THE SYNTHESIS OF INERT METAL NANOPARTICLES. |
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