CN109122678A - A kind of nano-silver loaded is in the nano-ag composite and its preparation method and purposes of amphipathic biological carbon material - Google Patents
A kind of nano-silver loaded is in the nano-ag composite and its preparation method and purposes of amphipathic biological carbon material Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/22—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients stabilising the active ingredients
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
- A01N47/42—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides containing —N=CX2 groups, e.g. isothiourea
- A01N47/44—Guanidine; Derivatives thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/22—Improving land use; Improving water use or availability; Controlling erosion
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
- Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures
Abstract
A kind of nano-silver loaded using Escherichia coli or yeast cells as amphiphilic biology carbon material made from raw material, and obtains nano-ag composite by electrostatic interaction loading nano silvery in the nano-ag composite of amphipathic biological carbon material.Amphipathic biological carbon material itself in the present invention is without antibacterial action, but its surface is rich in a large amount of carboxyl and the aromatic ring structure high degree of dispersion in polarity and nonpolar solvent.There is great specific surface area and excellent adsorption capacity simultaneously, this allows to load Nano silver grain as an ideal carrier and constructs a kind of novel antibacterial system.The two combination can improve its disadvantage respectively, make it have more excellent biological function.The invention discloses its preparation methods.
Description
Technical field
The present invention relates to material science and nanoscale science and technology field, in particular to two kinds based on amphipathic biological carbon material
Nano-ag composite.
Background technique
Nano silver material has both the good characteristic of nano material because of it, and brilliant bactericidal property itself is reported extensively
Road.It has been applied to conduit, prosthetic replacement operation, dentistry, food packaging, water treatment system and textile field.It is in biology
Medically there is very big exploitation potential, can be used for exploitation and prepare antibacterial medical instrument, medical dressing, man-made organ etc..Research
It was found that the medical material added with nano silver material is clinical to Escherichia coli, staphylococcus aureus, Candida albicans etc. common
Tens kinds of surgery easy infection bacteriums have strong inhibition and killing effect, and will not generate drug resistance.
Amphipathic biology carbon material surface is rich in a large amount of carboxyl and aromatic ring structure, and has excellent amphiphilic performance,
It can high degree of dispersion in polarity and nonpolar solvent.There is great specific surface area and excellent adsorption capacity simultaneously, this makes it can
To load Nano silver grain as an ideal carrier and construct a kind of novel antibacterial system.
Novel nano silver composite produced by the present invention is under the advantage for the anti-microbial property for remaining nano silver simultaneously in pole
Property and nonpolar solvent in still have high dispersion.Water dispersible nano silver broad spectrum antimicrobial agent is carried on amphipathic by the present invention
The biological obtained nano-ag composite of carbon material, can be compatible with various hydrophobic polymer substrate, as PMMA, TPU,
Silicon rubber, PU, PSF etc..Thus can be used as functional additive prepares various antimicrobial coating/film/surfaces, is producing
There is potential application with antibacterial field needed for life.
Summary of the invention
The object of the present invention is to provide a kind of nano-silver loadeds in the nano-ag composite of amphipathic biological carbon material and its
Preparation method.
Based on above-mentioned purpose, the present invention adopts the following technical scheme:
In the nano-ag composite of amphipathic biological carbon material, it is with Escherichia coli or saccharomycete for a kind of nano-silver loaded
Amphiphilic biological carbon Material cladding obtained has the material of nano silver.
A kind of preparation method of above-mentioned nano-ag composite, it includes the following steps:
The preparation of step 1, amphipathic biological carbon material: it takes Escherichia coli or yeast powder to be placed in a beaker, adds water dispersion equal
It is even, the impurity that upper solution discards beaker bottom is retained after standing, upper solution is added acetone, mixes, be placed on shaking table and shake
It swings, is centrifuged, discard supernatant liquid, repeat above-mentioned acetone cleaning operation, then wash, centrifugation washes away remaining acetone, substrate is used
PBS buffer solution containing 2% glutaraldehyde is uniformly dispersed, and pours into reaction kettle, sets in baking oven, 150~200 DEG C of reaction 8-10h, instead
It after answering, is cooled to room temperature, opens reaction kettle, discard supernatant, lower sediment is washed, it is dry to get amphipathic biological carbon
Material；
The preparation of step 2, cationic Nano silver solution: taking silver nitrate, and ultrapure water is added to dissolve, and is protected from light, under magnetic agitation,
Solution containing hexamethylene is added drop-wise in silver nitrate solution, is protected from light, reduction is added dropwise in magnetic agitation 1-3h
Agent sodium borohydride solution, is protected from light, and magnetic agitation 4-8h obtains cationic Nano silver solution；
The preparation of step 3, cationic nano-ag composite: the amphipathic biological carbon material in above-mentioned steps 1 is added
Into above-mentioned steps 2 in cationic Nano silver solution, ultrasonic disperse is uniform, is protected from light, and 8-12h is shaken at 0-10 DEG C, reaction
After, by the washing of above-mentioned mixed solution, drying, obtain cationic nano-ag composite.
The preparation method of above-mentioned nano-ag composite, the PBS buffer solution containing 2% glutaraldehyde described in step 1, pH=
6.0。
The preparation method of above-mentioned nano-ag composite, amphipathic biology carbon material described in step 2 and polyethyleneimine
Mass ratio is 1:(1~3).
The preparation method of above-mentioned nano-ag composite, the concentration of silver nitrate solution described in step 2 are 0.5mmol/L-
1.5mmol/L。
The preparation method of above-mentioned nano-ag composite, the concentration of hexamethylene described in step 2 are 10-
30μg mL-1。
Another preparation method of above-mentioned nano-ag composite, it includes the following steps:
Step 1 ', the preparation of amphipathic biological carbon material: take Escherichia coli or yeast powder to be placed in a beaker, add water dispersion equal
It is even, the impurity that upper solution discards beaker bottom is retained after standing, upper solution is added acetone, mixes, be placed on shaking table and shake
It swings, is centrifuged, discard supernatant liquid, repeat above-mentioned acetone cleaning operation, then wash, centrifugation washes away remaining acetone, substrate is used
PBS buffer solution containing 2% glutaraldehyde is uniformly dispersed, and pours into reaction kettle, sets in baking oven, 150~200 DEG C of reaction 8-10h, instead
It after answering, is cooled to room temperature, opens reaction kettle, discard supernatant, lower sediment is washed, it is dry to get amphipathic biological carbon
Material；
Step 2 ', amphipathic biological carbon material surface grafting polyethylene imine: take amphipathic biological carbon material to be scattered in pH
In=5.5 PBS buffer solution, 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride, N- hydroxyl fourth two are sequentially added
It is after acid imide is activated, it is evenly dispersed with the PBS buffer solution of pH=5.5, it is added molten with the PBS buffer solution of pH=5.5
The polyethylenimine solution of solution, 4~8h of oscillating reactions is washed after reaction, dry, obtains polyethyleneimine amino-functionalization
Amphipathic biology carbon material；
Step 3 ', the preparation of anionic Nano silver solution: take silver nitrate, ultrapure water added to dissolve, be protected from light, magnetic agitation
Under, the solution containing sodium apolate is added drop-wise in silver nitrate solution, is protected from light, reduction is added dropwise in magnetic agitation 10-30min
Agent sodium borohydride, is protected from light, and magnetic agitation 3-5h obtains anionic Nano silver solution；
Step 4 ', the preparation of anionic nano-ag composite: by two of polyethyleneimine amino-functionalization in above-mentioned steps 2 '
Parent's property biology carbon material is added in above-mentioned steps 3 ' in anionic Nano silver solution, and ultrasonic disperse is uniform, is protected from light, in 0-10
8-12h is shaken at DEG C, after reaction, by the washing of above-mentioned mixed solution, drying, obtains anionic nano-ag composite.
The preparation method of above-mentioned nano-ag composite, step 1 ' described in the PBS buffer solution containing 2% glutaraldehyde, pH=
6.0。
The preparation method of above-mentioned nano-ag composite, the step 2 ' in, amphipathic biology carbon material and 1- (3- diformazan ammonia
Base propyl) -3- ethyl-carbodiimide hydrochloride, N- hydroxysuccinimide mass ratio be 1:(1~4): (1~4).
The preparation method of above-mentioned nano-ag composite, step 2 ' described in amphipathic biological carbon material and polyethyleneimine
Mass ratio is 1:(1~3).
The preparation method of above-mentioned nano-ag composite, step 3 ' described in silver nitrate solution concentration be 1mmol/L-
3mmol/L。
The solution of sodium apolate is dense in the preparation method of above-mentioned nano-ag composite, step 3 ' described in step 3 '
Degree is 0.1mg mL-1-0.5mg mL-1。
Above-mentioned nano-ag composite can be compatible with various hydrophobic polymer substrate, can be used as functional additive preparation
Various antimicrobial coating/film/surfaces, the antibacterial field needed for producing and living have potential application.
The preparation method of novel nano silver composite of the present invention based on amphipathic biological carbon material, compared to more existing
Some technologies have the advantage that
(1) amphipathic biological carbon material itself is without antibacterial action, but its surface exists rich in a large amount of carboxyl and aromatic ring structure
High degree of dispersion in polarity and nonpolar solvent.There is great specific surface area and excellent adsorption capacity simultaneously, this allows to
Nano silver grain is loaded as an ideal carrier and constructs a kind of novel antibacterial system.It is each that the two combination can improve it
From the shortcomings that, make it have more excellent biological function；
(2) sodium apolate not only improves the stability of nano silver while as ligand, itself is excellent anti-
Solidifying characteristic generates " heparan effect " to improve the blood compatibility of material；Hexamethylene itself is as anti-
Microbial inoculum, preservative have been widely used, and greatly promote the antibacterial effect of nano silver.
(3) Nano silver solution has efficient bactericidal property, but its liquid condition is easily reunited, and influences its sterilization effect
Fruit, and it is not easy to maintain.Because its partial size is smaller, be generally centrifuged using Ultracentrifuge, not only wasted time in this way but also
Increase production cost.The present invention can make amphipathic biological carbon material and nano silver molten based on amphipathic biological carbon material
Both liquid is closely combined by Electrostatic Absorption, and equipment investment is few when the method mass production, and enforcement difficulty is small, and preparation side
Method is simple and easy, greatly reduces production cost, and this method has no too big influence to environment.
(4) the amphipathic and surface of amphipathic biological carbon material is made full use of to be rich in the characteristic of functional group in the present invention,
The method that the material of different charges is adsorbed onto amphipathic biological carbon material or the amphipathic biological carbon material surface of functionalization, can
A variety of materials (such as: amino, carboxyl, sulfonate radical etc.) rich in positive charge or negative electrical charge are used as in amphipathic biological carbon materials
Expect the load on surface, prepare the amphipathic biological carbon material of new functionization.
(5) present invention is by utilizing laser particle size and Zeta potential analyzer, ultraviolet-uisible spectrophotometer (UV), scanning
Electron microscope (SEM) carries out micromorphology analysis to prepared nano-ag composite, and nano silver produced by the present invention is compound
Object even particle size distribution, preferably, load capacity is high, and bactericidal effect is good, is remaining the anti-microbial property of nano silver brilliance for dispersibility
The still high degree of dispersion in polarity and nonpolar solvent simultaneously under advantage.The present invention loads water dispersible nano silver broad spectrum antimicrobial agent
, can be compatible with various hydrophobic polymer substrate in the amphipathic biological obtained nano-ag composite of carbon material, as PMMA,
TPU, silicon rubber, PU, PSF etc..Thus can be used as functional additive prepares various antimicrobial coating/film/surfaces,
Antibacterial field needed for production and life has potential application.
Detailed description of the invention
Fig. 1 is the uv-visible absorption spectra feature of PHMB-AgNPs Nano silver solution；
Fig. 2 is amphipathic biological carbon materials A CPs (a), cationic nano-ag composite ACPs-PHMB-AgNPs (b)
Scanning electron microscope (SEM) photograph；
The amphipathic analysis of Fig. 3 cationic nano-ag composite (ACPs-PHMB-AgNPs)；
Fig. 4 is the uv-visible absorption spectra feature of PVS-AgNPs Nano silver solution；
Fig. 5 is amphipathic biological carbon materials A CPs (a), anionic nano-ag composite ACPs-PEI-PVS-AgNPs
(b) scanning electron microscope (SEM) photograph；
Fig. 6 is the amphipathic analysis of anionic nano-ag composite (ACPs-PEI-PVS-AgNPs)；
Fig. 7 is cationic nano-ag composite (ACPs-PHMB-AgNPs) to three kinds of bacterium antibacterial situations.
Fig. 8 is anionic nano-ag composite (ACPs-PEI-PVS-AgNPs) to three kinds of bacterium antibacterial situations.
Specific embodiment
With reference to the accompanying drawing and specific embodiment, the present invention is described in detail.
Embodiment 1
Using amphipathic biological carbon material as the preparation of the novel cationic nano-ag composite of carrier:
(1) preparation of amphipathic biological carbon material (ACPs): take 10g saccharomyces cerevisiae (offer of Henan Losec brewery) in
In beaker, add water dispersion uniform, the impurity that upper solution discards beaker bottom is retained after standing.Suitable third is added into each pipe
Ketone mixes, and is placed in 180r/min on shaking table, vibrates 10-15min, and centrifugation outwells supernatant, repeats aforesaid operations with method
Three times.Washing, centrifugation, in triplicate, washes away remaining acetone.Substrate 100ml is contained to the PBS buffer solution of 2% glutaraldehyde
(pH 6.0) is uniformly dispersed, and pours into reaction kettle, sets in baking oven, 150~200 DEG C of reaction 8-10h.After reaction, it is cooled to
Room temperature opens reaction kettle, outwells supernatant, and with distilled water, supersound washing lower layer substrate for several times, removes residue and water-soluble sugar repeatedly
Ball.It is finally washed twice with dehydrated alcohol, 60 DEG C of dry 6~10h are labeled as ACPs up to amphipathic carbon material in baking oven.
(2) preparation of cationic Nano silver solution: weighing 16.9mg silver nitrate, adds 100ml ultrapure water to dissolve, and shift
Into the brown volumetric flask being protected from light, it is configured to the silver nitrate solution of 1mmol/L, the silver nitrate solution of preparation is kept in dark place.It takes
In the above-mentioned 1mmol/L silver nitrate solution and conical flask of 25ml, it is protected from light, magnetic agitation 0-1h, by 10 μ g ml of 15ml-1-30μg
ml-1Hexamethylene solution be added drop-wise in above-mentioned 1mmol/L silver nitrate solution dropwise, be protected from light, magnetic agitation
1-3h is then added reducing agent sodium borohydride with certain drop speed, is protected from light, magnetic agitation 4-8h, obtained yellow clear solution
As cationic Nano silver solution is labeled as PHMB-AgNPs.
(3) preparation of cationic nano-ag composite: the amphipathic biological carbon material weighed in 50mg above-mentioned (1) is added
To in 50ml above-mentioned (2) in cationic Nano silver solution, ultrasonic disperse is uniform, is protected from light, and 8-12h is shaken at 0-10 DEG C, instead
After answering, above-mentioned mixed solution is centrifuged with 8000r/min, discards upper solution, by precipitating washing 3~5 times, in baking oven
50 DEG C of dry 8~10h obtain cationic nano-ag composite labeled as ACPs-PHMB-AgNPs.
Embodiment 2
Using amphipathic biological carbon material as the preparation of the novel anionic type nano-ag composite of carrier:
(1) preparation of amphipathic carbon material (ACPs): take 10g saccharomyces cerevisiae (offer of Henan Losec brewery) in beaker
In, add water dispersion uniform, the impurity that upper solution discards beaker bottom is retained after standing.Suitable acetone is added into each pipe,
It mixes, is placed in 180r/min on shaking table, vibrate 10-15min, centrifugation outwells supernatant, repeats aforesaid operations three with method
It is secondary.Washing, centrifugation, in triplicate, washes away remaining acetone.Substrate 100ml is contained to the PBS buffer solution (pH of 2% glutaraldehyde
6.0) it is uniformly dispersed, pours into reaction kettle, set in baking oven, 150~200 DEG C of reaction 8-10h.After reaction, it is cooled to room temperature,
Reaction kettle is opened, supernatant is outwelled, supersound washing lower layer substrate for several times, removes residue and water-soluble sugar ball repeatedly with distilled water.Most
It is washed twice with dehydrated alcohol afterwards, 60 DEG C of dry 6~10h are labeled as ACPs up to amphipathic carbon material in baking oven.
(2) amphipathic carbon material surface grafting polyethylene imine: dry amphipathic carbon material 100mg is taken to be scattered in 10ml
In the PBS buffer solution of pH=5.5, sequentially add 100mg 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride and
The N- hydroxysuccinimide of 100mg, carries out 2~3h of activation.It is centrifuged after activation, discards supernatant liquid, with pH=5.5's
PBS buffer solution is washed 3~5 times, then the PBS buffer solution of 10ml pH=5.5 is added thereto, after ultrasonic disperse is uniform thereto
Be added dissolved with the PBS buffer solution of 5ml pH=5.5 50mg polyethyleneimine (aladdin, E107079, M.W.10000,
99%), 4~8h of oscillating reactions on shaking table, after reaction, centrifugation discards supernatant liquid, by washing of precipitate 3-5 times, in baking oven
In 50 DEG C of dry 8-10h, obtain the amphipathic carbon material of polyethyleneimine amino-functionalization.By the amphipathic of polyethyleneimine amino-functionalization
Carbon material is labeled as ACPs-PEI.
(3) preparation of anionic Nano silver solution: weighing 34mg silver nitrate, adds 100ml ultrapure water to dissolve, and be transferred to
In the brown volumetric flask being protected from light, it is configured to the silver nitrate solution of 2mmol/L, the silver nitrate solution of preparation is kept in dark place.It takes
In the above-mentioned 2mmol/L silver nitrate solution and conical flask of 46ml, it is protected from light, magnetic agitation 0-1h, by 2ml 0.1mg ml-1-0.5mg
ml-1Polyvinyl sulfonic acid sodium solution be added drop-wise in above-mentioned 2mmol/L silver nitrate solution dropwise, be protected from light, magnetic agitation 0-30min,
Then reducing agent sodium borohydride is added with certain drop speed, be protected from light, magnetic agitation 3-5h, obtained dark yellow clear solution is
Anionic Nano silver solution is labeled as PVS-AgNPs；
(4) preparation of anionic nano-ag composite: the amphipathic of grafting polyethylene imine in 50mg above-mentioned (2) is weighed
Biological carbon material is added in 50ml above-mentioned (3) in anionic Nano silver solution, and ultrasonic disperse is uniform, is protected from light, at 0-10 DEG C
Above-mentioned mixed solution is centrifuged with 8000r/min after reaction, discards upper solution by lower concussion 8-12h, by precipitating washing 3
~5 times, 50 DEG C of dry 8-10h in baking oven, anionic nano-ag composite is obtained labeled as ACPs-PEI-PVS-AgNPs.
For above-described embodiment 1, the present invention is molten to PHMB-AgNPs nano silver by ultraviolet-uisible spectrophotometer (UV)
Liquid is characterized.Fig. 1 is the uv-visible absorption spectra feature of cationic Nano silver solution PHMB-AgNPs；It is obtained to receive
The silver-colored solution of rice has maximum absorption band at λ=402nm, is consistent with document report, illustrates that cosmocil stearate is successfully made
The composite nano silver solution of hydrochlorate cladding.
For above-described embodiment 1, the present invention passes through laser particle size and Zeta potential analyzer to the load issue of nano silver
It is verified, test result is as shown in table 1:
Table 1
| PHMB-AgNPs | ACPs | ACPs-PHMB-AgNPs | |
| Zeta(mV) | +23.7 | -30.1 | 39.4 |
| Size(d.nm) | 57.29 | 642.8 | 753 |
Nano silver can be determined by the variation of amphipathic biological the carbon material current potential and partial size of nano-silver loaded in table 1
Successful load of the grain in amphipathic biological carbon material surface.
For above-described embodiment 1, the present invention carries out table to ACPs-PHMB-AgNPs by scanning electron microscope (SEM)
Sign.Fig. 2 is the scanning electron microscope (SEM) photograph of ACPs (a), ACPs-PHMB-AgNPs (b), visible in detail can be received in load from figure
The amphipathic biological carbon material surface of meter Yin be covered be evenly distributed, the Argent grain of uniform particle diameter, illustrate nano-Ag particles in amphiphilic
The successful load of property biology carbon material surface.
For above-described embodiment 1, the present invention characterizes ACPs-PHMB-AgNPs by dispersibility experiment, and Fig. 3 is
Dispersion implementations of the ACPs-PHMB-AgNPs in opposed polarity solvent.ACPs-PHMB-AgNPs Monodispersed in three kinds of solvents
It is uniform, illustrate its i.e. hydrophilic and oleophylic, is a kind of amphipathic nature material.Simultaneously in two kinds of solvents of opposed polarity, ACPs-
PHMB-AgNPs will be scattered in water-oil interface.It is possible thereby to prove the load of Argent grain without influencing the amphipathic of ACPs.
For above-described embodiment 2, the present invention is by ultraviolet-uisible spectrophotometer (UV) to PVS-AgNPs Nano silver solution
It is characterized.Fig. 4 is the uv-visible absorption spectra feature of anionic Nano silver solution PVS-AgNPs；Nano silver obtained
Solution has maximum absorption band at λ=390nm, is consistent with document report, illustrates that answering for sodium apolate cladding is successfully made
Close Nano silver solution.
For above-described embodiment 2, the present invention passes through the grafting of laser particle size and Zeta potential analyzer to polyethyleneimine
As a result and the load issue of nano silver is verified, and test result is as shown in table 2:
Table 2
Pass through the amphipathic biological carbon material current potential of the load of polyethyleneimine amino-functionalization and nano silver in table 2 and partial size
Variation can determine polyethyleneimine in the successful grafting of amphipathic biological carbon material surface, and nano-Ag particles are in amphipathic biology
The successful load of carbon material surface.
For above-described embodiment 2, the present invention carries out ACPs-PEI-PVS-AgNPs by scanning electron microscope (SEM)
Characterization.Fig. 5 be ACPs (a), ACPs-PEI-PVS-AgNPs (b) scanning electron microscope (SEM) photograph, from Fig. 5 can it is visible in detail
The amphipathic biological carbon material surface of loading nano silvery be covered be evenly distributed, the Argent grain of uniform particle diameter, illustrate nano-Ag particles
In the successful load of amphipathic biological carbon material surface.
For above-described embodiment 2, the present invention characterizes ACPs-PEI-PVS-AgNPs by dispersibility experiment, Fig. 6
The dispersion implementations for being ACPs-PEI-PVS-AgNPs in opposed polarity solvent.ACPs-PEI-PVS-AgNPs is in three kinds of solvents
Middle Monodispersed is uniform, illustrates its i.e. hydrophilic and oleophylic, is a kind of amphipathic nature material.Simultaneously in two kinds of solvents of opposed polarity,
ACPs-PEI-PVS-AgNPs will be scattered in water-oil interface.It is possible thereby to prove the load of Argent grain without influencing the two of ACPs
Parent's property.
Test example 1
Fungistatic effect test is carried out with ACPs-PHMB-AgNPs nano-ag composite prepared by embodiment:
It selects using staphylococcus aureus (S.aureus) separation strains as the gram-positive bacteria of representative, with Escherichia coli
(E.coli) separation strains are the Gram-negative bacteria represented and using Candida albicans (C.albicans) separation strains as the true of representative
Bacterium.Above-mentioned strain is provided by medical college of He'nan University.
This test use liquid antibiotic method, take respectively 0 μ g, 0.1 μ g, 0.2 μ g, 0.3 μ g, 0.4 μ g, 0.5 μ g, 0.6 μ g,
0.7 μ g, 0.8 μ g, 0.9 μ g ACPs-PHMB-AgNPs are placed in the 5mL centrifuge tube of sterilizing, are aseptically respectively added thereto
Enter 1mL and contains 105The bacterium solution of CFU, sealing are placed in 37 DEG C of shaking tables concussion 6h, after concussion, drawn respectively with liquid-transfering gun respectively from
100 μ L of suspension in heart pipe, and be spread evenly across in each solid plate, it seals, is placed in culture in 37 DEG C of incubators and for 24 hours, observes
Bacterium colony growing state, and count.Experimental result is shown in Fig. 7, ACPs-PHMB-AgNPs has stronger inhibition to make three kinds of bacteriums
With the MIC to S.aureus, E.coli, C.albicans is respectively 0.5 μ g/mL, 0.7 μ g/mL, 0.6 μ g/mL.
Test example 2
Fungistatic effect test is carried out with ACPs-PEI-PVS-AgNPs nano-ag composite prepared by embodiment:
It selects using staphylococcus aureus (S.aureus) separation strains as the gram-positive bacteria of representative, with Escherichia coli
(E.coli) separation strains are the Gram-negative bacteria represented and using Candida albicans (C.albicans) separation strains as the true of representative
Bacterium.Above-mentioned strain is provided by medical college of He'nan University.
This test use liquid antibiotic method, take respectively 0 μ g, 0.02 μ g, 0.04 μ g, 0.06 μ g, 0.08 μ g, 0.10 μ g,
0.13 μ g, 0.16 μ g, 0.19 μ g, 0.3 μ g ACPs-PEI-PVS-AgNPs are placed in the 5mL centrifuge tube of sterilizing, in aseptic condition
Under thereto respectively be added 1mL contain 105The bacterium solution of CFU, sealing are placed in 37 DEG C of shaking table concussion 6h, after concussion, use liquid-transfering gun
100 μ L of suspension in each centrifuge tube is drawn respectively, and is spread evenly across in each solid plate, is sealed, is placed in 37 DEG C of incubators
Culture for 24 hours, observes bacterium colony growing state, and count.Experimental result is shown in Fig. 8, ACPs-PEI-PVS-AgNPs is equal to three kinds of bacteriums
Have stronger inhibiting effect, the MIC to S.aureus, E.coli, C.albicans be respectively 0.13 μ g/mL, 0.19 μ g/mL,
0.16μg/mL。
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, without departing substantially from spirit of that invention
And its in the case where essence, made any modifications, equivalent replacements, and improvements etc. should be included in right appended by the present invention and want
Within the protection scope asked.
Claims (10)
1. a kind of nano-silver loaded is in the nano-ag composite of amphipathic biological carbon material, it is characterized in that: it is with Escherichia coli
Or amphiphilic biological carbon Material cladding made from saccharomycete has the material of nano silver.
2. a kind of preparation method of nano-ag composite described in claim 1, it is characterized in that it includes the following steps:
The preparation of step 1, amphipathic biological carbon material: taking Escherichia coli or yeast powder to be placed in a beaker, add water dispersion uniform, quiet
It postponing and retains the impurity that upper solution discards beaker bottom, acetone is added in upper solution, and it mixes, is placed on shaking table and vibrates, from
The heart, discards supernatant liquid, repeats above-mentioned acetone cleaning operation, then washes, and centrifugation washes away remaining acetone, by substrate with containing
The PBS buffer solution of 2% glutaraldehyde is uniformly dispersed, and pours into reaction kettle, sets in baking oven, 150~200 DEG C of reaction 8-10h, reaction knot
Shu Hou is cooled to room temperature, and is opened reaction kettle, is discarded supernatant, lower sediment is washed, dry to get amphipathic biological carbon material；
The preparation of step 2, cationic Nano silver solution: taking silver nitrate, and ultrapure water is added to dissolve, and is protected from light, and under magnetic agitation, will contain
There is the solution of hexamethylene to be added drop-wise in silver nitrate solution, the concentration of the silver nitrate solution is
0.5mmol/L-1.5mmol/L is protected from light, magnetic agitation 1-3h, and reducing agent sodium borohydride solution is added dropwise, is protected from light, magnetic agitation 4-
8h obtains cationic Nano silver solution；
The preparation of step 3, cationic nano-ag composite: the amphipathic biological carbon material in above-mentioned steps 1 is added to
It states in step 2 in cationic Nano silver solution, ultrasonic disperse is uniform, is protected from light, and 8-12h is shaken at 0-10 DEG C, and reaction terminates
Afterwards, by the washing of above-mentioned mixed solution, drying, cationic nano-ag composite is obtained.
3. the preparation method of above-mentioned nano-ag composite, the matter of amphipathic biology carbon material and polyethyleneimine described in step 2
Measuring ratio is 1:(1~3).
4. the preparation method of nano-ag composite according to claim 3, it is characterized in that: polyhexamethylene described in step 2
The concentration of biguanide hydrochloride is 10-30 μ g mL-1。
5. a kind of preparation method of nano-ag composite described in claim 1, it is characterized in that it includes the following steps:
Step 1 ', the preparation of amphipathic biological carbon material: take Escherichia coli or yeast powder to be placed in a beaker, add water dispersion uniform,
Retaining the impurity that upper solution discards beaker bottom after standing, upper solution is added acetone, mixes, be placed on shaking table and vibrate,
Centrifugation, discards supernatant liquid, repeats above-mentioned acetone cleaning operation, then washes, and centrifugation washes away remaining acetone, by substrate with containing
There is the PBS buffer solution of 2% glutaraldehyde to be uniformly dispersed, pour into reaction kettle, sets in baking oven, 150~200 DEG C of reaction 8-10h, reaction
After, it is cooled to room temperature, opens reaction kettle, discard supernatant, lower sediment is washed, it is dry to get amphipathic biological carbon materials
Material；
Step 2 ', amphipathic biological carbon material surface grafting polyethylene imine: take amphipathic biological carbon material to be scattered in pH=5.5
PBS buffer solution in, it is sub- to sequentially add 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride, N- maloyl
It is after amine is activated, it is evenly dispersed with the PBS buffer solution of pH=5.5, the PBS buffer solution dissolution for using pH=5.5 is added
Polyethylenimine solution, 4~8h of oscillating reactions is washed after reaction, dry, obtains the amphiphilic of polyethyleneimine amino-functionalization
Property biology carbon material；
Step 3 ', the preparation of anionic Nano silver solution: take silver nitrate, ultrapure water added to dissolve, silver nitrate solution obtained
Concentration is 1mmol/L-3mmol/L, is protected from light, and under magnetic agitation, it is molten that the solution containing sodium apolate is added drop-wise to silver nitrate
It in liquid, is protected from light, magnetic agitation 10-30min, reducing agent sodium borohydride is added dropwise, is protected from light, magnetic agitation 3-5h obtains anionic
Nano silver solution；
Step 4 ', the preparation of anionic nano-ag composite: by above-mentioned steps 2 ' polyethyleneimine amino-functionalization it is amphipathic
Biological carbon material is added in above-mentioned steps 3 ' in anionic Nano silver solution, and ultrasonic disperse is uniform, is protected from light, at 0-10 DEG C
8-12h is shaken, after reaction, by the washing of above-mentioned mixed solution, drying, obtains anionic nano-ag composite.
6. the preparation method of the nano-ag composite according to claim 2 or 6, it is characterized in that: step 1 or step 1 ' described in contain
There are the PBS buffer solution of 2% glutaraldehyde, pH=6.0.
7. the preparation method of nano-ag composite according to claim 8, it is characterized in that: the step 2 ' in, amphipathic life
Object carbon material and 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride, N- hydroxysuccinimide mass ratio are 1:
(1~4): (1~4).
8. the preparation method of nano-ag composite according to claim 8, it is characterized in that: step 2 ' described in amphipathic biology
The mass ratio of carbon material and polyethyleneimine is 1:(1~3).
Gather in ' described in step 3 ' 9. the preparation method of nano-ag composite according to claim 8, it is characterized in that: step 3
The concentration of the solution of vinyl sulfonic acid sodium is 0.1mg mL-1-0.5mg mL-1。
10. nano-ag composite described in claim 1 is preparing various antimicrobial coatings, film or surface as functional additive
In application.
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