CN106172386A - A kind of preparation method carrying silver conch meal antibacterial - Google Patents
A kind of preparation method carrying silver conch meal antibacterial Download PDFInfo
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- CN106172386A CN106172386A CN201610520834.4A CN201610520834A CN106172386A CN 106172386 A CN106172386 A CN 106172386A CN 201610520834 A CN201610520834 A CN 201610520834A CN 106172386 A CN106172386 A CN 106172386A
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
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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
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Abstract
This invention describes a kind of preparation method carrying silver conch meal antibacterial, by preparing conch meal, the conch meal obtained is mixed with sodium citrate solution and silver nitrate solution, and with obtaining carrying silver conch meal after the molten reduction of sodium borohydride, after centrifugal drying, both must carry silver conch meal Antibacterial Products.The inventive method is simple, and raw material sources are extensive, and the antimicrobial product minimal inhibitory concentration obtained has reached 48 μ g/ml, shows stronger fungistatic effect, is with a wide range of applications.
Description
Technical field
The invention belongs to the preparing technical field of antibacterial, be specifically related to a kind of preparation side carrying silver conch meal antibacterial
Method.
Background technology
Health is one of our most concerned topic, and antibacterial is as the extremely strong species of a kind of adaptive faculty, human lives's
Region, antibacterial is nearly ubiquitous.In recent years because the infection event that antibacterial causes also emerges in an endless stream, since the nearly century,
Antibiotic is widely used in various antibacterial field, but gos deep into antibiotic research recently as people, anti-owing to using
Raw element there is a possibility that antibacterial produces the drawback of drug resistance.Under abuse of antibiotics causes the overall background of various problems, antibiotic table
Reveal a certain degree of limitation.Then, people start sight to invest some traditional inorganic antiseptics, carry the most herein
The metal ion antibacterial agent nano silver antimicrobials arrived.
Along with the development of nanotechnology in modern age, nano level silver particles, due to the character that it is special, receive the biggest pass
Note.Simple-substance nano silvery volume is minimum, be not easy to store, use, present stage using nanometer silver as anti-biotic material uses be mainly
Silver particles is supported on carrier, plays antibacterial action.Nanometer silver barrier fabric (antibacterial gauze) is had to upper in terms of medical treatment
The treatment of wounds scalded can suppress bacterial infection, and effect can continue 3 days, has exceeded the effect of clinical conventional norfloxacin
Really.Loading nano silvery on fabric, can promote the healing of wound, makes damaged cell faster regenerate and repairs, it is possible to improving wound
Hinder the microcirculation of surrounding tissue, effectively activate and promote histiocytic growth, make wound recover faster, reduce and stay the hidden of scar
Suffer from.There are the stainless steel material carrying nanometer-level silver, water purification aspect active alumina adsorption nanometer silver on medical apparatus and instruments, process drinking-water
Swimming-pool water and industrial circulating water etc..Nanometer silver is also used on coating, makes antibiotic paint, remembers according to Patents document
Carrying, coating exposes 400h in the sunlight, and the performance of coating does not find change.
Coastal area shell aboundresources, but while a large amount of salvaging, leave a lot of waste shell, cause shell dirty
Dye.But shell but has the value much not noted by people, the such as concrete made as aggregate, it is possible to send out
Waving the ability of load-bearing, the present invention selects shell as support materials, also utilizes cheap, and the even shell as waste product provides
Source, turn waste into wealth considers.Shell is the biogenic mineral material that a kind of biomineralization is formed, and calcium carbonate accounts for its quality
95%, remaining 5% includes that the organic substrates such as protein, and chitin, shell are made up of calcium carbonate and biomacromolecule
Nano composite material, appropriately processed, some groups between biomacromolecule are destroyed, and some active function groups expose and table
Face, some groups on surface just provide place for silver-colored load, and meanwhile, the swelling degraded of few fibers albumen, chitin turns
Turn to chitosan, and chitosan also has certain anti-microbial property.
Summary of the invention
It is desirable to provide the preparation method carrying silver conch meal antibacterial that a kind of good anti-bacterial effect, broad spectrum activity are antibacterial,
This preparation method simple and fast, turns waste into wealth simultaneously, has market prospect widely.
The present invention realizes especially by techniques below scheme:
A kind of preparation method carrying silver conch meal antibacterial, mainly comprises the steps that
Step one, the preparation of conch meal
1.1 take mussel raw material, are beaten by shell and fragmentate, and are soaked in 12h in 0.5mol/g sodium hydroxide solution, Under Ultrasonic Vibration
Swing process 10min, rinse with clear water, dry under the conditions of 60 DEG C, pulverize with in Chinese medicine grinder；
1.2 will pulverize after shell be placed in sodium hydroxide solution, on the magnetic stirring apparatus of 60 DEG C keep 1h, reacted
After one-tenth, sucking filtration separates, and cleans with deionized water simultaneously, is dried；
The conch meal of isolated is carried out anaerobic calcining by 1.3, and cooling, the conch meal after calcining is grey black；
The conch meal that anaerobic is calcined is carried out aerobic sintering by 1.4, and cooling collection, the conch meal after calcination is white.
Step 2, the synthesis of load silver conch meal
2.1 take respectively concentration be the sodium citrate solution of 0.498mg/ml, concentration be that the silver nitrate solution of 0.5mg/ml mixes
Merge and add the conch meal obtained, mixed liquor is placed on magnetic stirring apparatus stirring, stirs on magnetic stirrer under ice bath state
Mix 3min；
2.2 dropwise dropping concentration be the sodium borohydride solution of 0.22mg/ml, stand；
After 2.3 reaction terminatings, take out mixing suspension, centrifugal 5min abandoning supernatant under 2000rpm, add distilled water and wash
Wash, centrifugal, product is placed in 60 DEG C of oven dryings and both must carry silver conch meal antibacterial.
Further,
In step 1.3 of the present invention, the condition of anaerobic calcining is: 550 DEG C, 1h.
In step 1.4 of the present invention, the condition of aerobic sintering is: 750 DEG C, 1h.
In step 2 of the present invention, sodium citrate solution, silver nitrate solution, the volume ratio of sodium borohydride solution are 4.5:5:3,
It is preferably sodium citrate solution 4.5ml, silver nitrate solution 5ml, sodium borohydride solution 3ml.
In step 2.1 of the present invention, the addition of conch meal and the mass volume ratio of sodium borohydride solution are 0.1g/ml, excellent
Elect 0.3g as.
The preparation process of conch meal of the present invention can not carry out the process of step 1.3 and 1.4, it is possible to only select step 1.3
Or the carrying out of 1.4 processes.
The present invention prepares in the method carrying silver conch meal antibacterial, when not carrying out step 1.3 in the preparation process of conch meal
With 1.4 process time, the process of step 1.3 and/or 1.4 can be carried out after the synthesis carrying silver conch meal.
Prepare it addition, the present invention carries silver conch meal antibacterial also by following methods:
Solution is prepared ibid, adds 5.0ml silver nitrate solution, 4.5ml PVP, 0.3g conch meal, in magnetic force in beaker
Stirring and evenly mixing on agitator, irradiates mixing suspension directly over high voltage mercury lamp, reacts 1h, when suspension color no longer changes, eventually
Only reaction, centrifugal 5min abandoning supernatant under 2000rpm, add distilled water washing, centrifugal, product is placed in 60 DEG C of baking ovens and does
Dry both must carry silver conch meal antibacterial.
The invention have the benefit that
The present invention uses chemical reduction method to prepare nano-Ag particles, utilizes local reduction way to prepare loading nano silvery
Conch meal, tests prove that carrying nano silver conch meal has certain bacteriostasis, meet the standard of antibacterial, by one timing
Between DIFFUSION TREATMENT (4 DEG C refrigerators place 12 hours), fungistatic effect can be strengthened to a certain extent, the inventive method uses two
The PROCESS FOR TREATMENT conch meal of secondary sintering, makes conch meal surface have the concavo-convex ridge of abundant fine hair shape, and silver is permissible after being reduced out
Being supported in gap, increase unit mass silver storage capacity to a certain extent, it is antibacterial that the inventive method gained carries silver conch meal
Agent antibacterial effect can continue 48h and be maintained at certain high intensity, has good sustained anti-microbial effect, the inventive method raw material simultaneously
In coastal area aboundresources, low cost, operating procedure is simple, and the nano silver antimicrobials prepared can have good anti-microbial property
And releasability, cosmetics can be applied to by carrying silver conch meal antibacterial and coating is medium, before having market application widely
Scape.
Accompanying drawing explanation
Fig. 1 is secondary calcination NaOH pretreatment conch meal；
Fig. 2 is NaOH pretreatment conch meal；
Fig. 3 is that AR conch meal combines 700 DEG C of calcining 1h products after nanometer silver；
Fig. 4 is ultraviolet reducing process secondary clacining conch meal.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described further, the following stated, is only the preferable enforcement to the present invention
Example, not does the restriction of other forms to the present invention, and any those skilled in the art are possibly also with the disclosure above
Technology contents be changed to the Equivalent embodiments that changes on an equal basis.Every without departing from the present invention program content, according to the present invention
Technical spirit any simple modification that following example are done or equivalent variations, all fall within protection scope of the present invention.
This invention describes a kind of preparation method carrying silver conch meal antibacterial, the preparation work of the present invention is specifically described below
Skill.
1, nanometer silver is prepared
Test and have two schemes: 1. sodium borohydride reduction.2. ultra-vioket radiation method
1. liquid phase reduction
AgNO3+NaBH4+3H2O=Ag+NaNO3+B(OH)3+3.5H2
Reagent: (Kermel Tianjin section is close europeanized for silver nitrate (Changzhou City Guoyu Environmental Science & Technology Co., Ltd.) sodium borohydride
Learn reagent company limited) two citric acid monohydrate trisodiums (Hangzhou Gao Jing Fine Chemical Co., Ltd) reagent purity standard is AR.
Instrument: (Shanghai instrument great waves bio-instruments have magnetic stirring apparatus (Hangzhou motor for instrument company) UV-Vis-NIR spectrogrph
Limit company) electronic balance (Beijing Sai Duolisi instrument system company limited).
Process: configuration solution: silver nitrate 0.5mg/ml bis-citric acid monohydrate trisodium 0.498mg/ml sodium borohydride 0.22mg/
ml
The water that experiment uses, is secondary deionized water.Silver nitrate solution is placed in brown volumetric flask, prevents because illumination is made
Become loss of reaction.
Take a certain amount of silver nitrate and appropriate sodium citrate (trying citric acid), to move to 100ml conical flask after water constant volume
In.On magnetic stirrer, it is stirred 5min under ice bath state is simultaneously added dropwise the sodium borohydride solution of a small amount of fresh configuration.Mixed
Polymer solution is transformed into grey black solution by colourless (some brown possible) rapidly.Extraction sample uses UV-Vis-NIR spectrogrph
The resonance absorbing peak of detection nano silver particles.When the amount of selected trisodium citrate and sodium borohydride is 4.5ml, 3ml.Silver nitrate is molten
When liquid takes 5ml, Nano silver grain is less.Nano silver grain absworption peak is minimum, and now the particle size of silver is smaller.
Changing borane reducing agent sodium hydride rate of addition, the resonance absorbing peak of silver colloid also can change, and drips in a certain degree
Adding the fastest, silver colloidal particles average-size tapers into.Reaction temperature also can affect Nano silver grain size, when temperature is relatively low,
Nano silver grain average-size is less.
2. ultra-vioket radiation method
Ag?+R-→Ag+R
R is reproducibility group, can directly utilize the anion of silver salt as reducing agent, it is possible to separately add reducing agent, the method
Preparing nanometer silver, the condition of every technique all has an impact, and yield is unstable, easily causes waste.
Reagent: (Hangzhou height is brilliant fine for silver nitrate (Changzhou City Guoyu Environmental Science & Technology Co., Ltd.) two citric acid monohydrate trisodium
Chemical Co., Ltd.).
Instrument: high voltage mercury lamp (Shanghai Ji Guang special lighting electrical apparatus factory) magnetic stirring apparatus (Hangzhou motor for instrument company) UV-
Vis-NIR spectrogrph (Shanghai Yi Tao bio-instruments company limited) electronic balance (Beijing Sai Duolisi instrument system company limited)
Process: silver nitrate is identical with sodium borohydride method with the proportioning of stabilizer.First mixed nitrate silver and trisodium citrate
Solution, is placed on magnetic stirring apparatus and is stirred, and irradiates under high voltage mercury lamp, and period covers ambient light, reduces interference.Mixing
The color of liquid, by substantially colorless transparent, crossfades into light brown → brown → black, shows to react termination.
2, conch meal produces
Instrument: Chinese medicine grinder (Wenling city Ao Li Chinese traditional medicine machine company) KQ-500E ultrasonic cleaning instrument (city of Kunshan's Ultrasound Instrument
Device company limited) baking oven (three, Shanghai Scientific Instruments Corporation) tube furnace
Selecting Mussel Powder, mussel contains horny layer due to its surface, can form one by processing reaction removal horny layer
Determine the cavity in degree or depression.
Take appropriate mussel raw material, substantially clean surface, wash away the impurity of absorption, after flushing, shell is beaten and fragmentates, leaching
Steep in 0.5mol/g sodium hydroxide solution 12 hours.Sonic oscillation processes 10min, substantially cleans the miscellaneous of shell surface attachment
Matter.Put into after rinsing 3 times with clear water in 60 DEG C of baking ovens and be dried.Choose appropriate shell fragment, be put in Chinese medicine grinder the most on a small quantity
Middle pulverizing, the most a collection of about pulverizes 3min.Pulverizing is collected pack after completing and is continued to employ.
Conch meal is placed in beaker, adds certain density sodium hydroxide solution (concentration is without being strict with) and be placed in magnetic force
On agitator, design temperature 60 DEG C, keep 1h.React rear sucking filtration separation conch meal, and clean 2 with deionized water simultaneously
Time.It is dried and continues to employ.
Processing intent: for making the horny layer in conch meal react, forms cavity, increases silver-colored portative area, on the one hand
Also silver can be allowed more securely to be combined on conch meal.
Anaerobic calcining Ar: use tube furnace, carries out anaerobic calcining, collects pack, the shell after calcining after 550 DEG C of 1h coolings
Powder is grey black.
Double sintering: use tube furnace, carries out the conch meal that anaerobic is calcined aerobic 750 DEG C of 1h of sintering, collects after cooling
Pack, the conch meal after calcination is white.
3, silver conch meal synthesis is carried
Preparing nanometer silver and have two schemes, carrying silver conch meal also has two schemes in synthesis general orientation.
1. liquid-phase reduction silver ion method
Various solution are prepared according to the concentration preparing nanometer silver scheme.4.5ml trisodium citrate is dripped molten in conical flask
Liquid, with 5.0ml silver nitrate solution, puts into 0.3g conch meal simultaneously.Conical flask is placed on magnetic stirring apparatus and is stirred, and
Ice bath.Mixing time about 3 minutes, it is therefore an objective to for making solution can penetrate conch meal, and mix.Dropwise dropping 3ml sodium borohydride is molten
Liquid, notes dripping too fast, otherwise reacts too fast, and silver cannot be supported on the space of conch meal, and antibacterial sample quality declines.
On agitator, stand a moment after dropping, reaction can be terminated.Take out and mix suspension, high speed centrifugation,
2000rpm is centrifuged 5min (rotating speed and time do not have strict regulations, can separate solid-liquid) abandoning supernatant, adds distilled water
Washing, centrifugal, washing operation 2 times, clean the impurity of residual.Product is placed in 60 DEG C of oven dryings.Take out sample, in Muffle furnace
In carry out secondary clacining, design temperature is 550 DEG C for the first time, time 1h, and after cooling, calcining heat is 700 DEG C for the second time, time
Between 1h, after cooling take out pack continue to employ as sample.
2. photoreduction silver ion method
Solution is prepared ibid, and as the stabilizer of reaction, trisodium citrate can replace with PVP.Prepare a 50ml to hold
The beaker of amount, adds 5.0ml silver nitrate solution in beaker, puts into 4.5ml stabilizer, 0.3g conch meal simultaneously, be placed in magnetic force
Stirring and evenly mixing is carried out on agitator.Opening high voltage mercury lamp, mixing suspension is irradiated in surface, react about 1h (kind of shell is different,
There is little difference in response time) reaction time shading, simultaneously note mercury lamp heating, need fan cooling.Treat that suspension color no longer becomes
During change, terminate reaction, close high voltage mercury lamp.Ensuing process is identical with solution phase chemical reduction, the sample pack after calcining
Continue to employ.
In the preparation process of conch meal the most of the present invention, the process technique for conch meal secondary clacining also can carry silver shellfish
Carry out after the synthesis of shell powder.That is, final sintetics course of reaction respectively includes following several:
1) secondary clacining after conch meal sodium borohydride method combines silver
2) secondary clacining after conch meal ultra-vioket radiation method combines silver
3) the conch meal sodium borohydride method of double sintering combines silver
4) the conch meal ultra-vioket radiation method of double sintering combines silver
5) an Ar sintering sodium borohydride method is calcined after combining silver.
Although the most all can be obtained sintetics of the present invention, the synthesis that the present invention finally selects by above synthesis path
The conch meal sodium borohydride method that the best approach is double sintering carrying silver conch meal antibacterial combines silver method, and its main cause is concrete
See effect test.
Embodiment 1 Bactericidal test
Instruction strain: escherichia coli.
Sterilizing prepares: tweezers, Oxford cup (internal diameter 6mm ± 0.2mm), culture dish, distilled water, calcium oxide compare (AR Tianjin
Bo Di Chemical Co., Ltd.).
Need instrument and equipment: biochemical cultivation case (Hitachi Hitachi, Ltd.), super-clean bench (Thermo Fisher
Scientific)。
Antibacterial prepares:
Take subzero 20 degrees Celsius of frozen strain Escherichia coli 1:100 and be diluted in fluid medium, 37 DEG C of shaking tables of 220rpm
Activated spawn 12-14h.Bacterium solution is stored in 4 DEG C of refrigerators after having activated.Continue to employ after treating.
Preparation of samples: every kind of sample takes equal in quality, is placed in EP pipe, after high temperature sterilize, goes out according to concentration proportioning dropping
Bacterium distilled water, and carry out ultrasonic DIFFUSION TREATMENT, make solid particle more careful, be more equally distributed in suspension.
Preparation culture medium:
Experiment LB solid culture based formulas 100ml:
Yeast extract: 0.5g (BR Hangzhou Basebio Bio-tech Co., Ltd.)
Peptone: 1.0g (BR Hangzhou Basebio Bio-tech Co., Ltd.)
NaCl:1.0g (AR Shishewei Chemical Co., Ltd., Shanghai)
Agar powder: 1-1.2g (BR Hangzhou Basebio Bio-tech Co., Ltd.)
PH controls 7.6 ± 0.2
121 DEG C of autoclaving 20min.Sterilizing carries out sterile working after terminating in super-clean bench.The Bacterial Plate of experiment is adopted
Use double-layer agar technique.(the most first make culture medium solidifying, then on culture medium solid, be coated with one layer of bacterium solution.)
Sample treatment: concentration as required, adds a certain amount of dd water in the sample after sterilizing, ultrasonic disperse processes,
Make particle dispersed.(dilute process needs sterile working).
It is down flat plate coating: every part of culture dish is uniformly poured 25ml LB solid medium, after culture medium solidifying, often into
200 μ l bacterium solution are dripped in ware culture medium, then with aseptic glass rake uniform for bacterium solution coating.Standing a period of time, the time, length was with bacterium
Liquid is absorbed, and media surface does not has obvious liquid to be as the criterion.
Placing Oxford cup: place 4 Oxford cups in each culture medium, spacing is uniform, and more than 24mm, with culture dish limit
Away from more than 15mm.Disposably to put level during placement to put, try not mobile.
Add antibacterial suspension: after Oxford cup disposes and stablizes, each Oxford cup drips the sample of 200 μ l respective concentration
Solution.Note not dripping to outside the cup of Oxford during dropping, immovable Oxford cup after dropping.
Diffusion and cultivation: carefully move culture dish, be put in 12h in 4 DEG C of refrigerators, DIFFUSION TREATMENT.Put unified for culture dish again
Enter in 37 DEG C of bacteriological incubators and carry out cultivating 24 hours.Take out culture dish, use slide gauge, measure antibacterial by decussation method
The diameter of circle.
The antibacterial diluted concentration that experiment uses is 1% without exception, inhibition zone size data (unit mm).
Sample number into spectrum:
1:Cao matched group
2: the raw shellfish powder matched group of secondary clacining
3: conch meal sodium borohydride method combines secondary clacining after silver
4: conch meal ultra-vioket radiation method combines secondary clacining after silver
5: double sintering shell powder supported sodium borohydride method reducing nano-silver
6: the shell powder supported ultra-vioket radiation method reducing nano-silver of double sintering
Calcine after 7: one times Ar sintering sodium borohydride method combines silver
Experimental result:
Table 1 Bactericidal test
Learnt by statistical data:
Under 1% concentration, sodium borohydride reduction silver ion combines sample antibacterial ability that the method for nanometer silver is fabricated to
By force, according to National Health Service's associated documents, " antibacterial circle diameter size at below 7mm, is then considered as without fungistatic effect, inhibition zone
More than 7mm, show weak fungistatic effect, and antibacterial circle diameter is at 10-20mm, has stronger inhibitory action.
Embodiment 2 minimal inhibitory concentration measures
From the point of view of embodiment 1 experimental result, the antimicrobial sample antibacterial ability that sodium borohydride reduction is made is the strongest, selects this
Class sample is further tested:
Preparing bacteria suspension: take the escherichia coli 10 μ L that above experiment activated, 37 DEG C of shaking tables cultivate exponential phase (about
20 minutes).
Preparation culture medium:
Nutrient broth NB culture medium prescription is as follows: (100ml)
Peptone 1.0g (BR Hangzhou Basebio Bio-tech Co., Ltd.)
Carnis Bovis seu Bubali cream 0.3g (BR Shanghai Sheng Gong biological engineering company limited)
NaCl 0.5g (AR Shishewei Chemical Co., Ltd., Shanghai)
PH 7.2±0.2(25℃)
Dilute sample antibacterial: take 13 sterilizing test tubes, adds 1.6ml culture medium in the first pipe.Remaining every Guan Junjia
Enter 1ml culture medium, add antimicrobial sample stock solution (1280 μ g/ml) 0.4ml, mixing at the first pipe, draw 1ml to second pipe, mixed
Draw 1ml to the 3rd pipe after even again, with the continuous doubling dilution of this rule to the 12nd pipe, and discard from the 12nd pipe absorption 1ml liquid.
13rd pipe is as blank.Each pipe drug level is followed successively by: 256,128,64,32,16,8,4,2,1,0.5,0.25,0.125
μg/ml.,
Inoculation bacterium solution:
In above-mentioned test tube, each pipe adds 20 μ l equivalent bacterium solution, mixing.
Cultivate:
After being stoppered stopper, test tube is placed in 37 DEG C of normal air incubators and cultivates.Incubation time 18 hours.
After 18h, in incubator, take out test tube, observe bacterial growth situation, test tube does not has bacterial growth, sample
The concentration that the minimum test tube of concentration is corresponding is minimal inhibitory concentration MIC of sample.
Experimental result such as table 2:
Table 2 bacterial growth quantity (+represent growth ,-represent not growth)
As known from Table 2, the minimal inhibitory concentration of sample between the concentration of 6--7 pipe, scope (4--8 μ g/ml).
Embodiment 3 bacteriostasis rate measures
Use solid medium to cultivate the method observing bacterium colony ratio, prepare according to the compound method of LB culture medium and cultivate
Base, after sterilizing, each culture dish uniformly culture medium of falling 25ml, after cooling, drip 100 μ l bacterium solution, pave bacterium solution with aseptic rake,
Then drip 100 μ l sample solutions, pave, be repeated 3 times, culture medium is placed in 37 DEG C of incubators and cultivates 24h, observe clump count,
Calculate bacteriostasis rate.
Bacteriostasis rate=(blank clump count-add antimicrobial sample clump count)/blank group clump count.
Experimental result such as table 3:
Table 3 bacteriostasis rate
Culture medium is put in 37 DEG C of incubators after measuring by experiment again, in 36h, the most again takes out observation thin when 48h, 60h
Bacteria growing situation, it was observed that the culture medium bacterium colony having added antibacterial after 48h is the most denumerable, and after 60h, clump count increases gradually, afterwards
Gradually it is similar to without antibacterial group.
Embodiment 4 characterizes experiment
Antibacterial sample needs after having prepared to carry out sample characterizing experiment, so that it is determined that some particularitys of sample
Matter.
1) scanning electronic microscope observation pattern
Take a little (trace) sample to be placed in EP pipe, add 2ml dehydrated alcohol, ultrasonic disperse about 20 minutes, make trace sample
Product disperse, and take a small amount of sample drop on silicon chip, to be dried after, deliver to scanning electron microscope, shoot pattern picture.
As shown in Fig. 1 and Fig. 2 contrasts, clear that, processing through calcination, conch meal particle surface produces fine hair
Shape the most concavo-convex, is beneficial to adhere to nano-Ag particles, and nanometer silver can be allowed to a certain extent to slowly release
Come.
As shown in Fig. 3 and Fig. 4 contrasts, in ultra-vioket radiation course of reaction, silver ion reduction becomes silver simple substance, and adsorbs in calcining
In the gap of conch meal.
Claims (6)
1. the preparation method carrying silver conch meal antibacterial, it is characterised in that comprise the following steps:
Step one, the preparation of conch meal
1.1 take mussel raw material, are beaten by shell and fragmentate, and are soaked in 12h in 0.5mol/g sodium hydroxide solution, at sonic oscillation
Reason 10min, rinses with clear water, dries under the conditions of 60 DEG C, pulverizes with in Chinese medicine grinder；
1.2 will pulverize after shell be placed in sodium hydroxide solution, on the magnetic stirring apparatus of 60 DEG C keep 1h, after having reacted
Sucking filtration separates, and cleans with deionized water simultaneously, is dried；
The conch meal of isolated is carried out anaerobic calcining by 1.3, and cooling, the conch meal after calcining is grey black；
The conch meal that anaerobic is calcined is carried out aerobic sintering by 1.4, and cooling collection, the conch meal after calcination is white；
Step 2, the synthesis of load silver conch meal
2.1 take respectively concentration be the sodium citrate solution of 0.498mg/ml, concentration be that the silver nitrate solution of 0.5mg/ml mixes also
Add the conch meal obtained, mixed liquor is placed on magnetic stirring apparatus stirring, stir on magnetic stirrer under ice bath state
3min；
2.2 dropwise dropping concentration be the sodium borohydride solution of 0.22mg/ml, stand；
After 2.3 reaction terminatings, take out mixing suspension, centrifugal 5min abandoning supernatant under 2000rpm, add distilled water washing,
Centrifugal, product is placed in 60 DEG C of oven dryings and both must carry silver conch meal antibacterial.
A kind of preparation method carrying silver conch meal antibacterial the most according to claim 1, it is characterised in that step of the present invention
In 1.3, the condition of anaerobic calcining is: 550 DEG C, 1h.
A kind of preparation method carrying silver conch meal antibacterial the most according to claim 1, it is characterised in that step of the present invention
In 1.4, the condition of aerobic sintering is: 750 DEG C, 1h.
A kind of preparation method carrying silver conch meal antibacterial the most according to claim 1, it is characterised in that in step 2,
Sodium citrate solution, silver nitrate solution, the volume ratio of sodium borohydride solution are 4.5:5:3.
A kind of preparation method carrying silver conch meal antibacterial the most according to claim 4, it is characterised in that sodium citrate is molten
Liquid consumption is 4.5ml, and silver nitrate solution consumption is 5ml, and sodium borohydride solution consumption is 3ml.
A kind of preparation method carrying silver conch meal antibacterial the most according to claim 1, it is characterised in that adding of conch meal
Dosage is 0.1g/ml with the mass volume ratio of sodium borohydride solution.
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Application publication date: 20161207 |