CN107671305A - The method that nano silver antibacterial agent is quickly prepared using Ligustrum quihoui fruit extracting solution - Google Patents
The method that nano silver antibacterial agent is quickly prepared using Ligustrum quihoui fruit extracting solution Download PDFInfo
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- CN107671305A CN107671305A CN201710864692.8A CN201710864692A CN107671305A CN 107671305 A CN107671305 A CN 107671305A CN 201710864692 A CN201710864692 A CN 201710864692A CN 107671305 A CN107671305 A CN 107671305A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
A kind of method that nano silver antibacterial agent is quickly prepared using Ligustrum quihoui fruit extracting solution, belongs to field of nano biotechnology, and its method is as follows：Ripe Ligustrum quihoui fruit is gathered, constant weight is dried to after cleaning, smashes；Ligustrum quihoui fruit powder is taken, the ultra-pure water of addition, is heated to reflux, after natural cooling, decompression filters, and centrifugation, finally gives Ligustrum quihoui fruit extracting solution；Ligustrum quihoui fruit extracting solution is taken, adds AgNO3Solution, ultra-pure water constant volume, solution after constant volume is placed in Ultrasound Instrument and is ultrasonically treated, while give sunlight, obtain nano silver antibacterial agent.This method is obviously improved, can completed in 1 15min using the light-catalyzed reaction of ultrasonic assistant, aggregate velocity with Ligustrum quihoui fruit extract biosynthesis Nano Silver.This method is green, and material is easy to get, and product has the higher uniformity and dispersiveness, and product quality is stable, and has significant fungistatic effect, and antimicrobial spectrum is wide, beneficial to popularization.
Description
Technical field
The present invention relates to field of nano biotechnology, is specially that a kind of quickly prepared using Ligustrum quihoui fruit extracting solution is received
The method of the silver-colored bacteriostatic agent of rice, it can be applicable in agricultural and aquatic products field.
Background technology
In recent years, a large amount of administrations with bacteriostatic agent in agricultural production, the increase of microorganism drug resistance, medicament residue are caused
Seriously, increasing environmental pollution etc. endangers.Therefore, develop and develop safety and environmental protection, be not likely to produce the new bacteriostatic agent of drug resistance extremely
Close important.With the continuous development of nanometer technology, common concern of the nano metal bacteriostatic agent by people.This kind of particle diameter 1~
Metal particle between 100nm all has strong suppression and killing action to a variety of pathogenic microorganisms, have specific surface area it is big,
Safe and non-toxic, has a broad antifungal spectrum, the advantages that having no drug resistance, it is widely used to medical treatment, food, purification of water quality, antibiotic paint and anti-
The multiple fields such as bacterium fabric.Wherein, Nano Silver being most widely used in antibacterial field, research show that Nano Silver can destroy carefully
Bacterium cell membrane enters intracellular, and can be combined with the sulfydryl of protein, destroys the activity of cell synzyme, disturbs DNA of bacteria
Synthesis, the silver ion of release can also suppress the respiratory chain of microorganism, ultimately result in bacterial death.Therefore Nano Silver is counted as one
The quite potential bacteriostatic agent of kind, turn into the study hotspot of new bacteriostatic agent.
The preparation of Nano Silver at present mainly uses Physical and chemical method, but physical method to equipment requirement and energy consumption compared with
Height, it is unfavorable for industrialized production；Chemical method needs to use substantial amounts of chemical reducing agent in operation, has one to human body and environment
Fixed harm.The biology that Nano Silver is prepared by the use of the active material in biomaterial as reducing agent and stabilizer of latest developments
Synthetic technology has the advantages that simple synthesis technique, safety and environmental protection, reaction condition are gentle, turns into the Nano Silver with development prospect
Synthetic method.It is cheap and easy to get especially with plant extracts synthesizing nano-silver material, it is suitable for large-scale industrialized production.So
And it is found that many vegetable materials reaction time for preparing Nano Silver is longer in actual production, and the plant of different batches
The Nano Silver reappearance of thing materials synthesis is bad, and stability is poor, and uniform particle sizes' degree is not ideal enough.
For these reasons, we screen to a large amount of natural plant materials first, finally find Ligustrum quihoui first
The fruit extract of (Ligustrum quihoui Carr.) has the excellent speciality of biosynthesis Nano Silver.It is and basic herein
On existing Nano Silver synthetic method is improved, with reference to ultrasonic wave and luminescence method, closed using Ligustrum quihoui extract biology
Into nano silver antibacterial agent.This method is without heating, and power consumption is low, and method is simple, is easy to promote.This method greatly improves synthesis effect
Rate, reacting can complete in 15min.In addition, in view of application of the Nano Silver in the fields such as aquatic products, agricultural is less, this patent
The primary study bacteriostatic agent is to agricultural and the fungistatic effect of aquatic pathogenic bacterium, the results showed that its antimicrobial spectrum is wide, to for trying cause of disease
Bacterium has significant suppression and killing effect, will have wide application and promotion prospect in the fields such as agricultural, aquatic products.
The content of the invention
The technical problem to be solved in the present invention is that provide one kind quickly prepares nanometer using Ligustrum quihoui fruit extracting solution
The method of silver-colored bacteriostatic agent, methods described use one-step method biosynthesis Nano Silver, and preparation process is simple.
The present invention is achieved by the following technical solution：
A kind of method that nano silver antibacterial agent is quickly prepared using Ligustrum quihoui fruit extracting solution, method are as follows：
1) the ripe Ligustrum quihoui fruit of collection, constant weight is dried to after cleaning, is smashed；
2) the Ligustrum quihoui fruit powder in step 1) is taken, adds 1-50% (g/100ml) ultra-pure water, 40-90 DEG C adds
Heat backflow 30-120min, after natural cooling, decompression filters, and centrifugation, finally gives Ligustrum quihoui fruit extracting solution；
3) the Ligustrum quihoui fruit extracting solution in step 2) is taken, adds AgNO3Solution, ultra-pure water constant volume, make silver nitrate whole
Concentration is 0.1-10mM, and Ligustrum quihoui fruit extracting solution accounts for the 5-25% of overall solution volume after constant volume, and solution after constant volume is placed in
It is ultrasonically treated in Ultrasound Instrument, while gives sunlight, the color of solution is changed into golden yellow i.e. termination instead from pale pink after constant volume
Should, obtain nano silver antibacterial agent.
Further, the ultrasonic power in the step 3) is 100-1000W.
Further, the sunlit intensity in the step 3) is 10000-100000lx.
Further, the reaction temperature in the step 3) is room temperature.
Further, the reaction time in the step 3) is 1-30min.
The beneficial effect of the present invention compared with prior art：
A kind of method of the photocatalysis Ligustrum quihoui biosynthesis Nano Silver of ultrasonic assistant provided by the present invention, is used
Ligustrum quihoui be common afforestation plant, material is easy to get.This method is with Ligustrum quihoui fruit extract biosynthesis
Nano Silver, and be obviously improved, can be completed in 1-15min using the light-catalyzed reaction of ultrasonic assistant, aggregate velocity.This method
Green, product has the higher uniformity and dispersiveness, and product quality is stable, avoids different batches of biosynthesis Nano Silver
The shortcomings that secondary poor reproducibility.Nano Silver is to Escherichia coli, staphylococcus aureus, pseudomonas syringae, vibrio parahemolyticus etc.
Pathogen is respectively provided with significant fungistatic effect, and antimicrobial spectrum is wide, beneficial to popularization.
Brief description of the drawings
Fig. 1：Using Ligustrum quihoui fruit extract under different ultrasonic power the agent of biosynthesis nano silver antibacterial it is ultraviolet
Visible absorption spectra figure；
Fig. 2：Can in the ultraviolet of differential responses time biosynthesis nano silver antibacterial agent using Ligustrum quihoui leaf extract
See abosrption spectrogram.
Embodiment
The technical scheme in the embodiment of the present invention is clearly and completely described below, described embodiment is only
Part of the embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art
The every other embodiment obtained under the premise of no creative work, belongs to the scope of protection of the invention.
The Ligustrum quihoui fruit extract of embodiment 1 prepares Nano Silver
A, the preparation of Ligustrum quihoui fruit extracting solution
Ripe Ligustrum quihoui fruit is gathered, after running water is cleaned, ultra-pure water rinses 3 times, and 60 DEG C are dried to constant weight, storage
It is standby.
Dry Ligustrum quihoui fruit is smashed, weighs powder 1g, adds 10mL ultra-pure waters, 90 DEG C are heated to reflux
30min.After natural cooling, decompression filters, and 12000rpm centrifugation 10min, collects supernatant, obtains Ligustrum quihoui extract solution, store
It is standby in 4 DEG C.
B, the biosynthesis of Nano Silver
1mM AgNO is added into 1mL Ligustrum quihoui fruit extracting solutions3Solution 19mL, after stirring, 100W is used respectively
Ultrasonic wave, illumination, 100W ultrasonic waves add photo-irradiation treatment 30min.
C, visible-ultraviolet sign of Nano Silver
The synthesis of Nano Silver is characterized by ultraviolet-visible spectrophotometer, scanning wavelength scope is 300-600nm.Accompanying drawing 1
It has been shown that, the product of three kinds of processing methods synthesis all occur near 450nm the characteristic absorption peak of Nano Silver (Nano silver grain due to
The surface plasma body resonant vibration of characteristic can produce characteristic absorption peak in the range of wavelength 400-500nm).Wherein ultrasonic wave adds
The product light absorption value of illumination synthesis is maximum, produces strong absworption peak.It is possible thereby to illustrate to add photocatalytic to produce in ultrasonic wave
The effect of Nano Silver is best.
The Ligustrum quihoui leaf extract of embodiment 2 prepares Nano Silver
A, the preparation of Ligustrum quihoui leaf extract
Ligustrum quihoui blade is gathered, after running water is cleaned, ultra-pure water rinses 3 times, and 60 DEG C are dried to constant weight, store for future use.
Ligustrum quihoui fruit powder 2g is weighed, adds 10mL ultra-pure waters, 50 DEG C are heated to reflux 2h.After natural cooling, decompression
Filter, 12000rpm centrifugation 10min, collect supernatant, obtain Ligustrum quihoui extract solution, be stored in 4 DEG C, it is standby.
B, the biosynthesis of Nano Silver
5mM AgNO is added into 2mL Ligustrum quihoui fruit extracting solutions3Solution 19mL, after stirring, with 100W ultrasounds
Ripple adds illumination to be sampled after handling 1min, 3min, 5min, 7min, 9min, 12min respectively.
C, visible-ultraviolet sign of Nano Silver
The synthesis of Nano Silver is characterized by ultraviolet-visible spectrophotometer, scanning wavelength scope is 300-600nm.Accompanying drawing 2
Shown, reaction solution does not have the characteristic absorption peak of Nano Silver when without ultrasound with sunlight in the range of 400-500nm, but
After ultrasound and photo-irradiation treatment, reaction solution produces characteristic absorption peak immediately, extends the ultraviolet of Nano Silver with the reaction time
Gradually increase is absorbed, increase trend slows down after 9min, illustrates that the synthetic reaction can reach higher synthesis effect in 10min
Rate.
The Ligustrum quihoui different tissues extract of embodiment 3 prepares Nano Silver
A, the preparation of Ligustrum quihoui extract solution
Ligustrum quihoui leaf, flower, fruit are gathered respectively, and after running water is cleaned, ultra-pure water rinses 3 times, and 60 DEG C are dried to perseverance
Weight, is stored for future use.
Weigh above-mentioned three kinds of Ligustrum quihoui tissues to smash, take 1g, add 10mL ultra-pure waters, 90 DEG C are heated to reflux 1h.
After natural cooling, decompression filters, and 12000rpm centrifugation 10min, collects supernatant, obtains Ligustrum quihoui extract solution, be stored in 4 DEG C,
It is standby.
B, the biosynthesis of Nano Silver
Above-mentioned three kinds of Ligustrum quihouis extract solution 3mL is respectively taken, adds 1mM AgNO3Solution 19mL, after stirring, respectively
Add photo-irradiation treatment 10min with 100W ultrasonic waves.
C, visible-ultraviolet sign of Nano Silver
All there is the characteristic absorption peak of Nano Silver near 450nm in the product of three kinds of different tissues synthesis, illustrates leaflet female
Loyal three kinds of tissue extracts can be by AgNO3Nano-Ag particles are reduced into, are used equally for the preparation of Nano Silver.
D, stability compares
By the Nano Silver of three kinds of different tissues synthesis, avoid light place finds to be synthesized by leaf and flower after one month at room temperature
Nano silver solution darken, brownish black, and solutions turbid are become by golden yellow, there is deposited phenomenon；And
The Nano Silver of Ligustrum quihoui fruit synthesis still keeps the distinctive golden yellow of Nano Silver, solution clear.
E, the evaluation of fungistatic effect
From the cause of disease indicator bacteria Escherichia coli and staphylococcus aureus of routine, inhibition zone is carried out using conventional cylinder plate method
Experiment detects the bacteriostatic activity after three kinds of Nano Silvers synthesized are placed one month.
Three kinds of Nano silver solutions that Bactericidal test shows newly to synthesize produce inhibition zone to pathogen, but place one month
The Nano silver solution synthesized afterwards by Ligustrum quihoui leaf and flower no longer produces inhibition zone to pathogen, illustrates that its bacteriostatic activity disappears
Lose, and still have obvious inhibition zone to two kinds of pathogens by the Nano Silver that Ligustrum quihoui fruit synthesizes.It can thus be appreciated that Ligustrum quihoui
The nano silver antibacterial agent of fruit synthesis is more stable, is particularly suited for the exploitation of new bacteriostatic agent.
The evaluation of the nano silver antibacterial agent fungistatic effect of embodiment 4
In order to fully investigate the present invention synthesis bacteriostatic agent fungistatic effect, respectively from analysis of clinic pathogenic microorganism (Escherichia coli and
Staphylococcus aureus), phytopathogen (pseudomonas syringae), aquatic pathogenic bacterium (Vibrio anguillarum, vibrio alginolyticus, Vibrio splindidus)
To by Ligustrum quihoui fruit extract GCMS computer Nano Silver be experiment material in embodiment 3, using conventional cups and dishes as indicator bacteria
Method carries out the bacteriostatic activity of the nano silver antibacterial agent of Bactericidal test detection synthesis.Experimental result is shown in Table 1, as can be seen from Table 1
No matter the Nano silver solution of synthesis is respectively provided with obvious antibacterial work to analysis of clinic pathogenic microorganism, phytopathogen or to aquatic pathogenic bacterium
Property, and physiological saline and Ligustrum quihoui fruit extracting solution control group for examination pathogen to not producing inhibitory action then.The above results
Show the Nano Silver of synthesis has broad-spectrum antibacterial active to a variety of pathogens, shows its wide application prospect.Also, different batches
The bacteriostatic agent of synthesis also there is similar fungistatic effect, illustrate the Nano Silver stable performance of this method synthesis, be adapted to batch production
Batch production.
Antibacterial circle diameter (n=3) of the Ligustrum quihoui fruit extracting solution synthesizing nano-silver of table 1 to 6 kinds of pathogens
Claims (5)
- A kind of 1. method that nano silver antibacterial agent is quickly prepared using Ligustrum quihoui fruit extracting solution, it is characterised in that its method It is as follows：1) the ripe Ligustrum quihoui fruit of collection, constant weight is dried to after cleaning, is smashed；2) the Ligustrum quihoui fruit powder in step 1) is taken, adds 1-50% (g/100ml) ultra-pure water, 40-90 DEG C is heated back 30-120min is flowed, after natural cooling, decompression filters, and centrifugation, finally gives Ligustrum quihoui fruit extracting solution；3) the Ligustrum quihoui fruit extracting solution in step 2) is taken, adds AgNO3Solution, ultra-pure water constant volume, make silver nitrate final concentration of 0.1-10mM, Ligustrum quihoui fruit extracting solution account for the 5-25% of overall solution volume after constant volume, and solution after constant volume is placed in into Ultrasound Instrument Middle supersound process, while give sunlight, the color of solution is changed into golden yellow i.e. terminating reaction from pale pink after constant volume, obtains Nano silver antibacterial agent.
- 2. according to the method for claim 1, it is characterised in that the ultrasonic power in the step 3) is 100-1000W.
- 3. according to the method for claim 1, it is characterised in that the sunlit intensity in the step 3) is 10000- 100000lx。
- 4. according to the method for claim 1, it is characterised in that the reaction temperature in step 3) is room temperature.
- 5. according to the method for claim 1, it is characterised in that the reaction time in step 3) is 1-30min.
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| CN113996800A (en) * | 2021-10-28 | 2022-02-01 | 广东省科学院微生物研究所(广东省微生物分析检测中心) | Method for preparing nano-silver based on gynura bicolor extract |
| CN118080872A (en) * | 2024-01-23 | 2024-05-28 | 江苏农林职业技术学院 | Method for rapidly and environmentally preparing nano silver by using gardenia extracting solution and application |
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| CN118080872A (en) * | 2024-01-23 | 2024-05-28 | 江苏农林职业技术学院 | Method for rapidly and environmentally preparing nano silver by using gardenia extracting solution and application |
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