CN107114655A - A kind of g C of corona treatment3N4Antiseptic and preparation method and purposes - Google Patents
A kind of g C of corona treatment3N4Antiseptic and preparation method and purposes Download PDFInfo
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- CN107114655A CN107114655A CN201710256147.0A CN201710256147A CN107114655A CN 107114655 A CN107114655 A CN 107114655A CN 201710256147 A CN201710256147 A CN 201710256147A CN 107114655 A CN107114655 A CN 107114655A
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- plasma
- corona treatment
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
- A23L3/358—Inorganic compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
- C01B21/0605—Binary compounds of nitrogen with carbon
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- Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
Abstract
The present invention relates to a kind of g C of corona treatment3N4Antiseptic and preparation method and purposes.G C are first synthesized by calcination method by urea3N4, then under nitrogen protection with high pressure plasma processing g C3N4, g C are improved with this3N4Antibacterial effect.G C of the present invention3N4Preparation technology, plasma treatment technique and the experiment of remaining bacterium number all relative maturities, it is plasma treated after g C3N4Antibacterial effect is significantly improved, with important value.
Description
Technical field
The invention belongs to field of food safety, and in particular to g-C3N4The preparation of antiseptic, plasma are to g-C3N4Place
Reason and remaining bacterium number experiment and application.
Background technology
In recent years, with expanding economy and the progress of society, the living standard of the people is gradually stepped up, and environmental pollution etc. is each
The problem of kind gradually shows.Novel nano-material has been obtained for extensive research as effective and environmentally friendly material, meanwhile, it is based on
Bacterium infection problem in some food is extremely serious, develops a kind of nano material and also very must as function antimicrobial
Will.Wherein, some semi-conducting materials have proved to be effective and environmentally friendly antiseptic.People are also more next to the quality requirement of food
Higher, Safety of Food Quality is increasingly subject to whole society's concern.Food pollution has seriously threatened the healthy and life of consumer
Safety, influence social stability and harmony.In consideration of it, researching and developing safe and efficient anti-biotic material and plasma treatment effect
As one of vital task for improving China's pollution degradation and food security.
The country has a lot on g-C3N4With the patent application of the method for plasma.CN101489923A discloses one kind
The preparation method of carbonitride.CN105028436A discloses graphite phase carbon nitride as the new application of anti-biotic material.
CN104311864A discloses fungi-proofing fresh-keeping plastic package material of a kind of efficient visible light and preparation method thereof, the efficient visible light
Fungi-proofing fresh-keeping plastic package material is one side attachment or two-sided attachment or is embedded in the poly- of g- carbonitrides/titania nanoparticles
Ethene packaging material.CN103839748A discloses plasma processing apparatus and method of plasma processing.
CN204337134U discloses a kind of air plasma wound disinfection and wound antibacterial coating unit.
g-C3N4As a kind of new nano material, because the driven band gap of its visible ray, high heat endurance, chemistry are steady
The characteristic such as qualitative and easily prepared, is widely used.But it is due to g-C3N4The high coincidence factor in light induced electron cave and low
Surface area, is subject to certain restrictions its antibacterial activity.The present invention improves g-C using plasma3N4Antibacterial activity.
The concept of plasma was suggested first in nineteen twenty-eight earliest, and pointed out that plasma is the collection of approximate electroneutral
Zoarium, is made up of ion with electronic population, and electric field and magnetic field can be responded.Utilize corona treatment g-C3N4, make
Its potential and particle diameter increase, its antibacterial activity are improved.By the g-C of corona treatment3N4To Escherichia coli and golden yellow
The staphylococcic antibacterial effect of color is significantly improved, and this new nano material is a kind of antibacterial effectively with environmental protection
Material, has great application in terms of production and life.
The content of the invention
The purpose of the present invention is to disclose a kind of g-C of corona treatment3N4The preparation method of antiseptic, passes through plasma
G-C after body processing3N4, its antibacterial activity is significantly improved, and enhances the antibacterial to Escherichia coli and staphylococcus aureus
Effect, to apply in actual production, reaches the purpose of food consumption safety.
The present invention prepares g-C in vacuum tube furnace by urea by calcination method3N4, heating rate is 5 DEG C/min, calcining
Temperature is 550~600 DEG C, and calcination time is 4~5h.
Using plasma treatment g-C3N4Method be：
Using plasma handles g-C3N4, power is in 500W, and the time is 1-5min；Or using plasma processing g-
C3N4, time 1min, power is 200-1000W.
Above-mentioned using plasma handles g-C3N4It is in N2The lower progress of protection.
The antibacterial experiment of the present invention is to use the method for plate culture count, determines g-C3N4To Escherichia coli and golden yellow grape
The remaining bacterium number of coccus.20mL PBS solution is added in bottle after sterilization, then is separately added into g-C3N4And corona treatment
The g-C crossed3N4, be made into 0.2% concentration, fully mix after, addition 105~106CFU/mL bacterium solution (Escherichia
Coli, Staphylococcus aureus), 37 DEG C of concussion and cultivates.Sterilized water is used as negative control.Each test tube is placed in gas
Bathe shaking table under the conditions of 37 DEG C, 150rpm concussion reaction.Appropriate nutrient solution is taken to carry out ten times of gradient dilutions to suitably after 24h
Concentration, coating is uniform, and culture is inverted in 37 DEG C of constant incubators.Colony counting is carried out after 24~48h, different time points are obtained
Total plate count in nutrient solution, so as to evaluate g-C3N4Antibacterial effect.Test, average in triplicate.
Brief description of the drawings
G-C under plasma processing times different Fig. 13N4To the antibacterial effect of Escherichia coli.
G-C under plasma treatment power different Fig. 23N4To the antibacterial effect of Escherichia coli.
G-C under plasma processing times different Fig. 33N4To the antibacterial effect of staphylococcus aureus.
G-C under plasma treatment power different Fig. 43N4To the antibacterial effect of staphylococcus aureus.
Embodiment
Illustrate the embodiment of the present invention, but the protection content of the present invention by Examples below, be not only limited to this
The g-C of embodiment 13N4To the antibacterial experiment of Escherichia coli
1 experiment material
2 experimental standard strains
Escherichia coli (Escherichia coli)
3 experimental methods
1)g-C3N4Preparation
1. 10g urea is weighed, is placed in crucible, and is closed the lid, is placed in vacuum tube furnace；
2. calcining heat and time are adjusted：550 DEG C are raised to 5 DEG C/min heating rate, then 4 are calcined at 550 DEG C
Hour, room temperature is cooled to, faint yellow solid g-C is obtained3N4, grind into powder is standby.
2) corona treatment g-C3N4
1. 50mg g-C are weighed3N4It is placed in culture dish；
2. culture dish is placed in plasma apparatus and handled, power in 500W, the time is 1,3,5min, or when
Between 1min, power be 200,300,400,500,750,1000W, obtained the g-C of different disposal condition3N4。
3) preparation of bacterium solution
Directly take after the strain being inoculated in nutrient broth medium test tube, Escherichia coli culture 24h, it is mixed with oscillator
After even, with 0 times of 0.03mol/L phosphate buffer 1s, 1000 times of gradient dilution (about 105cfu/mL)。
4) preparation of control group sample liquid
0.2mL dilution bacterium solution is drawn with liquid-transfering gun, the blue lid of the sterilized PBS solution containing 20mL is added to
In bottle.
5) preparation of test group sample liquid
The g-C of the above-mentioned preparations of 0.04g is weighed respectively3N4With the g-C of corona treatment3N4It is added to sterilized contain
Have in the 20mL blue lid bottle of PBS solution, be made into 0.2% concentration.Then, 0.2mL dilution is drawn with liquid-transfering gun
Bacterium solution liquid is added thereto, and fully shaking shakes up.
6) check sample " 0 " time of contact count plate
After mixing, by 10 times of control sample liquid, 100 times of gradient dilution, 0.1mL stostes, 10 are drawn respectively-1、10-2Times sample liquid is applied
It is distributed on nutritious agar medium flat board, per sample liquid, 2 plates of parallel coating, 37 DEG C ± 1 are inverted in by above-mentioned flat board
24h is cultivated in DEG C constant incubator, colony counting is done.
7) concussion contact culture
Bottle containing check sample and test sample is fixed on the shaking table of constant-temperature shaking incubator, in operative temperature 37
Under the conditions of DEG C ± 1 DEG C, with 150r/min speed, shake stand-by.
8) count plate after concussion contact certain time
After 24h after contact concussion, by the control sample liquid containing Escherichia coli after vibration and experiment sample liquid through 10 times
After 100 times of gradient dilution, 0.1mL stostes, 10 are drawn respectively-1、10-2Times sample liquid is coated on nutritious agar medium and put down
On plate, 2 plates of parallel coating per sample liquid are inverted in culture 24h in 37 DEG C of ± 1 DEG C of constant incubators and do viable bacteria culture counting.
4 data processings
According to the viable bacteria clump count recorded, the work of Escherichia coli in each sample liquid after contact concussion 24h is calculated
Bacterium sum, control, it was therefore concluded that.
5 experimental results
As a result as illustrated, plasma power select 500W when, with the extension of plasma processing time, g-C3N4To big
The antibacterial effect of enterobacteria is gradually stepped up, and when the processing time of plasma is 1min, sterilizing rate reaches 99.22%, plasma
When processing time is 3min, sterilizing rate reaches 99.91%, and when the processing time of plasma is 5min, sterilizing rate reaches
99.99%.When plasma processing time is 1min, g-C3N4It is notable with the rise of power to the antibacterial effect of Escherichia coli
Improve, when plasma treatment is 500W, sterilizing rate reaches 99.95%, and when plasma treatment power is 1000W, sterilizing rate is
99.96%, it is seen that power g-C after 500W3N4Too big difference is not had to the antibacterial effect of Escherichia coli.
The g-C of embodiment 23N4To the antibacterial experiment of staphylococcus aureus
1 experiment material
2 experimental standard strains
Staphylococcus aureus (Staphylococcus aureus)
3 experimental methods
1)g-C3N4Preparation
1. 10g urea is weighed, is placed in crucible, and is closed the lid, is placed in vacuum tube furnace；
2. calcining heat and time are adjusted：550 DEG C are raised to 5 DEG C/min heating rate, then 4 are calcined at 550 DEG C
Hour, room temperature is cooled to, faint yellow solid g-C is obtained3N4, smash standby.
2) corona treatment g-C3N4
1. 50mg g-C are weighed3N4It is placed in culture dish；
2. culture dish is placed in plasma apparatus and handled, power in 500W, the time is 1,3,5min, or when
Between 1min, power be 200,300,400,500,750,1000W, obtained the g-C of different disposal condition3N4。
3) preparation of bacterium solution
Directly the strain being inoculated in nutrient broth medium test tube is taken, after staphylococcus aureus culture 48h, with shaking
Swing after device mixing, with 0 times of 0.03mol/L phosphate buffer 1s, 1000 times of gradient dilution (about 105cfu/mL)。
4) preparation of control group sample liquid
0.2mL dilution bacterium solution is drawn with liquid-transfering gun, the blue lid of the sterilized PBS solution containing 20mL is added to
In bottle.
5) preparation of test group sample liquid
The g-C of the above-mentioned preparations of 0.04g is weighed respectively3N4With the g-C of corona treatment3N4It is added to sterilized contain
Have in the 20mL blue lid bottle of PBS solution, be made into 0.2% concentration.Then, 0.2mL dilution is drawn with liquid-transfering gun
Bacterium solution liquid is added thereto, and fully shaking shakes up.
6) check sample " 0 " time of contact count plate
After mixing, by 10 times of control sample liquid, 100 times of gradient dilution, 0.1mL stostes, 10 are drawn respectively-1、10-2Times sample liquid is applied
It is distributed on nutritious agar medium flat board, per sample liquid, 2 plates of parallel coating, 37 DEG C ± 1 are inverted in by above-mentioned flat board
48h is cultivated in DEG C constant incubator, colony counting is done.
7) concussion contact culture
Bottle containing check sample and test sample is fixed on the shaking table of constant-temperature shaking incubator, in operative temperature 37
Under the conditions of DEG C ± 1 DEG C, with 150r/min speed, shake stand-by.
8) count plate after concussion contact certain time
After 24h after contact concussion, by the control sample liquid containing staphylococcus aureus after vibration and experiment sample liquid
After 10 times of 100 times of gradient dilutions, 0.1mL stostes, 10 are drawn respectively-1、10-2Times sample liquid is coated on nutritious agar training
Support on base flat board, 2 plates of parallel coating per sample liquid, be inverted in culture 48h in 37 DEG C of ± 1 DEG C of constant incubators and do viable bacteria culture
Count.
4 data processings
According to the viable bacteria clump count recorded, Staphylococcus aureus in each sample liquid after contact concussion 48h is calculated
The total viable count of bacterium, control, it was therefore concluded that.
5 experimental results
As a result as illustrated, plasma power select 500W when, with the extension of plasma processing time, g-C3N4To gold
The antibacterial effect of staphylococcus aureus is gradually stepped up, and when the processing time of plasma is 1min, sterilizing rate reaches 99.38%, etc.
When the processing time of ion is 3min, sterilizing rate reaches 99.89%, and when the processing time of plasma is 5min, sterilizing rate reaches
99.90%.When plasma processing time is 1min, g-C3N4To the antibacterial effect of staphylococcus aureus with the rise of power
And significantly improve, when plasma treatment is 400W, sterilizing rate reaches 94.99%, when plasma treatment power is 500W, sterilizing rate
For 99.66%, when plasma treatment power is 750W, sterilizing rate is 99.93%, when plasma treatment power is 1000W, sterilization
Rate is 99.95%.
Claims (7)
1. a kind of g-C of corona treatment3N4Antiseptic, it is characterised in that：The g-C3N4Antiseptic is by plasma
The g-C of processing3N4, to improve g-C3N4Antibacterial activity.
2. a kind of g-C of corona treatment as claimed in claim 13N4Antiseptic, it is characterised in that：Using plasma
Handle g-C3N4, power is in 500W, and the time is 1-5min.
3. a kind of g-C of corona treatment as claimed in claim 13N4Antiseptic, it is characterised in that：Using plasma
Handle g-C3N4, time 1min, power is 200-1000W.
4. a kind of g-C of corona treatment as claimed in claim 13N4Antiseptic, it is characterised in that：Using plasma
Handle g-C3N4It is in N2The lower progress of protection.
5. a kind of g-C of corona treatment as claimed in claim 23N4Antiseptic, it is characterised in that：Time is 3min.
6. a kind of g-C of corona treatment as claimed in claim 33N4Antiseptic, it is characterised in that：Power is 750W.
7. a kind of g-C of corona treatment as claimed in claim 13N4Antiseptic, it is characterised in that：Corona treatment
G-C3N4Antimicrobial concentration be 0.2% (W/V, g/mL)；Bacterium is staphylococcus aureus and Escherichia coli.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108525693A (en) * | 2018-03-07 | 2018-09-14 | 中国科学院深圳先进技术研究院 | A kind of graphite phase carbon nitride photoelectricity composite catalyst and preparation method thereof |
| CN110240144A (en) * | 2018-03-07 | 2019-09-17 | 海南大学 | A kind of method of plasma discharging auxiliary pyrolysis preparation carbon nanotube |
| CN110506884A (en) * | 2019-08-30 | 2019-11-29 | 江苏大学 | A kind of double lysine antibacterial agents and preparation method and application |
| CN110583956A (en) * | 2019-08-30 | 2019-12-20 | 江苏大学 | Double-histidine antibacterial agent, preparation method and application |
| CN110637966A (en) * | 2019-08-30 | 2020-01-03 | 江苏大学 | Cold plasma treated bis-arginine antibacterial agent, preparation method and application |
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| CN103657699A (en) * | 2013-12-12 | 2014-03-26 | 上海师范大学 | G-C3N4 quantum dot modified titanium oxide nanotube catalyst as well as preparation method and application thereof |
| CN104874414A (en) * | 2015-01-21 | 2015-09-02 | 辽宁石油化工大学 | Large-specific surface area graphite-phase carbonitride photocatalyst and application thereof in photocatalytic degradation reaction of TCP and photocatalysis reaction for hydrogen production |
| CN105028436A (en) * | 2015-07-09 | 2015-11-11 | 东南大学 | Novel application of graphite-phase carbon nitride as antibacterial material |
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| CN101230540A (en) * | 2008-02-22 | 2008-07-30 | 东南大学 | Antibiotic polymer nano fibre and preparation method thereof |
| CN103657699A (en) * | 2013-12-12 | 2014-03-26 | 上海师范大学 | G-C3N4 quantum dot modified titanium oxide nanotube catalyst as well as preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108525693A (en) * | 2018-03-07 | 2018-09-14 | 中国科学院深圳先进技术研究院 | A kind of graphite phase carbon nitride photoelectricity composite catalyst and preparation method thereof |
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| CN108525693B (en) * | 2018-03-07 | 2021-04-09 | 中国科学院深圳先进技术研究院 | Graphite-phase carbon nitride photoelectric composite catalyst and preparation method thereof |
| CN110506884A (en) * | 2019-08-30 | 2019-11-29 | 江苏大学 | A kind of double lysine antibacterial agents and preparation method and application |
| CN110583956A (en) * | 2019-08-30 | 2019-12-20 | 江苏大学 | Double-histidine antibacterial agent, preparation method and application |
| CN110637966A (en) * | 2019-08-30 | 2020-01-03 | 江苏大学 | Cold plasma treated bis-arginine antibacterial agent, preparation method and application |
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