CN110240722A - A kind of chitosan composite antibiotic film and preparation method thereof of load wheat gliadin/nano silver - Google Patents
A kind of chitosan composite antibiotic film and preparation method thereof of load wheat gliadin/nano silver Download PDFInfo
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- CN110240722A CN110240722A CN201910581461.5A CN201910581461A CN110240722A CN 110240722 A CN110240722 A CN 110240722A CN 201910581461 A CN201910581461 A CN 201910581461A CN 110240722 A CN110240722 A CN 110240722A
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/0806—Silver
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Abstract
The invention discloses a kind of chitosan composite antibiotic films and preparation method thereof of load wheat gliadin/nano silver.The described method includes: chitosan is added in the aqueous solution of glacial acetic acid, it is uniformly mixed and obtains chitosan solution；Wheat gliadin/nano silver composite particles and glycerite are added in chitosan solution, stirs evenly, obtains into film liquid, then casting film, be dried to obtain the chitosan composite antibiotic film of the load wheat gliadin/nano silver.Preparation method provided by the invention, easy to operate, mild condition will not generate harm to environment and human body.Preparation method provided by the invention, with high production efficiency, high quality, wheat gliadin/nano silver composite particles have good dispersibility and stability in chitosan complex film, there is good bactericidal effect to Escherichia coli and staphylococcus aureus, have a good application prospect.
Description
Technical field
The invention belongs to antibiotic packaging material preparation technical fields, and in particular to a kind of load wheat gliadin/nanometer
The chitosan composite antibiotic film and preparation method thereof of silver.
Background technique
Social economy be showing improvement or progress day by day with people's living standard be continuously improved modern society, the topic that people most pay close attention to it
One is still Food Quality Safety, but the propagation and sprawling of the human pathogen being seen everywhere seriously threaten food
Quality safety, and then influence human health.So inhibiting the growth and proliferation of pathogenic bacteria, it is mitigated or eliminated what pathogenic bacteria were led to
The focus that antibiotic packaging material has been used as scientific research and production field is developed in harm.
In food transport storage by filmogen in conjunction with antibacterial agent, extension effective period of food quality can be reached, prevented
The purpose of food spoilage etc..Chitosan is biodegradable and biocompatible polymer, and with excellent antimicrobial
Activity is one of common packaging material for food.- NH2 and-OH rich in chitosan molecule, can form similar net
The cage molecule of network structure can be chelated by hydrogen bond or ionic bond and wheat gliadin, so that nano silver composite particles are equal
It is even to be scattered in chitosan basal body, nano silver/chitosan complex film is formed, nano silver composite particles and chitosan is cooperateed with and makees
With, and then improve its anti-microbial property.Nano silver/the chitosan film largely reported both at home and abroad is simple nano silver mostly
Grain.It is initially formed stable nano silver and meets particle, then composite particles are evenly spread into matrix and obtain into film liquid, re-form film
Preparation method is rarely reported at present.
Summary of the invention
In order to overcome deficiencies of the prior art, the object of the present invention is to provide a kind of molten eggs of load wheat alcohol
Chitosan composite antibiotic film of white/nano silver and preparation method thereof.
A kind of chitosan composite antibiotic film of load wheat gliadin/nano silver provided by the invention and its preparation side
Method is able to solve existing method production nano-Ag particles and is unevenly distributed in chitosan composite antibiotic film, disadvantage easy to reunite.It utilizes
Chitosan composite antibiotic film made from method provided by the invention has Escherichia coli and staphylococcus aureus to kill well
Bacterium effect.
Preparation method provided by the invention, using chitosan as matrix, addition gliadin/AgNPs composite particles are antibacterial
Agent achievees the purpose that suppress growth of microorganism, and has provided newly thinking for building bacteriostatic film.
The purpose of the present invention is realized at least through one of following technical solution.
A kind of preparation method of the chitosan composite antibiotic film of load wheat gliadin/nano silver provided by the invention,
Include the following steps:
(1) wheat gliadin is added in ethanol solution, is uniformly mixed and obtains Properties of Wheat Gliadin Solution；Silver nitrate is added
In water, it is uniformly mixed, obtains silver nitrate solution；
(2) carnosic acid is added in ethanol solution, is uniformly mixed and obtains carnosic acid solution；By step (1) silver nitrate
Solution is added in the Properties of Wheat Gliadin Solution, stirs evenly, obtains silver nitrate-Properties of Wheat Gliadin Solution；Then by mouse
Tail oxalic acid solution is added in silver nitrate-Properties of Wheat Gliadin Solution, stirs evenly, obtains mixed liquor；Under stirring, it will mix
It closes liquid and carries out heating water bath processing, be cooled to room temperature, purify, dialysis treatment obtains wheat gliadin/nano silver colloid particle
Suspension (gliadin/AgNPs colloidal solid)；
(3) chitosan is added in the aqueous solution of glacial acetic acid, is stirred evenly, centrifugal treating takes supernatant, and it is molten to obtain chitosan
Liquid；
(4) step (2) wheat gliadin/nano silver colloid particle suspension liquid addition step (3) described chitosan is molten
It in liquid, stirs evenly, obtains mixture；
(5) glycerol is added in step (4) described mixture, stirs evenly, obtains into film liquid, it will (can at film liquid casting film
Pour into polystyrene board and cast), it is dried (being carried out in climatic chamber), then Balance Treatment (the nitre in drier
Sour magnesium saturated solution, 58%RH), the chitosan composite antibiotic film of the load wheat gliadin/nano silver is made.
Further, the mass percent concentration of step (1) described ethanol solution is 70%, step (2) described ethanol solution
Mass percent concentration be 95%.
Further, in step (1) described Properties of Wheat Gliadin Solution, the mass percent concentration of wheat gliadin
For 0.1wt%-1.5wt%, preferably 0.5wt%；The concentration of step (1) described silver nitrate solution is 0.005mol/L-0.5mol/L
Preferably 0.05mol/L.
Further, in step (2) the carnosic acid solution, the mass percent concentration of the carnosic acid is
0.05wt%-1.5wt%, preferably 0.5wt%；The volume ratio of the silver nitrate solution and Properties of Wheat Gliadin Solution is 1-9:1-
9, preferably 1:1；The stirring rate under stirring is 300-600r/min, preferably 500r/min.
Further, the volume ratio of step (2) silver nitrate solution and carnosic acid solution is 1:1；The water-bath adds
The temperature of heat treatment is 37 degrees Celsius, and the time of heating water bath processing is 120min；The mode of step (2) described purifying is anti-molten
One or more of agent method and revolving method；The dialysis treatment is that molecular cut off is used to carry out for the bag filter of 10Da；Thoroughly
The time of analysis processing is 24 hours.
Further, the concentration of volume percent of the aqueous solution of step (3) described glacial acetic acid is 0.5%-2%；The shell is poly-
The mass volume ratio of sugar and the aqueous solution of glacial acetic acid is 1-5:100g/mL；The centrifugation rate of the centrifugal treating is 8000-
10000rpm, the time of centrifugal treating are 10-30min.
Preferably, step (3) mixing time stirred evenly is 12 hours, and the temperature of stirring is room temperature.
Further, step (4) wheat gliadin/nano silver colloid particle suspension liquid and chitosan solution body
Product is than being 5-15:100.
Preferably, the wheat gliadin/nano silver colloid particle suspension liquid volume is the body of chitosan aqueous solution
Long-pending 10%(v/v).
Preferably, the time of step (4) described stirring is 30min, and the temperature of stirring is room temperature.
Further, the quality of step (5) described glycerol is the 15%-25% of step (3) described chitosan mass；It is described dry
The temperature of dry processing is 37-60 degrees Celsius, and the time of drying process is -48h for 24 hours.
Further, the time of step (5) Balance Treatment in drier is two days or more, described in drier
The relative humidity of Balance Treatment is 58%RH.
Preferably, the wheat gliadin/nano silver colloid particle suspension liquid (gliadin/AgNPs colloidal solid)
In, Ag equivalent is content silver-colored in 32 ug/mL(wheat gliadins/nano-Ag particles solution).The wheat gliadin/
Nano silver colloid particle suspension liquid can be used liquid phase reduction and be made.
Preferably, it prepares the wheat gliadin/nano silver colloid particle and suspends (gliadin/AgNPs colloidal solid)
Include the following steps: wheat gliadin being added to 70%(w/v) ethanol solution in obtain 0.5%(w/v) wheat alcohol it is molten
Albumen alcoholic solution；Silver nitrate dissolution is obtained to the silver nitrate solution of 0.05 mol/L in aqueous solution；Carnosic acid is dissolved in
0.5% carnosic acid solution 95%(w/v) is obtained in ethanol water.Silver nitrate solution is added in Properties of Wheat Gliadin Solution
Stir 10 min.Then carnosic acid solution was being poured into according to pouring into silver nitrate-Properties of Wheat Gliadin Solution slowly
Cheng Zhongyong electronic stirrer ceaselessly stirs until being uniformly mixed, and then under the conditions of 37 DEG C, stirring in water bath reacts a period of time,
The color of solution becomes rufous from colourless, until solution colour is unchanged, cooled to room temperature, then to the molten egg of wheat alcohol
White/nano silver colloidal sol carries out the sequence of operations such as anti-solvent, revolving, and finally dialyse in the bag filter of 10 KD 24 h；To
Prepare wheat gliadin/nano silver colloid particle.
The chitosan that the present invention provides a kind of wheat gliadin of the load as made from above-mentioned preparation method/nano silver is answered
Close antibacterial film.
The chitosan composite antibiotic film of the load wheat gliadin/nano silver drier (magnesium nitrate saturated solution,
It 58%RH) reuses within balance two days or more, better effect.
Compared with prior art, the invention has the advantages that and the utility model has the advantages that
(1) preparation method provided by the invention, easy to operate, mild condition will not generate harm to environment and human body；
(2) preparation method provided by the invention has high production efficiency, high quality, wheat gliadin/nanometer
Silver-colored composite particles have good dispersibility and stability in chitosan complex film, to Escherichia coli and staphylococcus aureus
With good bactericidal effect, have a good application prospect.
Detailed description of the invention
Fig. 1 is the load wheat gliadin/nano silver chitosan composite antibiotic film and comparison that embodiment 1,2,3 provides
The CLSM figure for the chitosan complex film that example 1,2,3 provides.
Fig. 2 is the load wheat gliadin/nano silver chitosan composite antibiotic film and comparison that embodiment 1,2,3 provides
The SEM figure for the chitosan complex film that example 1,2,3 provides.
Specific embodiment
Specific implementation of the invention is described further below in conjunction with attached drawing and example, but implementation and protection of the invention
It is without being limited thereto.If it is existing to be that those skilled in the art can refer to it is noted that there is the not special process of detailed description below
Technology realize or understand.Reagents or instruments used without specified manufacturer, be considered as can by it is commercially available be commercially available it is normal
Advise product.
Embodiment 1
A kind of preparation method of the chitosan composite antibiotic film of load wheat gliadin/nano silver, includes the following steps:
(1) by 1g wheat gliadin be added 10mL mass percent concentration be 70% ethanol solution in, be uniformly mixed obtain it is small
Gliadin solution (wheat gliadin mass percent concentration is 0.5%)；1g silver nitrate is added to the water, is uniformly mixed,
Obtain silver nitrate solution (concentration 0.05mol/L)；
(2) ethanol solution that mass percent concentration is 95% is added in carnosic acid, is uniformly mixed and obtains carnosic acid solution
(mass percent concentration of carnosic acid is 0.5%)；Step (1) silver nitrate solution is added to the wheat gliadin of 4mL
It in solution, stirs evenly, obtains silver nitrate-Properties of Wheat Gliadin Solution；Then silver nitrate-wheat is added in carnosic acid solution
The volume ratio of alcohol soluble protein solution, silver nitrate solution and carnosic acid solution is 1:1, stirs evenly, obtains mixed liquor；In rate
Mixed liquor to be carried out heating water bath processing, the temperature of heating water bath processing is 37 DEG C, water-bath under the stirring of 500r/min
The time of heat treatment be 120min, be cooled to room temperature, purify, dialysis treatment, dialysis treatment use molecular cut off for
The bag filter of 10Da carries out, and the time of dialysis treatment is 24 hours, obtains wheat gliadin/nano silver colloid particle and suspends
Liquid；
(3) 1g chitosan is added in the aqueous solution for the glacial acetic acid that 70mL concentration of volume percent is 1%, is stirred evenly, at centrifugation
Reason, the rate of centrifugal treating are 10000rpm, and the time of centrifugal treating is 20min, takes supernatant, obtains chitosan solution；
(4) step (2) wheat gliadin/nano silver colloid particle suspension liquid addition step (3) described chitosan is molten
In liquid, the volume ratio of wheat gliadin/nano silver colloid particle suspension liquid and chitosan solution is 1:10, stirs evenly, obtains
To mixture；
(5) 0.2g glycerol is added in step (4) described mixture, is stirred evenly at room temperature, the time of stirring is 30min, is obtained
To at film liquid, casting film in the polystyrene board of 18 × 21cm will be poured at film liquid, be done in climatic chamber (50%RH)
Dry processing, dry temperature be 37 degrees Celsius, the dry time be 48h, then drier (magnesium nitrate saturated solution, 58%
RH balance two days, are made the chitosan composite antibiotic film of the load wheat gliadin/nano silver in).
Embodiment 2
A kind of preparation method of the chitosan composite antibiotic film of load wheat gliadin/nano silver, includes the following steps:
(1) by 1g wheat gliadin be added 10mL mass percent concentration be 70% ethanol solution in, be uniformly mixed obtain it is small
Gliadin solution (wheat gliadin mass percent concentration is 0.5%)；1g silver nitrate is added to the water, is uniformly mixed,
Obtain silver nitrate solution (silver nitrate solution concentration 0.05mol/L)；
(2) carnosic acid is added in the ethanol solution that mass percent concentration is 95%, is uniformly mixed and obtains carnosic acid solution
(mass percent concentration of carnosic acid is 0.5%)；It is molten that 4mL wheat gliadin is added in step (1) silver nitrate solution
It in liquid, stirs evenly, obtains silver nitrate-Properties of Wheat Gliadin Solution；Then silver nitrate-wheat alcohol is added in carnosic acid solution
In molten protein solution, the volume ratio of silver nitrate solution and carnosic acid solution is 1:1, stirs evenly, obtains mixed liquor；In rate
Mixed liquor to be carried out heating water bath processing, the temperature of heating water bath processing is 37 DEG C, water-bath under the stirring of 500r/min
The time of heat treatment be 120min, be cooled to room temperature, purify, dialysis treatment, dialysis treatment use molecular cut off for
The bag filter of 10Da carries out, and the time of dialysis treatment is 24 hours, obtains wheat gliadin/nano silver colloid particle and suspends
Liquid；
(3) 1g chitosan is added in the aqueous solution for the glacial acetic acid that 70mL concentration of volume percent is 1%, is stirred evenly, at centrifugation
Reason, the rate of centrifugal treating are 8000rpm, and the time of centrifugal treating is 30min, takes supernatant, obtains chitosan solution；
(4) step (2) wheat gliadin/nano silver colloid particle suspension liquid addition step (3) described chitosan is molten
In liquid, the volume ratio of wheat gliadin/nano silver colloid particle suspension liquid and chitosan solution is 1:20, stirs evenly, obtains
To mixture；
(5) 0.2g glycerol is added in step (4) described mixture, is stirred evenly at room temperature, the time of stirring is 30min, is obtained
To at film liquid, casting film in the polystyrene board of 18 × 21cm will be poured at film liquid, be done in climatic chamber (50%RH)
Dry processing, dry temperature be 37 degrees Celsius, the dry time be 48h, then drier (magnesium nitrate saturated solution, 58%
RH balance two days, are made the chitosan composite antibiotic film of the load wheat gliadin/nano silver in).
Embodiment 3
A kind of preparation method of the chitosan composite antibiotic film of load wheat gliadin/nano silver, includes the following steps:
(1) by 1g wheat gliadin be added 10mL mass percent concentration be 70% ethanol solution in, be uniformly mixed obtain it is small
Gliadin solution (wheat gliadin mass percent concentration is 0.5%)；1g silver nitrate is added to the water, is uniformly mixed,
Obtain silver nitrate solution (silver nitrate solution concentration is 0.05mol/L)；
(2) carnosic acid is added in the ethanol solution that mass percent concentration is 95%, is uniformly mixed and obtains carnosic acid solution
(carnosic acid mass percent concentration is 0.5%)；4mL Properties of Wheat Gliadin Solution is added in step (1) silver nitrate solution
In, it stirs evenly, obtains silver nitrate-Properties of Wheat Gliadin Solution；Then it is molten silver nitrate-wheat alcohol to be added in carnosic acid solution
In protein solution, the volume ratio of silver nitrate solution and carnosic acid solution is 1:1, stirs evenly, obtains mixed liquor；It is in rate
Under the stirring of 500r/min, mixed liquor is subjected to heating water bath processing, the temperature of heating water bath processing is 37 DEG C, and water-bath adds
The time of heat treatment is 120min, is cooled to room temperature, and is purified, and dialysis treatment, dialysis treatment uses molecular cut off as 10Da
Bag filter carry out, time of dialysis treatment is 24 hours, obtains wheat gliadin/nano silver colloid particle suspension liquid；
(3) 1g chitosan is added in the aqueous solution for the glacial acetic acid that 70mL concentration of volume percent is 1%, is stirred evenly, at centrifugation
Reason, the rate of centrifugal treating are 9000rpm, and the time of centrifugal treating is 10min, takes supernatant, obtains chitosan solution；
(4) step (2) wheat gliadin/nano silver colloid particle suspension liquid addition step (3) described chitosan is molten
In liquid, the volume ratio of wheat gliadin/nano silver colloid particle suspension liquid and chitosan solution is 3:20, stirs evenly, obtains
To mixture；
(5) 0.2g glycerol is added in step (4) described mixture, is stirred evenly at room temperature, the time of stirring is 30min, is obtained
To at film liquid, casting film in the polystyrene board of 18 × 21cm will be poured at film liquid, be done in climatic chamber (50%RH)
Dry processing, dry temperature be 37 degrees Celsius, the dry time be 48h, then drier (magnesium nitrate saturated solution, 58%
RH balance two days, are made the chitosan composite antibiotic film of the load wheat gliadin/nano silver in).
Comparative example 1
A kind of preparation method of the chitosan composite antibiotic film of load carnosic acid, includes the following steps:
(1) 1g chitosan is added in the aqueous solution for the glacial acetic acid that 70mL concentration of volume percent is 1%, is stirred evenly at room temperature,
The time of stirring is 12 hours, centrifugal treating, and the rate of centrifugal treating is 10000rpm, and the time of centrifugal treating is 20min, is taken
Supernatant obtains chitosan solution；
(2) carnosic acid is added in the ethanol solution that mass percent concentration is 95%, is uniformly mixed and obtains carnosic acid solution
(carnosic acid mass percent concentration is 0.05%)；Step (1) described chitosan solution is added in the carnosic acid solution
In, the volume ratio of carnosic acid solution and chitosan solution is 1:10, is stirred evenly at room temperature, mixing time 30min is obtained
Mixed liquor；
(3) step (2) described mixing is added in 0.2g glycerol (glycerol additive amount is the 20% of step (1) described chitosan mass)
It in liquid, stirs evenly at room temperature, the time of stirring is 30min, obtains into film liquid, the polyphenyl second of 18 × 21cm will be poured at film liquid
Casting film on alkene plate, it is dry in climatic chamber (50%RH) that the carnosic acid-chitosan complex film is made, drying
Temperature is 37 degrees Celsius, and the dry time is 48h；
(4) step (3) carnosic acid-chitosan complex film is balanced two at drier (magnesium nitrate saturated solution, 58%RH)
It, obtains the chitosan composite antibiotic film of the load carnosic acid.
Comparative example 2
A kind of preparation method of the chitosan composite antibiotic film of load silver nitrate, includes the following steps:
(1) 1g chitosan is added in the aqueous solution for the glacial acetic acid that 70mL concentration of volume percent is 1%, is stirred evenly at room temperature,
The time of stirring is 12 hours, centrifugal treating, and the rate of centrifugal treating is 10000rpm, and the time of centrifugal treating is 20min, is taken
Supernatant obtains chitosan solution；
(2) by silver nitrate solution (concentration 0.05mol/mL) be added step (1) described chitosan solution in, silver nitrate solution with
The volume ratio of chitosan solution is 1:10, is stirred evenly at room temperature, mixing time 30min obtains mixed liquor；
(3) 0.2g glycerol (qualities of glycerin is the 20% of chitosan mass) is added in step (2) described mixed liquor, is stirred at room temperature
It mixes uniformly, the time of stirring is 30min, obtains into film liquid, is cast into pouring into the polystyrene board of 18 × 21cm at film liquid
Film, dry in climatic chamber (50%RH) that the carnosic acid-chitosan complex film is made, dry temperature is 37 Celsius
Degree, dry time are 48h；
(4) step (3) silver nitrate-chitosan complex film is balanced two at drier (magnesium nitrate saturated solution, 58%RH)
It, obtains the chitosan composite antibiotic film of the load silver nitrate.
Comparative example 3
A kind of preparation method of chitosan film, includes the following steps:
(1) 1g chitosan is added in the aqueous solution for the glacial acetic acid that 70mL concentration of volume percent is 1%, is stirred evenly at room temperature,
The time of stirring is 12 hours, centrifugal treating, and the rate of centrifugal treating is 10000rpm, and the time of centrifugal treating is 20min, is taken
Supernatant obtains chitosan solution；
(2) 0.2g glycerol (qualities of glycerin is the 20% of chitosan mass) is added in step (1) described mixed liquor, is stirred at room temperature
It mixes uniformly, the time of stirring is 30min, obtains into film liquid, is cast into pouring into the polystyrene board of 18 × 21cm at film liquid
Film, dry in climatic chamber (50%RH) that the carnosic acid-chitosan complex film is made, dry temperature is 37 Celsius
Degree, dry time are 48h；
(3) step (2) silver nitrate-chitosan complex film is balanced two at drier (magnesium nitrate saturated solution, 58%RH)
It, obtains the chitosan film.
Measure of merit is embodied
Using the biocidal property of confocal laser scanning microscope chitosan complex film, as a result as shown in Figure 1.Fluorescence intensity and cell
Interior ROS production quantity is directly proportional, and ROS is induced cell apoptosis even dead by cellular oxidation stress reaction；And bacterial cell is dead
After have a degree of aggregation.
The test includes the following steps:
A bacterium colony of Escherichia coli ATCC8739 and staphylococcus aureus ATCC6538 is taken to disperse respectively and in nutrient broth
In in 37 DEG C incubate 16 hours, be diluted to 10 with sterile water5-106The bacterial density of cfu/mL, obtains bacteria suspension.Use punch
Composite membrane (sample to be tested that embodiment and comparative example provide) is cut into diameter as the diaphragm of 6mm and places it in 24
In orifice plate.1mL bacteria suspension (OD600=0.01) is added into 24 orifice plates, then cultivates bacterium under the conditions of 37 DEG C with insulating box
24h.After for 24 hours, 24 orifice plates are taken out, wash composite membrane three times with the sodium chloride solution that the concentration of 1mL pH=6.5 is 0.9wt%, then use
10uM DCFDA(2,7- dichlorofluorescein) dyeing 30min.Ready sample is placed under laser confocal microscope and is observed,
The measurement of sample carries out at room temperature, a length of 488 nm of excitation light wave, and wavelength of transmitted light is 550 nm, slit 4nm.Using 40
× and 10 × eyepiece, 1024 × 1024 resolution ratio carries out Image Acquisition.
Fig. 1 is the optical microscope of antibacterial composite membrane；Wherein A, B respectively indicate Escherichia coli and Staphylococcus aureus
Bacterium；A1, B1 are that the wheat gliadin/nano silver-chitosan complex film provided using embodiment 1 carries out the micro- of bacteriostatic experiment
Mirror figure (volume ratio of wheat gliadin/nano silver colloid particle solution and chitosan suspension that embodiment 1 provides is 1:
10)；A2, B2 are that the wheat gliadin/nano silver-chitosan complex film provided using embodiment 2 carries out the aobvious of bacteriostatic experiment
Micro mirror figure (volume ratio of wheat gliadin/nano silver colloid particle suspension liquid and chitosan solution that embodiment 2 provides is 1:
20)；A3, B3 are that the wheat gliadin/nano silver-chitosan complex film provided using only embodiment 3 carries out bacteriostatic experiment
Microscope figure (embodiment 3 provide wheat gliadin/nano silver colloid particle solution and the volume ratio of chitosan suspension be
3:20)；A4, B4 are that the chitosan composite antibiotic film of the load carnosic acid provided using comparative example 1 carries out the aobvious of bacteriostatic experiment
Micro mirror figure；A5, B5 are that the chitosan composite antibiotic film of the load silver nitrate provided using comparative example 2 carries out the micro- of bacteriostatic experiment
Mirror figure；A6, B6 are that the chitosan film provided using comparative example 3 carries out the microscope figure of bacteriostatic experiment；The scale of Fig. 1: 10 μm.
As shown in Figure 1, compared with comparative example, gliadin/nano silver-chitosan complex film of embodiment offer
Antibacterial effect is more preferable, load wheat gliadin/nano silver chitosan composite antibiotic film (wheat that wherein embodiment 1 provides
Alcohol soluble protein/nano silver colloid particle solution and the volume ratio of chitosan solution are best for 1:10) antibacterial effect.
The dispersibility of loading substance in the film provided using scanning electron microscopic observation embodiment 1 and comparative example, as a result such as Fig. 2 institute
Show.Sample is fixed on special stainless steel sample platform surface by double-sided adhesive by field emission scanning electron microscope (TE-SEM), is used
Gold spraying instrument sprays coating of the thickness less than 20 nm, plated film time 150s in sample surfaces.Sample is taken out, LEO is passed through
1530 VP field emission microscopy observation environmental microbes carry out observation under 15 k V acceleration voltages and take pictures.
Fig. 2 be antibacterial composite membrane scanning electron microscope (SEM) photograph (A, B, C are respectively what embodiment 1, embodiment 2 and embodiment 3 provided
Wheat gliadin/nano silver-chitosan complex film scanning electron microscope (SEM) photograph, wherein wheat gliadin/nano silver colloid particle
The volume ratio of solution and chitosan solution is respectively 1:10,1:20 and 3:20；D, E, F are respectively the load mouse that comparative example 1 provides
The chitosan composite antibiotic film and comparative example 3 for the load silver nitrate that the chitosan composite antibiotic film of tail oxalic acid, comparative example 2 provide mention
The scanning electron microscope (SEM) photograph of the chitosan film of confession；Scale: 1 μm.
As shown in Fig. 2, the film smoother in D, E, F, load has wheat gliadin/nano-Ag particles in A, B, C film,
In contrast rough, the wherein colloidal solid distribution uniform in A film.
Above embodiments are only preferrred embodiment of the present invention, for explaining only the invention, are not intended to limit the present invention, this
Field technical staff should belong to guarantor of the invention without departing from change made under spirit of the invention, replacement, modification etc.
Protect range.
Claims (10)
1. a kind of preparation method of the chitosan composite antibiotic film of load wheat gliadin/nano silver, which is characterized in that including
Following steps:
(1) wheat gliadin is added in ethanol solution, is uniformly mixed and obtains Properties of Wheat Gliadin Solution；Silver nitrate is added
In water, it is uniformly mixed, obtains silver nitrate solution；
(2) carnosic acid is added in ethanol solution, is uniformly mixed and obtains carnosic acid solution；By step (1) silver nitrate
Solution is added in the Properties of Wheat Gliadin Solution, stirs evenly, obtains silver nitrate-Properties of Wheat Gliadin Solution；Then by mouse
Tail oxalic acid solution is added in silver nitrate-Properties of Wheat Gliadin Solution, stirs evenly, obtains mixed liquor；Under stirring, it will mix
It closes liquid and carries out heating water bath processing, be cooled to room temperature, purify, dialysis treatment obtains wheat gliadin/nano silver colloid particle
Suspension；
(3) chitosan is added in the aqueous solution of glacial acetic acid, is stirred evenly, centrifugal treating takes supernatant, and it is molten to obtain chitosan
Liquid；
(4) step (2) wheat gliadin/nano silver colloid particle suspension liquid addition step (3) described chitosan is molten
It in liquid, stirs evenly, obtains mixture；
(5) glycerol is added in step (4) described mixture, stirs evenly, obtains into film liquid, will done at film liquid casting film
Dry processing, then the Balance Treatment in drier, is made the chitosan composite antibiotic of the load wheat gliadin/nano silver
Film.
2. preparation method according to claim 1, which is characterized in that in step (1) described Properties of Wheat Gliadin Solution,
The mass percent concentration of wheat gliadin is 0.1%-1.5%；The concentration of step (1) described silver nitrate solution is
0.005mol/L-0.5mol/L。
3. preparation method according to claim 1, which is characterized in that the mass percent of step (1) described ethanol solution
Concentration is 70%, and the mass percent concentration of step (2) described ethanol solution is 95%.
4. preparation method according to claim 1, which is characterized in that described in step (2) the carnosic acid solution
The mass percent concentration of carnosic acid is 0.05%-1.5%；The volume ratio of the silver nitrate solution and Properties of Wheat Gliadin Solution
For 1-9:1-9；The stirring rate under stirring is 300-600r/min.
5. preparation method according to claim 1, which is characterized in that step (2) silver nitrate solution and carnosic acid
The volume ratio of solution is 1:1；The temperature of heating water bath processing is 37 degrees Celsius, and the time of heating water bath processing is
120min；The mode of step (2) described purifying is one or more of anti-solvent method and revolving method；The dialysis treatment is to use
The bag filter that molecular cut off is 10Da carries out, and the time of dialysis treatment is 24 hours.
6. preparation method according to claim 1, which is characterized in that the volume of the aqueous solution of step (3) described glacial acetic acid
Percent concentration is 0.5%-2%；The mass volume ratio of the aqueous solution of the chitosan and glacial acetic acid is 1-5:100g/mL；It is described
The centrifugation rate of centrifugal treating is 8000-10000rpm, and the time of centrifugal treating is 10-30min.
7. preparation method according to claim 1, which is characterized in that step (4) wheat gliadin/nano-silver colloid
The volume ratio of body particle suspension liquid and chitosan solution is 5-15:100.
8. preparation method according to claim 1, which is characterized in that the quality of step (5) described glycerol is step (3) institute
State the 15%-25% of chitosan mass；The temperature of the drying process is 37-60 degrees Celsius, time of drying process be for 24 hours-
48h。
9. preparation method according to claim 1, which is characterized in that step (5) Balance Treatment in drier
Time is two days or more, and the relative humidity of the Balance Treatment in drier is 58%RH.
10. a kind of load wheat gliadin/nano silver shell as made from claim 1-9 described in any item preparation methods
Glycan composite antibacterial film.
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| CN116023716A (en) * | 2022-10-31 | 2023-04-28 | 华中农业大学 | Layer-by-layer nanoparticle filled fresh-keeping-indicating composite film, preparation method and application |
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Application publication date: 20190917 |