CN107177044A - A kind of collagen-Tea Polyphenols antibacterial film and preparation method thereof - Google Patents
A kind of collagen-Tea Polyphenols antibacterial film and preparation method thereof Download PDFInfo
- Publication number
- CN107177044A CN107177044A CN201610131170.2A CN201610131170A CN107177044A CN 107177044 A CN107177044 A CN 107177044A CN 201610131170 A CN201610131170 A CN 201610131170A CN 107177044 A CN107177044 A CN 107177044A
- Authority
- CN
- China
- Prior art keywords
- tea polyphenols
- collagen
- concentration
- blended liquid
- antibacterial film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
- B65D65/46—Applications of disintegrable, dissolvable or edible materials
- B65D65/463—Edible packaging materials
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
- B65D65/46—Applications of disintegrable, dissolvable or edible materials
- B65D65/466—Bio- or photodegradable packaging materials
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1545—Six-membered rings
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12Q—MEASURING OR TESTING PROCESSES INVOLVING ENZYMES, NUCLEIC ACIDS OR MICROORGANISMS; COMPOSITIONS OR TEST PAPERS THEREFOR; PROCESSES OF PREPARING SUCH COMPOSITIONS; CONDITION-RESPONSIVE CONTROL IN MICROBIOLOGICAL OR ENZYMOLOGICAL PROCESSES
- C12Q1/00—Measuring or testing processes involving enzymes, nucleic acids or microorganisms; Compositions therefor; Processes of preparing such compositions
- C12Q1/02—Measuring or testing processes involving enzymes, nucleic acids or microorganisms; Compositions therefor; Processes of preparing such compositions involving viable microorganisms
- C12Q1/18—Testing for antimicrobial activity of a material
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2389/00—Characterised by the use of proteins; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Zoology (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Immunology (AREA)
- Materials Engineering (AREA)
- Biophysics (AREA)
- Physics & Mathematics (AREA)
- Biotechnology (AREA)
- Toxicology (AREA)
- Microbiology (AREA)
- Molecular Biology (AREA)
- Biodiversity & Conservation Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Food Preservation Except Freezing, Refrigeration, And Drying (AREA)
- Medicinal Preparation (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention provides a kind of preparation method of collagen Tea Polyphenols antibacterial film, comprise the following steps：Modified collagen solution is taken, the Tea Polyphenols of different quality is dissolved in respectively in modified collagen solution, after stirring, the collagen Tea Polyphenols blended liquid of various concentrations is obtained；Collagen Tea Polyphenols blended liquid is subjected to minimal inhibitory concentration experiment, the minimal inhibitory concentration of Tea Polyphenols is obtained；The collagen Tea Polyphenols blended liquid for being more than minimal inhibitory concentration with minimal inhibitory concentration and concentration is subjected to Minimum Bactericidal, the minimum bactericidal concentration of Tea Polyphenols is obtained；Film is taken off after vacuum outgas, casting film-forming will be carried out with minimum bactericidal concentration and close to the collagen Tea Polyphenols blended liquid of minimum bactericidal concentration, collagen Tea Polyphenols antibacterial film is made.The preparation method is drawn after minimal inhibitory concentration and minimum bactericidal concentration, is used to refer to the preparation of impedance mycoderm, and method is simple and easy to apply.
Description
Technical field
The present invention relates to packaging material for food field, and in particular to a kind of collagen-Tea Polyphenols antibacterial film and its system
Preparation Method.
Background technology
Edible packing membrane is scattered and disappeared and nutritional ingredient consumption due to that can reduce the flavor substance of food, prevents micro- life
Thing infects, can effectively extend food storage it is fresh-keeping and sale the time limit, so as to receive significant attention.Numerous
Edible packaging membrane carrier in, collagen is gentle because of its safety non-toxic, nutritious, good film forming
Body barrier property and enjoy favor.But collagen does not have antibacterial activity, to food surface in processing, storage
The microorganism of pollution in fortune and processing procedure is without the effect for suppressing or killing, thus it is in shelf life storage
There is limitation in the length of limit.
In addition, prior art is during packaging film is prepared, packaging film finished-product material is typically first prepared, then will
Finished-product material uses Odontothrips loti to measure the inhibition zone to Escherichia coli or staphylococcus aureus etc. to test into
The antibacterial effect of product material, if the anti-bacterial result that test is obtained is bad, also needs the concentration of adjustment antiseptic again
Packaging film is prepared, then re-test antibacterial effect, until the good packaging film finished-product material of antibacterial effect is obtained,
The preparation method lacks the guidance of science, and preparation method is complicated, time-consuming longer, wastes substantial amounts of time and essence
Power.
The content of the invention
To solve the above problems, the invention provides a kind of preparation method of collagen-Tea Polyphenols antibacterial film, should
Method is first tested the antibacterial effect of Tea Polyphenols, is drawn after minimal inhibitory concentration and minimum bactericidal concentration, is used
To instruct the preparation of antibacterial film, make preparation method more purposive and specific aim, while saving the substantial amounts of time
And energy.
First aspect present invention provides a kind of preparation method of collagen-Tea Polyphenols antibacterial film, including following step
Suddenly：
Modified collagen solution is taken, the Tea Polyphenols of different quality is dissolved in the collagen egg of the modification respectively
In white solution, after stirring, collagen-Tea Polyphenols blended liquid of different Tea Polyphenols concentration is obtained；
The collagen-Tea Polyphenols blended liquid is subjected to minimal inhibitory concentration experiment, the Tea Polyphenols is obtained most
Small Mlc；
To be more than with the minimal inhibitory concentration and concentration the collagen of the minimal inhibitory concentration-
Tea Polyphenols blended liquid carries out Minimum Bactericidal, obtains the minimum bactericidal concentration of the Tea Polyphenols；
Collagen-tea with the minimum bactericidal concentration and concentration close to the minimum bactericidal concentration is more
Phenol blended liquid takes off film after carrying out vacuum outgas, casting film-forming, and collagen-Tea Polyphenols antibacterial film is made.
Wherein, the minimal inhibitory concentration test method is：
The Tea Polyphenols of different quality is dissolved into respectively in modified collagen solution, after stirring, obtained
Tea Polyphenols concentration is respectively 10,5,2.5,1.25,0.625,0.313,0.156,0.078,0.039,0.02
With 0.01mg/mL collagen-Tea Polyphenols blended liquid, hanged by Escherichia coli or with staphylococcus aureus bacterium
Liquid is added in the collagen-Tea Polyphenols blended liquid, and observing in the collagen-Tea Polyphenols blended liquid is
It is no to have macroscopic bacterial precipitation, it is visible by naked eyes the collagen-Tea Polyphenols blended liquid pair of bacterial precipitation
The minimum Tea Polyphenols concentration answered be in collagen-Tea Polyphenols blended liquid Tea Polyphenols to Escherichia coli or to gold
The minimal inhibitory concentration of staphylococcus aureus.
Wherein, in the collagen-Tea Polyphenols blended liquid Tea Polyphenols to Escherichia coli or to staphylococcus aureus
Minimal inhibitory concentration be 0.078-0.156mg/mL.
Wherein, the Minimum Bactericidal method is：
Collagen with the minimal inhibitory concentration-Tea Polyphenols blended liquid and concentration are more than the minimum
The collagen of Mlc-Tea Polyphenols blended liquid is added separately in culture dish and Escherichia coli or golden yellow Portugal
37 DEG C of co-cultivation 24-48h of grape coccus, then observe the bacterial growth situation in the culture dish, no growth bacterium
The corresponding minimum Tea Polyphenols concentration of culture dish fallen be in collagen-Tea Polyphenols blended liquid Tea Polyphenols to big
Enterobacteria or the minimum bactericidal concentration to staphylococcus aureus.
Wherein, in the collagen-Tea Polyphenols blended liquid Tea Polyphenols to Escherichia coli or to staphylococcus aureus
Minimum bactericidal concentration be 0.156-0.313mg/mL.
Wherein, the method for the vacuum outgas is：By the collagen in the environment of vacuum 0.08-0.09Mpa
Albumen-Tea Polyphenols blended liquid degassing 3-6min, repeats after deaerating three times, stands 0.5-1h.
Wherein, after the vacuum outgas, the collagen-Tea Polyphenols blended liquid is subjected to casting film-forming, then
4-20h is dried at 30-60 DEG C, film is taken off after cooling, obtains collagen-Tea Polyphenols antibacterial film.
Wherein, the preparation method of the collagen solution of the modification is：Collagen is dissolved in distilled water,
5-30min is heat-treated at a temperature of 20 DEG C -60 DEG C, the collagen solution of the modification is obtained.
The preparation method for collagen-Tea Polyphenols antibacterial film that first aspect present invention is provided, this method is first more to tea
The antibacterial effect of phenol is tested, and is drawn after minimal inhibitory concentration and minimum bactericidal concentration, is used to refer to impedance mycoderm
Preparation, make preparation method more purposive and specific aim, while saving substantial amounts of time and efforts.
Second aspect of the present invention provides a kind of collagen-Tea Polyphenols antibacterial film, and it is by above-mentioned preparation method system
.
Wherein, the thickness of the collagen-Tea Polyphenols antibacterial film is 0.08-0.12mm.
The collagen that second aspect of the present invention is provided-Tea Polyphenols antibacterial film, including collagen and Tea Polyphenols, two
Person is biodegradable, and biocompatibility is preferable, in addition, the anti-microbial property of Tea Polyphenols is preferably, obtained collagen
Albumen-Tea Polyphenols antibacterial film has Antimicrobial preservative characteristic, can suppress the growth of food microorganisms in storage simultaneously
The secondary pollution of food is avoided, so as to extend the shelf-life of food.
To sum up, beneficial effect of the present invention includes the following aspects：
1st, the invention provides a kind of preparation method of collagen-Tea Polyphenols antibacterial film, the preparation method is advanced
Row bacteriostatic test and sterilization test, are then filmed again, preparation method is had purpose and specific aim, section
Substantial amounts of time and efforts is saved；
2nd, the invention provides a kind of collagen-Tea Polyphenols antibacterial film, with Antimicrobial preservative characteristic, it can press down
The growth of food microorganisms and the secondary pollution of food is avoided in storage processed, so as to extend guaranteeing the quality for food
Phase.
Brief description of the drawings
Fig. 1 is the flow chart of the preparation method of collagen-Tea Polyphenols antibacterial film of the embodiment of the present invention 1；
Fig. 2 is that the embodiment of the present invention 1 tests Tissue Culture Plate of the Tea Polyphenols to the minimal inhibitory concentration of Escherichia coli
Figure；
Fig. 3 is that the embodiment of the present invention 1 tests cell of the Tea Polyphenols to the minimal inhibitory concentration of staphylococcus aureus
Culture plate figure；
Fig. 4 is that the embodiment of the present invention 1 tests culture dish figure of the Tea Polyphenols to the minimum bactericidal concentration of Escherichia coli；
Fig. 5 is that the embodiment of the present invention 1 tests culture of the Tea Polyphenols to the minimum bactericidal concentration of staphylococcus aureus
Ware figure.
Embodiment
As described below is the preferred embodiment of the present invention, it is noted that for the ordinary skill of the art
For personnel, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these change
Enter and retouching is also considered as protection scope of the present invention.
First aspect present invention provides a kind of preparation method of collagen-Tea Polyphenols antibacterial film, including following step
Suddenly：
Modified collagen solution is taken, it is molten that the Tea Polyphenols of different quality is dissolved in into modified collagen respectively
In liquid, after stirring, collagen-Tea Polyphenols blended liquid of different Tea Polyphenols concentration is obtained；
Collagen-Tea Polyphenols blended liquid is subjected to minimal inhibitory concentration experiment, the minimum antibacterial dense of Tea Polyphenols is obtained
Degree；
Collagen-Tea Polyphenols blended liquid of minimal inhibitory concentration will be more than with minimal inhibitory concentration and concentration
Minimum Bactericidal is carried out, the minimum bactericidal concentration of Tea Polyphenols is obtained；
By with minimum bactericidal concentration and concentration close to minimum bactericidal concentration collagen-Tea Polyphenols blended liquid
Film is taken off after carrying out vacuum outgas, casting film-forming, collagen-Tea Polyphenols antibacterial film is made.
In embodiment of the present invention, collagen is NTx albumen.
In embodiment of the present invention, collagen is extracted from fish scale, ox-hide or pigskin and obtained.
In a preferred embodiment of the invention, collagen is fish scale collagen, the purity of fish scale collagen
More than 90%.
Tea Polyphenols, also known as tea tannin, tea boots matter, are the general names of light base class compound more than the class contained by tealeaves.
It is highly profitable to healthy.Natural Antioxidant Tea Polyphenol, be proved to antibacterial, it is anti-oxidant, anti-cancer,
Reduce plurality of health care functions and the pharmacodynamics effects such as cholesterol.
Collagen and Tea Polyphenols are mixed for preparing collagen-Tea Polyphenols antibacterial film by the present invention, can suppress food
The growth of product surface microorganism, so as to reach food fresh keeping and the effect of Shelf-life.Meanwhile, collagen
- Tea Polyphenols antibacterial film can be biodegradable, and environment will not be polluted.
In embodiment of the present invention, modified collagen solution obtains collagen progress heat modification.
In embodiment of the present invention, thermally-denatured method is：Collagen is dissolved in distilled water,
5-30min is heat-treated at a temperature of 20 DEG C -60 DEG C, modified collagen solution is obtained.
Unmodified collagen is insoluble in water, and mechanical property and film forming ability are poor, modified, collagen
The degree of cross linking is higher, mechanical strength and it is thermally-stabilised preferably, while may be uniformly dispersed in distilled water, it is easy to film forming.
In embodiment of the present invention, the concentration of modified collagen solution is 0.03g/mL-0.07g/mL.If
Collagen content is less in collagen solution, it may be difficult to the preferable antibacterial film of bridging property is obtained, if collagen
Albumen is higher, and being prepared into for antibacterial film is originally considerably improved, therefore, the modified collagen solution of the present invention
Concentration is 0.03g/mL-0.07g/mL.
In a preferred embodiment of the invention, the concentration of modified collagen solution is 0.05g/mL.
In embodiment of the present invention, mixing speed is 2000-5000r/min.
In embodiment of the present invention, the concentration difference of Tea Polyphenols in collagen-Tea Polyphenols blended liquid of various concentrations
For 10,5,2.5,1.25,0.625,0.313,0.156,0.078,0.039,0.02 and 0.01mg/mL.
In embodiment of the present invention, minimal inhibitory concentration method of testing is：
The Tea Polyphenols of different quality is dissolved into respectively in modified collagen solution, after stirring, obtained
Tea Polyphenols concentration is respectively 10,5,2.5,1.25,0.625,0.313,0.156,0.078,0.039,0.02
With 0.01mg/mL collagen-Tea Polyphenols blended liquid, hanged by Escherichia coli or with staphylococcus aureus bacterium
Liquid is added in collagen-Tea Polyphenols blended liquid, whether has naked eyes in observation collagen-Tea Polyphenols blended liquid
Visible bacterial precipitation, is visible by naked eyes collagen-corresponding Cmin of Tea Polyphenols blended liquid of bacterial precipitation
As Tea Polyphenols is to Escherichia coli or to the minimal inhibitory concentration of staphylococcus aureus.
The minimal inhibitory concentration method of testing that embodiment of the present invention is provided, by collagen-Tea Polyphenols blended liquid and
Whether after bacteria suspension mixing, need to only visually observe in collagen-Tea Polyphenols blended liquid can obtain containing bacterial precipitation
To minimal inhibitory concentration, method of testing is simply, intuitively, it is not necessary to which bacterium and collagen-Tea Polyphenols is common
Mix liquid culture re-test for a period of time, it is easy to operate.
In embodiment of the present invention, the collagen of various concentrations-Tea Polyphenols blended liquid is placed in 96 orifice plates.
It is usually to be operated in test tube when testing minimal inhibitory concentration, but when using tube manipulation, the solution body of consuming
Generally tens milliliters of product, is wasted more serious.The present invention carries out minimal inhibitory concentration experiment using 96 orifice plates,
The liquor capacity added per hole is only several milliliters, greatlys save experimentation cost.
In embodiment of the present invention, the clump count of Escherichia coli is 10 in 96 orifice plates4-106cfu/mL。
In embodiment of the present invention, the clump count of staphylococcus aureus is 10 in 96 orifice plates4-106cfu/mL。
In embodiment of the present invention, minimum bactericidal concentration method of testing is：
Collagen with minimal inhibitory concentration-Tea Polyphenols blended liquid and concentration are more than minimal inhibitory concentration
Collagen-Tea Polyphenols blended liquid be added separately in culture dish and Escherichia coli or staphylococcus aureus
37 DEG C of co-cultivation 24-48h, then observe the bacterial growth situation in culture dish, the culture dish pair of no growth bacterium colony
The Cmin answered as minimum bactericidal concentration.
In embodiment of the present invention, the clump count of the Escherichia coli in culture dish is 104-106cfu/mL。
In embodiment of the present invention, the clump count of the staphylococcus aureus in culture dish is 104-106cfu/mL。
In embodiment of the present invention, agar medium is contained in culture dish.
The minimum bactericidal concentration method of testing that embodiment of the present invention is provided, is obtaining minimal inhibitory concentration result
Afterwards, minimum bactericidal concentration is tested according to minimal inhibitory concentration, method is simple, directly perceived, is not required to from multiple different
Test obtains minimum bactericidal concentration in the collagen of concentration-Tea Polyphenols blended liquid, and process of the test is more brief.
In embodiment of the present invention, the minimal inhibitory concentration of Tea Polyphenols is in collagen-Tea Polyphenols blended liquid
0.078-0.156mg/mL。
In embodiment of the present invention, the minimum bactericidal concentration of Tea Polyphenols is in collagen-Tea Polyphenols blended liquid
0.156-0.313mg/mL。
In specific experiment or production process, final collagen-Tea Polyphenols can be selected common according to the actual requirements
The concentration of Tea Polyphenols in mixed liquid, it is such as more preferable for the antibacterial effect of collagen-Tea Polyphenols antibacterial film, it can select
Concentration is more than collagen-Tea Polyphenols blended liquid of minimum bactericidal concentration.
When collagen is mixed with Tea Polyphenols, easily chemically react, such as the carboxylic in collagen
The hydroxyl of base and Tea Polyphenols reacts, so that antibacterial effect can be influenceed, therefore collagen-Tea Polyphenols antibacterial film
Antibacterial effect and the antibacterial effect of independent Tea Polyphenols be different.Prior art tests the antibacterial effect of Tea Polyphenols
When, it is usually that Tea Polyphenols is soluble in water, so as to test the antibacterial effect of the Tea Polyphenols aqueous solution.And the present invention is surveyed
The antibacterial effect of Tea Polyphenols in collagen-Tea Polyphenols blended liquid is tried, it is as a result more accurate.
In embodiment of the present invention, the method that collagen-Tea Polyphenols blended liquid is carried out into vacuum outgas is：True
By collagen-Tea Polyphenols blended liquid degassing 3-6min in the environment of reciprocal of duty cycle 0.08-0.09Mpa, degassing three is repeated
After secondary, 0.5-1h is stood.The purpose of degassing is the gas to be wrapped up in removing coating liquid, helps to be distributed
Uniform antibacterial film.
In embodiment of the present invention, collagen-Tea Polyphenols blended liquid is subjected to casting film-forming, at 30-60 DEG C
4-20h is dried, film is taken off after cooling, obtains collagen-Tea Polyphenols antibacterial film.
In embodiment of the present invention, by collagen-Tea Polyphenols blended liquid casting film-forming on poly (methyl methacrylate) plate.
In embodiment of the present invention, collagen-Tea Polyphenols blended liquid is settled to after 100mL, then is cast into
Film.
In embodiment of the present invention, film is taken off after drying cooling, in 25 ± 1 DEG C of temperature, humidity is 50 ± 1% perseverance
48h is balanced in constant temperature and humidity case, collagen-Tea Polyphenols antibacterial film is obtained.
In embodiment of the present invention, the thickness of collagen-Tea Polyphenols antibacterial film is 0.08-0.12mm.
It is antibacterial using testing again that the preparation method for the antibacterial film that prior art is generally provided needs first to prepare finished product
The method of loop diameter carrys out anti-microbial property test, and antibacterial test method generally requires the completion of aptitude test in 3 days, in addition,
This method can only be qualitative, it is impossible to directly obtains the minimal inhibitory concentration and minimum bactericidal concentration of antibacterial film.If anti-
Bacterium test effect is bad, and also adjusting the proportioning of raw material, re-test prepares antibacterial film again, subsequently also to be resisted
Bacterium is tested, and the preparation method more blindly, lacks and instructed, and preparation method complexity is cumbersome.
First aspect present invention provide collagen-Tea Polyphenols antibacterial film preparation method, prepare antibacterial film it
The minimal inhibitory concentration and minimum bactericidal concentration of Tea Polyphenols in preceding first test collagen-Tea Polyphenols blended liquid,
To after minimal inhibitory concentration and minimum bactericidal concentration, the preparation of impedance mycoderm can be used to refer to, such as be can confirm that anti-
Antibacterial effect preferably, makes the preparation of antibacterial film more purposive and is directed to when polyphenol content is how many in mycoderm
Property, it is to avoid prior art needs repeatedly to prepare the problem of preparation method that antibacterial film causes is complicated, method
Simply, intuitively.
Second aspect of the present invention provides a kind of collagen-Tea Polyphenols antibacterial film, and it is by above-mentioned preparation method system
.
In embodiment of the present invention, the thickness of collagen-Tea Polyphenols antibacterial film is 0.08-0.12mm.
The collagen that the present invention is provided-Tea Polyphenols antibacterial film, available for packaging for foodstuff, be particularly suitable for use in deep-sea fish
Packaging.
The collagen that second aspect of the present invention is provided-Tea Polyphenols antibacterial film, including collagen and Tea Polyphenols, two
Person is biodegradable, and biocompatibility is preferable, in addition, the anti-microbial property of Tea Polyphenols is preferably, obtained collagen
Albumen-Tea Polyphenols antibacterial film has Antimicrobial preservative characteristic, can suppress the growth of food microorganisms in storage simultaneously
The secondary pollution of food is avoided, so as to extend the shelf-life of food.Collagen-Tea Polyphenols that the present invention is obtained resists
Mycoderm can apply to the fresh-keeping of food.
Embodiment 1：
The preparation method schematic flow sheet of reference picture 1, a kind of preparation method of collagen-Tea Polyphenols antibacterial film,
Comprise the following steps：
(1) collagen heat modification：Weigh 5g fish scale collagens to be dissolved in 95mL distilled water, heat modification temperature
Spend for 20 DEG C, the heat modification time is 30min, obtains modified collagen solution；
(2) Tea Polyphenols minimal inhibitory concentration is tested：A certain amount of Tea Polyphenols is weighed, modified glue is dissolved in respectively
Former protein solution, speed of agitator is 2000r/min, the ultimate density for obtaining Tea Polyphenols is respectively 10,5,2.5,
1.25th, 0.625,0.313,0.156,0.078,0.039,0.02 and 0.01mg/mL collagen-Tea Polyphenols
Blended liquid；
Take sterile 96 porocyte culture plates, by Tea Polyphenols concentration be respectively 10,5,2.5,1.25,0.625,0.313,
0.156th, 0.078,0.039,0.02 and 0.01mg/mL collagen-Tea Polyphenols blended liquid is respectively placed in 96 holes
The 1st in Tissue Culture Plate arrange the 1st pipe into the 11st pipe and the 2nd row the 1st pipe into the 11st pipe, then
2 arrange in the often pipe of the 1st pipe to the 11st pipe Escherichia coli in addition Escherichia coli bacteria suspension, 96 porocyte culture plates
Clump count is about 105CFU/ml；Whether compare in the 1st row, the 2nd row's culture plate of observation has macroscopic bacterium
Precipitation, is visible by naked eyes the corresponding Cmin of the culture plate as Tea Polyphenols that the culture plate of bacterial precipitation is clarified
To the minimal inhibitory concentration of Escherichia coli.In the same manner, test Tea Polyphenols is to staphylococcus aureus
The clump count of staphylococcus aureus is about 10 in minimal inhibitory concentration, 96 porocyte culture plates5CFU/ml.Fig. 2
Tissue Culture Plate figure of the Tea Polyphenols to the minimal inhibitory concentration of Escherichia coli is tested for the embodiment of the present invention 1；From Fig. 2
In as can be seen that the 2nd arrange 1-7 pipe for clarification, since the 8th pipe, solution is more muddy, therefore, it can really
Fixed 7th concentration for managing corresponding Tea Polyphenols is minimal inhibitory concentration, and Tea Polyphenols is to the minimum antibacterial dense of Escherichia coli
Spend for 0.156mg/mL.Fig. 3 is that the embodiment of the present invention 1 tests Tea Polyphenols to the minimum antibacterial of staphylococcus aureus
The Tissue Culture Plate figure of concentration；From figure 3, it can be seen that the 2nd arranges test tube of the 1-7 pipes for clarification, from the 8th pipe
Start, solution is more muddy, hence, it can be determined that the concentration of the corresponding Tea Polyphenols of the 7th pipe is minimum antibacterial dense
Degree, Tea Polyphenols is 0.156mg/mL to the minimal inhibitory concentration of staphylococcus aureus.
(3) Tea Polyphenols Minimum Bactericidal：
The collagen for being 0.156mg/mL by concentration-Tea Polyphenols blended liquid and concentration are 10,5,2.5,1.25,
0.625 and 0.313mg/mL collagen-Tea Polyphenols blended liquid is added separately in 7 agar plates, in training
By drawing board method inoculation Escherichia coli in foster ware, the clump count of Escherichia coli is about 10 in culture dish5CFU/ml；
37 DEG C are incubated the bacterial growth situation after 24h in observation culture dish, the corresponding minimum of culture dish of no growth bacterium colony
Concentration is minimum bactericidal concentration of the Tea Polyphenols to Escherichia coli.Fig. 4 is that the embodiment of the present invention 1 tests Tea Polyphenols pair
The culture dish figure of the minimum bactericidal concentration of Escherichia coli；Figure 4, it is seen that not given birth in 7 culture dishes
Long E. coli clones, it may be determined that minimal inhibitory concentration is that minimum bactericidal concentration is 0.156mg/mL.Press
According to identical method, concentration is by test Tea Polyphenols to the minimum bactericidal concentration of staphylococcus aureus
0.156mg/mL collagen-Tea Polyphenols blended liquid and concentration are 10,5,2.5,1.25,0.625 and
0.313mg/mL collagen-Tea Polyphenols blended liquid is added separately in 7 agar plates, in culture dish
The clump count for being inoculated with staphylococcus aureus in staphylococcus aureus, culture dish is about 105CFU/ml；37℃
It is incubated the bacterial growth situation in observation culture dish after 24h.Fig. 5 is that the embodiment of the present invention 1 tests Tea Polyphenols to gold
The culture dish figure of the minimum bactericidal concentration of staphylococcus aureus.From figure 5 it can be seen that not having in 7 culture dishes
There are growth E. coli clones, hence, it can be determined that minimum bactericidal concentration of the Tea Polyphenols to staphylococcus aureus
For 0.156mg/mL.
(4) vacuum outgas：By collagen-Tea Polyphenols blended liquid cooling of the Tea Polyphenols concentration for 0.156mg/mL
To room temperature (23 DEG C), deaerate 6min under vacuum 0.08Mpa environment, in triplicate, then stands 0.5h.
(5) casting film-forming：Collagen-Tea Polyphenols blended liquid is settled to 100mL, that is, takes 100mL vacuum
Tea Polyphenols concentration after degassing is cast to poly (methyl methacrylate) plate for 0.156mg/mL collagen-Tea Polyphenols blended liquid
On, 20h is dried at 30 DEG C, notices that poly (methyl methacrylate) plate keeps level.Film is taken off after drying cooling, in temperature 25
± 1 DEG C, 48h is balanced in the climatic chamber of humidity 50 ± 1%, and collagen-Tea Polyphenols antibacterial film is made,
The thickness of the collagen-Tea Polyphenols antibacterial film is 0.08mm.
Embodiment 2：
A kind of preparation method of collagen-Tea Polyphenols antibacterial film, comprises the following steps：
(1) collagen heat modification：Weigh 3g fish scale collagens to be dissolved in 97mL distilled water, heat modification temperature
Spend for 60 DEG C, the heat modification time is 5min, obtains modified collagen solution；
(2) the step of be the same as Example 1 (2)；
(3) the step of be the same as Example 1 (3)；
(4) vacuum outgas：By collagen-Tea Polyphenols blended liquid cooling of the Tea Polyphenols concentration for 0.156mg/mL
To room temperature (23 DEG C), deaerate 3min under vacuum 0.09Mpa environment, in triplicate, then stands 1h；
(5) casting film-forming：Collagen-Tea Polyphenols blended liquid is settled to 100mL, that is, takes 100mL vacuum
Tea Polyphenols concentration after degassing is cast to poly (methyl methacrylate) plate for 0.156mg/mL collagen-Tea Polyphenols blended liquid
On, 4h is dried at 60 DEG C, notices that poly (methyl methacrylate) plate keeps level.Dry cooling after take off film, temperature 25 ±
1 DEG C, 48h is balanced in the climatic chamber of humidity 50 ± 1%, and collagen-Tea Polyphenols antibacterial film is made, should
The thickness of collagen-Tea Polyphenols antibacterial film is 0.10mm.
Embodiment 3：
A kind of preparation method of collagen-Tea Polyphenols antibacterial film, comprises the following steps：
(1) collagen heat modification：Weigh 7g fish scale collagens to be dissolved in 93mL distilled water, heat modification temperature
Spend for 40 DEG C, the heat modification time is 10min, obtains modified collagen solution；
(2) the step of be the same as Example 1 (2)；
(3) the step of be the same as Example 1 (3)；
(4) vacuum outgas：By collagen-Tea Polyphenols blended liquid cooling of the Tea Polyphenols concentration for 0.156mg/mL
To room temperature (23 DEG C), deaerate 4min under vacuum 0.09Mpa environment, in triplicate, then stands 0.7h；
(5) casting film-forming：Collagen-Tea Polyphenols blended liquid is settled to 100mL, that is, takes 100mL vacuum
Tea Polyphenols concentration after degassing is cast to poly (methyl methacrylate) plate for 0.156mg/mL collagen-Tea Polyphenols blended liquid
On, 10h is dried at 40 DEG C, notices that poly (methyl methacrylate) plate keeps level.Film is taken off after drying cooling, in temperature 25
± 1 DEG C, 48h is balanced in the climatic chamber of humidity 50 ± 1%, and collagen-Tea Polyphenols antibacterial film is made,
The thickness of the collagen-Tea Polyphenols antibacterial film is 0.12mm.
Effect example：
It is as follows there is provided effect example for the beneficial effect that provides powerful support for the embodiment of the present invention, to evaluate and test this hair
The performance for the product that bright embodiment is provided.
Collagen made from embodiment 1-Tea Polyphenols antibacterial film is used for the salmon of packaging fresh, set simultaneously
Blank sample, blank sample refers to not cooking the salmon of any processing, always micro- in the salmon of test 0-7 days
Biological indicators.
Table 1
Remarks：N represents that bacterium colony is too many, leads to not count.
From table 1 it follows that using the bacterial content in the salmon of collagen-Tea Polyphenols antibacterial film packaging
To be substantially reduced than blank sample, this can illustrate, using collagen made from the inventive method-Tea Polyphenols antibacterial
The antibacterial effect of film preferably, can be advantageously applied to the packaging of food.
Embodiment described above only expresses the several embodiments of the present invention, and it describes more specific and detailed,
But therefore it can not be interpreted as the limitation to the scope of the claims of the present invention.It should be pointed out that for this area
For those of ordinary skill, without departing from the inventive concept of the premise, various modifications and improvements can be made,
These belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be with appended claims
It is defined.
Claims (10)
1. the preparation method of a kind of collagen-Tea Polyphenols antibacterial film, it is characterised in that comprise the following steps：
Modified collagen solution is taken, the Tea Polyphenols of different quality is dissolved in the collagen of the modification respectively
In protein solution, after stirring, collagen-Tea Polyphenols blended liquid of different Tea Polyphenols concentration is obtained；
The collagen-Tea Polyphenols blended liquid is subjected to minimal inhibitory concentration experiment, the Tea Polyphenols is obtained
Minimal inhibitory concentration；
To be more than with the minimal inhibitory concentration and concentration the collagen of the minimal inhibitory concentration-
Tea Polyphenols blended liquid carries out Minimum Bactericidal, obtains the minimum bactericidal concentration of the Tea Polyphenols；
Collagen-tea with the minimum bactericidal concentration and concentration close to the minimum bactericidal concentration is more
Phenol blended liquid takes off film after carrying out vacuum outgas, casting film-forming, and collagen-Tea Polyphenols antibacterial film is made.
2. the preparation method of collagen as claimed in claim 1-Tea Polyphenols antibacterial film, it is characterised in that
The minimal inhibitory concentration test method is：
The Tea Polyphenols of different quality is dissolved into respectively in modified collagen solution, after stirring, obtained
To Tea Polyphenols concentration be respectively 10,5,2.5,1.25,0.625,0.313,0.156,0.078,0.039,
0.02 and 0.01mg/mL collagen-Tea Polyphenols blended liquid, by Escherichia coli or and staphylococcus aureus
Bacteria suspension is added in the collagen-Tea Polyphenols blended liquid, observes the collagen-Tea Polyphenols blended liquid
In whether have macroscopic bacterial precipitation, the collagen-Tea Polyphenols for being visible by naked eyes bacterial precipitation is common
The mixed corresponding minimum Tea Polyphenols concentration of liquid be in collagen-Tea Polyphenols blended liquid Tea Polyphenols to Escherichia coli
Or to the minimal inhibitory concentration of staphylococcus aureus.
3. the preparation method of collagen as claimed in claim 2-Tea Polyphenols antibacterial film, it is characterised in that
Tea Polyphenols presses down to Escherichia coli or to the minimum of staphylococcus aureus in the collagen-Tea Polyphenols blended liquid
Bacteria concentration is 0.078-0.156mg/mL.
4. the preparation method of collagen as claimed in claim 1-Tea Polyphenols antibacterial film, it is characterised in that
The Minimum Bactericidal method is：
Collagen with the minimal inhibitory concentration-Tea Polyphenols blended liquid and concentration are more than the minimum
The collagen of Mlc-Tea Polyphenols blended liquid is added separately in culture dish and Escherichia coli or golden yellow Portugal
37 DEG C of co-cultivation 24-48h of grape coccus, then observe the bacterial growth situation in the culture dish, no growth bacterium
The corresponding minimum Tea Polyphenols concentration of culture dish fallen be in collagen-Tea Polyphenols blended liquid Tea Polyphenols to big
Enterobacteria or the minimum bactericidal concentration to staphylococcus aureus.
5. the preparation method of collagen as claimed in claim 4-Tea Polyphenols antibacterial film, it is characterised in that
Tea Polyphenols is killed to Escherichia coli or to the minimum of staphylococcus aureus in the collagen-Tea Polyphenols blended liquid
Bacteria concentration is 0.156-0.313mg/mL.
6. the preparation method of collagen as claimed in claim 1-Tea Polyphenols antibacterial film, it is characterised in that
The method of the vacuum outgas is：It is in the environment of vacuum 0.08-0.09Mpa that the collagen-tea is more
Phenol blended liquid degassing 3-6min, repeats after deaerating three times, stands 0.5-1h.
7. the preparation method of collagen as claimed in claim 1-Tea Polyphenols antibacterial film, it is characterised in that
After the vacuum outgas, the collagen-Tea Polyphenols blended liquid is subjected to casting film-forming, then at 30-60 DEG C
Lower dry 4-20h, film is taken off after cooling, obtains collagen-Tea Polyphenols antibacterial film.
8. the preparation method of collagen as claimed in claim 1-Tea Polyphenols antibacterial film, it is characterised in that
The preparation method of the collagen solution of the modification is：Collagen is dissolved in distilled water,
5-30min is heat-treated at a temperature of 20 DEG C -60 DEG C, the collagen solution of the modification is obtained.
9. a kind of collagen-Tea Polyphenols antibacterial film, it is characterised in that the collagen-Tea Polyphenols antibacterial
Film is as made from any one of the claim 1-8 preparation methods.
10. collagen as claimed in claim 9-Tea Polyphenols antibacterial film, it is characterised in that the collagen egg
The thickness of in vain-Tea Polyphenols antibacterial film is 0.08-0.12mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610131170.2A CN107177044A (en) | 2016-03-09 | 2016-03-09 | A kind of collagen-Tea Polyphenols antibacterial film and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610131170.2A CN107177044A (en) | 2016-03-09 | 2016-03-09 | A kind of collagen-Tea Polyphenols antibacterial film and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107177044A true CN107177044A (en) | 2017-09-19 |
Family
ID=59829818
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610131170.2A Pending CN107177044A (en) | 2016-03-09 | 2016-03-09 | A kind of collagen-Tea Polyphenols antibacterial film and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107177044A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111607114A (en) * | 2020-06-16 | 2020-09-01 | 陕西科技大学 | Preparation method of green degradable multifunctional collagen-based nano composite membrane |
| CN114938847A (en) * | 2022-05-24 | 2022-08-26 | 江南大学 | Processing method of high-quality instant fish gelatin and instant fish gelatin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020779A (en) * | 2010-11-17 | 2011-04-20 | 河南工业大学 | Preparation method of edible anti-bacterial packaging film |
| CN102250368A (en) * | 2011-05-19 | 2011-11-23 | 四川大学 | Edible collagen-based food packaging film and preparation method thereof |
| CN104974531A (en) * | 2015-07-09 | 2015-10-14 | 浙江海洋学院 | Method for preparing antibacterial and antioxidant composite film by using scale |
-
2016
- 2016-03-09 CN CN201610131170.2A patent/CN107177044A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102020779A (en) * | 2010-11-17 | 2011-04-20 | 河南工业大学 | Preparation method of edible anti-bacterial packaging film |
| CN102250368A (en) * | 2011-05-19 | 2011-11-23 | 四川大学 | Edible collagen-based food packaging film and preparation method thereof |
| CN104974531A (en) * | 2015-07-09 | 2015-10-14 | 浙江海洋学院 | Method for preparing antibacterial and antioxidant composite film by using scale |
Non-Patent Citations (2)
| Title |
|---|
| 李凡 刘永茂 主编: "《基础医学实验教程》", 30 September 2002 * |
| 胡建平 编著: "《鱼胶原蛋白的开发与应用》", 31 March 2014 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111607114A (en) * | 2020-06-16 | 2020-09-01 | 陕西科技大学 | Preparation method of green degradable multifunctional collagen-based nano composite membrane |
| CN111607114B (en) * | 2020-06-16 | 2022-09-27 | 陕西科技大学 | Preparation method of green degradable multifunctional collagen-based nano composite membrane |
| US11613616B2 (en) | 2020-06-16 | 2023-03-28 | Shaanxi University Of Science & Technology | Preparation method of green, biodegradable, and multifunctional collagen-based nanocomposite film |
| CN114938847A (en) * | 2022-05-24 | 2022-08-26 | 江南大学 | Processing method of high-quality instant fish gelatin and instant fish gelatin |
| CN114938847B (en) * | 2022-05-24 | 2024-03-22 | 江南大学 | Processing method of high-quality instant fish gelatin and instant fish gelatin |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108434954B (en) | It is a kind of multi-functional except formaldehyde deodorization eliminating smell agent | |
| CN103012827B (en) | Manufacturing method of chitosan-PE double-layer bacteriostatic preservative film | |
| JP2008278890A (en) | New microorganism | |
| CN104756983A (en) | Fresh flower antistaling agent and preparation method thereof | |
| CN107582459B (en) | A kind of preservative and preparation method thereof containing Fructus Forsythiae | |
| CN106236772B (en) | Pasture disinfectant for nipples of dairy cows and its preparation method and application | |
| CN113351125A (en) | Citrus essential oil microcapsule and preparation method and application thereof | |
| CN108714138A (en) | Betagen Solution and preparation method thereof | |
| CN107177044A (en) | A kind of collagen-Tea Polyphenols antibacterial film and preparation method thereof | |
| CN107177046A (en) | A kind of collagen-Herba Origani Vulgaris quintessence oil antibacterial film and preparation method thereof | |
| CN107177045A (en) | A kind of collagen-lysozyme antibiotic film and preparation method thereof | |
| CN102640781B (en) | Fresh meat composite biological preservative and preparation method of fresh meat composite biological preservative | |
| Jensen et al. | Nutritional yeast culture has specific anti-microbial properties without affecting healthy flora. Preliminary results | |
| CN107853377A (en) | The bio-preservative of cold freshly-slaughtered poultry | |
| CN101297658A (en) | Method for reducing survival rate of salmonella on egg surface by ozonated water | |
| Cibik et al. | The antibacterial effect of silver anode treatment on raw milk | |
| CN109645101A (en) | A kind of composite preservative and preparation method thereof for birds, beasts and eggs storage | |
| CN105124714B (en) | A kind of low temperature pre-cooling extends the preservation technology of fresh flour normal-temperature shelf life | |
| CN105001431B (en) | The preparation method of the edibility antibacterial film liquid of the chelating agent containing tfe polymer and application | |
| ElNasri et al. | Packaging type and their effects on the chemical and microbial quality of Sudanese white cheese (Gibna bayda) | |
| Duran et al. | The Evaluation of the Antibacterial Effect of Silver Anode Treatment on Raw Milk | |
| CN108329630A (en) | A kind of aquatic products antibacterial deodorization preservative film and preparation method thereof | |
| CN109122815A (en) | The fresh-keeping film liquid of hydrophobically modified gel-type and preparation containing glycine betaine for meat | |
| CN105801666B (en) | Preparation method and application of miichthys miiuy swim bladder protein peptide | |
| Renur et al. | Application of chitosan and Chinese lemon extract (Citrus mitis) based edible coating on tuna fillet |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170919 |