CN111073188A - Preparation method and application of antibacterial composite membrane for fresh aquatic products - Google Patents
Preparation method and application of antibacterial composite membrane for fresh aquatic products Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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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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- 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
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- 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
- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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Abstract
The invention discloses a preparation method of an antibacterial composite film for fresh aquatic products, which comprises the following steps: preparing a polyvinyl alcohol aqueous solution and a chitosan acetic acid solution, uniformly mixing the polyvinyl alcohol aqueous solution and the chitosan acetic acid solution, flatly paving the mixture in a container, and cooling to 20-25 ℃ to obtain hydrogel; and repeatedly freezing and thawing the hydrogel to prepare the antibacterial composite membrane for the fresh aquatic products. The preparation method of the antibacterial composite film for fresh aquatic products is simple, economic and strong in operability, has good mechanical properties, can be used for inhibiting the growth of putrefying bacteria and pathogenic bacteria, can ensure the quality and economic value of food, can ensure the edible safety of the food, and has good application prospects in the aspects of fresh aquatic product packaging and the like.
Description
Technical Field
The invention belongs to the technical field of food packaging and the field of polymer film materials, and particularly relates to a preparation method and application of an antibacterial composite film for fresh aquatic products.
Background
The aquatic product has rich nutrition, fine meat quality and easy absorption by human body, thereby gaining the favor of consumers. With the continuous improvement of living standard, the proportion of the fresh food and aquatic products in the market is increased year by year in recent years. However, fresh food and aquatic products are not treated in a violent processing and sterilization mode, so that the fresh food and aquatic products are easily polluted by putrefying bacteria and the like, and if the fresh food and aquatic products are polluted by the putrefying bacteria, the problems of production quality such as generation of bad smell, reduction of food quality and the like can be caused, so that the edible value and the economic value of the fresh food and aquatic products are lost; and the pathogenic bacteria pollution can directly threaten the physical health of consumers. Therefore, in order to effectively inhibit the growth of spoilage bacteria and pathogenic bacteria in fresh aquatic products and guarantee the use safety of the fresh aquatic products, the development of an antibacterial preservative film with application value is urgently needed.
Chitosan (CS) is a natural polysaccharide consisting of glucosamine and N-acetylglucosamine units. The chitosan has cationic property, can interact with microbial cell membranes with negative charges to cause the osmotic pressure of microbial cell walls to change and substances in cells to leak, thereby playing a role in bacteriostasis and being a good food fresh-keeping bacteriostat. However, chitosan has poor mechanical properties and low stretchability, and still has the problems of poor adhesion with food and the like in the process of preparing the preservative film.
At present, in order to ensure that film products have good stretchability and elasticity, most of preservative films in the market are PE films, PVC films and PVDC films, but the films are difficult to degrade and even cause environmental pollution and food safety problems. Polyvinyl alcohol (PVA) is a polyhydroxy polymer, has no toxicity, stable performance, good wear resistance, bonding force and solvent resistance, and can form a film with smooth, tough and tear-resistant surface. And the water solubility and the biodegradability of the polyvinyl alcohol have no toxic or side effect on a human body, so that the polyvinyl alcohol can be used as an environment-friendly packaging material, but the polyvinyl alcohol has no antibacterial property and cannot be used as an antibacterial composite film.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and better ensure the quality and the safety of food. On the premise of considering the environmental protection problem, the antibacterial composite film for fresh aquatic products is prepared from polyvinyl alcohol and chitosan, so that the defect that the polyvinyl alcohol film has no antibacterial property can be improved, and the defect that the mechanical property of the chitosan film is insufficient is overcome.
In order to achieve the purpose, the invention provides a preparation method of an antibacterial composite film for fresh aquatic products, and the composite film prepared by the method has higher mechanical strength and antibacterial performance, and can greatly solve the problem of food spoilage caused by microorganisms in the processes of food processing, transportation and storage.
A preparation method of an antibacterial composite membrane for fresh aquatic products comprises the following steps:
s1, preparing a polyvinyl alcohol aqueous solution: preparing a polyvinyl alcohol aqueous solution with the polyvinyl alcohol concentration of 25-250 g/L by using polyvinyl alcohol and water;
s2, preparing a chitosan acetic acid solution: diluting glacial acetic acid into an acetic acid solution with the volume fraction of 0.1-10%, adding chitosan into the acetic acid solution, and uniformly stirring to prepare a chitosan acetic acid solution with the chitosan concentration of 10-100 g/L;
s3, mixing: mixing the polyvinyl alcohol aqueous solution obtained in the step S1 with the chitosan acetic acid solution obtained in the step S2, and stirring and uniformly mixing at 90-100 ℃ to obtain a mixed solution; flatly paving the mixed solution in a container, wherein the depth of the mixed solution is 1-2 mm, and cooling to 20-25 ℃ to obtain hydrogel; the mixed solution consists of polyvinyl alcohol aqueous solution and chitosan acetic acid solution according to the following volume percentage: 33.4 to 66.6 percent of polyvinyl alcohol aqueous solution and 33.4 to 66.6 percent of chitosan acetic acid solution;
s4, freeze thawing: placing the hydrogel obtained in the step S3 in an environment with the temperature of-20 to-80 ℃ for freezing for 3 to 34 hours, and then placing the hydrogel at the temperature of 4 to 30 ℃ for thawing for 2 to 24 hours;
s5: and (5) repeating the freeze thawing of the step S4 for 5-10 times to obtain the antibacterial composite membrane for the fresh aquatic products.
In a preferred embodiment, the preparing the aqueous solution of polyvinyl alcohol in step S1 specifically includes: adding polyvinyl alcohol into water, stirring at 90-100 ℃ and 300-800 rpm for 1-3 h, and preparing a polyvinyl alcohol aqueous solution with the polyvinyl alcohol concentration of 25-250 g/L.
In a preferable mode, the stirring and blending in step S2 is: stirring at 300-800 rpm for 1-3 h.
In a preferable mode, the stirring and blending in step S3 is: stirring at 300-800 rpm for 1-3 h.
In a preferred mode, the preparation method of the antibacterial composite membrane for fresh aquatic products comprises the following steps:
s1, preparing a polyvinyl alcohol aqueous solution: weighing 4g of polyvinyl alcohol, adding the polyvinyl alcohol into 40mL of deionized water, stirring at 100 ℃ and 400rpm for 2h until the polyvinyl alcohol is dissolved, and preparing a polyvinyl alcohol aqueous solution with the polyvinyl alcohol concentration of 100 g/L;
s2, preparing a chitosan acetic acid solution: diluting glacial acetic acid into 2% acetic acid solution by using deionized water, weighing 3.2g of chitosan, adding the chitosan into 80mL of acetic acid solution, continuously stirring at 400rpm for 3h until the chitosan is dissolved, and preparing the chitosan acetic acid solution with the chitosan concentration of 40 g/L;
s3, mixing: mixing 40mL of the polyvinyl alcohol aqueous solution obtained in the step S1 and 80mL of the chitosan acetic acid solution obtained in the step S2, and stirring at 400rpm and 100 ℃ for 3 hours; spreading 120mL of mixed solution in a culture dish with the length of 30cm multiplied by the width of 25cm, wherein the depth of the mixed solution is 0.16cm, and cooling to 20 ℃ to obtain hydrogel;
s4, freeze thawing: freezing the hydrogel obtained in the step S3 at-80 ℃ for 8h, and then placing the hydrogel at 20 ℃ for 4h for thawing;
s5: and (5) repeating the freeze thawing of the step S4 for 8 times to prepare the antibacterial composite membrane for the fresh aquatic products.
The invention also provides an application of the antibacterial composite membrane for fresh aquatic products, which is characterized in that the antibacterial composite membrane for fresh aquatic products can be used for inhibiting the growth of bacteria, wherein the bacteria are Hafnia alvei (Hafnia alive H4), Escherichia coli (CICC 10670), Staphylococcus aureus (Staphylococcus aureus, ATCC6538) and Salmonella (ATCC 14028); the fresh aquatic product antibacterial composite film is used for wrapping the aquatic product, and the aquatic product is stored at 4 ℃ and used for inhibiting the total number of bacterial colonies and the generation of volatile basic nitrogen in the aquatic product.
In a preferred mode, the aquatic product is salmon.
The invention has the beneficial effects that:
the invention provides a preparation method of an antibacterial composite film for fresh aquatic products, which has the advantages that:
1. the polyvinyl alcohol molecular structure is stable, and the composite film can be endowed with excellent mechanical properties; the chitosan has the cationic electrostatic property, so that the composite membrane has excellent antibacterial performance and has obvious inhibition effect on the growth of spoilage bacteria and pathogenic bacteria.
2. The preparation method of the composite membrane has the advantages of simple process, low cost and easy operation, and greatly reduces human resources and material resources.
3. The composite membrane prepared by the invention is easy to degrade, nontoxic and environment-friendly.
The polyvinyl alcohol-chitosan composite film has good inhibition effect on spoilage bacteria and pathogenic bacteria, effectively prolongs the shelf life of fresh food and water products, and ensures the mechanical property and environmental greenness. In addition, the composite membrane has simple preparation process and mild reaction conditions, so the composite membrane has strong application and popularization, can provide good theoretical basis for the selection of food packaging materials, and has wide application prospect and value in the field of membrane materials.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) image of a cross section of the antibacterial composite membrane for fresh aquatic products prepared in example 1 of the present invention.
Fig. 2 is a scanning electron microscope image of a cross section of the antibacterial composite membrane for fresh aquatic products prepared in example 2 of the present invention.
Fig. 3 is a scanning electron microscope image of a cross section of the antibacterial composite membrane for fresh aquatic products prepared in example 3 of the present invention.
Fig. 4 is a scanning electron microscope image of a cross section of the antibacterial composite membrane for fresh aquatic products prepared in example 4 of the present invention.
FIG. 5 shows the inhibition rate of the antibacterial composite membrane for fresh aquatic products prepared by the invention on the growth of four strains for 24h (a, b, c, d represent the difference between the groups of each example, and p is less than 0.05).
Fig. 6 shows the total number of colonies in the salmon packaged with the antibacterial composite film for fresh aquatic products prepared by the present invention after the salmon is stored for different time periods (the control group is the salmon without packaging).
Fig. 7 shows The Volatile Basic Nitrogen (TVBN) of salmon packaged with antibacterial composite film for fresh aquatic products prepared according to the present invention after storing for different time (control group is non-packaged salmon).
Detailed Description
The present invention is further illustrated by the following specific examples.
1. A preparation method of an antibacterial composite membrane for fresh aquatic products comprises the following steps:
s1, preparing a polyvinyl alcohol aqueous solution: adding polyvinyl alcohol into water, stirring at 90-100 ℃ until the polyvinyl alcohol is dissolved, and preparing a polyvinyl alcohol aqueous solution with the polyvinyl alcohol concentration of 25-250 g/L;
s2, preparing a chitosan acetic acid solution: diluting glacial acetic acid into an acetic acid solution with the volume fraction of 0.1-10%, adding chitosan into the acetic acid solution, and uniformly stirring to prepare a chitosan acetic acid solution with the chitosan concentration of 10-100 g/L;
s3, mixing: mixing the polyvinyl alcohol aqueous solution obtained in the step S1 with the chitosan acetic acid solution obtained in the step S2, stirring and uniformly mixing at 90-100 ℃ to obtain a mixed solution, and spreading and standing the mixed solution in a culture dish to form a film; the polyvinyl alcohol aqueous solution accounts for 33.4-66.6% of the mixed solution by mass, and the chitosan acetic acid solution accounts for 33.4-66.6% of the total mixed solution by mass;
s4, freeze thawing: and (4) freezing the membrane obtained in the step S3 in an environment of-20 to-80 ℃ for 3 to 34 hours, and then placing the membrane at 4 to 30 ℃ for 2 to 24 hours for unfreezing. S5: and (5) repeating the freeze thawing of the step S4 for 5-10 times to obtain the antibacterial composite membrane for the fresh aquatic products.
Preferably, the stirring to dissolve in step S1 is specifically: stirring at 300-800 rpm for 1-3 h.
In a preferable mode, the stirring and blending in step S2 is: stirring at 300-800 rpm for 1-3 h.
In a preferable mode, the stirring and blending in step S3 is: stirring at 300-800 rpm for 1-3 h.
Example 1
A preparation method of an antibacterial composite membrane for fresh aquatic products comprises the following steps:
s1, preparing a polyvinyl alcohol aqueous solution: weighing 8g of polyvinyl alcohol, adding the polyvinyl alcohol into 80mL of deionized water, stirring at 90 ℃ and 400rpm for 3h until the polyvinyl alcohol is dissolved, and preparing a polyvinyl alcohol aqueous solution with the polyvinyl alcohol concentration of 100 g/L;
s2, preparing a chitosan acetic acid solution: diluting glacial acetic acid into 2% acetic acid solution by using deionized water, weighing 1.6g of chitosan, adding the chitosan into 40mL of acetic acid solution, continuously stirring at 400rpm for 3h until the chitosan is dissolved, and preparing the chitosan acetic acid solution with the chitosan concentration of 40 g/L;
s3, mixing: mixing 80mL of the polyvinyl alcohol aqueous solution obtained in the step S1 and 40mL of the chitosan acetic acid solution obtained in the step S2, and stirring at 400rpm and 90 ℃ for 3 hours; spreading 120mL of mixed solution in a culture dish with the length of 30cm multiplied by the width of 25cm, wherein the depth of the mixed solution is 0.16cm, and cooling to 20 ℃ to obtain hydrogel;
s4, freeze thawing: placing the hydrogel obtained in the step S3 in an environment with the temperature of-80 ℃ for freezing for 3h, and then placing the hydrogel at the temperature of 20 ℃ for thawing for 3 h;
s5: and (5) repeating the freeze thawing of the step S4 for 8 times to prepare the antibacterial composite membrane for the fresh aquatic products.
The cross section of the antibacterial composite membrane for fresh aquatic products obtained in example 1 was observed (1000 times) by using a Scanning Electron Microscope (SEM), and the result shows that the polyvinyl alcohol makes the cross section of the composite membrane compact and the chitosan makes the composite membrane form pores. The antibacterial composite film obtained in example 1 is tested for mechanical properties according to GB13022-91, and the antibacterial composite film is proved to have good mechanical properties, wherein the tensile strength is 0.417MPa, the elongation at break is 110.23%, and the elastic modulus is 0.095 MPa. The growth inhibition rates of the antibacterial composite membrane in the embodiment 1 on Hafnia alvei, Escherichia coli, Staphylococcus aureus and Salmonella are respectively 2.23%, 10.5%, 27.57% and 15.1% by adopting a growth curve method, which shows that the embodiment has good inhibition effect on the growth of putrefying bacteria and pathogenic bacteria. Fresh salmon meat is packaged by adopting the composite membrane, stored for different time at 4 ℃, the total number of bacterial colonies of the sample is determined according to GB4789.2-2016, and after 10 days, compared with a control group, the antibacterial composite membrane in the example 1 can inhibit 73.13% of the total number of bacterial colonies in the salmon sample. After The Volatile Basic Nitrogen (TVBN) of the sample is measured according to GB5009.228-2016, after 10 days at 4 ℃, the antibacterial composite membrane of example 1 can inhibit 48.78% of TVBN generation of salmon body compared with a control group. Texture Profiling (TPA) was performed on salmon samples, setting the texture analyzer parameters to: return distance (mm): 30, of a nitrogen-containing gas; return speed (mm/sec): 15; contact force (g): 5; after 10 days at 4 ℃, the hardness, elasticity, cohesiveness, chewiness and recoverability of the sample without being packaged by the antibacterial composite film of the example 1 are respectively 301.4g, 0.36, 0.20, 46.4g and 0.06, and the hardness, elasticity, cohesiveness, chewiness and recoverability of the sample packaged by the antibacterial composite film of the example 1 are respectively 410.8g, 0.39, 0.22, 72.0g and 0.07, which shows that the antibacterial composite film for fresh aquatic products prepared by the embodiment can effectively ensure the texture and quality characteristics of fish bodies. Therefore, the antibacterial composite film for fresh aquatic products prepared in the embodiment 1 has good mechanical properties, has a remarkable antibacterial effect, and has a good protection effect on food quality and taste.
Example 2
A preparation method of an antibacterial composite membrane for fresh aquatic products comprises the following steps:
s1, preparing a polyvinyl alcohol aqueous solution: weighing 6g of polyvinyl alcohol, adding the polyvinyl alcohol into 60mL of deionized water, stirring at 100 ℃ and 500rpm for 2h until the polyvinyl alcohol is dissolved, and preparing a polyvinyl alcohol aqueous solution with the polyvinyl alcohol concentration of 100 g/L;
s2, preparing a chitosan acetic acid solution: diluting glacial acetic acid into 2% acetic acid solution by using deionized water, weighing 2.4g of chitosan, adding the chitosan into 60mL of acetic acid solution, continuously stirring at 500rpm for 3h until the chitosan is dissolved, and preparing the chitosan acetic acid solution with the chitosan concentration of 40 g/L;
s3, mixing: mixing 60mL of the polyvinyl alcohol aqueous solution obtained in the step S1 and 60mL of the chitosan acetic acid solution obtained in the step S2, and stirring at 500rpm and 100 ℃ for 2 hours; spreading 120mL of mixed solution in a culture dish with the length of 30cm multiplied by the width of 25cm, wherein the depth of the mixed solution is 0.16cm, and cooling to 20 ℃ to obtain hydrogel;
s4, freeze thawing: placing the hydrogel obtained in the step S3 in an environment with the temperature of-80 ℃ for freezing for 10h, and then placing the hydrogel at the temperature of 20 ℃ for thawing for 2 h;
s5: and (5) repeating the freeze thawing of the step S4 for 8 times to prepare the antibacterial composite membrane for the fresh aquatic products.
The cross section of the antibacterial composite membrane for fresh aquatic products obtained in example 2 was observed (1000 times) by using a Scanning Electron Microscope (SEM), and the result shows that the polyvinyl alcohol makes the cross section of the composite membrane compact and the chitosan makes the composite membrane form pores. The antibacterial composite film obtained in example 2 is tested for mechanical properties according to GB13022-91, and the antibacterial composite film is proved to have good mechanical properties, wherein the tensile strength is 0.344MPa, the elongation at break is 91.82%, and the elastic modulus is 0.077 MPa. The growth curve method is adopted to determine that the growth inhibition rates of the antibacterial composite membrane in the embodiment 2 on Hafnia alvei, Escherichia coli, Staphylococcus aureus and Salmonella are 69.2%, 62%, 53.73% and 55.05% respectively, which shows that the embodiment has good inhibition effect on the growth of putrefying bacteria and pathogenic bacteria. Fresh salmon meat is packaged by adopting the composite membrane, stored for different time at 4 ℃, the total number of bacterial colonies of the sample is determined according to GB4789.2-2016, and after 10 days, compared with a control group, the antibacterial composite membrane in the example 2 can inhibit 86.07% of the total number of bacterial colonies in the salmon sample. After The Volatile Basic Nitrogen (TVBN) of the sample is measured according to GB5009.228-2016, after 10 days at 4 ℃, the antibacterial composite membrane of example 2 can inhibit 65.85% of TVBN generation of salmon body compared with a control group. Texture Profiling (TPA) was performed on salmon samples, setting the texture analyzer parameters to: return distance (mm): 30, of a nitrogen-containing gas; return speed (mm/sec): 15; contact force (g): 5; after the temperature is 4 ℃ and 10 days, the hardness, elasticity, cohesiveness, chewiness and recoverability of the sample without being packaged by the antibacterial composite film in the embodiment 2 are respectively 301.4g, 0.36, 0.20, 46.4g and 0.06, and the hardness, elasticity, cohesiveness, chewiness and recoverability of the sample packaged by the antibacterial composite film in the embodiment 2 are respectively 502.3g, 0.50, 0.24, 94.3g and 0.08, which shows that the antibacterial composite film for fresh food and aquatic products prepared by the embodiment can effectively ensure the texture and quality characteristics of fish bodies. Therefore, the antibacterial composite film for fresh aquatic products prepared in the embodiment 2 has good mechanical properties, has a remarkable antibacterial effect, and has a good protection effect on food quality and taste.
Example 3
A preparation method of an antibacterial composite membrane for fresh aquatic products comprises the following steps:
s1, preparing a polyvinyl alcohol aqueous solution: weighing 4.8g of polyvinyl alcohol, adding the polyvinyl alcohol into 48mL of deionized water, stirring at 90 ℃ and 500rpm for 2h until the polyvinyl alcohol is dissolved, and preparing a polyvinyl alcohol aqueous solution with the polyvinyl alcohol concentration of 100 g/L;
s2, preparing a chitosan acetic acid solution: diluting glacial acetic acid into 2% acetic acid solution by using deionized water, weighing 2.88g of chitosan, adding the chitosan into 72mL of acetic acid solution, continuously stirring at 500rpm for 3h until the chitosan is dissolved, and preparing the chitosan acetic acid solution with the chitosan concentration of 40 g/L;
s3, mixing: mixing 48mL of the polyvinyl alcohol aqueous solution obtained in the step S1 and 72mL of the chitosan acetic acid solution obtained in the step S2, and stirring at 500rpm and 90 ℃ for 2 hours; spreading 120mL of mixed solution in a culture dish with the length of 30cm multiplied by the width of 25cm, wherein the depth of the mixed solution is 0.16cm, and cooling to 20 ℃ to obtain hydrogel;
s4, freeze thawing: freezing the hydrogel obtained in the step S3 at-80 ℃ for 6h, and then placing the hydrogel at 20 ℃ for 2h for thawing;
s5: and (5) repeating the freeze thawing of the step S4 for 8 times to prepare the antibacterial composite membrane for the fresh aquatic products.
The cross section of the antibacterial composite membrane for fresh aquatic products obtained in example 3 was observed by a Scanning Electron Microscope (SEM) (1000 times), and the results showed that the cross section of the composite membrane was loose and the chitosan caused pores to form. The antibacterial composite film obtained in example 3 is tested for mechanical properties according to GB13022-91, and the antibacterial composite film is proved to have good mechanical properties, wherein the tensile strength is 0.254MPa, the elongation at break is 134.09%, and the elastic modulus is 0.041 MPa. The growth curve method is adopted to determine that the growth inhibition rates of the antibacterial composite membrane in the embodiment 3 on Hafnia alvei, Escherichia coli, Staphylococcus aureus and Salmonella are 94.5%, 81.17%, 81% and 78.57% respectively, which shows that the embodiment has obvious inhibition effect on the growth of putrefying bacteria and pathogenic bacteria. Fresh salmon meat is packaged by adopting the composite membrane, stored for different time at 4 ℃, the total number of bacterial colonies of the sample is determined according to GB4789.2-2016, and after 10 days, compared with a control group, the antibacterial composite membrane in the example 3 can inhibit 93.28% of the total number of bacterial colonies in the salmon sample. After The Volatile Basic Nitrogen (TVBN) of the sample is measured according to GB5009.228-2016, after 10 days at 4 ℃, the antibacterial composite membrane of example 3 can inhibit 78.66% of TVBN generation of salmon body compared with a control group. Texture Profiling (TPA) was performed on salmon samples, setting the texture analyzer parameters to: return distance (mm): 30, of a nitrogen-containing gas; return speed (mm/sec): 15; contact force (g): 5; after the temperature is 4 ℃ and 10 days, the hardness, elasticity, cohesiveness, chewiness and recoverability of the sample without being packaged by the antibacterial composite film in the embodiment 3 are respectively 301.4g, 0.36, 0.20, 46.4g and 0.06, and the hardness, elasticity, cohesiveness, chewiness and recoverability of the sample packaged by the antibacterial composite film in the embodiment 3 are respectively 609.0g, 0.59, 0.27, 113.5g and 0.1, which shows that the antibacterial composite film for fresh food and aquatic products prepared by the embodiment can effectively ensure the texture and quality characteristics of fish bodies. Therefore, the antibacterial composite film for fresh aquatic products prepared in the embodiment 3 has good mechanical properties, has a remarkable antibacterial effect, and has a remarkable protection effect on food quality and taste.
Example 4
A preparation method of an antibacterial composite membrane for fresh aquatic products comprises the following steps:
s1, preparing a polyvinyl alcohol aqueous solution: weighing 4g of polyvinyl alcohol, adding the polyvinyl alcohol into 40mL of deionized water, stirring at 100 ℃ and 400rpm for 2h until the polyvinyl alcohol is dissolved, and preparing a polyvinyl alcohol aqueous solution with the polyvinyl alcohol concentration of 100 g/L;
s2, preparing a chitosan acetic acid solution: diluting glacial acetic acid into 2% acetic acid solution by using deionized water, weighing 3.2g of chitosan, adding the chitosan into 80mL of acetic acid solution, continuously stirring at 400rpm for 3h until the chitosan is dissolved, and preparing the chitosan acetic acid solution with the chitosan concentration of 40 g/L;
s3, mixing: mixing 40mL of the polyvinyl alcohol aqueous solution obtained in the step S1 and 80mL of the chitosan acetic acid solution obtained in the step S2, and stirring at 400rpm and 100 ℃ for 3 hours; spreading 120mL of mixed solution in a culture dish with the length of 30cm multiplied by the width of 25cm, wherein the depth of the mixed solution is 0.16cm, and cooling to 20 ℃ to obtain hydrogel;
s4, freeze thawing: freezing the hydrogel obtained in the step S3 at-80 ℃ for 8h, and then placing the hydrogel at 20 ℃ for 4h for thawing;
s5: and (5) repeating the freeze thawing of the step S4 for 8 times to prepare the antibacterial composite membrane for the fresh aquatic products.
The cross section of the antibacterial composite membrane for fresh aquatic products obtained in example 4 is observed by a Scanning Electron Microscope (SEM) (1000 times), and the result shows that the cross section of the composite membrane is loose and the chitosan causes the composite membrane to form pores. The antibacterial composite film obtained in example 4 is tested for mechanical properties according to GB13022-91, and the antibacterial composite film is proved to have good mechanical properties, wherein the tensile strength is 0.136MPa, the elongation at break is 103.94%, and the elastic modulus is 0.036 MPa. The growth curve method is adopted to determine that the growth inhibition rates of the antibacterial composite membrane in the embodiment 4 on Hafnia alvei, Escherichia coli, Staphylococcus aureus and Salmonella are respectively 97.9%, 92.23%, 93% and 90.47%, which shows that the embodiment has obvious inhibition effect on the growth of putrefying bacteria and pathogenic bacteria. Fresh salmon meat is packaged by adopting the composite membrane, stored for different time at 4 ℃, the total number of bacterial colonies of the sample is measured according to GB4789.2-2016, and after 10 days, the antibacterial composite membrane in the example 4 can inhibit 97.76 percent of the total number of bacterial colonies in the salmon sample compared with a control group. After The Volatile Basic Nitrogen (TVBN) of the sample is measured according to GB5009.228-2016, after 10 days at 4 ℃, the antibacterial composite membrane of example 4 can inhibit 88.41% of TVBN generation of salmon body compared with a control group. Texture Profiling (TPA) was performed on salmon samples, setting the texture analyzer parameters to: return distance (mm): 30, of a nitrogen-containing gas; return speed (mm/sec): 15; contact force (g): 5; after the temperature is 4 ℃ and 10 days, the hardness, elasticity, cohesiveness, chewiness and recoverability of the sample without being packaged by the antibacterial composite film of the embodiment 4 are respectively 301.4g, 0.36, 0.20, 46.4g and 0.06, and the hardness, elasticity, cohesiveness, chewiness and recoverability of the sample packaged by the antibacterial composite film of the embodiment 4 are respectively 723.3g, 0.73, 0.31, 142.8g and 0.12, which shows that the antibacterial composite film for fresh food and aquatic products prepared by the embodiment can effectively ensure the texture and quality characteristics of fish bodies. Therefore, the antibacterial composite film for fresh aquatic products prepared in the embodiment 4 has good mechanical properties, has a remarkable antibacterial effect, and has a remarkable protection effect on food quality and taste.
The mechanical properties of the antibacterial composite membrane for fresh aquatic products prepared by the embodiments of the invention are shown in table 1; results of Texture Analysis (TPA) of salmon stored at 4 ℃ for different times using the antibacterial composite membrane for fresh aquatic products prepared in each example of the present invention are shown in Table 2, wherein a, b, c and d represent differences among the examples, and p is less than 0.05.
TABLE 1 mechanical Properties of the composite films of the examples
| Tensile strength MPa | Elongation at break% | Modulus of elasticity MPa | |
| Example 1 | 0.42±0.01 | 110.23±3.54 | 0.09±0.00 |
| Example 2 | 0.34±0.04 | 91.82±9.23 | 0.08±0.00 |
| Example 3 | 0.25±0.01 | 134.09±9.64 | 0.04±0.00 |
| Example 4 | 0.14±0.01 | 103.94±12.41 | 0.04±0.00 |
Table 2 analysis of meat texture of salmon stored with composite film for various periods of time in each example
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (8)
1. A preparation method of an antibacterial composite film for fresh aquatic products is characterized by comprising the following steps:
s1, preparing a polyvinyl alcohol aqueous solution: preparing a polyvinyl alcohol aqueous solution with the polyvinyl alcohol concentration of 25-250 g/L by using polyvinyl alcohol and water;
s2, preparing a chitosan acetic acid solution: diluting glacial acetic acid into an acetic acid solution with the volume fraction of 0.1-10%, adding chitosan into the acetic acid solution, and uniformly stirring to prepare a chitosan acetic acid solution with the chitosan concentration of 10-100 g/L;
s3, mixing: mixing the polyvinyl alcohol aqueous solution obtained in the step S1 with the chitosan acetic acid solution obtained in the step S2, and stirring and uniformly mixing at 90-100 ℃ to obtain a mixed solution; flatly paving the mixed solution in a container, wherein the depth of the mixed solution is 1-2 mm, and cooling to 20-25 ℃ to obtain hydrogel; the mixed solution consists of polyvinyl alcohol aqueous solution and chitosan acetic acid solution according to the following volume percentage: 33.4 to 66.6 percent of polyvinyl alcohol aqueous solution and 33.4 to 66.6 percent of chitosan acetic acid solution;
s4, freeze thawing: freezing the hydrogel obtained in the step S3 at-20 to-80 ℃ for 3 to 34 hours, and then placing the hydrogel at 4 to 30 ℃ for 2 to 24 hours;
s5: and (5) repeating the freeze thawing of the step S4 for 5-10 times to obtain the antibacterial composite membrane for the fresh aquatic products.
2. The preparation method of the antibacterial composite membrane for fresh aquatic products according to claim 1, wherein the step S1 of preparing the aqueous solution of polyvinyl alcohol specifically comprises: adding polyvinyl alcohol into water, stirring at 90-100 ℃ and 300-800 rpm for 1-3 h, and preparing a polyvinyl alcohol aqueous solution with the polyvinyl alcohol concentration of 25-250 g/L.
3. The preparation method of the antibacterial composite membrane for fresh aquatic products according to claim 1, wherein the step S2 is to stir and mix uniformly: stirring at 300-800 rpm for 1-3 h.
4. The preparation method of the antibacterial composite membrane for fresh aquatic products according to claim 1, wherein the step S3 is to stir and mix uniformly: stirring at 300-800 rpm for 1-3 h.
5. The preparation method of the antibacterial composite membrane for fresh aquatic products according to claim 1, comprising the steps of:
s1, preparing a polyvinyl alcohol aqueous solution: weighing 4g of polyvinyl alcohol, adding the polyvinyl alcohol into 40mL of deionized water, stirring at 100 ℃ and 400rpm for 2h, and preparing a polyvinyl alcohol aqueous solution with the polyvinyl alcohol concentration of 100 g/L;
s2, preparing a chitosan acetic acid solution: diluting glacial acetic acid into 2% acetic acid solution by using deionized water, weighing 3.2g of chitosan, adding the chitosan into 80mL of the acetic acid solution, and stirring at 400rpm for 3h to prepare chitosan acetic acid solution with the chitosan concentration of 40 g/L;
s3, mixing: mixing 40mL of the polyvinyl alcohol aqueous solution obtained in the step S1 and 80mL of the chitosan acetic acid solution obtained in the step S2, and stirring at 400rpm and 100 ℃ for 3 hours; spreading 120mL of the mixed solution in a culture dish with the length of 30cm and the width of 25cm, wherein the depth of the mixed solution in the culture dish is 0.16cm, and cooling to 20 ℃ to obtain hydrogel;
s4, freeze thawing: freezing the hydrogel obtained in the step S3 at-80 ℃ for 8h, and then placing the hydrogel at 20 ℃ for 4 h;
s5: and (5) repeating the freeze thawing of the step S4 for 8 times to prepare the antibacterial composite membrane for the fresh aquatic products.
6. Use of the fresh aquatic product antimicrobial composite membrane prepared according to any one of claims 1 to 5 for inhibiting the growth of bacteria selected from the group consisting of Hafniaalvei (Hafniaalive), Escherichia coli (Escherichia coli), Staphylococcus aureus (Staphylococcus aureus), and Salmonella (Salmonella).
7. Use of an antimicrobial composite film according to any one of claims 1 to 5 in the manufacture of a fresh aquatic product, wherein the antimicrobial composite film is used to coat an aquatic product and stored at 4 ℃ to inhibit the formation of total bacterial colonies and volatile basic nitrogen in the aquatic product.
8. The application of the antibacterial composite membrane for fresh aquatic products according to claim 7, wherein the aquatic products are salmon.
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