CN110790987B - Chitosan-silk fibroin edible film and preparation method thereof - Google Patents
Chitosan-silk fibroin edible film and preparation method thereof Download PDFInfo
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- 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
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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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- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/04—Alginic acid; Derivatives thereof
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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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- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention relates to a preparation method of a chitosan-silk fibroin edible film, which is characterized by comprising the following steps: step S1, preparing a quaternized chitosan solution; step S2, preparing a silk fibroin solution; step S3, preparing chitosan-silk fibroin; and S4, preparing the chitosan-silk fibroin edible film. The invention also discloses a chitosan-silk fibroin edible film prepared by the preparation method of the chitosan-silk fibroin edible film. The chitosan-silk fibroin edible film disclosed by the invention has good moisture resistance, can effectively delay the aging and browning of fruits and vegetables, inhibits the growth of microorganisms in the fruits and vegetables, improves the storage period of the fruits and vegetables, keeps the original quality and commodity value of the fruits and vegetables to the maximum extent, is safe and environment-friendly to use, and has higher economic value, social value and ecological value.
Description
Technical Field
The invention relates to the technical field of edible films, in particular to a chitosan-silk fibroin edible film and a preparation method thereof.
Background
The fresh fruits and vegetables have high nutritive value and are deeply loved by consumers, but the fresh fruits and vegetables have short shelf life at room temperature and are easy to rot. With the improvement of the cognition degree of people on green food, how to improve the storage period of fruits and vegetables and keep the original quality and commodity value of the fruits and vegetables to the maximum degree becomes one of the focuses of research in the field of food science.
The edible film is an edible preservative film for short, has the characteristics of good preservation effect, convenient use, good practicability and the like, is simple in manufacturing process, low in cost, edible, easy to degrade and free of environmental pollution, is a food packaging material with great development potential, is a preservative material frequently used in a coating preservation technology, is usually coated on the surface of a fruit by a preservative with a film forming function, is formed on the surface of the fruit after standing for a period of time, and can block gas exchange between the fruit and air, so that the nutrient consumption is reduced, and the aging is delayed.
Although the edible preservative film used at present achieves remarkable results in fruit and vegetable preservation, the edible preservative film also has the problems that the polysaccharide has strong hydrophilicity, so that the film has poor moisture resistance and is easy to absorb moisture and become sticky in a high-humidity environment; the protein membrane has strong hydrophilicity and poor water resistance.
Tujie et al, in food and machinery, vol.26, No. 6, 11 months 2010, Chitosan-glycerol-fibroin blend film preparation and Performance research, Chitosan-glycerol-fibroin blend film was prepared by the sialorrhea method, and the influence of the blending ratio of each component on the film performance was examined with the elongation strength and elongation at break of the film as the index. The results show that: the chitosan can enhance the tensile strength of the film, but when the concentration of the chitosan is more than or equal to 10g/L, the elongation at break of the film is reduced; the tensile strength and the elongation at break of the film can be improved by adding the glycerol; the tensile strength of the membrane can be slightly increased by adding the silk fibroin, and the breaking elongation is obviously improved. Further adopting 10g/L chitosan, 10g/L glycerin and 0-10 g/L silk fibroin to form a film, and investigating the antibacterial performance. The results show that: the blended membrane containing 5g/L of silk fibroin can completely inhibit the growth of staphylococcus aureus, the blended membrane containing 20g/L of silk fibroin can completely inhibit the growth of escherichia coli, and the antibacterial performance of the chitosan blended membrane is greatly improved by adding the silk fibroin. In the paper, the mechanical property and the antibacterial property of the blend film are only researched, but the food fresh-keeping effect is not demonstrated; it is not an edible film; because no surfactant and plasticizer are added, the film formed by blending pure chitosan solution and silk fibroin solution is easy to age and crack and poor in moisture resistance.
Therefore, the development of the edible film which has good moisture resistance, can effectively delay the aging and browning of the fruits and vegetables, inhibits the growth of microorganisms in the fruits and vegetables, improves the storage period of the fruits and vegetables and keeps the original quality and commodity value of the fruits and vegetables to the maximum extent has very important significance for promoting the development of a coating preservation technology.
Disclosure of Invention
The invention aims to provide a chitosan-silk fibroin edible film for overcoming the defects of the prior art; the edible film has good moisture resistance, can effectively delay the aging and browning of fruits and vegetables, inhibits the growth of microorganisms in the fruits and vegetables, improves the storage period of the fruits and vegetables, keeps the original quality and commodity value of the fruits and vegetables to the maximum extent, is safe and environment-friendly to use, and has higher economic value, social value and ecological value; meanwhile, the invention also provides a preparation method of the chitosan-silk fibroin edible film.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a chitosan-silk fibroin edible film is characterized by comprising the following steps:
step S1, preparation of quaternized chitosan solution: dissolving quaternized chitosan in deionized water, stirring for 15-30 minutes at 50-60 ℃ to form a solution, then adding glacial acetic acid with the mass percentage concentration of 1-3% into the solution, continuing to perform heat preservation and mechanical stirring for 35-45 minutes at the rotation speed of 450-550rpm, and then standing to obtain a clear and transparent yellowish quaternized chitosan solution;
step S2, preparation of silk fibroin solution: dissolving nano silk fibroin in deionized water, stirring for 20-35 minutes at 55-65 ℃ to form a solution, then adding glacial acetic acid with the mass percentage concentration of 0.5-1.5% into the solution, continuing to perform heat preservation and mechanical stirring for 25-35 minutes at the rotating speed of 500rpm, and then standing to obtain a silk fibroin solution;
step S3, preparation of chitosan-silk fibroin: mixing the quaternized chitosan solution prepared in the step S1 with the silk fibroin solution prepared in the step S2, uniformly stirring, adding glycerol, polyethylene glycol and a surfactant, stirring for 30-40 minutes on a magnetic stirrer, homogenizing for 3-5 times by using a homogenizer, vacuum-filtering, cooling for later use, and freeze-drying to obtain a sample;
step S4, preparing the chitosan-silk fibroin edible film: dissolving the chitosan-silk fibroin prepared in the step S3 in water, adding alginic acid, magnetically stirring for 2-3 hours in a water bath at 60-80 ℃ to obtain a mixed solution, then exhausting air by using a vacuum pump to remove air bubbles in the solution, pouring the solution on an acrylic plate, drying the acrylic plate at 60-80 ℃ to form a film, and finally uncovering the film for storage to obtain the chitosan-silk fibroin edible film.
Furthermore, in step S1, the mixture ratio of the quaternized chitosan, the deionized water and the glacial acetic acid is 10g (1-1.5L): 8-12 mL.
Furthermore, in step S2, the ratio of the nano silk fibroin, the deionized water and the glacial acetic acid is (9-11g): (1-1.5L): 8-12 mL.
Preferably, the mass ratio of the quaternized chitosan solution, the silk fibroin solution, the glycerol, the polyethylene glycol and the surfactant in the step S3 is 1:1 (0.02-0.05):0.03: 0.02.
Preferably, the surfactant is at least one of tween 20 and tween 80.
Further, in step S4, the mass ratio of chitosan-silk fibroin, water and alginic acid is (2-5):100: 0.3.
The invention also aims to provide the chitosan-silk fibroin edible film prepared by the preparation method of the chitosan-silk fibroin edible film.
Further, the chitosan-silk fibroin edible film is used as a fruit and vegetable coating fresh-keeping material.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages: the edible film has good moisture resistance, can effectively delay the aging and browning of fruits and vegetables, inhibits the growth of microorganisms in the fruits and vegetables, improves the storage period of the fruits and vegetables, keeps the original quality and commodity value of the fruits and vegetables to the maximum extent, is safe and environment-friendly to use, and has higher economic value, social value and ecological value; the preparation method of the chitosan-silk fibroin edible film is simple and easy to operate, the reaction condition is mild, and the dependence on equipment is not high.
Detailed Description
The invention relates to a preparation method of a chitosan-silk fibroin edible film, which is characterized by comprising the following steps:
step S1, preparation of quaternized chitosan solution: dissolving quaternized chitosan in deionized water, stirring for 15-30 minutes at 50-60 ℃ to form a solution, then adding glacial acetic acid with the mass percentage concentration of 1-3% into the solution, continuing to perform heat preservation and mechanical stirring for 35-45 minutes at the rotation speed of 450-550rpm, and then standing to obtain a clear and transparent yellowish quaternized chitosan solution;
step S2, preparation of silk fibroin solution: dissolving nano silk fibroin in deionized water, stirring for 20-35 minutes at 55-65 ℃ to form a solution, then adding glacial acetic acid with the mass percentage concentration of 0.5-1.5% into the solution, continuing to perform heat preservation and mechanical stirring for 25-35 minutes at the rotating speed of 500rpm, and then standing to obtain a silk fibroin solution;
step S3, preparation of chitosan-silk fibroin: mixing the quaternized chitosan solution prepared in the step S1 with the silk fibroin solution prepared in the step S2, uniformly stirring, adding glycerol, polyethylene glycol and a surfactant, stirring for 30-40 minutes on a magnetic stirrer, homogenizing for 3-5 times by using a homogenizer, vacuum-filtering, cooling for later use, and freeze-drying to obtain a sample;
step S4, preparing the chitosan-silk fibroin edible film: dissolving the chitosan-silk fibroin prepared in the step S3 in water, adding alginic acid, magnetically stirring for 2-3 hours in a water bath at 60-80 ℃ to obtain a mixed solution, then exhausting air by using a vacuum pump to remove air bubbles in the solution, pouring the solution on an acrylic plate, drying the acrylic plate at 60-80 ℃ to form a film, and finally uncovering the film for storage to obtain the chitosan-silk fibroin edible film.
Further, the mixture ratio of the quaternized chitosan, the deionized water and the glacial acetic acid in the step S1 is 10g (1-1.5L): 8-12 mL); in the step S2, the ratio of the nano silk fibroin, the deionized water and the glacial acetic acid is (9-11g): (1-1.5L): 8-12 mL); in the step S3, the mass ratio of the quaternized chitosan solution to the silk fibroin solution to the glycerol to the polyethylene glycol to the surfactant is 1:1 (0.02-0.05) to 0.03: 0.02; the surfactant is at least one of Tween 20 and Tween 80; in the step S4, the mass ratio of the chitosan-silk fibroin, the water and the alginic acid is (2-5) to 100: 0.3.
The invention also aims to provide the chitosan-silk fibroin edible film prepared by the preparation method of the chitosan-silk fibroin edible film.
Further, the chitosan-silk fibroin edible film is used as a fruit and vegetable coating fresh-keeping material; the edible film has good moisture resistance, can effectively delay the aging and browning of fruits and vegetables, inhibits the growth of microorganisms in the fruits and vegetables, improves the storage period of the fruits and vegetables, keeps the original quality and commodity value of the fruits and vegetables to the maximum extent, is safe and environment-friendly to use, and has higher economic value, social value and ecological value; the preparation method of the chitosan-silk fibroin edible film is simple and easy to operate, the reaction condition is mild, and the dependence on equipment is not high.
The invention will be further described with reference to specific examples, but the scope of protection of the invention is not limited thereto:
example 1
The embodiment provides a preparation method of a chitosan-silk fibroin edible film, which is characterized by comprising the following steps:
step S1, preparation of quaternized chitosan solution: dissolving 10g of quaternized chitosan into 1L of deionized water, stirring for 15 minutes at 50 ℃ to form a solution, then adding 8mL of glacial acetic acid with the mass percentage concentration of 1%, continuing to mechanically stir for 35 minutes at the rotating speed of 450rpm by heat preservation, and standing to obtain a clear and transparent yellowish quaternized chitosan solution;
step S2, preparation of silk fibroin solution: dissolving 9g of nano silk fibroin in 1L of deionized water, stirring for 20 minutes at 55 ℃ to form a solution, then adding 8mL of glacial acetic acid with the mass percentage concentration of 0.5% into the solution, continuing to perform heat preservation and mechanical stirring for 25 minutes at the rotating speed of 500rpm, and then standing to obtain a silk fibroin solution;
step S3, preparation of chitosan-silk fibroin: mixing 100g of the quaternized chitosan solution prepared in the step S1 with 100g of the silk fibroin solution prepared in the step S2, stirring uniformly, adding 2g of glycerol, 3g of polyethylene glycol and 202 g of tween into the mixture, stirring for 30 minutes on a magnetic stirrer, homogenizing for 3 times by using a homogenizer, carrying out vacuum filtration, cooling for later use, and carrying out freeze drying to obtain a sample;
step S4, preparing the chitosan-silk fibroin edible film: dissolving 2g of chitosan-silk fibroin prepared in the step S3 in 100g of water, adding 0.3g of alginic acid, magnetically stirring for 2 hours in a water bath at 60 ℃ to obtain a mixed solution, pumping air by using a vacuum pump to remove air bubbles in the solution, pouring the solution on an acrylic plate, drying the acrylic plate at 60 ℃ to form a film, and finally peeling off the film and storing to obtain the chitosan-silk fibroin edible film.
The invention also aims to provide the chitosan-silk fibroin edible film prepared by the preparation method of the chitosan-silk fibroin edible film.
The chitosan-silk fibroin edible film is used as a coating preservation material for fruits and vegetables.
Example 2
This example provides a chitosan-silk fibroin edible film, which is substantially the same as that in example 1, except that the ratio of the quaternized chitosan, deionized water, and glacial acetic acid in step S1 is 10g:1.2L:9 mL; the ratio of the nano silk fibroin, the deionized water and the glacial acetic acid in the step S2 is 9.5g:1.1L:9 mL; in the step S3, the mass ratio of the quaternized chitosan solution to the silk fibroin solution to the glycerol to the polyethylene glycol to the surfactant is 1:1:0.03:0.03: 0.02; the surfactant is tween 80; in the step S4, the mass ratio of the chitosan-silk fibroin, the water and the alginic acid is 3:100: 0.3.
Example 3
This example provides a chitosan-silk fibroin edible film, which is substantially the same as that in example 1, except that the ratio of the quaternized chitosan, deionized water, and glacial acetic acid in step S1 is 10g:1.3L:10 mL; in the step S2, the ratio of the nano silk fibroin to the deionized water to the glacial acetic acid is 10g to 1.3L to 10 mL; in the step S3, the mass ratio of the quaternized chitosan solution to the silk fibroin solution to the glycerol to the polyethylene glycol to the surfactant is 1:1:0.035:0.03: 0.02; the surfactant is tween 20; in step S4, the mass ratio of chitosan-silk fibroin, water and alginic acid is 3.5:100: 0.3.
Example 4
This example provides a chitosan-silk fibroin edible film, which is substantially the same as that in example 1, except that the ratio of the quaternized chitosan, deionized water, and glacial acetic acid in step S1 is 10g:1.4L:11 mL; in the step S2, the ratio of the nano silk fibroin to the deionized water to the glacial acetic acid is 10.5g to 1.4L to 11 mL; in the step S3, the mass ratio of the quaternized chitosan solution to the silk fibroin solution to the glycerol to the polyethylene glycol to the surfactant is 1:1:0.04:0.03: 0.02; the surfactant is formed by mixing Tween 20 and Tween 80 according to the mass ratio of 2: 3; in the step S4, the mass ratio of the chitosan-silk fibroin, the water and the alginic acid is 4:100: 0.3.
Example 5
This example provides a chitosan-silk fibroin edible film, which is substantially the same as that in example 1, except that the ratio of the quaternized chitosan, deionized water, and glacial acetic acid in step S1 is 10g:1.5L:12 mL; in the step S2, the ratio of the nano silk fibroin to the deionized water to the glacial acetic acid is 11g:1.5L:12 mL; in the step S3, the mass ratio of the quaternized chitosan solution to the silk fibroin solution to the glycerol to the polyethylene glycol to the surfactant is 1:1:0.05:0.03: 0.02; the surfactant is tween 20; in the step S4, the mass ratio of the chitosan-silk fibroin, the water and the alginic acid is 5:100: 0.3.
Comparative example 1
This example provides a chitosan-silk fibroin edible film, which is substantially identical to that of example 1, except that: in step S1, the quaternary ammonium salt chitosan is replaced with water-soluble chitosan.
Comparative example 2
This example provides a chitosan-silk fibroin edible film, which is substantially identical to that of example 1, except that: in step S3, no polyethylene glycol is added.
Comparative example 3
This example provides a chitosan-silk fibroin edible film, which is substantially identical to that of example 1, except that: alginic acid was not added in step S3.
To further illustrate the technical effects of the embodiments of the present invention, the chitosan-silk fibroin edible films prepared by the embodiments 1-5 and the comparative examples 1-3 of the present invention were subjected to performance tests, the test results are shown in table 1, and the test methods are as follows:
(1) tensile strength: the tensile rate is 100mm/min and the test temperature is 25 ℃ according to the test method of the tensile property of the GB/T1040-1992 plastics.
(2) And (3) VC content determination: the measurements were carried out according to the national standard GB 61951986 using the 2,6 dichloroindophenol titration method and were measured on film coatings and on tomato surfaces stored for 15 days.
(3) And (3) testing antibacterial performance: the strains tested were selected as E.coli and S.aureus as determined by FZ/T73023-2006.
TABLE 1
As can be seen from table 1, the chitosan-silk fibroin edible film disclosed by the embodiment of the invention has more excellent mechanical properties and antibacterial properties, and when the chitosan-silk fibroin edible film is used for preserving the surfaces of fruits and vegetables, the storage period of the fruits and vegetables can be effectively prolonged, and the preservation effect can be improved.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (3)
1. A preparation method of a chitosan-silk fibroin edible film is characterized by comprising the following steps:
step S1, preparation of quaternized chitosan solution: dissolving quaternized chitosan in deionized water, stirring for 15-30 minutes at 50-60 ℃ to form a solution, then adding glacial acetic acid with the mass percentage concentration of 1-3% into the solution, continuing to perform heat preservation and mechanical stirring for 35-45 minutes at the rotation speed of 450-550rpm, and then standing to obtain a clear and transparent yellowish quaternized chitosan solution;
step S2, preparation of silk fibroin solution: dissolving nano silk fibroin in deionized water, stirring for 20-35 minutes at 55-65 ℃ to form a solution, then adding glacial acetic acid with the mass percentage concentration of 0.5-1.5% into the solution, continuing to perform heat preservation and mechanical stirring for 25-35 minutes at the rotating speed of 500rpm, and then standing to obtain a silk fibroin solution;
step S3, preparation of chitosan-silk fibroin: mixing the quaternized chitosan solution prepared in the step S1 with the silk fibroin solution prepared in the step S2, uniformly stirring, adding glycerol, polyethylene glycol and a surfactant, stirring for 30-40 minutes on a magnetic stirrer, homogenizing for 3-5 times by using a homogenizer, vacuum-filtering, cooling for later use, and freeze-drying to obtain a sample;
step S4, preparing the chitosan-silk fibroin edible film: dissolving the chitosan-silk fibroin prepared in the step S3 in water, adding alginic acid, magnetically stirring for 2-3 hours in a water bath at 60-80 ℃ to obtain a mixed solution, then exhausting air by using a vacuum pump to remove air bubbles in the solution, pouring the solution on an acrylic plate, drying the acrylic plate at 60-80 ℃ to form a film, and finally uncovering the film for storage to obtain the chitosan-silk fibroin edible film;
in the step S1, the mixture ratio of the quaternized chitosan, the deionized water and the glacial acetic acid is 10g (1-1.5L) to 8-12 mL; in the step S2, the ratio of the nano silk fibroin, the deionized water and the glacial acetic acid is (9-11g): (1-1.5L): 8-12 mL); in the step S3, the mass ratio of the quaternized chitosan solution to the silk fibroin solution to the glycerol to the polyethylene glycol to the surfactant is 1:1 (0.02-0.05) to 0.03: 0.02; in the step S4, the mass ratio of the chitosan-silk fibroin, the water and the alginic acid is (2-5) to 100: 0.3.
2. The method for preparing the chitosan-silk fibroin edible film according to claim 1, wherein the surfactant is at least one of tween 20 and tween 80.
3. The chitosan-silk fibroin edible film prepared by the preparation method of the chitosan-silk fibroin edible film as claimed in any one of claims 1-2.
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