CN114381042A - Bio-based food freshness indicating film and preparation method thereof - Google Patents
Bio-based food freshness indicating film and preparation method thereof Download PDFInfo
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- 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
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- 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
- C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2303/02—Starch; Degradation products thereof, e.g. dextrin
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- 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
- 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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- 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
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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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
- 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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- 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
- 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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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- 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
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Abstract
The invention discloses a bio-based food freshness indicating film which is prepared from the following raw materials in parts by weight: anthocyanin powder: 5-10 parts of sodium alginate: 30 to 40 portions of CaCl2: 20-30 parts of soluble starch: 20-35 parts of chitosan: 20-35 parts of glycerol: 5-15 parts of acetic acid: 2-5 parts; the preparation method comprises the following process steps of preparing anthocyanin powder, anthocyanin microcapsules, chitosan solution, starch solution, mixed membrane solution and drying. The inventionThe intelligent indicating film is prepared from the starch, the chitosan and the natural anthocyanin microcapsules, has no biotoxicity and antibacterial property and is low in cost, the stability of the indicating film can be improved by the anthocyanin microcapsules, and meanwhile, the chitosan and the anthocyanin in the indicating film have strong antibacterial property and oxidation resistance, so that the freshness retaining capability of the indicating film can be endowed, and the shelf life of food is prolonged.
Description
Technical Field
The invention relates to the technical field of intelligent food packaging, in particular to a bio-based food freshness indicating film and a preparation method thereof.
Background
For food, the package can reduce the influence of external factors such as low temperature, light, humidity and the like which can cause food deterioration, simultaneously can prevent the food from being damaged, and can effectively ensure the safety of the food. However, in the storage of meat products, nutrients such as proteins and fats in the food are easily decomposed and metabolized by microorganisms and enzymes, which leads to deterioration in quality and deterioration in freshness.
The Chinese patent with publication number CN112378906A discloses a preparation method of a meat freshness indication label based on natural pigment, which comprises the following steps: dissolving carrageenan powder in deionized water, fully stirring, and adding glycerol to obtain a carrageenan solution; dissolving natural pigment to obtain an indicator solution; adding the indicator solution into the carrageenan solution, degassing, and pouring into a polystyrene culture dish to obtain a completely gelled indicator membrane; dissolving konjac glucomannan in deionized water, stirring, and adding glycerol; adding camellia oil into konjac glucomannan solution, dispersing the mixture with a high-speed disperser, performing ultrasonic treatment to obtain film-forming emulsion, degassing, pouring onto a completely gelled indicator film, and drying. According to the technical scheme, the freshness of meat can be detected, but the stability of anthocyanin is poor, so that the indication effect of the label can be influenced; and the indicating label has limited performance, can only display the freshness of meat, has no antibacterial property and can not prevent food damage.
Disclosure of Invention
The invention aims to provide a biological-based food freshness indicating film aiming at the defects in the prior art, which is added with natural anthocyanin powder, has good stability, can show the freshness of meat foods through color, has antibacterial property and can prolong the shelf life of the foods.
Another object of the present invention is to provide a method for preparing the above bio-based food freshness indicating film.
The purpose of the invention is realized by the following technical scheme:
the bio-based food freshness indicating film is characterized by being prepared from the following raw materials in parts by weight: anthocyanin powder: 5-10 parts of sodium alginate: 30 to 40 portions of CaCl2: 20-30 parts of soluble starch: 20-35 parts of chitosan: 20-35 parts of glycerol: 5-15 parts of acetic acid: 2-5 parts.
Further, the anthocyanin powder is prepared from the following raw materials in parts by weight: dehydrated purple cabbage powder: 5-10 parts of acetic acid/70% ethanol aqueous solution: 48-70 parts.
Further, the anthocyanin microcapsule is prepared from the following raw materials in parts by weight: anthocyanin powder: 5-10 parts of sodium alginate: 30 to 40 portions of CaCl2: 20-30 parts of deionized water: 500-600 parts.
A preparation method of the bio-based food freshness indicating film comprises the following steps:
s1, dehydrating and drying the cleaned purple cabbage, then smashing the purple cabbage into powder, adding the purple cabbage powder into an acetic acid/70% ethanol water solution, carrying out ultrasonic wave synergistic heating extraction, filtering and centrifuging to obtain an extracting solution, purifying the extracting solution, and carrying out vacuum freeze drying to obtain anthocyanin powder;
s2, adding anthocyanin powder into deionized water to obtain an anthocyanin solution; adding sodium alginate into deionized water, stirring and degassing to obtain a sodium alginate solution, and mixing the anthocyanin solution and the sodium alginate solution to obtain a mixed solution; then preparing CaCl2Adding sodium alginate dropwise into CaCl2Obtaining anthocyanin microcapsules in the solution;
s3, adding chitosan and acetic acid into deionized water, uniformly stirring, and then carrying out ultrasonic treatment and degassing to obtain a chitosan solution;
s4, adding soluble starch into deionized water, heating and stirring in a water bath to obtain a starch solution, carrying out ultrasonic treatment and degassing on the starch solution, and then cooling the starch solution to the normal temperature and continuing stirring;
s5, mixing the treated chitosan solution and the starch solution, adding glycerol, uniformly stirring, adding anthocyanin powder, and performing ultrasonic oscillation degassing treatment, stirring and ultrasonic degassing treatment to obtain a mixed membrane solution;
and S6, pouring the mixed membrane solution into a horizontally placed glass culture dish, and drying to obtain the bio-based food freshness indicating membrane.
Further, the purification treatment in step S1 is to purify the extract by using a macroporous resin.
Further, the pH value of the acetic acid/70% ethanol water solution is 2.8-3.0.
Further, in the step S1, the temperature in the dehydration drying process is 40-50 ℃, the drying time is 20-30 hours, the temperature in the heating extraction process is 50-60 ℃, and the extraction time is 30-60 min.
Further, in the step S2, the concentration of the anthocyanin solution is 1-2 mg/mL, and the mass ratio of the anthocyanin solution to the sodium alginate solution is 1: 3.
Further, in the step S4, the water bath stirring temperature is 50-65 ℃, and the stirring time is 1-2 hours.
Further, in the step S6, the temperature of the drying process is 35-45 ℃, and the time is 20-24 hours.
A bio-based food freshness indicating film prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
according to the method, the anthocyanin is extracted by ultrasonic wave in a synergistic manner, so that the extraction rate of the anthocyanin is further improved, then the mixed solution is purified by macroporous resin to further remove impurities in the extracted anthocyanin, the purity of the anthocyanin is improved, and the sensitivity of the indicator film for monitoring the freshness of food is further improved. The invention also adopts sodium alginate solution and CaCl2Solution microcrystallization of anthocyaninsEncapsulation is carried out, and the stability of the anthocyanin is improved.
The intelligent indicating film is prepared from the starch, the chitosan and the natural anthocyanin, and compared with other indicating films, the chitosan has better antibacterial property, so that the indicating film has no biotoxicity, antibacterial property, low cost, good film forming property, better antibacterial property and good biodegradability, and accords with the trends of green packaging and sustainable development. The anthocyanin has strong oxidation resistance, can endow the indicating film with fresh-keeping capacity, and prolongs the shelf life of food.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention;
fig. 2 is a diagram illustrating the effect of the present invention.
Detailed Description
In order to facilitate understanding of the present invention, the present invention will be described in more detail with reference to the following examples, but the scope of the present invention is not limited to the following specific examples.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
The embodiment provides a preparation method of a bio-based food freshness indicating film, which is prepared from the following raw materials in parts by weight: anthocyanin powder: 8 parts of sodium alginate: 30 portions of CaCl2: 20 parts of soluble starch: 35 parts of chitosan: 25 parts of glycerol: 10 parts of acetic acid: 5 parts of a mixture; the anthocyanin powder is prepared from the following raw materials in parts by weight: dehydrated purple cabbage powder: 10 parts, acetic acid/70% ethanol aqueous solution: 60 parts. The preparation method comprises the following steps:
s1, putting the cleaned purple cabbage into a 40 ℃ oven for dehydration and drying for 24h, then crushing into powder, adding 10 parts of dehydrated purple cabbage powder into 60 parts of acetic acid/70% ethanol water solution (pH is 2.8-3.0), performing ultrasonic wave synergistic heating extraction at 50 ℃ for 30min, filtering and centrifuging to obtain an extracting solution, purifying the extracting solution by using macroporous resin HPD100A, and performing vacuum freeze drying to obtain anthocyanin powder;
s2, adding 8 parts of anthocyanin powder into 200 parts of deionized water to obtain an anthocyanin solution; adding 30 parts of sodium alginate into 400 parts of deionized water, stirring and degassing to obtain a sodium alginate solution, and mixing the anthocyanin solution and the sodium alginate solution according to a mass ratio of 1:3 to obtain a mixed solution; then 20 parts of CaCl2Adding into 350 parts of deionized water to obtain CaCl2Adding sodium alginate dropwise into CaCl2Obtaining anthocyanin microcapsules in the solution;
s3, adding 35 parts of chitosan and 5 parts of acetic acid into 300 parts of deionized water, stirring, and performing ultrasonic treatment for 10min to degas to obtain a chitosan solution;
s4, adding 35 parts of soluble starch into 400 parts of deionized water, stirring for 1 hour in a water bath at 50 ℃ to obtain a starch solution, carrying out ultrasonic treatment on the starch solution for 15min to degas, cooling the starch solution to normal temperature, and continuing stirring for 20 min;
s5, mixing the treated chitosan solution and the starch solution, adding 10 parts of glycerol, uniformly stirring, adding the anthocyanin microcapsules, carrying out ultrasonic oscillation treatment for 40min, stirring for 5h, and carrying out ultrasonic treatment for 5min for degassing to obtain a mixed membrane solution;
s6, pouring the mixed membrane solution into a horizontally placed stripping culture dish, and then placing the culture dish in a 35-DEG C air-blast drying oven for drying for 20 hours to obtain the bio-based food freshness indicating membrane.
Example 2
The embodiment provides a preparation method of a bio-based food freshness indicating film, which is prepared from the following raw materials in parts by weight: anthocyanin powder: 5 parts of sodium alginate: 35 portions of CaCl2: 25 parts of soluble starch: 35 parts of chitosan: 28 parts of glycerol: 15 parts of acetic acid: 5 parts of a mixture; wherein the anthocyanin powder is prepared from the following raw materials in parts by weightThe material is prepared by the following steps: dehydrated purple cabbage powder: 8 parts, acetic acid/70% ethanol aqueous solution: 60 parts. The preparation method comprises the following steps:
s1, putting the cleaned purple cabbage into a 50 ℃ oven for dehydration and drying for 28h, then crushing into powder, adding 8 parts of dehydrated purple cabbage powder into 60 parts of acetic acid/70% ethanol water solution (pH is 2.8-3.0), performing ultrasonic wave synergistic heating extraction for 50min at 60 ℃, filtering and centrifuging to obtain an extracting solution, purifying the extracting solution by using macroporous resin HPD100A, and performing vacuum freeze drying to obtain anthocyanin powder;
s2, adding 5 parts of anthocyanin powder into 200 parts of deionized water to obtain an anthocyanin solution; adding 35 parts of sodium alginate into 400 parts of deionized water, stirring and degassing to obtain a sodium alginate solution, and mixing the anthocyanin solution and the sodium alginate solution according to a mass ratio of 1:3 to obtain a mixed solution; then 25 parts of CaCl2Adding into 350 parts of deionized water to obtain CaCl2Adding sodium alginate dropwise into CaCl2Obtaining anthocyanin microcapsules in the solution;
s3, adding 35 parts of chitosan and 5 parts of acetic acid into 300 parts of deionized water, stirring, and performing ultrasonic treatment for 10min to degas to obtain a chitosan solution;
s4, adding 35 parts of soluble starch into 400 parts of deionized water, stirring for 2 hours in a water bath at 60 ℃ to obtain a starch solution, carrying out ultrasonic treatment on the starch solution for 15 minutes to degas, cooling the starch solution to normal temperature, and continuing stirring for 20 minutes;
s5, mixing the treated chitosan solution and the starch solution, adding 15 parts of glycerol, uniformly stirring, adding the anthocyanin microcapsules, carrying out ultrasonic oscillation treatment for 40min, stirring for 5h, and carrying out ultrasonic treatment for 5min for degassing to obtain a mixed membrane solution;
s6, pouring the mixed membrane solution into a horizontally placed stripping culture dish, and then placing the culture dish in a forced air drying oven at 40 ℃ for drying for 24 hours to obtain the bio-based food freshness indicating membrane.
The biological-based food freshness indicating film prepared by the embodiment has the advantages that the addition amount of anthocyanin is small, the color of the corresponding freshness intelligent indicating film is light purple, and the color change is more sensitive and the effect is more obvious in the monitoring of the freshness of meat products.
Example 3
This example provides a method for preparing a bio-based food freshness indicating film, which is similar to example 1, and is different from example 1 in that the raw material composition is as follows: anthocyanin powder: 10 parts of sodium alginate: 40 portions of CaCl2: 25 parts of soluble starch: 35 parts of chitosan: 30 parts of glycerol: 15 parts of acetic acid: 5 parts of a mixture; the anthocyanin powder is prepared from the following raw materials in parts by weight: dehydrated purple cabbage powder: 8 parts, acetic acid/70% ethanol aqueous solution: 70 parts of (B); the anthocyanin microcapsule is prepared from the following raw materials in parts by weight: anthocyanin powder: 10 parts of sodium alginate: 40 portions of CaCl2: 25 parts of deionized water: 500 parts.
The biological base food freshness indicator film anthocyanin addition amount that this embodiment prepared is more, and the colour of corresponding freshness intelligence indicator film is dark purple, and the discoloration is comparatively slow in the monitoring of meat food freshness.
Example 4
This example provides a method for preparing a bio-based food freshness indicating film, which is similar to example 1, and is different from example 1 in that the raw material composition is as follows: anthocyanin powder: 8 parts of sodium alginate: 40 portions of CaCl2: 30 parts of soluble starch: 35 parts of chitosan: 35 parts of glycerol: 5 parts of acetic acid: 5 parts of a mixture; the anthocyanin powder is prepared from the following raw materials in parts by weight: dehydrated purple cabbage powder: 10 parts, acetic acid/70% ethanol aqueous solution: 60 parts; the anthocyanin microcapsule is prepared from the following raw materials in parts by weight: anthocyanin powder: 8 parts of sodium alginate: 40 portions of CaCl2: 30 parts of deionized water: 600 parts.
The bio-based food freshness indicating film prepared by the embodiment has less glycerol addition amount, and the corresponding freshness intelligent indicating film has higher tensile strength but larger brittleness.
Example 5
This example provides a bio-based food freshness indicator film, according to example 1The preparation method is the same as that of the example 1, and is different from the example 1 in that the raw materials comprise the following components: anthocyanin powder: 8 parts of sodium alginate: 35 portions of CaCl2: 30 parts of soluble starch: 353 parts and chitosan: 35 parts of glycerol: 15 parts of acetic acid: 5 parts of a mixture; the anthocyanin powder is prepared from the following raw materials in parts by weight: dehydrated purple cabbage powder: 10 parts, acetic acid/70% ethanol aqueous solution: 60 parts; the anthocyanin microcapsule is prepared from the following raw materials in parts by weight: anthocyanin powder: 8 parts of sodium alginate: 35 portions of CaCl2: 30 parts of deionized water: 550 parts of the raw materials.
The bio-based food freshness indication film prepared by the embodiment has higher glycerol addition amount, and the corresponding freshness intelligent indication film has lower tensile strength but better toughness.
The bacteriostatic property of the bio-based food freshness indicating film in the application is tested by a flat plate bacterial colony counting method, and the specific experimental steps are as follows:
a certain amount (106CFU/mL) of escherichia coli and staphylococcus aureus suspension is dripped on the surface of the antibacterial preservative film, is evenly coated and is placed in an incubator at 37 +/-1 ℃ for culture for 4 hours. Then soaking the bacteria in a centrifuge tube of PBS buffer solution, shaking the bacteria on a constant temperature shaking table at 37 +/-1 ℃ for 10min, and then diluting the bacteria in the PBS buffer solution. 60 μ L of diluted PBS buffer was pipetted onto agar medium plates and incubated at 37. + -. 1 ℃ for 24h, each of which was repeated 3 times. The bacterial suspension without the preservative film is taken as a control group.
The bacteriostatic rates of the bio-based food freshness indicating films prepared in examples 1-5 are shown in the following table:
it should be understood that the above examples are only for clearly illustrating the technical solutions of the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The bio-based food freshness indicating film is characterized by being prepared from the following raw materials in parts by weight: anthocyanin powder: 5-10 parts of sodium alginate: 30 to 40 portions of CaCl2: 20-30 parts of soluble starch: 20-35 parts of chitosan: 20-35 parts of glycerol: 5-15 parts of acetic acid: 2-5 parts.
2. The bio-based food freshness indicating film according to claim 1, wherein the anthocyanin powder is prepared from the following raw materials in parts by weight: dehydrated purple cabbage powder: 5-10 parts of acetic acid/70% ethanol aqueous solution: 48-70 parts.
3. A method of making a bio-based food freshness indicating film according to claim 1 or 2, comprising the steps of:
s1, dehydrating and drying the cleaned purple cabbage, then smashing the purple cabbage into powder, adding the purple cabbage powder into an acetic acid/70% ethanol water solution, carrying out ultrasonic wave synergistic heating extraction, filtering and centrifuging the obtained extract, purifying the extract, and carrying out vacuum freeze drying to obtain anthocyanin powder;
s2, adding anthocyanin powder into deionized water to obtain an anthocyanin solution; adding sodium alginate into deionized water, stirring and degassing to obtain a sodium alginate solution, and mixing the anthocyanin solution and the sodium alginate solution to obtain a mixed solution; then preparing CaCl2Adding sodium alginate dropwise into CaCl2Obtaining anthocyanin microcapsules in the solution;
s3, adding chitosan and acetic acid into deionized water, uniformly stirring, and then carrying out ultrasonic treatment and degassing to obtain a chitosan solution;
s4, adding soluble starch into deionized water, heating and stirring in a water bath to obtain a starch solution, carrying out ultrasonic treatment and degassing on the starch solution, and then cooling the starch solution to the normal temperature and continuing stirring;
s5, mixing the treated chitosan solution and the starch solution, adding glycerol, uniformly stirring, adding anthocyanin microcapsules, and performing oscillation degassing treatment, stirring and ultrasonic degassing treatment to obtain a mixed membrane solution;
and S6, pouring the mixed membrane solution into a horizontally placed stripping culture dish, and drying to obtain the bio-based food freshness indicating membrane.
4. The method according to claim 3, wherein the purification treatment in step S1 is to purify the extract by using a macroporous resin.
5. The method according to claim 3, wherein the pH of the acetic acid/70% ethanol aqueous solution in step S1 is 2.8 to 3.0.
6. The preparation method according to claim 3, wherein the temperature of the dehydration drying process in the step S1 is 40-50 ℃, the drying time is 20-30 h, the temperature of the heating extraction process is 50-60 ℃, and the extraction time is 30-60 min.
7. The preparation method of claim 3, wherein the concentration of the anthocyanin solution in the step S2 is 1-2 mg/mL, and the mass ratio of the anthocyanin solution to the sodium alginate solution is 1: 3.
8. The preparation method of claim 3, wherein the water bath stirring temperature in the step S4 is 50-65 ℃, and the stirring time is 1-2 h.
9. The method according to claim 3, wherein the drying process in step S6 is carried out at a temperature of 35-45 ℃ for 20-24 hours.
10. A bio-based food freshness indicating film prepared by the preparation method of any one of claims 3 to 9.
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