CN111286056B - Preparation method of nano antioxidant film - Google Patents
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Abstract
The invention provides a preparation method of a nano oxidation resistant film. According to the technical scheme, gelatin, glycerol, tocopherol, tween and deionized water in a specific ratio are used as raw materials, a gelatin-glycerol aqueous solution and an oily solution are respectively prepared, the gelatin-glycerol aqueous solution and the oily solution are mixed and then are firstly subjected to homogenization treatment to obtain a composite gelatin membrane solution, and then the composite gelatin membrane solution is treated by combining high-pressure homogenization and ultrasound, so that the membrane solution is subjected to mechanical effect from the high-pressure homogenization and cavitation from ultrasound at the same time. The shearing force generated by high-pressure homogenization and bubbles generated by ultrasonic cavitation enable oil drops in the composite gelatin solution to form nano particles which are uniformly dispersed in the solution, so that the formed nano antioxidant gelatin film has high tensile strength, elongation at break and light barrier property, low film thickness and water vapor permeability and high oxidation resistance, and can be used as a functional food packaging material to be applied to the food industry.
Description
Technical Field
The invention relates to the technical field of gelatin films, in particular to a preparation method of a nano antioxidant film.
Background
In recent years, edible films have been a hot spot in the field of food packaging due to their edible safety and environmental degradability. Gelatin is a biological material derived from protein, and has good film forming property and biocompatibility. The physical properties of the pure gelatin film are poor, the bioactivity is low, the tensile strength, the light barrier property, the film thickness, the water vapor permeability and the like are not ideal, and the oxidation resistance is poor, so that the pure gelatin film needs to be modified to meet the process requirements in the field of food packaging.
At present, a common additive for preparing the antioxidant gelatin film is essential oil, and the strong smell of the essential oil influences the application of the gelatin film in the food field; meanwhile, the large oil component (essential oil) particles dispersed in the gelatin film hinder the interaction between protein and protein, and the mechanical property and the biological activity of the composite film are not brought into the best state.
Disclosure of Invention
The invention aims to provide a preparation method of a nano antioxidant film aiming at the technical defects of the prior art, and aims to solve the technical problem that the physical property of a conventional gelatin film needs to be improved in the prior art.
The invention also aims to solve the technical problem that the conventional gelatin film has poor oxidation resistance.
The invention further solves the technical problem of how to avoid introducing the prominent smell of essential oil while realizing the oxidation resistance of the gelatin film.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a preparation method of a nano oxidation resistant film comprises the following steps:
1) the formula comprises the following components in percentage by weight: 8% of gelatin, 1% of glycerol, 4% of tocopherol, 0.8% of tween and the balance of deionized water;
2) mixing gelatin and water, dissolving at 60 deg.C for 90min, and stirring until gelatin is completely dissolved;
3) cooling the gelatin solution obtained in the step 2) to room temperature, adding glycerol with the formula amount, and uniformly mixing to obtain a gelatin-glycerol aqueous solution;
4) mixing tocopherol and tween according to the formula amount, and fully oscillating by using an oscillator to obtain an oily solution;
5) mixing the gelatin-glycerol aqueous solution obtained in the step 3) with the oily solution obtained in the step 4), and carrying out homogenization treatment for 3min by using a homogenizer at 13000rpm to obtain a composite gelatin membrane liquid;
6) mixing the composite gelatin membrane liquid (also called as gelatin emulsion) obtained in the step 5) under the high-pressure homogenizing condition of 80-100 MPa
7) Carrying out ultrasonic treatment on the mixed product obtained in the step 6) for 10min under the condition of 400-600 w to obtain a membrane liquid before membrane forming;
8) and (3) forming a film by using the film liquid obtained in the step (7) before film forming.
Preferably, the film formation in step 8) includes: pouring the membrane liquid before membrane forming into a plate, and drying for 48 hours under the condition of room temperature ventilation; and (3) putting the dried membrane into a closed environment with the relative humidity of 50% for balancing for 24h, and removing the membrane to obtain the nano antioxidant membrane.
Preferably, the dish is a 90mm × 90mm plastic dish, and the amount of the membrane solution poured into the dish before membrane formation is 4 mL.
Preferably, the tween is tween 80.
Preferably, the freezing force of the gelatin in the step 1) and the step 2) is 260-270.
Preferably, in step 2), during the dissolving process, the port of the container is continuously closed by a preservative film (for preventing the moisture in the solution from volatilizing due to a long-time heating process and influencing the concentration of the gelatin in the solution).
Preferably, the number of high pressure cycles in step 6) is 3.
Preferably, the ultrasonic treatment in step 7) is carried out by using an ultrasonic disruptor, with a frequency of 20kHz, with a 6mm horn being selected, and stopped for 2s per 2s of ultrasonic treatment.
Preferably, the drying is carried out for 48 hours at a temperature of 25. + -. 2 ℃ and a relative humidity of 50. + -. 5%.
The invention provides a preparation method of a nano oxidation resistant film. According to the technical scheme, gelatin, glycerol, tocopherol, tween and deionized water in a specific ratio are used as raw materials, a gelatin-glycerol aqueous solution and an oily solution are respectively prepared, the gelatin-glycerol aqueous solution and the oily solution are mixed and then are firstly subjected to homogenization treatment to obtain a composite gelatin membrane solution, and then the composite gelatin membrane solution is treated by combining high-pressure homogenization and ultrasound, so that the membrane solution is subjected to mechanical effect from the high-pressure homogenization and cavitation from ultrasound at the same time. The shearing force generated by high-pressure homogenization and bubbles generated by ultrasonic cavitation enable oil drops in the composite gelatin solution to form nano particles which are uniformly dispersed in the solution, so that the formed nano oxidation-resistant gelatin film has high tensile strength, elongation at break, light barrier property, low film thickness, low water vapor permeability and high oxidation resistance, and can be used as a functional food packaging material to be applied to the food industry.
In order to improve the performance of the pure gelatin film, the tocopherol of an oily component is added in the preparation process of the gelatin film, so that the breaking elongation and the light barrier property of the film can be enhanced, and meanwhile, the oxidation resistance of the gelatin film is also enhanced due to the addition of the tocopherol; meanwhile, the physical property and the biological activity of the composite membrane are influenced by the size and the distribution of oily particles (tocopherol), and the nano-grade composite membrane is prepared by high-pressure homogenization and ultrasonic assistance, so that the physical property and the biological activity of the nano-grade composite membrane are further enhanced.
The nano oxidation resistant film prepared by the method has no unpleasant prominent smell, simultaneously has better mechanical property, waterproof property and light barrier property, has higher oxidation resistance than a non-nano oxidation resistant film, and can be used as a functional food packaging material to be applied to the field of food industry.
The beneficial effects of the invention are reflected in the following aspects: the invention prepares the nano oil drop particles by combining high-pressure homogenization and ultrasound, thereby having the following effects on the formation of the composite gelatin film: 1. the nano-level oil drop particles are uniformly distributed in the gelatin film, so that a film with a low film thickness can be formed; 2. the nano-level oil drops have small particle size, reduce the blocking effect between the gelatin protein and the protein and enhance the interaction between the protein and the protein, thereby increasing the tensile strength and the elongation at break of the gelatin film; 3. the nanometer level oil drop particles enhance the dispersion capability of the oil drops, thereby enhancing the barrier capability of the film to light; 4. the nano-level oil drop particles increase the specific surface area of oil drops, increase the difficulty of water vapor molecules to permeate the membrane, and increase the contact area of tocopherol oil drop particles and an oxidizing substance, so that the water vapor permeability of the membrane is reduced, and the oxidation resistance is enhanced. The invention can be used as a functional material in the field of food packaging.
Compared with the preparation method of the common composite membrane, the preparation method can greatly reduce the use amount of surface activity, and the product safety coefficient is high; compared with the preparation method of the conventional antioxidant gelatin film, the method uses the tocopherol as the antioxidant material, so that the adverse effect of the prominent smell of the conventional antioxidant (essential oil) on the gelatin film is avoided; compared with the product performance of the traditional composite gelatin film, the nano oxidation-resistant gelatin film prepared by the method has higher tensile strength and light barrier property, lower film thickness and water vapor permeability and higher oxidation resistance, and the functionality and the application value of the composite gelatin film are improved.
Drawings
FIG. 1 is a graph showing the oxidation resistance of the composite gelatin films obtained in the examples and comparative examples according to the embodiment of the present invention.
Detailed Description
Hereinafter, specific embodiments of the present invention will be described in detail. Well-known structures or functions may not be described in detail in the following embodiments in order to avoid unnecessarily obscuring the details. Approximating language, as used herein in the following examples, may be applied to identify quantitative representations that could permissibly vary in number without resulting in a change in the basic function. Unless defined otherwise, technical and scientific terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
A preparation method of a nano oxidation resistant film comprises the following steps:
(1) the following materials are selected in parts by weight: 8% of gelatin, 1% of glycerol, 4% of tocopherol, 0.8% of tween and the balance of deionized water, wherein the total amount is 100%.
(2) Mixing gelatin and water according to weight parts, and dissolving in 60 deg.C water solution for 90min while stirring until gelatin is completely dissolved.
(3) Cooling the gelatin water solution obtained in the step (2) to room temperature, adding a glycerol solution according to the weight part, and uniformly mixing to obtain a gelatin-glycerol water solution;
(4) mixing tocopherol and tween 80 in parts by weight, and sufficiently shaking by using a shaker to obtain an oily solution;
(5) mixing the aqueous solution in the step (3) and the oily solution in the step (4), and homogenizing for 3min by a homogenizer at 13000rpm to obtain a composite gelatin membrane liquid;
(6) mixing the gelatin emulsion obtained in the step (5) under a high-pressure homogenizing condition of 80-100 MPa;
(7) performing ultrasonic treatment on the gelatin emulsion obtained in the step (6) for 10min under the condition of 400-600 w to obtain a membrane liquid before membrane forming;
(8) pouring 4ml of the membrane liquid into a plastic plate with the thickness of 90mm by 90mm, and drying for 48 hours under the ventilation condition at room temperature;
(9) and (3) putting the dried membrane into a closed environment with the relative humidity of 50% for balancing for 24h, and removing the membrane to obtain the nano antioxidant membrane.
Wherein the gelatin freezing force in the step (1) is 260-270.
And (3) when the gelatin in the step (2) is heated in the water solution at the temperature of 60 ℃, sealing by using a preservative film to prevent the water in the solution from volatilizing in a long-time heating process to influence the concentration of the gelatin in the solution.
The number of high-pressure cycles in step (6) was 3.
And (4) selecting an ultrasonic crusher as ultrasonic equipment in the step (7), wherein the frequency is 20kHz, selecting a 6mm amplitude transformer, carrying out ultrasonic treatment for 2s, and stopping the ultrasonic treatment for 2 s.
The drying condition in the step (8) is carried out at 25. + -. 2 ℃ and a relative humidity of 50. + -. 5%.
The method adopts a mode of combining high-pressure homogenization and ultrasound to process the composite gelatin membrane liquid to prepare the nano-scale antioxidant gelatin membrane. The high-pressure homogenization and the ultrasound are combined to enable oil drops in the gelatin film to form nano particles, so that the nano-scale antioxidant gelatin film is prepared. On one hand, the gelatin film added with the tocopherol endows the gelatin film with good oxidation resistance, and simultaneously, the breaking elongation of the gelatin film is increased; on the other hand, compared with the non-nano-scale antioxidant gelatin film, the nano gelatin film prepared by combining high-pressure homogenization and ultrasound has higher antioxidant property, tensile strength and elongation at break and lower water vapor permeability. The nanometer level antioxidant gelatin film prepared by the method has good physical properties and high oxidation resistance, and can be used as a functional packaging material in the field of food packaging. The nano antioxidant gelatin film prepared by the method has good mechanical property, water vapor permeability and light barrier property, and the film has high antioxidant property, and can be used as a functional food packaging material.
Example 1
(1) The following materials are selected in parts by weight: 8% of gelatin, 1% of glycerol, 4% of tocopherol, 0.8% of tween and the balance of deionized water, wherein the total amount is 100%.
(2) Mixing gelatin and water according to weight parts, and dissolving in 60 deg.C water solution for 90min while stirring until gelatin is completely dissolved.
(3) Cooling the gelatin water solution obtained in the step (2) to room temperature, adding a glycerol solution according to the weight part, and uniformly mixing to obtain a gelatin-glycerol water solution;
(4) mixing tocopherol and tween 80 in parts by weight, and sufficiently shaking by using a shaker to obtain an oily solution;
(5) mixing the aqueous solution in the step (3) and the oily solution in the step (4), and homogenizing for 3min by a homogenizer at 13000rpm to obtain a composite gelatin membrane liquid;
(6) mixing the gelatin emulsion obtained in the step (5) under the high-pressure homogenization condition of 80 MPa;
(7) performing ultrasonic treatment on the gelatin emulsion obtained in the step (6) for 10min under the condition of 400w to obtain membrane liquid before membrane forming;
(8) pouring 4ml of the membrane liquid into a plastic plate with the thickness of 90mm by 90mm, and drying for 48 hours under the ventilation condition at room temperature;
(9) and (3) putting the dried membrane into a closed environment with the relative humidity of 50% for balancing for 24h, and removing the membrane to obtain the nano antioxidant membrane.
Example 2
(1) The following materials are selected in parts by weight: gelatin 8%, glycerol 1%, tocopherol 4%, tween 0.8%, and the balance of deionized water, the total being 100%.
(2) Mixing gelatin and water according to weight parts, and dissolving in 60 deg.C water solution for 90min while stirring until gelatin is completely dissolved.
(3) Cooling the gelatin water solution obtained in the step (2) to room temperature, adding a glycerol solution according to the weight part, and uniformly mixing to obtain a gelatin-glycerol water solution;
(4) mixing tocopherol and tween 80 in parts by weight, and sufficiently shaking by using a shaker to obtain an oily solution;
(5) mixing the aqueous solution in the step (3) and the oily solution in the step (4), and homogenizing for 3min by a homogenizer at 13000rpm to obtain a composite gelatin membrane liquid;
(6) mixing the gelatin emulsion obtained in the step (5) under the high-pressure homogenization condition of 80 MPa;
(7) performing ultrasonic treatment on the gelatin emulsion obtained in the step (6) for 10min under the condition of 600w to obtain membrane liquid before membrane forming;
(8) 4ml of the membrane liquid is poured into a plastic plate with 90mm to 90mm, and the plastic plate is dried for 48 hours under the ventilation condition at room temperature;
(9) and (3) putting the dried membrane into a closed environment with the relative humidity of 50% for balancing for 24h, and removing the membrane to obtain the nano antioxidant membrane.
Example 3
(1) The following materials are selected in parts by weight: 8% of gelatin, 1% of glycerol, 4% of tocopherol, 0.8% of tween and the balance of deionized water, wherein the total amount is 100%.
(2) Mixing gelatin and water according to weight parts, and dissolving in 60 deg.C water solution for 90min while stirring until gelatin is completely dissolved.
(3) Cooling the gelatin water solution obtained in the step (2) to room temperature, adding a glycerol solution according to the weight part, and uniformly mixing to obtain a gelatin-glycerol water solution;
(4) mixing tocopherol and tween 80 in parts by weight, and sufficiently shaking by using a shaker to obtain an oily solution;
(5) mixing the aqueous solution in the step (3) and the oily solution in the step (4), and homogenizing for 3min by a homogenizer at 13000rpm to obtain a composite gelatin membrane liquid;
(6) mixing the gelatin emulsion obtained in the step (5) under the high-pressure homogenization condition of 100 MPa;
(7) performing ultrasonic treatment on the gelatin emulsion obtained in the step (6) for 10min under the condition of 400w to obtain membrane liquid before membrane forming;
(8) pouring 4ml of the membrane liquid into a plastic plate with the thickness of 90mm by 90mm, and drying for 48 hours under the ventilation condition at room temperature;
(9) and (3) putting the dried membrane into a closed environment with the relative humidity of 50% for balancing for 24h, and removing the membrane to obtain the nano antioxidant membrane.
Example 4
(1) The following materials are selected in parts by weight: gelatin 8%, glycerol 1%, tocopherol 4%, tween 0.8%, and the balance of deionized water, the total being 100%.
(2) Mixing gelatin and water according to weight parts, and dissolving in 60 deg.C water solution for 90min while stirring until gelatin is completely dissolved.
(3) Cooling the gelatin water solution obtained in the step (2) to room temperature, adding a glycerol solution according to the weight part, and uniformly mixing to obtain a gelatin-glycerol water solution;
(4) mixing tocopherol and tween 80 in parts by weight, and sufficiently shaking by using a shaker to obtain an oily solution;
(5) mixing the aqueous solution in the step (3) and the oily solution in the step (4), and homogenizing for 3min by a homogenizer at 13000rpm to obtain a composite gelatin membrane liquid;
(6) mixing the gelatin emulsion obtained in the step (5) under the high-pressure homogenization condition of 100 MPa;
(7) performing ultrasonic treatment on the gelatin emulsion obtained in the step (6) for 10min under the condition of 600w to obtain membrane liquid before membrane forming;
(8) pouring 4ml of the membrane liquid into a plastic plate with the thickness of 90mm by 90mm, and drying for 48 hours under the ventilation condition at room temperature;
(9) and (3) putting the dried membrane into a closed environment with the relative humidity of 50% for balancing for 24h, and removing the membrane to obtain the nano antioxidant membrane.
Comparative example 1
(1) The following materials are selected in parts by weight: gelatin 8%, glycerol 1%, tocopherol 4%, tween 0.8%, and the balance of deionized water, the total being 100%.
(2) Mixing gelatin and water according to weight parts, and dissolving in 60 deg.C water solution for 90min while stirring until gelatin is completely dissolved.
(3) Cooling the gelatin water solution obtained in the step (2) to room temperature, adding a glycerol solution according to the weight part, and uniformly mixing to obtain a gelatin-glycerol water solution;
(4) mixing tocopherol and tween 80 in parts by weight, and sufficiently shaking by using a shaker to obtain an oily solution;
(5) mixing the aqueous solution in the step (3) and the oily solution in the step (4), and homogenizing for 3min by a homogenizer at 13000rpm to obtain a composite gelatin membrane liquid;
(6) 4ml of the membrane liquid is poured into a plastic plate with 90mm to 90mm, and the plastic plate is dried for 48 hours under the ventilation condition at room temperature;
(7) and (3) placing the dried film into a closed environment with the relative humidity of 50% for balancing for 24h, and removing the film to obtain the composite gelatin film.
Comparative example 2
(1) The following materials are selected in parts by weight: 8% of gelatin, 1% of glycerol, 4% of tocopherol, 0.8% of tween and the balance of deionized water, wherein the total amount is 100%.
(2) Mixing gelatin and water according to weight parts, and dissolving in 60 deg.C water solution for 90min while stirring until gelatin is completely dissolved.
(3) Cooling the gelatin aqueous solution obtained in the step (2) to room temperature, adding a glycerol solution according to parts by weight, and uniformly mixing to obtain a gelatin-glycerol aqueous solution;
(4) mixing tocopherol and tween 80 in parts by weight, and sufficiently shaking by using a shaker to obtain an oily solution;
(5) mixing the aqueous solution in the step (3) and the oily solution in the step (4), and homogenizing for 3min by a homogenizer at 13000rpm to obtain a composite gelatin membrane liquid;
(6) mixing the gelatin emulsion obtained in the step (5) under the high-pressure homogenization condition of 100 MPa;
(7) pouring 4ml of the membrane liquid into a plastic plate with the thickness of 90mm by 90mm, and drying for 48 hours under the ventilation condition at room temperature;
(8) and (3) placing the dried film into a closed environment with the relative humidity of 50% for balancing for 24h, and removing the film to obtain the composite gelatin film.
Comparative example 3
(1) The following materials are selected in parts by weight: 8% of gelatin, 1% of glycerol, 4% of tocopherol, 0.8% of tween and the balance of deionized water, wherein the total amount is 100%.
(2) Mixing gelatin and water according to weight parts, and dissolving in 60 deg.C water solution for 90min while stirring until gelatin is completely dissolved.
(3) Cooling the gelatin water solution obtained in the step (2) to room temperature, adding a glycerol solution according to the weight part, and uniformly mixing to obtain a gelatin-glycerol water solution;
(4) mixing tocopherol and tween 80 in parts by weight, and fully oscillating by using an oscillator to obtain an oily solution;
(5) mixing the aqueous solution in the step (3) and the oily solution in the step (4), and homogenizing for 3min by a homogenizer at 13000rpm to obtain a composite gelatin membrane liquid;
(6) performing ultrasonic treatment on the gelatin emulsion obtained in the step (6) for 10min under the condition of 600w to obtain membrane liquid before membrane forming;
(7) pouring 4ml of the membrane liquid into a plastic plate with the thickness of 90mm by 90mm, and drying for 48 hours under the ventilation condition at room temperature;
(8) and (3) placing the dried film into a closed environment with the relative humidity of 50% for balancing for 24h, and removing the film to obtain the composite gelatin film.
Example 5
The nano oxidation-resistant films prepared according to examples 1-4 and the common composite gelatin films prepared according to comparative examples 1-3 were subjected to detection of film thickness, water vapor transmission rate, tensile strength, elongation at break, water solubility and light transmittance.
The detection method comprises the following steps:
measurement of thickness of mono-and nano-gelatin films
The thickness of the film was measured by an electronic micrometer screw, and the measurement results are shown in table 1.
Second, testing the mechanical properties of the nano gelatin film
The composite gelatin film was tested for Tensile Strength (TS) and Elongation At Break (EAB) using a texture analyzer. The membrane is cut into strips with the width of 20mm and the length of 50mm, the membrane is fixed at two ends of a handle of the instrument, the distance between the two ends of the handle is adjusted to be 30mm, the testing speed is 1mm/s, and the hair promoting force is 20.0 g. The test structures are shown in table 1.
TS(MPa)＝F max /A
EAB(％)＝(L 0 /ΔL)×100％
Wherein, F max Is the maximum load (N) required for separating the strip-like membrane sample, and A is the cross-sectional area (m) of the sample membrane 2 )，L 0 Is the initial stretched length of the film,. DELTA.L is the stretched length after breaking of the film, L 0 ＝30mm。
Test of water vapor permeability of nanometer gelatin film
Dried CaCl was placed in a glass cup having a diameter of 40mm and a depth of 25mm 2 The glass was sealed with a film. The glass cup was placed in a closed container containing deionized water and the ambient temperature was adjusted to 30 ℃. The weight of the glass was measured every hour until there was no significant change in the weight of the glass, and the measurement was stopped. The water vapor permeability of the membrane was calculated by the following formula:
WVP(g m -1 s -1 Pa -1 )＝wlA -1 t -1 (P 2 –P 1 ) -1 ,
w represents the weight of growth of the glass (g), l is the thickness of the film (m), A is the area of the film seal (m) 2 ) T is the time(s) of change in weight of the glass, P 2 -P 1 Is the vapor pressure difference across the membrane (4244.9Pa at 30 ℃). The test structures are shown in table 1.
Fourth, testing the light barrier property of the nano gelatin film
The light barrier properties of the films were measured with a spectrophotometer with the visible light oriented between 200nm and 800 nm. The test structures are shown in table 2.
Free radical scavenging ability of DPPH
Preparing 0.1mmol/l DPPH solution with absolute ethyl alcohol, and storing in dark. Adding 2ml test sample solution and 2ml DPPH solution into the same test tube, shaking, standing in dark at room temperature for 30minMeasuring the absorbance A 1 Simultaneously measuring the absorbance A of 2ml of DPPH solution mixed with 2ml of solvent 0 The calculation formula of DPPH is:
A 0 absorbance at 520nm of DPPH without sample addition, A 1 The absorbance of the sample with the DPPH reagent at 520 nm. The test results are shown in fig. 1.
TABLE 1 composite gelatin film thickness, tensile strength, elongation at break, water vapor permeability data
TABLE 2 composite gelatin film light barrier data
The embodiments of the present invention have been described in detail, but the description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. Any modification, equivalent replacement, and improvement made within the scope of the application of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation method of a nano oxidation resistant film is characterized by comprising the following steps:
1) the formula comprises the following components in percentage by weight: 8% of gelatin, 1% of glycerol, 4% of tocopherol, 0.8% of tween and the balance of deionized water;
2) mixing gelatin and water, dissolving at 60 deg.C for 90min, and stirring until gelatin is completely dissolved;
3) cooling the gelatin solution obtained in the step 2) to room temperature, adding glycerol with the formula amount, and uniformly mixing to obtain a gelatin-glycerol aqueous solution;
4) mixing tocopherol and tween according to the formula amount, and fully oscillating by using an oscillator to obtain an oily solution;
5) mixing the gelatin-glycerol aqueous solution obtained in the step 3) with the oily solution obtained in the step 4), and carrying out homogenization treatment for 3min by using a homogenizer at 13000rpm to obtain a composite gelatin membrane liquid;
6) mixing the composite gelatin membrane liquid obtained in the step 5) under the high-pressure homogenizing condition of 80-100 MPa;
7) carrying out ultrasonic treatment on the product mixed in the step 6) for 10min under the condition of 400-600 w to obtain a membrane liquid before membrane forming;
8) and (3) forming a film by using the film liquid obtained in the step (7) before film forming.
2. The method for preparing a nano oxidation-resistant film according to claim 1, wherein the step of forming the film in step 8) comprises: pouring the membrane liquid before membrane forming into a flat dish, and drying for 48 hours under the ventilation condition at room temperature; and (3) putting the dried membrane into a closed environment with the relative humidity of 50% for balancing for 24h, and removing the membrane to obtain the nano anti-oxidation membrane.
3. The method for preparing a nano antioxidant membrane as claimed in claim 2, wherein the dish is a plastic dish of 90mm x 90mm, and the pouring amount of the membrane solution before membrane formation into the dish is 4 mL.
4. The method for preparing a nano antioxidant membrane as claimed in claim 1, wherein the tween is tween 80.
5. The method for preparing a nano antioxidant film according to claim 1, wherein the freezing force of the gelatin in step 1) and step 2) is 260-270.
6. The method for preparing a nano antioxidant film as claimed in claim 1, wherein in the step 2), a port of the container is continuously closed with a preservative film during the dissolution.
7. The method for preparing a nano antioxidant film as claimed in claim 1, wherein the number of high pressure cycles in step 6) is 3.
8. The method for preparing a nano antioxidant film as claimed in claim 1, wherein the ultrasonic treatment in step 7) is performed by using an ultrasonicator, the frequency is 20kHz, a horn of 6mm is selected, and 2s of treatment is stopped every 2s of ultrasonic treatment.
9. The method for preparing a nano anti-oxidation film according to claim 2, wherein the drying is performed at a temperature of 25 ± 2 ℃ and a relative humidity of 50 ± 5% for 48 hours.
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| CN104194354A (en) * | 2014-09-05 | 2014-12-10 | 山东省海洋生物研究院 | Edible biological preservative film and preparation method thereof |
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