CN114316379B - Degradable antibacterial and antioxidant film and preparation method thereof - Google Patents
Degradable antibacterial and antioxidant film and preparation method thereof Download PDFInfo
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- CN114316379B CN114316379B CN202210030835.6A CN202210030835A CN114316379B CN 114316379 B CN114316379 B CN 114316379B CN 202210030835 A CN202210030835 A CN 202210030835A CN 114316379 B CN114316379 B CN 114316379B
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Abstract
The invention discloses a degradable antibacterial and antioxidant film and a preparation method thereof, and relates to the technical field of preservative films, wherein the degradable antibacterial and antioxidant film is prepared from the following raw materials in percentage by weight: the weight ratio of chitosan, zein, volatile oil and glycerol is (0.8-1.2): (0.8-1.2): (0.8-1.2): (0.4 to 0.6); the preparation method of the degradable antibacterial and antioxidant film comprises the following steps of S1: preparing volatile oil: s2: preparation of chitosan solution and zein solution: s3: embedding volatile oil in zein; s4: preparation of the film: the biological regenerated degradable corn protein solution and chitosan are adopted as the base materials of the film, so that the environmental problems of white pollution caused by discarding the traditional film, atmospheric pollution caused by burning and the like are solved, the antibacterial and antioxidant functions of the film are enhanced by adopting the volatile oil, and the food spoilage and rancidity are delayed.
Description
Technical Field
The invention relates to the technology in the field of preservative films, in particular to a degradable antibacterial and antioxidant film and a preparation method thereof.
Background
Food safety problems are always serious global health problems, and are directly related to life and health of people and are hot topics of social attention at home and abroad. With the improvement of people living water, people pay more and more attention to the safety of food storage, and the research on food preservation technology is a hot spot problem of research in recent years. The food preservative film technology is also receiving more and more attention, the traditional preservative film is often made of petroleum products such as polyethylene, polyvinyl alcohol and the like, and the environmental problems such as white pollution and the like are easy to cause due to the characteristic of difficult degradation, and in addition, a large amount of carbon dioxide gas is released when the film is burnt, so that the greenhouse effect of the earth is increased to a certain extent. In this regard, development of novel degradable preservative films is becoming a development direction of preservative films. The main market is still petroleum-based preservative films, and the major disadvantages of the petroleum-based preservative films are easy environmental pollution and lack of functionality. At present, research and development of novel film materials and film functionality are faster, but the problems of single function, complex production and preparation process and the like are also commonly existed.
Volatile oil is also called essential oil, is an oily liquid with volatility and can be distilled out along with water vapor, has special fragrance, and mainly exists in plants of Labiatae, umbelliferae, compositae, rutaceae, zingiberaceae and the like. Volatile oil mainly comprises aliphatic and aromatic compounds, has strong biological activities such as antibiosis and antioxidation, and has been widely used in the fields of medicine, food and the like. Meanwhile, volatile oils are considered to be generally safe and have been widely added to foods and medicines.
However, volatile oil has the characteristics of instability, volatility and the like, is sensitive to light, heat and air, and is easy to volatilize and oxidize and deteriorate after long-term exposure, so that the related efficacy and effect are lost, and the application of the volatile oil is limited. For this reason, in order to increase the stability of the volatile oil, certain technical means, such as inclusion, emulsification, encapsulation, etc., are required to stabilize the volatile oil in the carrier material, thereby achieving the activity and effect of the volatile oil.
Based on the importance of environmental and food safety at home and abroad, the volatile oil is reported to be integrated into the degradable film, but the existing integrated antibacterial degradable film has the defects of complex process and multiple procedures; or the volatile oil is directly added into the film. The complex process leads to high cost, the volatile oil is directly added into the film, and the volatile oil is easy to volatilize in the subsequent drying process of the film due to the characteristic of thermal instability of the volatile oil; volatile oils volatilize, resulting in a film with a matte surface, even perforations, limiting the application of the film.
Disclosure of Invention
In view of the above, the present invention aims at overcoming the disadvantages of the prior art, and its main object is to provide a degradable antibacterial and antioxidant film and a preparation method thereof, which solves the environmental problems of white pollution caused by discarding the traditional film and atmospheric pollution caused by incineration by using a bio-renewable degradable zein solution and chitosan as the base materials of the film; the volatile oil is adopted to enhance the antibacterial and antioxidant functions of the film and delay food spoilage and rancidity.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the degradable antibacterial and antioxidant film is prepared from the following raw materials in percentage by weight: the weight ratio of chitosan, zein, volatile oil and glycerol is (0.8-1.2): (0.8-1.2): (0.8-1.2): (0.4 to 0.6).
As a preferred embodiment: the weight ratio of the chitosan to the zein to the volatile oil to the glycerol is 1:1:1:0.6.
as a preferred embodiment: the volatile oil is Jiang Xiangru volatile oil.
The preparation method of the degradable antibacterial and antioxidant film comprises the following steps:
s1: preparing volatile oil: placing the medicinal materials containing the volatile oil into a volatile oil extractor, adding 6-10 times of water by weight, heating, distilling and extracting for 2-8 h; stopping heating to obtain a water layer and a volatile oil layer respectively, and adding a drying agent into the volatile oil layer to dehydrate and dry to obtain volatile oil;
s2: preparation of chitosan solution and zein solution: adding chitosan into acetic acid solution, stirring to form transparent chitosan solution, centrifuging, filtering insoluble substances, and collecting upper chitosan solution for use; dissolving zein in ethanol solution, stirring to form transparent zein solution, centrifuging, filtering insoluble substances, and collecting upper zein solution for use;
s3: embedding volatile oil in zein;
s4: preparation of the film: adding chitosan and glycerol solution into the product obtained by embedding the volatile oil into S3 zein, and homogenizing for 5min at 13000rpm to obtain film forming solution; pouring the film forming solution into a culture dish, vacuum degassing the film forming solution in the culture dish, and drying in a drying oven at 30-50 ℃ for 36h to obtain the film.
As a preferred embodiment: and (3) embedding the volatile oil by using the zein in the step S3 to form nanoemulsion embedded volatile oil or nanoparticle embedded volatile oil.
As a preferred embodiment: the specific steps of forming the nanoemulsion embedded volatile oil are as follows: dropwise adding the upper-layer zein solution obtained in the step S2 into ultrapure water, homogenizing while dropwise adding, and separating out zein nanoparticles from the zein solution; adding the volatile oil obtained in the step S1 into zein nanoparticles, homogenizing while dripping, and adsorbing the zein nanoparticles on the surface of the volatile oil droplets to form nanoemulsion embedded volatile oil.
As a preferred embodiment: the homogenizing speed is 10000rpm-15000rpm, the homogenizing time is 5min-30min, and the weight ratio of volatile oil to zein nanoparticles is 0-1.5.
As a preferred embodiment: the specific steps of forming the nanoparticle embedded volatile oil are as follows: adding the volatile oil obtained in the step S1 into the upper-layer zein solution obtained in the step S2, wherein the weight ratio of the volatile oil to the zein solution is 0-1.5, homogenizing while dripping, the homogenizing speed is 13000rpm, the homogenizing time is 15min, and the volatile oil and the zein solution are fully dissolved to form a uniform solution; dripping the solution into ultrapure water, homogenizing while dripping, homogenizing at 13000rpm for 5-30 min, and separating out nanoparticles by dissolving volatile oil and zein in water to obtain nanoparticle-embedded volatile oil.
As a preferred embodiment: the mass concentration of the acetic acid solution in the S2 is 1% -5%, the mass concentration of the chitosan solution is 1% -5%, the volume concentration of the ethanol solution is 70% -90%, and the mass concentration of the formed corn protein solution is 1% -5%.
As a preferred embodiment: the dryer in the S1 is anhydrous sodium sulfate or anhydrous calcium sulfate.
Compared with the prior art, the invention has obvious advantages and beneficial effects:
1. the biological regenerated degradable corn protein solution and chitosan are used as the base materials of the film, so that the environmental problems of white pollution caused by discarding the traditional film, atmospheric pollution caused by burning and the like are solved, and the safety of the packaging material is greatly improved;
2. the volatile oil is adopted to enhance the antibacterial and antioxidant functions of the film, delay food spoilage and rancidity and solve the problems of food safety and food waste to a certain extent;
3. the preparation method provided by the invention overcomes the technical problems of complex production process of the degradable antibacterial and antioxidant film in the prior art; meanwhile, the problem that volatile oil is easy to volatilize in the subsequent drying process of the film due to the characteristic of thermal instability of the volatile oil by directly adding the volatile oil into the film in the prior art is solved; the degradable antibacterial and antioxidant film provided by the invention has the advantages of smooth surface, high tensile strength and good antibacterial and antioxidant effects.
In order to more clearly illustrate the structural features and efficacy of the present invention, a detailed description thereof will be given below with reference to the accompanying drawings and examples.
Drawings
FIG. 1 is a graph showing the transmittance of the films prepared in examples 1-6 and comparative examples according to the present invention as a function of wavelength;
FIG. 2 is a scanning electron microscope image of the surface morphology of a comparative film of the present invention;
FIG. 3 is a scanning electron microscope image of a broken cross section of a comparative film of the present invention;
FIG. 4 is a scanning electron microscope image of the surface morphology of the thin film of example 1 of the present invention;
FIG. 5 is a scanning electron microscope image of the surface morphology of the thin film of example 2 of the present invention;
FIG. 6 is a scanning electron microscope image of a broken cross section of a film according to example 2 of the present invention;
FIG. 7 is a scanning electron microscope image of the surface morphology of the thin film of example 3 of the present invention;
FIG. 8 is a scanning electron microscope image of the surface morphology of the thin film of example 4 of the present invention;
FIG. 9 is a scanning electron microscope image of the surface morphology of the thin film of example 5 of the present invention;
FIG. 10 is a scanning electron microscope image of a broken section of a film according to example 5 of the present invention;
FIG. 11 is a scanning electron microscope image of the surface morphology of the thin film of example 6 of the present invention;
FIG. 12 is a graph showing the oxidation resistance of the films prepared in examples 1-6 and comparative examples of the present invention.
Detailed Description
The invention discloses a degradable antibacterial and antioxidant film, which is shown in figures 1 to 12 and is prepared from the following raw materials in percentage by weight: the weight ratio of chitosan, zein, volatile oil and glycerol is (0.8-1.2): (0.8-1.2): (0.8-1.2): (0.4 to 0.6).
The weight ratio of the chitosan, the zein, the volatile oil and the glycerol is 1:1:1:0.6.
the volatile oil is Jiang Xiangru volatile oil.
The preparation method of the degradable antibacterial and antioxidant film comprises the following steps:
s1: preparing volatile oil: placing the medicinal materials containing the volatile oil into a volatile oil extractor, adding 6-10 times of water by weight, heating, distilling and extracting for 2-8 h; stopping heating to obtain a water layer and a volatile oil layer respectively, and adding a drying agent into the volatile oil layer to dehydrate and dry to obtain volatile oil; wherein the drying agent is anhydrous sodium sulfate or anhydrous calcium sulfate;
s2: preparation of chitosan solution and zein solution: adding chitosan into acetic acid solution, stirring to form transparent chitosan solution, centrifuging, filtering insoluble substances, and collecting upper chitosan solution for use; dissolving zein in ethanol solution, stirring to form transparent zein solution, centrifuging, filtering insoluble substances, and collecting upper zein solution for use; wherein the mass concentration of the acetic acid solution is 1% -5%, the mass concentration of the chitosan solution is 1% -5%, the volume concentration of the ethanol solution is 70% -90%, and the mass concentration of the corn protein solution is 1% -5%.
S3: embedding volatile oil in zein;
and S3, embedding the volatile oil by using zein to form nanoemulsion embedded volatile oil, wherein the specific steps of forming the nanoemulsion embedded volatile oil are as follows: dropwise adding the upper-layer zein solution obtained in the step S2 into ultrapure water, homogenizing while dropwise adding, and separating out zein nanoparticles from the zein solution; adding the volatile oil obtained in the step S1 into the zein nanoparticles, wherein the weight ratio of the volatile oil to the zein nanoparticles is 0-1.5; homogenizing while dripping, wherein zein nanoparticles are adsorbed on the surface of the volatile oil drops to form nanoemulsion embedded volatile oil, wherein the homogenizing speed is 10000-15000 rpm, and the homogenizing time is 5-30 min.
And S3, embedding volatile oil by using zein to form nanoparticle embedded volatile oil, wherein the specific steps of forming the nanoparticle embedded volatile oil are as follows: adding the volatile oil obtained in the step S1 into the upper-layer zein solution obtained in the step S2, wherein the weight ratio of the volatile oil to the zein solution is 0-1.5, homogenizing while dripping, the homogenizing speed is 13000rpm, the homogenizing time is 15min, and the volatile oil and the zein solution are fully dissolved to form a uniform solution; dripping the solution into ultrapure water, homogenizing while dripping, homogenizing at 13000rpm for 5-30 min, and separating out nanoparticles by dissolving volatile oil and zein in water to obtain nanoparticle-embedded volatile oil.
S4: preparation of the film: adding chitosan and glycerol solution into the product obtained by embedding the volatile oil into S3 zein, and homogenizing for 5min at 13000rpm to obtain film forming solution; pouring the film forming solution into a culture dish, vacuum degassing the film forming solution in the culture dish, and drying in a drying oven at 30-50 ℃ for 36h to obtain the film.
Example 1
The preparation method of the degradable antibacterial and antioxidant film comprises the following steps:
s1: preparing volatile oil: extracting Jiang Xiangru with 8 times of water for 5 hr, stopping heating to obtain water layer and volatile oil layer, adding anhydrous sodium sulfate or anhydrous calcium sulfate, and dehydrating and drying to obtain Jiang Xiangru volatile oil;
s2: preparation of chitosan solution and zein solution: adding chitosan into acetic acid solution with the mass concentration of 1%, stirring to form transparent chitosan solution with the mass fraction of 1%, centrifuging, filtering insoluble substances, and taking upper chitosan solution for later use; dissolving zein in 90% ethanol solution, stirring to form transparent zein solution with mass concentration of 5%, centrifuging, filtering to remove insoluble, and collecting upper zein solution;
s3: preparing the nanoemulsion embedded volatile oil: dripping the upper layer zein solution obtained by 30mLS into 120mL of ultrapure water, homogenizing while dripping, wherein the homogenizing speed is 13000rpm, the homogenizing time is 5min, and separating out zein nanoparticles from the zein solution; adding the volatile oil obtained in the step S1 into the zein nanoparticles, wherein the weight ratio of the volatile oil to the zein is 0.5, homogenizing while dripping, the homogenizing speed is 13000rpm, the homogenizing time is 15min, and the zein nanoparticles are adsorbed on the surfaces of the volatile oil droplets to form nanoemulsion embedded volatile oil.
S4: preparation of the film: adding 150mL of chitosan and 0.9g of glycerol solution into the nanoemulsion embedded volatile oil formed in the step S3, and homogenizing for 5min at the rotating speed of 13000rpm to obtain a film forming solution; pouring 80g of film forming solution into a plastic culture dish with the diameter of 11cm, vacuum degassing the film forming solution in the culture dish, drying in a drying oven at 40 ℃ for 36h, and demoulding to obtain the film embedded with the volatile oil.
Example 2
The preparation method of the degradable antibacterial and antioxidant film comprises the following steps:
s1: preparing volatile oil: extracting Jiang Xiangru with 8 times of water for 5 hr, stopping heating to obtain water layer and volatile oil layer, adding anhydrous sodium sulfate or anhydrous calcium sulfate, and dehydrating and drying to obtain Jiang Xiangru volatile oil;
s2: preparation of chitosan solution and zein solution: adding chitosan into acetic acid solution with the mass concentration of 1%, stirring to form transparent chitosan solution with the mass fraction of 1%, centrifuging, filtering insoluble substances, and taking upper chitosan solution for later use; dissolving zein in 90% ethanol solution, stirring to form transparent zein solution with mass concentration of 5%, centrifuging, filtering to remove insoluble, and collecting upper zein solution;
s3: preparing the nanoemulsion embedded volatile oil: dripping the upper layer zein solution obtained by 30mLS into 120mL of ultrapure water, homogenizing while dripping, wherein the homogenizing speed is 13000rpm, the homogenizing time is 5min, and separating out zein nanoparticles from the zein solution; adding the volatile oil obtained in the step S1 into the zein nanoparticles, wherein the weight ratio of the volatile oil to the zein is 1, homogenizing while dripping, the homogenizing rotating speed is 13000rpm, the homogenizing time is 15min, and the zein nanoparticles are adsorbed on the surfaces of the volatile oil droplets to form nanoemulsion embedded volatile oil.
S4: preparation of the film: adding 150mL of chitosan and 0.9g of glycerol solution into the nanoemulsion embedded volatile oil formed in the step S3, and homogenizing for 5min at the rotating speed of 13000rpm to obtain a film forming solution; pouring 80g of film forming solution into a plastic culture dish with the diameter of 11cm, vacuum degassing the film forming solution in the culture dish, drying in a drying oven at 40 ℃ for 36h, and demoulding to obtain the film embedded with the volatile oil.
Example 3
The preparation method of the degradable antibacterial and antioxidant film comprises the following steps:
s1: preparing volatile oil: extracting Jiang Xiangru with 8 times of water for 5 hr, stopping heating to obtain water layer and volatile oil layer, adding anhydrous sodium sulfate or anhydrous calcium sulfate, and dehydrating and drying to obtain Jiang Xiangru volatile oil;
s2: preparation of chitosan solution and zein solution: adding chitosan into acetic acid solution with the mass concentration of 1%, stirring to form transparent chitosan solution with the mass fraction of 1%, centrifuging, filtering insoluble substances, and taking upper chitosan solution for later use; dissolving zein in 90% ethanol solution, stirring to form transparent zein solution with mass concentration of 5%, centrifuging, filtering to remove insoluble, and collecting upper zein solution;
s3: preparing the nanoemulsion embedded volatile oil: dripping the upper layer zein solution obtained by 30mLS into 120mL of ultrapure water, homogenizing while dripping, wherein the homogenizing speed is 13000rpm, the homogenizing time is 5min, and separating out zein nanoparticles from the zein solution; adding the volatile oil obtained in the step S1 into the zein nanoparticles, wherein the weight ratio of the volatile oil to the zein is 1.5, homogenizing while dripping, the homogenizing speed is 13000rpm, the homogenizing time is 15min, and the zein nanoparticles are adsorbed on the surfaces of the volatile oil droplets to form nanoemulsion embedded volatile oil.
S4: preparation of the film: adding 150mL of chitosan and 0.9g of glycerol solution into the nanoemulsion embedded volatile oil formed in the step S3, and homogenizing for 5min at the rotating speed of 13000rpm to obtain a film forming solution; pouring 80g of film forming solution into a plastic culture dish with the diameter of 11cm, vacuum degassing the film forming solution in the culture dish, drying in a drying oven at 40 ℃ for 36h, and demoulding to obtain the film embedded with the volatile oil.
Example 4
The preparation method of the degradable antibacterial and antioxidant film comprises the following steps:
s1: preparing volatile oil: extracting Jiang Xiangru with 8 times of water for 5 hr, stopping heating to obtain water layer and volatile oil layer, adding anhydrous sodium sulfate or anhydrous calcium sulfate, and dehydrating and drying to obtain Jiang Xiangru volatile oil;
s2: preparation of chitosan solution and zein solution: adding chitosan into acetic acid solution with the mass concentration of 1%, stirring to form transparent chitosan solution with the mass fraction of 1%, centrifuging, filtering insoluble substances, and taking upper chitosan solution for later use; dissolving zein in 90% ethanol solution, stirring to form transparent zein solution with mass concentration of 5%, centrifuging, filtering to remove insoluble, and collecting upper zein solution;
s3: preparing nanoparticle embedded volatile oil: adding the volatile oil obtained in 30mLS to the upper-layer zein solution obtained in S2, wherein the weight ratio of the volatile oil to the zein solution is 0.5, homogenizing while dripping, the homogenizing speed is 13000rpm, the homogenizing time is 15min, and the volatile oil and the zein solution are fully dissolved to form a uniform solution; the solution is dripped into 120mL of ultrapure water, and is homogenized while dripping, the homogenizing speed is 13000rpm, the homogenizing time is 5, and the volatile oil and the zein are insoluble in water to separate out nanoparticles, thus forming the nanoparticle embedded volatile oil.
S4: preparation of the film: adding 150mL of chitosan and 0.9g of glycerol solution into the nanoparticle embedded volatile oil formed in the step S3, and homogenizing for 5min at the rotating speed of 13000rpm to obtain a film forming solution; pouring 80g of film forming solution into a plastic culture dish with the diameter of 11cm, vacuum degassing the film forming solution in the culture dish, drying in a drying oven at 40 ℃ for 36h, and demoulding to obtain the film embedded with the volatile oil.
Example 5
The preparation method of the degradable antibacterial and antioxidant film comprises the following steps:
s1: preparing volatile oil: extracting Jiang Xiangru with 8 times of water for 5 hr, stopping heating to obtain water layer and volatile oil layer, adding anhydrous sodium sulfate or anhydrous calcium sulfate, and dehydrating and drying to obtain Jiang Xiangru volatile oil;
s2: preparation of chitosan solution and zein solution: adding chitosan into acetic acid solution with the mass concentration of 1%, stirring to form transparent chitosan solution with the mass fraction of 1%, centrifuging, filtering insoluble substances, and taking upper chitosan solution for later use; dissolving zein in 90% ethanol solution, stirring to form transparent zein solution with mass concentration of 5%, centrifuging, filtering to remove insoluble, and collecting upper zein solution;
s3: preparing nanoparticle embedded volatile oil: adding the volatile oil obtained in 30mLS to the upper-layer zein solution obtained in S2, wherein the weight ratio of the volatile oil to the zein solution is 1, homogenizing while dripping, the homogenizing speed is 13000rpm, the homogenizing time is 15min, and the volatile oil and the zein solution are fully dissolved to form a uniform solution; the solution is dripped into 120mL of ultrapure water, and is homogenized while dripping, the homogenizing speed is 13000rpm, the homogenizing time is 5, and the volatile oil and the zein are insoluble in water to separate out nanoparticles, thus forming the nanoparticle embedded volatile oil.
S4: preparation of the film: adding 150mL of chitosan and 0.9g of glycerol solution into the nanoparticle embedded volatile oil formed in the step S3, and homogenizing for 5min at the rotating speed of 13000rpm to obtain a film forming solution; pouring 80g of film forming solution into a plastic culture dish with the diameter of 11cm, vacuum degassing the film forming solution in the culture dish, drying in a drying oven at 40 ℃ for 36h, and demoulding to obtain the film embedded with the volatile oil.
Example 6
The preparation method of the degradable antibacterial and antioxidant film comprises the following steps:
s1: preparing volatile oil: extracting Jiang Xiangru with 8 times of water for 5 hr, stopping heating to obtain water layer and volatile oil layer, adding anhydrous sodium sulfate or anhydrous calcium sulfate, and dehydrating and drying to obtain Jiang Xiangru volatile oil;
s2: preparation of chitosan solution and zein solution: adding chitosan into acetic acid solution with the mass concentration of 1%, stirring to form transparent chitosan solution with the mass fraction of 1%, centrifuging, filtering insoluble substances, and taking upper chitosan solution for later use; dissolving zein in 90% ethanol solution, stirring to form transparent zein solution with mass concentration of 5%, centrifuging, filtering to remove insoluble, and collecting upper zein solution;
s3: preparing nanoparticle embedded volatile oil: adding the volatile oil obtained in 30mLS to the upper-layer zein solution obtained in S2, wherein the weight ratio of the volatile oil to the zein solution is 1.5, homogenizing while dripping, the homogenizing speed is 13000rpm, the homogenizing time is 15min, and the volatile oil and the zein solution are fully dissolved to form a uniform solution; dripping the solution into 120mL of ultrapure water, homogenizing while dripping, wherein the homogenizing speed is 13000rpm, the homogenizing time is 5, and the volatile oil and the zein are insoluble in water to separate out nanoparticles to form nanoparticle-embedded volatile oil;
s4: preparation of the film: adding 150mL of chitosan and 0.9g of glycerol solution into the nanoparticle embedded volatile oil formed in the step S3, and homogenizing for 5min at the rotating speed of 13000rpm to obtain a film forming solution; pouring 80g of film forming solution into a plastic culture dish with the diameter of 11cm, vacuum degassing the film forming solution in the culture dish, drying in a drying oven at 40 ℃ for 36h, and demoulding to obtain the film embedded with the volatile oil.
Comparative example
The preparation method of the blank film without volatile oil in the embodiment comprises the following steps:
s1: preparation of chitosan solution and zein solution: adding chitosan into acetic acid solution with the mass concentration of 1%, stirring to form transparent chitosan solution with the mass fraction of 1%, centrifuging, filtering insoluble substances, and taking upper chitosan solution for later use; dissolving zein in 90% ethanol solution, stirring to form transparent zein solution with mass concentration of 5%, centrifuging, filtering to remove insoluble, and collecting upper zein solution;
s2: precipitation of nanoparticles: 30mLS to obtain upper zein solution, dripping the solution into 120mL ultrapure water, homogenizing while dripping, homogenizing at 13000rpm for 5 times, and separating nanoparticles out while insoluble zein;
s3: preparation of the film: adding 150mL of chitosan and 0.9g of glycerol solution into the nano particles separated out from the S2, and homogenizing for 5min at the rotating speed of 13000rpm to obtain a film forming solution; pouring 80g of film forming solution into a plastic culture dish with the diameter of 11cm, vacuum degassing the film forming solution in the culture dish, drying in a drying oven at 40 ℃ for 36h, and demoulding to obtain the blank film without volatile oil.
Effect example 1
Nanoparticle and nanoemulsion particle size distribution assay:
the sizes of the thin film particle diameters, particle size dispersibility and potential values in examples 1 to 6 and comparative examples were analyzed using a malvern particle diameter analyzer; the results of the present invention on the size, particle size distribution and potential values of the particle diameters of the films obtained in examples 1 to 6 and comparative examples are shown in Table 1 below;
TABLE 1 results of particle size, particle size dispersibility and potential values of films
Analysis of results:
as can be seen from the data in table 1: the particle sizes of the films in examples 1-6 and comparative examples are all nano-scale, the potential value of the film is between 40.8mV and 59.8mV, and the film can exist stably; in the films prepared by embedding the volatile oil in the nanoemulsion in the examples 1-3, the grain size of the films is slowly increased along with the increase of the weight ratio of the volatile oil to the zein solution; examples 4-6 films prepared by embedding volatile oil in nanoparticles, wherein the particle size of the films is obviously increased along with the increase of the weight ratio of the volatile oil to the zein solution; compared with the films prepared by embedding volatile oil in nano-particles in examples 1-3 and the films prepared by embedding volatile oil in nano-particles in examples 4-6, the films prepared by embedding volatile oil in nano-particles have high potential values when the weight ratio of volatile oil to zein solution is the same.
Effect example 2
Light transmittance test:
the transmittance of the films prepared in examples 1 to 6 and comparative example was measured in a wavelength range of 200nm to 800nm using an ultraviolet-visible spectrophotometer (UV-2600, shimadzu, japan), and the result is shown in FIG. 1;
analysis of results:
as can be seen from fig. 1: the films prepared in examples 1 to 6 and comparative examples have light transmittance increased in sequence as the wavelength increases; when the wavelength is in the range of 300-800 nm, the light transmittance is the highest, namely the blank film without the volatile oil prepared in the comparative example has the light transmittance of 37%; the lowest transmittance is the film prepared in example 6, which has a transmittance of 16%; the films prepared by embedding volatile oil in nanoemulsion in examples 1-3 have small light transmittance increase range and small fluctuation along with the increase of wavelength; the films prepared by embedding volatile oil in nanoparticles in examples 4-6 have large light transmittance increasing range and large fluctuation along with the increase of wavelength; the higher the light transmittance, the lower the blocking efficiency to light, and the easier the light penetrates through the film; the film has a certain blocking effect on light.
Effect example 3
Water vapor permeation test:
seven centrifuge tubes with the same specification are taken, and 1.0g of anhydrous calcium chloride is placed in each centrifuge tube with the cover removed; seven of sevenFixing the films prepared in examples 1-6 and comparative example, which correspond to each other one by one, on top of the centrifuge tube, recording mass m 1 The method comprises the steps of carrying out a first treatment on the surface of the Placing the centrifuge tube in a dryer containing saturated NaCl solution, placing the dryer in 25deg.C for 2 days, and calculating total water absorption m 2 A method of calculating Water Vapor Permeability (WVP) of the formula:
wherein: deltaW is weight gain mass (m 2 -m 1 ) The method comprises the steps of carrying out a first treatment on the surface of the t is time (h); x is film thickness (mm); a is the effective area (m 2 ) The method comprises the steps of carrying out a first treatment on the surface of the Δp is saturated vapor pressure (Pa); the results of the film water vapor permeation test are shown in Table 2;
table 2 film water vapor permeation test results
Analysis of results:
as can be seen from the data in table 2: the water permeability of the volatile oil-embedded films prepared in examples 1 to 6 is lower than that of the blank film in comparative example; the films prepared by embedding the volatile oil in the nanoemulsions in examples 1-3 have lower water permeability than the films prepared by embedding the volatile oil in the nanoparticles in examples 4-6; the film prepared by embedding the volatile oil in the nanoemulsion in example 2 has the lowest water permeability and the best water vapor blocking effect when the weight ratio of the volatile oil to the zein is 1 along with the increase of the addition amount of the volatile oil and the increase of the water permeability of the film.
Effect example 4
Mechanical strength test:
to determine the mechanical properties of the film, the force required to tear the film strip was determined by a texture gauge (ta. Xt plus, stable Micro System company, uk); firstly, cutting a film into a sheet shape (20 mm), measuring the mechanical properties of the film by using a probe at a speed of 1 mm/s in a measuring process through SMS (short message service) P/5s, and measuring each film sample prepared in examples 1-6 and comparative examples for 3 times by using Tensile Strength (TS) and elongation at break (EAB%) to obtain an average value; the TS (tensile strength) and EAB (elongation at break) are calculated as follows:
wherein: f (N) is the maximum force at which the film breaks; a (mm 2) is the cross-sectional area of the film;
wherein: d is the distance (mm) the probe travels to the rupture of the membrane when in contact with the membrane, and R is the radius of the supporting membrane Kong Bankong, which is also the radius (mm) of the membrane in contact with the probe.
The tensile strength and elongation at break results of the films are shown in Table 3;
TABLE 3 tensile Strength and elongation at break of films
Analysis of results:
as can be seen from the data in table 3: the films prepared by embedding the volatile oil in the examples 1-6 have improved tensile strength by nearly 200% to the maximum compared with the blank film of the comparative example; the elongation at break is also enhanced, the toughness is higher, and the tensile strength of the film prepared by embedding volatile oil in nanoemulsion in examples 1-3 is between 0.88N/mm and 1.04N/mm, and the elongation at break is 38.43% -69.67%; with the increase of the content of the volatile oil, the tensile strength and the breaking elongation are increased firstly and then reach the plateau or are reduced, and in the film prepared by embedding the volatile oil by adopting the nanoemulsion in the embodiment 2, when the weight ratio of the volatile oil to the zein is 1, the tensile strength of the film is 1.02N/mm, and the breaking elongation is 69.67%; the tensile strength of the film prepared by embedding volatile oil in nanoparticles in examples 4-6 is between 0.26N/mm and 1.02N/mm, the breaking elongation is between 14.18% and 58.88%, the weight ratio of volatile oil to zein in example 5 is 1.0, and the tensile strength and the breaking elongation are the maximum and are 1.07 and 58.88 respectively; for the film, the larger the tensile strength is, the better the tensile strength is, and the moderate and optimum elongation at break is, so the film prepared by embedding the volatile oil in the nanoemulsion is better than the film prepared by embedding the volatile oil in the nanoemulsion, the film prepared by embedding the volatile oil in the nanoemulsion in the embodiment 2 has the weight ratio of the volatile oil to the zein of 1, and the film has the optimum mechanical strength.
Effect example 5
Scanning electron microscope test:
the surface morphology of the films of examples 1 to 6 and comparative example was observed by a scanning electron microscope (Quanta 250, fei company, agile), and the cross-sectional structures of the films of example 2, example 5 and comparative example, which were frozen and brittle with liquid nitrogen and naturally broken, were observed by a scanning electron microscope; prior to measurement, each sample was sputter gold plated to increase conductivity, and the film samples were imaged at an accelerating voltage of 15 kV; the scanning electron microscope results are shown in figures 2-11;
analysis of results:
as can be seen from fig. 2-11: the films prepared by embedding volatile oil in examples 1-6 have smoother surfaces than the blank films of the comparative examples, and the films prepared by examples 2 and 5 have smoother fracture cross sections than the films of the comparative examples.
Effect example 6
Thickness measurement test:
the thickness of the film was measured by a hand-held digital display screw micrometer (three-volume company, china) with an accuracy of 0.001 mm, 3 thickness values were randomly obtained at different positions of the film in examples 1 to 6 and comparative example films, the measurement was repeated 3 times, the result was averaged, and the thickness measurement results are shown in table 4;
table 4 shows the measurement results of the film thickness
Analysis of results:
as can be seen from table 4: the films prepared in examples 1-6 had an average thickness of 0.1mm.
Effect example 7
Antioxidation test:
the antioxidant activity of the film was determined by scavenging 2, 2-diphenyl-1-picrylhydrazine (DPPH) free radical: the film samples of examples 1-6 and comparative example were weighed 20.0. 20.0 mg, respectively, dissolved in 10 mL methanol, and immersed in 24h at room temperature; filtering the soaking solution by a filter head (0.22 mu m), and then transferring 2 mL of 2, 2-diphenyl-1-picrylhydrazine and 1 mL methanol to mix; then, the mixed solution is vortexed on a vortex oscillator for 3 min and reacts for 30min in a dark place; finally, the absorbance of the sample at 517 and nm is measured by an ultraviolet spectrophotometer, and the DPPH free radical removing capacity of the sample is calculated.
Wherein: a is that 0 Absorbance values at 517 nm for DPPH methanol blank solution; a is the absorbance value of the different sample solutions at 517 and nm, the antioxidant activity results are shown in FIG. 12, and (a) in FIG. 12 is volatile oil (concentration is 175.4 μg/mL); (b) is a comparative film; (c) is the film of example 1; (d) is the film of example 2; (e) is the film of example 3; (f) is the film of example 4; (g) is the film of example 5; (h) A film of example 6.
Analysis of results:
as can be seen from fig. 12: the films prepared in examples 1 to 6 were stronger in antioxidant activity than the blank films of comparative examples, and FIG. 12 shows that in examples 1 to 3, the antioxidant activity of the films increases with the volatile oil content; FIG. 12 shows that in examples 4 to 6, the antioxidant activity of the film increases and decreases with increasing volatile oil content; example 3A film prepared by embedding volatile oil in nanoemulsion has the strongest antioxidant activity when the weight ratio of volatile oil to zein is 1.5; the order of magnitude of the antioxidant activity of the film is: example 3> example 5> example 2> example 6> example 4> example 1> comparative example, but the antioxidant activity of example 2 was not much different from that of example 3, and the film was prepared in example 2 by comprehensively considering factors such as the amount of volatile oil to be added.
Effect example 8
Antibacterial test:
the antibacterial effect of different films on staphylococcus aureus and escherichia coli is measured by adopting a diffusion method, the staphylococcus aureus and escherichia coli are respectively inoculated on a nutrient agar culture medium by using a sterilized coating rod on an ultra-clean workbench, the films of examples 1-6 and comparative example are respectively sheared into small discs with the diameter of 10mm and then are attached to a bacteria-containing plane, after culturing and culturing for 24 hours at 37 ℃, the diameter of a bacteria inhibition zone is measured, and the result is shown in Table 5;
TABLE 5 diameter measurement results of film inhibition zone
Analysis of results:
as can be seen from the data in table 5: the antibacterial effect of the film is evaluated according to the diameter of the antibacterial ring, and the larger the diameter is, the better the antibacterial effect is; the films prepared by embedding the volatile oil in examples 1-6 have stronger antibacterial capability; the blank film prepared in the comparative example does not show antibacterial activity, and after the volatile oil is embedded, the film shows the capability of resisting staphylococcus aureus and escherichia coli; the antibacterial effect of the film prepared by embedding volatile oil in nanoemulsion in examples 1-3 is integrally larger than that of the film prepared by embedding volatile oil in nanoparticles in examples 4-6; in examples 1-3, the anti-staphylococcus aureus and escherichia coli capabilities of the film are enhanced along with the increase of the content of the volatile oil, and the film prepared in example 3 has the strongest antibacterial capability; in examples 4-6, the antibacterial activity of the film increased and then stabilized with the increase of the content of the volatile oil, and the antibacterial activity of the film prepared in example 5 was strongest, but still weaker than that of the film prepared in example 2, wherein the weight ratio of the volatile oil to the zein is also 1; in consideration of comprehensive cost and the like, the weight ratio of the volatile oil to the zein is 1, and the film prepared by embedding the volatile oil in the nanoemulsion has strong mechanical property and physicochemical property and also has excellent antibacterial and antioxidant properties.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so any minor modifications, equivalent changes and modifications made to the above embodiments according to the technical principles of the present invention still fall within the scope of the technical solutions of the present invention.
Claims (7)
1. A degradable antibacterial and antioxidant film, which is characterized in that; is prepared from the following raw materials: chitosan, zein, volatile oil and glycerol, wherein the weight ratio of the chitosan to the zein to the volatile oil to the glycerol is 1:1:1:0.6.
2. the degradable antibacterial antioxidant film of claim 1, wherein the film comprises a polymer; the volatile oil is Jiang Xiangru volatile oil.
3. A method for preparing the degradable antibacterial antioxidant film according to any one of claims 1 to 2, characterized in that; the method comprises the following steps:
s1: preparing volatile oil: placing the medicinal materials containing the volatile oil into a volatile oil extractor, adding 6-10 times of water by weight, heating, distilling and extracting for 2-8 h; stopping heating to obtain a water layer and a volatile oil layer respectively, and adding a drying agent into the volatile oil layer to dehydrate and dry to obtain volatile oil;
s2: preparation of chitosan solution and zein solution: adding chitosan into acetic acid solution, stirring to form transparent chitosan solution, centrifuging, filtering insoluble substances, and collecting upper chitosan solution for use; dissolving zein in ethanol solution, stirring to form transparent zein solution, centrifuging, filtering insoluble substances, and collecting upper zein solution for use; the mass concentration of the acetic acid solution is 1% -5%, the mass concentration of the chitosan solution is 1% -5%, the volume concentration of the ethanol solution is 70% -90%, and the mass concentration of the formed corn protein solution is 1% -5%;
s3: embedding volatile oil in zein; the zein embedded volatile oil forms nanoemulsion embedded volatile oil or nanoparticle embedded volatile oil;
s4: preparation of the film: adding chitosan and glycerol solution into the product obtained by embedding the volatile oil into S3 zein, and homogenizing for 5min at 13000rpm to obtain film forming solution; pouring the film forming solution into a culture dish, vacuum degassing the film forming solution in the culture dish, and drying in a drying oven at 30-50 ℃ for 36h to obtain the film.
4. The method for preparing the degradable antibacterial antioxidant film according to claim 3, wherein the method comprises the steps of; the specific steps of forming the nanoemulsion embedded volatile oil are as follows: dropwise adding the upper-layer zein solution obtained in the step S2 into ultrapure water, homogenizing while dropwise adding, and separating out zein nanoparticles from the zein solution; adding the volatile oil obtained in the step S1 into zein nanoparticles, homogenizing while dripping, and adsorbing the zein nanoparticles on the surface of the volatile oil droplets to form nanoemulsion embedded volatile oil.
5. The method for preparing the degradable antibacterial antioxidant film according to claim 4, wherein the method comprises the following steps of; the homogenizing speed is 10000rpm-15000rpm, the homogenizing time is 5min-30min, and the weight ratio of volatile oil to zein nanoparticles is 0-1.5.
6. The method for preparing the degradable antibacterial antioxidant film according to claim 3, wherein the method comprises the steps of; the specific steps of forming the nanoparticle embedded volatile oil are as follows: adding the volatile oil obtained in the step S1 into the upper-layer zein solution obtained in the step S2, wherein the weight ratio of the volatile oil to the zein solution is 0-1.5, homogenizing while dripping, the homogenizing speed is 13000rpm, the homogenizing time is 15min, and the volatile oil and the zein solution are fully dissolved to form a uniform solution; dripping the solution into ultrapure water, homogenizing while dripping, homogenizing at 13000rpm for 5-30 min, and separating out nanoparticles by dissolving volatile oil and zein in water to obtain nanoparticle-embedded volatile oil.
7. The method for preparing the degradable antibacterial antioxidant film according to claim 3, wherein the method comprises the steps of; the dryer in the S1 is anhydrous sodium sulfate or anhydrous calcium sulfate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107141518A (en) * | 2017-06-07 | 2017-09-08 | 安徽中盛食用油科技有限公司 | A kind of edibility antibacterial film for wrapping up tea-seed oil and preparation method thereof |
| CN110771772A (en) * | 2019-11-11 | 2020-02-11 | 扬州冶春食品生产配送股份有限公司 | Nano composite emulsified essential oil coating film and preparation method and application thereof |
| CN113712072A (en) * | 2021-09-02 | 2021-11-30 | 合肥工业大学 | Clove essential oil pickering emulsion coating preservative and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107141518A (en) * | 2017-06-07 | 2017-09-08 | 安徽中盛食用油科技有限公司 | A kind of edibility antibacterial film for wrapping up tea-seed oil and preparation method thereof |
| CN110771772A (en) * | 2019-11-11 | 2020-02-11 | 扬州冶春食品生产配送股份有限公司 | Nano composite emulsified essential oil coating film and preparation method and application thereof |
| CN113712072A (en) * | 2021-09-02 | 2021-11-30 | 合肥工业大学 | Clove essential oil pickering emulsion coating preservative and preparation method and application thereof |
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| Improving the functionality of chitosan-based packaging films by crosslinking with nanoencapsulated clove essential oil;Lu Hua等;《International Journal of Biological Macromolecules》;20211007;第192卷;第627-634页 * |
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