CN114561045A - Edible active food fresh-keeping pad and preparation method thereof - Google Patents
Edible active food fresh-keeping pad and preparation method thereof Download PDFInfo
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Abstract
The invention provides an edible active food fresh-keeping pad and a preparation method thereof, and relates to the technical field of fresh-keeping pad processing. The fresh-keeping cushion of the invention takes natural degradable food processing by-products, namely nano chitin and nano cellulose, as main raw materials, and ferulic acid as a cross-linking agent, and induces the molecules in a composite system to form stable covalent bonds and non-covalent cross-links, thereby forming the stable three-dimensional network structure aerogel. On the basis, the active substances epsilon-polylysine and cinnamon essential oil are embedded in the aerogel, so that the aerogel is endowed with strong antibacterial and antioxidant properties, and the controlled release property of the aerogel is combined, so that the breeding of microorganisms can be effectively inhibited, and the shelf life of food is prolonged.
Description
Technical Field
The invention relates to the technical field of preparation of freshness-retaining pads, and relates to an edible active food freshness-retaining pad and a preparation method thereof.
Background
Food spoilage is a serious problem that plagues the food industry, and studies by the international society for refrigeration indicate that spoiled food accounts for 45% of the total annual food production worldwide for a variety of reasons. In the process of food storage, the performance of the fresh-keeping material often has a great influence on the shelf life of the food. The current fresh-keeping materials are mainly polyethylene, polypropylene and the like, but the non-degradability of the materials causes serious environmental pollution problems. In addition, the safety of some freshness-retaining materials remains questionable.
In recent years, the research on natural fresh-keeping materials provides a new scheme for solving the problem of food fresh keeping. Cellulose and chitin are two kinds of polysaccharides with the most abundant content in nature, and have the advantages of easy preparation, wide sources, degradability and the like. The deacetylated nano chitin and carboxymethyl nano cellulose prepared by taking the deacetylated nano chitin and carboxymethyl nano cellulose as raw materials are novel nano materials, have the characteristics of high length-diameter ratio and high specific surface area of the nano materials on the basis of the original advantages, can be well dispersed in a solution, enhances the mechanical property of a composite material, and has wide development prospect in the field of food preservation.
The growth and propagation of microorganisms are the main factors that cause food spoilage. The preservation of food by adding active substances to inhibit bacterial growth is a common preservation means. Epsilon-poly-L-lysine (Epsilon-PL) is a natural antibacterial peptide, has the advantages of strong heat stability, wide antibacterial spectrum and the like, and is mainly produced by fermenting glucose by streptomyces albus. The epsilon-polylysine has obvious inhibition effect on most gram-negative bacteria, gram-positive bacteria, saccharomycete and mould. Meanwhile, the epsilon-polylysine has high safety, is easy to biodegrade, and has wide development potential in the fields of food preservation and corrosion prevention. The plant essential oil is an important secondary metabolite in plants, has antibacterial and antioxidant capabilities, is low in dosage, and is economical and applicable. The application of the essential oil on the food fresh-keeping pad is more and more extensive, and the plant essential oil is added into the fresh-keeping pad, so that the water vapor barrier property, the mechanical property and the antibacterial property of the fresh-keeping pad can be improved.
Chinese patent CN105638851A discloses a method for preparing a food fresh-keeping pad, which is mainly made by sandwiching a water-soluble polyvinyl alcohol film between two layers of non-woven fabrics coated with carbon dioxide releasing reactant materials, and bonding and hot-pressing the two layers to form the fresh-keeping pad. The freshness-retaining mat can release CO2The concentration of the active ingredients in the fresh-keeping agent is kept fresh, and meanwhile, the active ingredients have a certain bacteriostatic action. But CO is difficult to control in the fresh-keeping process2The release amount and release rate of the active ingredients cannot well ensure the fresh-keeping effect. In addition, the non-woven fabric is easy to crack and expensive, so that the large-scale application of the fresh-keeping mat is limited.
Chinese patent CN101156620A discloses a method for preparing a food fresh-keeping pad, which can release carbon dioxide and chlorine dioxide gas with multiple functions of fresh-keeping, preservation, deodorization, etc., and also comprises a liquid absorbing material for absorbing liquid exuded from meat, so as to achieve the bacteriostatic and antiseptic effects. But the specific concentration of the gas can not be controlled, and meanwhile, the gas can be rapidly diffused into the air after being released, so that the action time is short, the bacteriostatic atmosphere is difficult to form around the food, and the fresh-keeping effect has certain limitation.
Therefore, the development of an economic, green and good-preservation-effect preservation pad is an important problem in the current food industry, and has wide application prospect and remarkable economic value.
Disclosure of Invention
The invention aims to solve the problems that the existing fresh-keeping pad has poor fresh-keeping effect, is difficult to degrade and pollutes the environment and the like. The fresh-keeping pad provided by the invention has broad-spectrum antibacterial capability, better moisture retention performance, the advantages of greenness, safety, no toxicity and low cost, and can better meet the application of the fresh-keeping pad in the aspect of antibacterial fresh keeping of food.
In order to achieve the above object, the present invention provides the following technical solutions:
the preparation method of the edible active food fresh-keeping cushion comprises the following steps:
s1, preparation of deacetylated nano chitin:
dispersing chitin powder in 33% sodium hydroxide aqueous solution, adding sodium borohydride accounting for 0.3% of the mass of the chitin, and magnetically stirring for 4 hours in a water bath at 90 ℃ to obtain deacetylated chitin solution; carrying out suction filtration and washing to obtain a solid product, and then drying in a 45 ℃ oven for 1 h; dissolving the dried solid product in 1 v/v% acetic acid aqueous solution, performing ultrasonic treatment for 1h, standing for 0.5h, collecting supernatant, and freeze-drying to obtain deacetylated nano chitin;
s2, preparing carboxymethyl nanocellulose:
mixing carboxymethyl cellulose and water according to the mass ratio of 1:100, homogenizing by using a homogenizer, collecting supernatant, and freeze-drying to obtain carboxymethyl nano-cellulose;
s3, the ferulic acid induces deacetylation nano chitin/carboxymethyl nano cellulose to carry out cross-linking, and the synthetic route is as follows:
the concrete method comprises the following steps
The carboxymethyl nano-cellulose prepared in the step S2 is dissolved in deionized water to prepare a solution with the mass volume concentration of 2%, and the deacetylated nano chitin-acetic acid mixed solution is added while stirring to obtain a uniform and transparent solution; the deacetylated nano chitin-acetic acid mixed solution is prepared by mixing deacetylated nano chitin with an acetic acid aqueous solution, wherein the mass volume concentration of the deacetylated nano chitin in the mixed solution is 2%;
adding ferulic acid for induced crosslinking, wherein the addition amount of the ferulic acid accounts for 3% of the dry matter amount of the deacetylated nano chitin and the carboxymethyl nano cellulose, and then reacting and stirring for 1h under the condition of 500rpm/min to obtain a crosslinking solution;
s4, preparing a finished product of the freshness protection pad:
respectively and slowly adding epsilon-polylysine and cinnamon essential oil solution into the cross-linking solution to ensure that the final concentrations of the epsilon-polylysine and the cinnamon essential oil in the system are respectively 25mg/L and 2 mg/L; stirring at 500rpm/min for 1h, and standing at room temperature for 12h to obtain hydrogel; finally, the hydrogel is soaked in deionized water until the system is neutral, and then the edible active food fresh-keeping cushion is prepared by freeze drying.
Preferably, deionized water is used for washing the solid product for multiple times in the suction filtration process in the step S1 until the washed filtrate is colorless.
Preferably, the freeze-drying process of steps S1, S2 and S4 is to wrap the solution in a clean glass dish with a preservative film and freeze the wrapped solution in a freezer at-80 ℃ for 12 hours, and then freeze-dry the wrapped solution for 24 to 72 hours at-80 ℃ to-85 ℃ under the conditions of a vacuum degree of 10 to 15.
Preferably, the homogenization condition in step S2 is to select a high-pressure nozzle with a diameter of D8, and homogenize the carboxymethylation pretreatment solution under 5000psi pressure for 2 times, and then under 20000psi pressure for 1 time.
Preferably, the concentration of acetic acid in step S3 is 1%.
Preferably, the mass ratio of the carboxymethyl nano-cellulose aqueous solution to the deacetylated nano chitin-acetic acid mixed solution in the step S3 is 4-6: 4-6. More preferably, the mass ratio of the carboxymethyl nano cellulose aqueous solution to the deacetylated nano chitin-acetic acid mixed solution is 4: 6, 5: 5, 6: 4.
Another object of the present invention is to provide an edible active food freshness-retaining mat prepared by the above method.
Compared with the prior art, the invention has the following beneficial effects:
the invention uses natural degradable food processing by-products, namely nano chitin and nano cellulose, as main raw materials, and ferulic acid as a cross-linking agent, and induces the molecules in a composite system to form stable covalent bonds and non-covalent cross-links so as to form the stable three-dimensional network structure aerogel. On the basis, the active substances epsilon-polylysine and cinnamon essential oil are embedded in the aerogel, so that the aerogel is endowed with strong antibacterial and antioxidant properties, and the controlled release property of the aerogel is combined, so that the breeding of microorganisms can be effectively inhibited, and the shelf life of food is prolonged.
The invention has simple preparation process, rich and safe raw material sources and low cost, is suitable for modern industrial production, can be combined with the existing physical preservation technology for use, is widely applied to the food industry and has wide prospect.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
An edible active food fresh-keeping cushion is prepared by the following steps:
preparation of S1 deacetylated chitin nanoparticles:
dispersing chitin powder in 33% sodium hydroxide aqueous solution, adding sodium borohydride accounting for 0.3% of the mass of the chitin powder, and magnetically stirring for 4h in a water bath at 90 ℃ to obtain deacetylated chitin solution. And (3) carrying out suction filtration and washing to obtain a solid product (the solid product is washed by deionized water for multiple times in the suction filtration process until the washed filtrate is colorless), and then drying in an oven at 45 ℃ for 1 h. Dissolving in 1% acetic acid water solution, ultrasonic treating for 1 hr, standing for 0.5 hr, collecting supernatant, and freeze drying to obtain deacetylated nanometer chitin;
s2 preparation of carboxymethyl nanocellulose:
carboxymethyl cellulose was dispersed in water to prepare a dispersion solution having a solid content of 1 wt%. Homogenizing with a high-pressure homogenizer, collecting supernatant, freeze drying to obtain carboxymethyl nanocellulose, wherein the homogenizing condition is that a high-pressure nozzle with D8 caliber is selected, the carboxymethylation pretreatment solution is homogenized for 2 times under the pressure condition of 5000psi, and then homogenized for 1 time under the pressure condition of 20000 psi;
s3 ferulic acid induces deacetylation nano chitin/carboxymethyl nano cellulose to crosslink:
dissolving the carboxymethyl nano-cellulose in the step S2 in deionized water to prepare a solution with the concentration of 2% (w/v), and adding a deacetylated nano-chitin-acetic acid mixed solution in proportion while stirring to obtain a uniform and transparent solution, wherein the deacetylated nano-chitin-acetic acid mixed solution is formed by mixing deacetylated nano-chitin with an acetic acid aqueous solution, the mass volume concentration of the deacetylated nano-chitin in the mixed solution is 2%, and the concentration of the acetic acid aqueous solution is 1%. Then adding 3% (w/w, accounting for the dry matter weight of the deacetylated nano chitin and the carboxymethyl nano cellulose) of ferulic acid for induced crosslinking, and reacting and stirring for 1h at 500 rpm/min. Wherein the volume ratio of the carboxymethyl nano-cellulose aqueous solution to the deacetylated nano chitin-acetic acid mixed solution is 4: 6, and a cross-linking solution is obtained.
Preparation of S4 finished product of fresh-keeping pad
Respectively and slowly adding epsilon-polylysine and cinnamon essential oil solution into the cross-linking solution to ensure that the final concentrations of the epsilon-polylysine and the cinnamon essential oil in the system are respectively 25mg/L and 2 mg/L. Stirring the mixture for 1 hour at the speed of 500rpm/min, and standing the mixture for 12 hours at room temperature to obtain hydrogel. Soaking the hydrogel in deionized water until the system is neutral, and freeze-drying to obtain the edible active food fresh-keeping pad.
The freeze drying method in the preparation process comprises placing the solution in a clean glass dish, wrapping with preservative film, freezing in a freezer at-80 deg.C for 12h, and freeze drying at-85 deg.C under vacuum degree of 12 for 30 h.
Example 2
An edible active food fresh-keeping pad is prepared by the following steps:
preparation of S1 deacetylated chitin nanoparticles:
dispersing chitin powder in 33% sodium hydroxide aqueous solution, adding sodium borohydride accounting for 0.3% of the mass of the chitin powder, and magnetically stirring for 4h in a water bath at 90 ℃ to obtain deacetylated chitin solution. And (3) carrying out suction filtration and washing to obtain a solid product (the solid product is washed by deionized water for multiple times in the suction filtration process until the washed filtrate is colorless), and then drying in an oven at 45 ℃ for 1 h. Dissolving in 1% acetic acid water solution, ultrasonic treating for 1 hr, standing for 0.5 hr, collecting supernatant, and freeze drying to obtain deacetylated nanometer chitin;
s2 preparation of carboxymethyl nanocellulose:
carboxymethyl cellulose was dispersed in water to prepare a dispersion solution having a solid content of 1 wt%. Homogenizing with a high-pressure homogenizer, collecting supernatant, freeze drying to obtain carboxymethyl nanocellulose, wherein the homogenizing condition is that a high-pressure nozzle with D8 caliber is selected, the carboxymethylation pretreatment solution is homogenized for 2 times under the pressure condition of 5000psi, and then homogenized for 1 time under the pressure condition of 20000 psi;
s3 ferulic acid induces deacetylation nano chitin/carboxymethyl nano cellulose to crosslink:
dissolving the carboxymethyl nano-cellulose in the step S2 in deionized water to prepare a solution with the concentration of 2% (w/v), and adding a deacetylated nano-chitin-acetic acid mixed solution in proportion while stirring to obtain a uniform and transparent solution, wherein the deacetylated nano-chitin-acetic acid mixed solution is formed by mixing deacetylated nano-chitin with an acetic acid aqueous solution, the mass volume concentration of the deacetylated nano-chitin in the mixed solution is 2%, and the concentration of the acetic acid aqueous solution is 1%. Then adding 3% (w/w, accounting for the dry matter weight of the deacetylated nano chitin and the carboxymethyl nano cellulose) of ferulic acid for induced crosslinking, and reacting and stirring for 1h at 500 rpm/min. Wherein the volume ratio of the carboxymethyl nano-cellulose aqueous solution to the deacetylated nano chitin-acetic acid mixed solution is 5: 5, and a cross-linking solution is obtained.
Preparation of S4 fresh-keeping pad finished product
Respectively and slowly adding epsilon-polylysine and cinnamon essential oil solution into the cross-linking solution to ensure that the final concentrations of the epsilon-polylysine and the cinnamon essential oil in the system are respectively 25mg/L and 2 mg/L. Stirring at 500rpm/min for 1 hr, and standing at room temperature for 12 hr to obtain hydrogel. Soaking the hydrogel in deionized water until the system is neutral, and freeze-drying to obtain the edible active food fresh-keeping pad.
The freeze drying method in the preparation process comprises placing the solution in a clean glass dish, wrapping with preservative film, freezing in a freezer at-80 deg.C for 12h, and freeze drying at-85 deg.C under vacuum degree of 12 for 30 h.
Example 3
An edible active food fresh-keeping cushion is prepared by the following steps:
preparation of S1 deacetylated chitin nanoparticles:
dispersing chitin powder in 33% sodium hydroxide aqueous solution, adding sodium borohydride accounting for 0.3% of the mass of the chitin powder, and magnetically stirring for 4h in a water bath at 90 ℃ to obtain deacetylated chitin solution. And (4) performing suction filtration and washing to obtain a solid product (the solid product is washed by deionized water for multiple times in the suction filtration process until the washed filtrate is colorless), and then drying in an oven at 45 ℃ for 1 h. Dissolving in 1% acetic acid water solution, ultrasonic treating for 1 hr, standing for 0.5 hr, collecting supernatant, and freeze drying to obtain deacetylated nanometer chitin;
s2 preparation of carboxymethyl nanocellulose:
carboxymethyl cellulose was dispersed in water to prepare a dispersion solution having a solid content of 1 wt%. Homogenizing with a high-pressure homogenizer, collecting supernatant, freeze drying to obtain carboxymethyl nanocellulose, wherein the homogenizing condition is that a high-pressure nozzle with D8 caliber is selected, the carboxymethylation pretreatment solution is homogenized for 2 times under the pressure condition of 5000psi, and then homogenized for 1 time under the pressure condition of 20000 psi;
s3 ferulic acid induces deacetylation nano chitin/carboxymethyl nano cellulose to crosslink:
dissolving the carboxymethyl nano-cellulose in the step S2 in deionized water to prepare a solution with the concentration of 2% (w/v), and adding a deacetylated nano-chitin-acetic acid mixed solution in proportion while stirring to obtain a uniform and transparent solution, wherein the deacetylated nano-chitin-acetic acid mixed solution is formed by mixing deacetylated nano-chitin with an acetic acid aqueous solution, the mass volume concentration of the deacetylated nano-chitin in the mixed solution is 2%, and the concentration of the acetic acid aqueous solution is 1%. Then adding 3% (w/w, accounting for the dry matter of the deacetylated nano chitin and the carboxymethyl nano cellulose) of ferulic acid for induced crosslinking, and reacting and stirring for 1h under the condition of 500 rpm/min. Wherein the volume ratio of the carboxymethyl nano-cellulose aqueous solution to the deacetylated nano chitin-acetic acid mixed solution is 6: 4, and a cross-linking solution is obtained.
Preparation of S4 fresh-keeping pad finished product
Respectively and slowly adding epsilon-polylysine and cinnamon essential oil solution into the cross-linking solution to ensure that the final concentrations of the epsilon-polylysine and the cinnamon essential oil in the system are respectively 25mg/L and 2 mg/L. Stirring at 500rpm/min for 1 hr, and standing at room temperature for 12 hr to obtain hydrogel. Soaking the hydrogel in deionized water until the system is neutral, and freeze-drying to obtain the edible active food fresh-keeping pad.
The freeze drying method in the preparation process comprises placing the solution in a clean glass dish, wrapping with preservative film, freezing in a freezer at-80 deg.C for 12h, and freeze drying at-85 deg.C under vacuum degree of 12 for 30 h.
The performance of the freshness pads prepared in examples 1 to 3 was tested as follows:
(1) antibacterial rate
The bacteriostatic effect of the safety pad was tested by the shake flask method (AATCC 100-. The bacteria used in this study were gram-negative escherichia coli (ATCC 25922) and gram-positive staphylococcus aureus (ATCC 6538). 0.75g of the sample was put into a conical flask equipped with a 70mL phosphate buffered saline stopper, 5mL of the bacterial solution was added, and the sample was shaken at 200rmp/min for 1 hour to sufficiently contact the bacteria. 0.5mL of the treated solution was placed on the medium and left at 37 ℃ for 48 hours. Blank samples (no ready samples added) were used to calculate the bacterial reduction rate. The reduction of bacteria was calculated according to equation (1).
R＝(B-A)/B×100％ (1)
R is an inhibition ratio (%), A is the number of bacteria on the medium inoculated with the sample-treated solution, and B is the number of bacteria on the medium inoculated with the non-sample-treated solution. As shown in table 1.
TABLE 1 comparison of antibacterial Effect of freshness-retaining pads
(2) Compression test
The compressive mechanical properties of the sponge were tested in a room temperature dry state using a universal tester (CTM 2100, shanghai assisted Strength instrumentation technologies, ltd.). The aerogel was cut into cubes of 10mm by 10 mm. The crosshead speed was set at 5mm/min, and the compressive stress acting on each of the aerogels when the compressive strain became 80% was compared, as shown in Table 2.
TABLE 2 compressive stress of the freshness pad at 80% compressive strain
(3) Experiment of preservation Effect
Fresh pork wrapped with the freshness pad prepared in example 1 and a commercially available freshness pad was stored in a refrigerator at 4 ℃ and compared after 5 days as shown in table 3.
TABLE 3 comparison of the freshness-retaining effect of the freshness-retaining pad of example 1 with that of a commercially available freshness-retaining pad
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A preparation method of an edible active food fresh-keeping cushion is characterized by comprising the following steps:
s1, preparation of deacetylated nano chitin:
dispersing chitin powder in 33% sodium hydroxide aqueous solution, adding sodium borohydride accounting for 0.3% of the mass of the chitin, and magnetically stirring for 4 hours in a water bath at 90 ℃ to obtain deacetylated chitin solution; carrying out suction filtration and washing to obtain a solid product, and then drying in a 45 ℃ oven for 1 h; dissolving the dried solid product in 1 v/v% acetic acid aqueous solution, performing ultrasonic treatment for 1h, standing for 0.5h, collecting supernatant, and freeze-drying to obtain deacetylated nano chitin;
s2, preparing carboxymethyl nanocellulose:
mixing carboxymethyl cellulose and water according to the mass ratio of 1:100, homogenizing by using a homogenizer, collecting supernatant, and freeze-drying to obtain carboxymethyl nano-cellulose;
s3, crosslinking the nano chitosan/carboxymethyl cellulose induced by ferulic acid:
dissolving the carboxymethyl nano-cellulose prepared in the step S2 in deionized water to prepare a solution with the mass volume concentration of 2%, and adding the deacetylated nano chitin-acetic acid mixed solution while stirring to obtain a uniform and transparent solution; the deacetylated nano chitin-acetic acid mixed solution is prepared by mixing deacetylated nano chitin with an acetic acid aqueous solution, wherein the mass volume concentration of the deacetylated nano chitin in the mixed solution is 2%;
adding ferulic acid for induced crosslinking, wherein the addition amount of the ferulic acid accounts for 3% of the dry matter amount of the deacetylated nano chitin and the carboxymethyl nano cellulose, and then reacting and stirring for 1h under the condition of 500rpm/min to obtain a crosslinking solution;
s4, preparing a finished product of the freshness protection pad:
respectively and slowly adding epsilon-polylysine and cinnamon essential oil into the cross-linking solution to ensure that the final concentrations of the epsilon-polylysine and the cinnamon essential oil in the system are respectively 25mg/L and 2 mg/L; then stirring for 1h at 500rpm/min, and standing for 12h at room temperature to obtain hydrogel; finally, the hydrogel is soaked in deionized water until the system is neutral, and then the edible active food fresh-keeping pad is prepared by freeze drying.
2. The method of claim 1, wherein the solid product is washed with deionized water several times during the suction filtration process of step S1 until the rinsing filtrate is colorless.
3. The method of claim 1, wherein the step of freeze-drying comprises steps of S1, S2 and S4, wherein the step of freeze-drying comprises placing the solution in a clean glass dish, wrapping the solution with a plastic wrap, freezing the coated solution in a freezer at-80 ℃ for 12 hours, and freeze-drying the coated solution at-80 ℃ to-85 ℃ for 24 hours to 72 hours under a vacuum degree of 10 to 15.
4. The method of claim 1, wherein the homogenization conditions of step S2 are selected from a high pressure nozzle with a D8 caliber, and the carboxymethylation pretreatment solution is homogenized under 5000psi pressure for 2 times, and then under 20000psi pressure for 1 time.
5. The method of claim 1, wherein the acetic acid concentration of step S3 is 1%.
6. The edible active food fresh-keeping pad and the preparation method thereof according to claim 1, wherein the mass ratio of the carboxymethyl nano cellulose aqueous solution to the deacetylated nano chitin-acetic acid mixed solution in the step S3 is 4-6: 4-6.
7. An edible active food freshness-retaining mat, characterized in that it is produced by the method of any one of claims 1 to 6.
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