CN114246285A - Microcapsule preservative and preparation method and application thereof - Google Patents

Microcapsule preservative and preparation method and application thereof Download PDF

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Publication number
CN114246285A
CN114246285A CN202111585090.1A CN202111585090A CN114246285A CN 114246285 A CN114246285 A CN 114246285A CN 202111585090 A CN202111585090 A CN 202111585090A CN 114246285 A CN114246285 A CN 114246285A
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preservative
microcapsule
core material
methacrylic acid
hydrogel
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CN114246285B (en
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陈国安
杨盛荣
张显久
赵樾
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SOUTHERN YANGZE UNIVERSITY BIOTECH
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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3481—Organic compounds containing oxygen
    • A23L3/3508—Organic compounds containing oxygen containing carboxyl groups
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3472—Compounds of undetermined constitution obtained from animals or plants
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3481—Organic compounds containing oxygen
    • A23L3/3499—Organic compounds containing oxygen with doubly-bound oxygen
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3535—Organic compounds containing sulfur
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
    • A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3454—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of liquids or solids
    • A23L3/3463—Organic compounds; Microorganisms; Enzymes
    • A23L3/3553—Organic compounds containing phosphorus
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
    • A23P20/00—Coating of foodstuffs; Coatings therefor; Making laminated, multi-layered, stuffed or hollow foodstuffs
    • A23P20/20—Making of laminated, multi-layered, stuffed or hollow foodstuffs, e.g. by wrapping in preformed edible dough sheets or in edible food containers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
    • C08H1/00—Macromolecular products derived from proteins
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs

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Abstract

The application relates to the field of food additives, and particularly discloses a microcapsule preservative as well as a preparation method and application thereof. A microcapsule preservative comprises an inner layer core material and an outer layer wall material which coats the inner layer core material by a photocuring method, wherein the outer layer wall material is methacrylic acid hydrogel, and the inner layer core material comprises tea polyphenol, astaxanthin, allicin and soybean phosphatidylcholine; wherein the weight ratio of the tea polyphenol, the astaxanthin, the allicin and the soybean phosphatidylcholine is 1 (1-3) to 0.2-0.8 to 5-10. The prepared microcapsule preservative has long-acting preservative property, does not influence the flavor of food, is safe and non-toxic, has wide application range, is not limited by the variety of the food, also has certain health-care function, and improves the nutritive value of the food.

Description

Microcapsule preservative and preparation method and application thereof
Technical Field
The application relates to the technical field of food additives, in particular to a microcapsule preservative and a preparation method and application thereof.
Background
With the development of economy, the living standard of people is continuously improved, and consumers put forward higher requirements on the food preservation degree and the food safety, so the food preservation technology needs to be further developed.
The food preservation technology at the present stage mainly adopts the following steps of adding food preservatives: potassium sorbate, benzoic acid and sodium salts thereof are often added in the traditional food preservation technology, and the chemical preservatives have certain toxicity and are easy to damage human bodies. Therefore, although chemical preservatives have the advantage of low cost, in view of their potential safety hazards to the human body, chemical preservatives have been gradually replaced by biological food preservatives in recent years.
The following biological food preservatives are mainly developed at present:
the first is nisin, which is a polypeptide compound consisting of various amino acids and can be absorbed and utilized by human body as a nutrient substance, but the bacteriostatic and preservative effectiveness of nisin is influenced by pH value and can stably exist in an acidic environment, but the bacteriostatic activity is obviously reduced in an alkaline environment, so that the bacteriostatic and preservative effect is lost in a short period.
The second is epsilon-polylysine which is a natural biological metabolic product, and the epsilon-polylysine is matched with other natural bacteriostatic agents to have obvious synergistic interaction effect, but the practice shows that the epsilon-polylysine can interact with protein or acidic polysaccharide in food to cause the loss of antibacterial ability; and epsilon-polylysine has weak emulsifying capacity; thus, epsilon-polylysine is limited to starchy foods.
In view of the above-mentioned related technologies, the applicant believes that the preservative performance of the biological food preservative is unstable and is difficult to achieve a long-term effective preservative effect, and therefore the biological food preservative needs to be further developed, and a food preservative with a long-lasting preservative performance needs to be prepared.
Disclosure of Invention
In order to further improve the long-acting preservative performance of the food preservative, the application provides a microcapsule preservative and a preparation method and application thereof.
In a first aspect, the microcapsule preservative provided by the present application adopts the following technical scheme:
a microcapsule preservative comprises an inner layer core material and an outer layer wall material which coats the inner layer core material by a photocuring method, wherein the outer layer wall material is methacrylic acid hydrogel, and the inner layer core material comprises tea polyphenol, astaxanthin, allicin and soybean phosphatidylcholine; wherein the weight ratio of the tea polyphenol, the astaxanthin, the allicin and the soybean phosphatidylcholine is 1 (1-3) to 0.2-0.8 to 5-10.
By adopting the technical scheme, the methacrylic acid hydrogel is formed by modifying gelatin through methacrylic anhydride, and carbon-carbon double bonds are introduced into the gelatin through the reaction of carboxyl of the methacrylic anhydride and hydroxyl on the gelatin, so that the methacrylic acid hydrogel can coat natural antibacterial and antioxidant substances (namely inner core materials) under the action of a photoinitiator through a photocuring principle to form a microcapsule structure, and the microcapsule preservative is obtained; the methacrylated hydrogel contains a large amount of polar groups such as carboxyl, amino and the like, has strong water absorption and retention capacity, and releases the core material of the inner layer after water absorption, swelling and cracking or thermal degradation. When the microcapsule preservative is coated on the surface of food, the methacrylated hydrogel forms a protective layer on the surface of the food, so that external moisture and oxygen are isolated, and the rancidity of free fatty acid and the bacterial reproduction process in the food are inhibited;
the inner core material permeates into food, and the main components of the inner core material, such as tea polyphenol, astaxanthin, allicin, soybean phosphatidylcholine and the like, have synergistic effect in the aspects of antibiosis and antioxidation:
the tea polyphenol has high-efficiency bactericidal performance, can reduce blood fat, block the synthesis of nitroso compounds in food in vivo, and eliminate the strong pungent flavor of volatile sulfur-containing compounds such as garlicin, so that the preservative does not influence the flavor of the food;
the astaxanthin has excellent oxidation resistance, the photostability of the allicin and the tea polyphenol can be improved, the situation that the allicin and the tea polyphenol lose effectiveness due to photooxidation in the microcapsule preparation process and the astaxanthin is only degraded under the illumination is avoided, the astaxanthin obtained by degradation still has a good function of removing free radicals, and after being absorbed by a human body, the immunity of a matrix can be enhanced;
the allicin has excellent sterilization performance and good volatility, and can ensure that the core material can be quickly diffused into the food; the soybean phosphatidylcholine wraps the tea polyphenol, so that the tea polyphenol is fully coated by the outer wall material in the preparation process, and the loss of the tea polyphenol in the preparation process is reduced;
when the microcapsule preservative is added into food, the microcapsule preservative is degraded by heating in the food processing process, the core material is released, the possibility of fatty acid rancidity and bacterial breeding in the food processing process is reduced, and the preservative effect is realized radically; therefore, the microcapsule preservative can play a long-acting preservative role. In addition, the addition mode of the microcapsule preservative is diversified, so that the microcapsule preservative is not limited by the environment and can be widely used.
And secondly, the tea polyphenol, the astaxanthin, the allicin and the soybean phosphatidylcholine are all nutrient components extracted from natural substances, have a certain health-care effect, and the methacrylated hydrogel is safe and non-toxic, so that the microcapsule preservative has high safety.
In conclusion, the microcapsule preservative has long-acting preservative property, does not influence the flavor of food, is safe and non-toxic, has wide application range, is not limited by the variety of the food, has a certain health-care function, and improves the nutritional value of the food.
Optionally, the methacrylated hydrogel is prepared by the following process:
weighing gelatin and methacrylic acid, wherein the weight ratio of the gelatin to the methacrylic acid is 1 (0.6-0.8);
dissolving gelatin to prepare a gelatin aqueous solution, adding methacrylic acid into the gelatin aqueous solution, adjusting the pH to 7 +/-0.4, heating to 55-65 ℃ under the nitrogen atmosphere, carrying out heat preservation reaction for 2.5-3.5h, and carrying out freeze drying to obtain the methacrylic acid hydrogel.
By adopting the technical scheme, the weight ratio of the gelatin to the methacrylic acid is adjusted, so that the double bond content of the methacrylic acid hydrogel is moderate, the photocuring rate of the subsequent methacrylic acid hydrogel is improved, the embedding rate of the core material of the inner layer is improved, and the prepared microcapsule preservative has a better preservative effect; when the weight ratio is less than the above range, the content of methacrylic acid is reduced, and the embedding rate of the core material of the inner layer is reduced; above this weight ratio range, the methacrylic acid content increases, leading to a prolonged swelling time of the subsequent methacrylated hydrogel core material, which is detrimental to the release of the core material of the inner layer.
Preferably, the weight ratio of the tea polyphenol, the astaxanthin, the allicin and the soybean phosphatidylcholine in the inner core material is 1:2:0.6: 8.
By adopting the technical scheme, the weight ratio of the components of the core material of the inner layer is controlled, so that the synergistic effect of the four substances is optimal.
In a second aspect, the application provides a preparation method of a microcapsule preservative, which adopts the following technical scheme:
a preparation method of microcapsule preservative comprises the following steps:
preparing an outer-layer wall material: dissolving the methacrylated hydrogel in water to prepare a methacrylated hydrogel solution with the concentration of 5wt% -10 wt%;
preparing an inner layer core material: weighing tea polyphenol, astaxanthin, allicin and soybean phosphatidylcholine according to a weight ratio, and uniformly stirring at 10-20 ℃ to obtain an inner core material;
and (3) photocuring: adding an inner layer core material into a methacrylic acid hydrogel solution, wherein the weight ratio of the inner layer core material to the methacrylic acid hydrogel is 1 (10-20), stirring and emulsifying, adding a photoinitiator with the concentration of 0.5-1 wt%, and then using light irradiation with the irradiation dose of 0.8-1.2W/cm2Ultraviolet curing for 1-10s, filtering, and freeze drying to obtain microcapsule preservative.
By adopting the technical scheme, the soybean phosphatidylcholine in the inner core material has better emulsification effect, so that the inner core material can be fully dispersed in the methacrylic acid hydrogel to form small droplets, and the methacrylic acid hydrogel can be rapidly cured in a short time under the initiation action of the photoinitiator, so that the inner core material is better embedded, and the corrosion prevention time of the microcapsule preservative is further prolonged.
Preferably, the photoinitiator is ethyl pyruvate.
By adopting the technical scheme, the ethyl pyruvate has the characteristics of low cost and no toxicity, and the initiation efficiency of the ethyl pyruvate on the methacrylic acid hydrogel is high, so that the core material of the inner layer is better embedded; the alpha-hydroxy ester product generated by photo-cracking in the process of initiating the ethyl pyruvate is harmless to human bodies, and the ethyl pyruvate is safe and harmless in the using process; and meanwhile, ethyl pyruvate is a preservative which is approved by FDA, the microcapsule preservative does not need to be purified in the preparation process, and the preservative effect of the microcapsule preservative can be further improved.
Preferably, the photocuring step is performed in an oxygen-free environment.
By adopting the technical scheme, the soybean phosphatidylcholine can be protected in an anaerobic environment, and the possibility of oxidation of the soybean phosphatidylcholine is reduced, so that the embedding rate of the inner core material is further improved, and the corrosion prevention time of the microcapsule preservative is further prolonged.
Preferably, the stirring speed in the photocuring step is 200-600 rpm.
By adopting the technical scheme, the low-speed stirring dispersion is adopted, and the heat generated in the stirring dispersion process is reduced, so that the loss of the inner-layer core material is reduced, and the embedding rate of the inner-layer core material is improved.
In a third aspect, the application provides an application of a microcapsule preservative, which adopts the following technical scheme: the application of the microcapsule preservative is to coat the surface of the food and/or add the microcapsule preservative into the food.
By adopting the technical scheme, the microcapsule preservative wall material has good water-absorbing swelling property, is very easy to absorb water, can keep the surface of food dry, and inhibits the growth of bacteria on the surface of the food;
meanwhile, after the wall material absorbs water and swells, a water-proof oxygen-isolating membrane can be formed on the surface of food, and the wall material is matched with an inner core material to permeate in the food, so that pathogenic bacteria such as mold, escherichia coli and the like such as aspergillus flavus and the like in the food can be eliminated, the synthesis of harmful substances such as nitrite-based compounds and the like is inhibited, and the total number of bacterial colonies is remarkably reduced.
In summary, the present application has the following beneficial effects:
1. according to the method, the natural antioxidant and antibacterial substances are embedded by adopting the methacrylic acid hydrogel through a photocuring method, so that the natural antioxidant and antibacterial substances can be fully reserved, and when the methacrylic acid hydrogel is used as a food additive in food, the methacrylic acid hydrogel can fully absorb water in the food and inhibit the food from putrefaction; the inner core material is matched for use, and the rancidity of grease, the synthesis of nitroso compounds and the breeding of bacteria of food are inhibited, so that the long-acting preservative effect on the food is achieved.
2. In the application, ethyl pyruvate is preferably used as a light curing agent, the photoinitiation effect of the ethyl pyruvate on the methacrylic acid hydrogel is good, the ethyl pyruvate is safe and harmless in the initiation process, and the ethyl pyruvate remained on the microcapsule preservative can further improve the preservative effect of the microcapsule preservative.
3. The method can ensure that the heat-sensitive natural antioxidant antibacterial substance is not easy to deteriorate and lose efficacy in the preparation process, fully exerts the antibacterial and antioxidant effects and plays a long-acting antiseptic role.
Detailed Description
Unless otherwise stated, the sources of the raw materials used in the preparation examples, examples and comparative examples in this application are as follows: gelatin is food grade gelatin, CAS No.: 9000-70-8, purchased from Jiujia biotechnology limited, Jiangsu; tea polyphenol, astaxanthin, allicin and soybean phosphatidylcholine are all self-made products.
Preparation example of methacrylated hydrogel
Preparation example 1
A methacrylated hydrogel prepared by the following steps:
weighing 10kg of gelatin and 6kg of methacrylic acid monomer;
putting gelatin into 30kg of deionized water, swelling for 0.5h at 20 ℃, heating the deionized water to 50 ℃, and stirring while keeping the temperature until the gelatin is completely dissolved to obtain a gelatin water solution;
under the condition of keeping out of the sun, adding methacrylic acid into the gelatin aqueous solution, stirring uniformly, dissolving the methacrylic acid, and adjusting the pH value of the system to be 7 by using a disodium hydrogen phosphate-potassium dihydrogen phosphate buffer solution;
and (3) heating to 55 ℃ in the nitrogen atmosphere, carrying out heat preservation reaction for 2.5h, and carrying out freeze drying to obtain the methacrylic acid hydrogel.
Preparation examples 2 to 5
The methacrylated hydrogel differs from preparation example 1 in the weight ratio of gelatin to methacrylic acid: the weight ratio of gelatin to methacrylic acid in preparation example 2 was 1: 0.7; the weight ratio of gelatin to methacrylic acid in preparation example 3 was 1: 0.8; the weight ratio of gelatin to methacrylic acid in preparation example 3 was 1: 0.4; the weight ratio of gelatin to methacrylic acid in preparation example 3 was 1: 1.
Preparation example 6
The methacrylated hydrogel is different from the preparation example 1 in that the temperature is raised to 65 ℃ in a nitrogen atmosphere, the reaction is carried out for 3.5 hours under the heat preservation condition, and the methacrylated hydrogel is obtained by freeze drying.
Examples
Example 1
A microcapsule preservative is prepared by the following preparation steps:
preparing an outer-layer wall material: weighing 100g of methacrylated hydrogel, dissolving the methacrylated hydrogel in 1kg of water, and uniformly stirring to prepare a 10wt% methacrylated hydrogel solution;
preparing an inner layer core material: weighing 10g of tea polyphenol, 10g of astaxanthin, 2g of allicin and 50g of soybean phosphatidylcholine; adding tea polyphenols, astaxanthin and allicin into soybean phosphatidylcholine at 10-20 deg.C, stirring to obtain inner core material;
and (3) photocuring: adding 50g of inner layer core material into the methacrylic acid-treated hydrogel solution to ensure that the weight ratio of the inner layer core material to the methacrylic acid-treated hydrogel is 1:2, stirring and emulsifying at the rotating speed of 200rpm, and adding 0.5g of ethyl pyruvate photoinitiatorContinuously stirring and uniformly mixing at the rotating speed of 200rpm, and then using light irradiation with the irradiation dose of 0.8W/cm2Ultraviolet curing for 10s, filtering, and freeze drying to obtain microcapsule preservative.
Examples 2 to 7
A microcapsule preservative is different from example 1 in the weight ratio of tea polyphenol, astaxanthin, allicin and soybean phosphatidylcholine in the inner core material, and the specific weight ratio is shown in the following table 1.
TABLE 1 weight ratio of the respective components of the core material of the inner layer
Examples Tea polyphenols/g Astaxanthin/g Allicin/g Soybean phosphatidyl choline/g
Example 1 10 10 2 50
Example 2 10 30 2 50
Example 3 10 20 2 50
Example 4 10 20 8 50
Example 5 10 20 6 50
Example 6 10 20 6 100
Example 7 10 20 6 80
Examples 8 to 12
A microencapsulated preservative as distinguished from example 7 by the different origin of the methacrylated hydrogel: wherein the methacrylated hydrogel of example 8 was derived from preparation 2; the methacrylated hydrogel in example 9 was derived from preparation 3; the methacrylated hydrogel in example 10 was derived from preparation 4; the methacrylated hydrogel in example 11 was derived from preparation 5; the methacrylated hydrogel in example 12 was derived from preparation 6.
Example 13
A microcapsule preservative was different from example 9 in that in the photocuring step, the weight ratio of the core material of the inner layer to the methacrylated hydrogel was 1:5, and 0.5g of ethyl pyruvate photoinitiator was added after stirring and emulsification at 600 rpm.
Example 14
A microcapsule preservative differing from example 9 in that the weight of ethylpyruvate in the photocuring step was 1wt% of the weight of the methacrylated hydrogel.
Example 15
A microcapsule preservative was distinguished from example 9 in that the irradiation amount of an ultraviolet lamp in the photocuring step was 1.2W/cm2The irradiation time was 5 s.
Example 16
A microcapsule preservative as distinguished from example 9 in that nitrogen gas was introduced before the photocuring step, so that the photocuring step was performed under a nitrogen atmosphere.
Example 17
A microcapsule preservative is different from that in example 9 in that in the step of preparing the outer-layer wall material, 100g of methacrylated hydrogel is weighed and dissolved in 2kg of water, and the mixture is stirred uniformly to prepare a methacrylated hydrogel solution with the concentration of 5 wt%.
Comparative example
Comparative examples 1 to 4
A microcapsule preservative differs from example 9 in that the composition of the inner core material is different, and the specific composition is shown in table 2 below.
TABLE 2 composition of inner core
Comparative example Tea polyphenols/g Astaxanthin/g Allicin/g Soybean phosphatidyl choline/g
Comparative example 1 / 10 2 60
Comparative example 2 10 / 2 60
Comparative example 3 10 10 / 52
Comparative example 4 26 26 20 /
Comparative example 5
A preservative is prepared by the following steps:
weighing 10g of tea polyphenol, 10g of astaxanthin, 2g of allicin and 50g of soybean phosphatidylcholine; adding tea polyphenols, astaxanthin and garlicin into soybean phosphatidylcholine at 10-20 deg.C, and stirring to obtain antiseptic.
Performance test
And (3) testing antibacterial and anticorrosive performances: 50 μ L of 10 was taken8CFU/mL E.coli, 50. mu.L 108CFU/mL Staphylococcus aureus and 50 uL 108Uniformly mixing the bacterial liquid of CFU/mL aspergillus flavus, and coating the mixture on an aseptic LB plate to prepare 22 aseptic LB plates with the bacterial liquid;
weighing 0.01g of each of examples 1-17 and comparative examples 1-5, and respectively adding the weighed materials into the bacterial liquid of different sterile LB plates; sealing the LB plate, culturing in a constant temperature incubator at 37 deg.C for 24h, and measuring the diameter of the zone with a vernier caliper. The larger the diameter of the inhibition zone is, the better the antibacterial performance is.
And (3) corrosion resistance aging test: sealing the LB plate, culturing in a constant temperature incubator at 37 deg.C for 120h, and measuring the diameter of the zone with a vernier caliper.
And (3) testing thermal stability: sealing the LB plate, culturing in a constant temperature incubator at 50 deg.C for 24h, and measuring the diameter of the zone with a vernier caliper.
And (3) detecting the anticorrosion effect: taking fresh pork with the size of 2cm multiplied by 2cm and fresh bean curd with the size of 2cm multiplied by 2cm, respectively and uniformly coating the surfaces of the fresh pork and the fresh bean curd with the pork and the bean curd of examples 1-17 and comparative examples 1-5, placing the pork and the bean curd in a culture dish, preserving for 24 hours at the temperature of 20 ℃, and then carrying out grade evaluation on the moisture, the color change and the peculiar smell of the pork and the bean curd;
moisture content: a shows that the water retention effect is very good;
b shows that the water retention effect is good;
c represents that the water retention effect is general;
d represents that the water retention effect is poor;
e represents very poor water retention;
color change: a shows that the surface of the product has no green and black mildew and the primary color is bright;
b shows that the surface of the product has no green and black mildew and the primary color is slightly brown;
c represents that the surface of the product has no green and black mildew and the primary color is seriously browned;
d represents that a small amount of green and black mildew spots appear on the surface of the product;
e represents that a great amount of green and black mildew spots appear on the surface of the product;
peculiar smell: a represents that the product has no peculiar smell such as sour taste and/or stink;
b represents that the product emits peculiar smell such as slight sour and/or stink, but the peculiar smell is not obvious;
c represents that the product emits peculiar smell such as sour and/or stink, and the peculiar smell is clearer;
d shows that the product emits peculiar smell such as sour and/or stink, and the peculiar smell is stronger.
The result of the detection
TABLE 3 results of the antibacterial and antiseptic properties and the antiseptic aging test
Figure BDA0003427565410000091
TABLE 4.50 ℃ diameter of zone of inhibition (mm)
Figure BDA0003427565410000092
Note: "/" indicates no zone of inhibition, the inhibition was ineffective.
TABLE 5 examination of the preservative effect on fresh pork
Detecting an object Moisture content Color change Peculiar smell Detecting an object Moisture content Color change Peculiar smell
Example 1 A B B Example 12 B A A
Example 2 A B B Example 13 A B B
Example 3 A B B Example 14 A A A
Example 4 A B B Example 15 A A A
Example 5 A B B Example 16 A A A
Example 6 A B B Example 17 A A A
Example 7 A B B Comparative example 1 A B C
Example 8 A B B Comparative example 2 A C C
Example 9 A A A Comparative example 3 A B D
Example 10 A A A Comparative example 4 A B D
Example 11 B A A Comparative example 5 E E D
TABLE 6 examination of fresh Bean curd preservation Effect
Detecting an object Moisture content Color change Peculiar smell Detecting an object Moisture content Color change Peculiar smell
Example 1 A A B Example 12 B A A
Example 2 A A B Example 13 A A B
Example 3 A A B Example 14 A A A
Example 4 A A B Example 15 A A A
Example 5 A A B Example 16 A A A
Example 6 A A B Example 17 A A A
Example 7 A A B Comparative example 1 A B C
Example 8 A A B Comparative example 2 A C C
Example 9 A A A Comparative example 3 A B C
Example 10 A A A Comparative example 4 A B D
Example 11 B A A Comparative example 5 E C D
By combining the example 1 and the comparative examples 1-5 and combining the tables 3-6, the antibacterial and antiseptic effects of the comparative examples 1 and 1-5 are known, the antibacterial and antiseptic effects of the example 1 and the comparative examples 1-5 are obvious in the aspect of inhibiting harmful pathogenic bacteria such as escherichia coli, staphylococcus aureus, aspergillus flavus and the like within 24h, and the diameter of the antibacterial ring is larger, because the comparative examples 1-4 do not contain tea polyphenol, astaxanthin, allicin and soybean phosphatidylcholine in sequence, and the comparative example 5 does not contain an outer wall material to coat an inner core material; even if the culture time of the bacteria liquid is prolonged to 120h, the diameters of the inhibition zones of escherichia coli, staphylococcus aureus and aspergillus flavus are only slightly reduced by 0.5-1.1cm, while the diameters of the inhibition zones in comparative examples 1-5 are reduced by at least 1cm, and the antibacterial, antiseptic and aging effects are short;
even if the bacterial liquid is cultured at the temperature of 50 ℃, the diameter change of the bacteriostatic circle of the escherichia coli, the staphylococcus aureus and the aspergillus flavus is small, while the diameter reduction amount of the bacteriostatic circle in the comparative examples 1-5 is large, particularly the comparative example 5 fails at the temperature of 50 ℃;
example 1 the water content of pork and bean curd can be effectively maintained and the deterioration time of pork and bean curd can be delayed by using the water content of pork and bean curd.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.

Claims (8)

1. The microcapsule preservative is characterized by comprising an inner-layer core material and an outer-layer wall material which coats the inner-layer core material by a photocuring method, wherein the outer-layer wall material is methacrylic acid hydrogel, and the inner-layer core material comprises tea polyphenol, astaxanthin, allicin and soybean phosphatidylcholine; wherein the weight ratio of the tea polyphenol, the astaxanthin, the allicin and the soybean phosphatidylcholine is 1 (1-3) to 0.2-0.8 to 5-10.
2. A microcapsule preservative according to claim 1, wherein: the methacrylated hydrogel is prepared by the following process:
weighing gelatin and methacrylic acid, wherein the weight ratio of the gelatin to the methacrylic acid is 1 (0.6-0.8);
dissolving gelatin to prepare a gelatin aqueous solution, adding methacrylic acid into the gelatin aqueous solution, adjusting the pH to 7 +/-0.4, heating to 55-65 ℃ under the nitrogen atmosphere, carrying out heat preservation reaction for 2.5-3.5h, and carrying out freeze drying to obtain the methacrylic acid hydrogel.
3. A microcapsule preservative according to claim 1, wherein: the weight ratio of the tea polyphenol, the astaxanthin, the allicin and the soybean phosphatidylcholine in the inner-layer core material is 1:2:0.6: 8.
4. A process for preparing a microcapsule preservative according to claims 1 to 3, characterized in that: the method comprises the following steps:
preparing an outer-layer wall material: dissolving the methacrylated hydrogel in water to prepare a methacrylated hydrogel solution with the concentration of 5wt% -10 wt%;
preparing an inner layer core material: weighing tea polyphenol, astaxanthin, allicin and soybean phosphatidylcholine according to a weight ratio, and uniformly stirring at 10-20 ℃ to obtain an inner core material;
and (3) photocuring: adding an inner layer core material into a methacrylic acid-treated hydrogel solution, wherein the weight ratio of the inner layer core material to the methacrylic acid-treated hydrogel is 1 (2-5), stirring and emulsifying, adding a photoinitiator, wherein the weight of the photoinitiator is 0.5-1 wt% of that of the methacrylic acid-treated hydrogel, and then using light irradiation with the irradiation dose of 0.8-1.2W/cm2Ultraviolet curing for 5-10s, filtering, and freeze drying to obtain microcapsule preservative.
5. The method for preparing a microcapsule preservative according to claim 4, wherein: the photoinitiator is ethyl pyruvate.
6. The method for preparing a microcapsule preservative according to claim 4, wherein: the photocuring step is performed in an oxygen-free environment.
7. The method for preparing a microcapsule preservative according to claim 1, wherein: the stirring speed in the photocuring step is 200-600 rpm.
8. The application of microcapsule preservative is characterized in that: a microencapsulated preservative as defined in claim 1 applied to the surface of a food product and/or added to the interior of a food product.
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