CN112237215A - Application of natural essential oil nano liposome preservative in sturgeon caviar storage - Google Patents
Application of natural essential oil nano liposome preservative in sturgeon caviar storage Download PDFInfo
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Images
Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23B—PRESERVING, e.g. BY CANNING, MEAT, FISH, EGGS, FRUIT, VEGETABLES, EDIBLE SEEDS; CHEMICAL RIPENING OF FRUIT OR VEGETABLES; THE PRESERVED, RIPENED, OR CANNED PRODUCTS
- A23B4/00—General methods for preserving meat, sausages, fish or fish products
- A23B4/14—Preserving with chemicals not covered by groups A23B4/02 or A23B4/12
- A23B4/18—Preserving with chemicals not covered by groups A23B4/02 or A23B4/12 in the form of liquids or solids
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- 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
Abstract
The invention discloses an application of a natural essential oil nanoliposome (EO-NPs-Lps) preservative in sturgeon caviar storage, wherein the preparation method of the natural essential oil nanoliposome preservative comprises the following steps: (1) stirring and heating natural plant essential oil, stopping heating after a period of time, and cooling to room temperature; filtering and collecting filtrate to obtain natural essential oil microparticle solution; (2) dissolving the natural essential oil microparticle solution in ethanol, mixing with lecithin, magnetically stirring at room temperature, fully mixing, and storing at 4 ℃ for 12-24 h; heating, decompressing and removing the solvent, dispersing in deionized water, carrying out dynamic ultrahigh pressure micro-jet treatment, and freeze-drying to obtain the natural essential oil nanoliposome preservative. The natural essential oil nanoliposome has fresh keeping, antiseptic and antioxidant effects, and can delay the quality reduction rate of caviar; meanwhile, the health care tea also has the health care effect. The processing method is simple and convenient, the equipment investment is low, the safety is realized, and the production cost is low.
Description
Technical Field
The invention belongs to the related technical fields of food preservatives, aquatic product storage and preservation, nano materials and the like, and particularly relates to a preparation method of a natural essential oil nano liposome preservative and application of the natural essential oil nano liposome preservative in sturgeon caviar food.
Background
China is one of the countries with the most sturgeon varieties, so that the development of sturgeon products in China has the advantages of resource conditions. Sturgeon Caviar (Caviar), also known as Caviar, is generally prepared from sturgeon roe by lightly salting. Because of its rich nutrient components of EPA, DHA, EPA and DHA, omega 3 polyunsaturated fatty acid, etc., it is generally compared with black soft gold. Caviar is used as a high-grade consumer product in the international market, and the consumer market of China is further expanded in recent years. In addition, the application of caviar in the fields of health care products and cosmetics is receiving more and more attention. The preservation of caviar is an important issue in the production, transportation and storage processes. At present, the aim of corrosion prevention is fulfilled by directly adding excessive non-polar salt, the method has poor fresh-keeping effect and poor flavor, and the fresh-keeping agent can not be stored basically after being packaged and opened; meanwhile, the aim of modern human health nutrition is also violated by the addition of high-concentration inorganic salt, so that the development and application of the safe and efficient natural food preservative which can be applied to the preservation of caviar are widely concerned.
The natural preservatives can be divided into plant-source preservatives, animal-source preservatives and microbial-source preservatives according to different sources. The plant source biological antistaling agent comprises natural extracts, such as tea polyphenol, garlicin, spice extract, etc.; also plant essential oils, such as tea tree essential oil, cinnamon essential oil, clove essential oil, oregano essential oil, etc. After the plant essential oil reaches a certain concentration, as the effective components are concentrated, the effective action sites are more, the cell contents of the microorganisms or ions in the cells can leak and flow out, the normal growth activity of the microorganisms is influenced, and when the concentration exceeds the tolerance range, the microorganisms are possibly killed. For example, the tea tree essential oil has obvious bacteriostatic effect on various bacteria (escherichia coli and golden yellow wine bacteria), mould and microzyme. Literature research shows that the type and content of active ingredients of plant essential oil influence the bacteriostatic action (different from strain to strain). The plant essential oil contains various components with synergistic effect, the effect is superior to the effect of the independent action of each effective component, and the synergistic effect is more beneficial to the application of the plant essential oil in food processing and storage. The effective active components of the plant essential oil are key factors of antibiosis and antioxidation, and directly influence the activity and antibiosis mode of the essential oil. Because the components of the plant essential oil are complex, the bacteriostasis mechanism of the plant essential oil is also various, and for bacteria, the bacteriostasis mechanism is mainly the degradation of cell walls; disrupting the cell membrane; membrane proteins are disrupted, etc. Further research results of this subject group show that some kinds of essential oils are subjected to special heat treatment to form essential oil nanoparticles, and the bacteriostatic effect of the essential oil nanoparticles is far better than that of untreated essential oils.
The effective components of the plant essential oil are volatile, generally contain strong peculiar smell of the plant, are sensitive to temperature, generally need low temperature to be kept away from a heat source, the essential oil is sensitive to sunlight, crystallization can be separated out at low temperature, and the essential oil is almost insoluble in water. These characteristics all become limitations when the bactericidal performance of the essential oil is applied to practical production. Thus, to overcome this limitation of use of essential oils, liposomes can be used to entrap the essential oils. Liposomes are vesicles with a bilayer structure formed from lipid molecules in aqueous solution. In recent years, research into liposomes has been greatly advanced, and liposomes are used as various drug carriers in many fields such as foods, cosmetics, and medicines. Due to the unique molecular structure and physicochemical properties of the liposome, the basic characteristics of the liposome are mainly shown in that hydrophilic and hydrophobic substances are embedded in a double way, and the water dispersibility is good; the biocompatibility is good, and no toxicity exists; the core material has low diffusion rate, slow release property and long-acting property. In the process of preparing the liposome, the properties of particle size, surface charge and the like can be changed to improve the universality of the liposome product.
Sturgeon products are high value-added products with rich nutrition, but the storage and preservation problems of products related to caviar are always the key points of academic and enterprise attention; the subject group is engaged in the preparation and application research work of novel functional food additives for a long time, and the natural essential oil nano liposome preservative is developed, so that the quality of caviar products is not influenced, the addition of chemical inorganic salt is avoided, the continuous and efficient antibacterial and antioxidant characteristics are realized, the storage time of the products can be effectively prolonged, the preservative is green and safe in source, and the sustainable development requirement is met.
Disclosure of Invention
According to the defects of the prior art, the invention aims to provide the application of the natural essential oil nanoliposome preservative in the storage of the sturgeon caviar, the preservative has the characteristics of high efficiency, continuous antioxidation and bacteriostasis, excellent biocompatibility, healthy and safe use, can effectively prolong the storage life of the sturgeon caviar, reduce the fishy smell of the caviar and avoid the use of chemical additives, and has the health-care functions of resisting inflammation, softening blood vessels, reducing blood pressure and the like, thereby having wide application prospect.
In order to achieve the purpose, the technical scheme of the invention is as follows:
provides an application of natural essential oil nanoliposome composite preservative in sturgeon caviar storage. Test results show that the natural essential oil nanoliposome preservative added into the sturgeon caviar in a certain proportion can achieve better antibacterial and antioxidant effects.
Preferably, the preparation steps of the natural essential oil nanoliposome (EO-NPs-Lps) are as follows:
adding 4mL of natural tea Tree Essential Oil (TEO) into a glass sample bottle, magnetically stirring at 1200rpm, heating at 160 ℃ for 0.5h, stopping heating, continuing stirring, and naturally cooling to room temperature; filtering with PVDF microporous membrane with pore diameter of 0.45 μm, collecting natural tea tree essential oil microparticle solution (TEO-NPs) containing nano-nanoparticles, and storing at 4 deg.C. Dissolving the 36mg natural tea tree essential oil microparticle solution (TEO-NPs) in 12mL ethanol (96%), fully mixing with 60mg lecithin, stirring under magnetic force at room temperature, fully mixing, storing in a refrigerator at 4 deg.C overnight, standing at 60 deg.C, and removing solvent by rotary evaporation under reduced pressure until a thin layer of uniform dry film is formed at the bottom of a round-bottomed flask; dispersing the liposome in 10mL deionized water, wherein the microjet pressure is 120Mpa, and the microjet frequency is 2 times, so as to obtain a monolayer stable liposome meeting the particle size requirement, freeze-drying at-65 ℃, collecting the product (EO-NPs-Lps), and storing at 4 ℃ for later use.
When the sturgeon caviar is preserved, the method specifically comprises the following steps of adding a proper amount of natural essential oil nano liposome preservative into unprocessed fresh caviar, and fully and uniformly mixing. And (3) performing heat-seal packaging, namely filling the caviar into a vacuum packaging bag, and performing vacuum heat-seal packaging by using an inclined vacuum packaging machine with the frequency of 50Hz, wherein the power of the inclined vacuum packaging machine is 2-3 KW, and the vacuum degree is 0.1-0.2 MPa.
In order to keep a good preservation effect, the content of the natural essential oil nano liposome preservative in the sturgeon caviar is 0.5-2 wt% during storage.
Compared with the prior art, the invention has the beneficial effects that:
(1) the natural essential oil nanoliposome (EO-NPs-Lps) preservative is used as a durable and efficient preservative, and has good antibacterial and antioxidant effects. The antibacterial effect of the essential oil nanoparticles contained in the liposome is far superior to that of the traditional essential oil. The source is green and safe, the environment is protected, the sanitation is realized, and the degradable advantage is realized.
(2) The essential oil component embedded in the liposome has the effects of bacteriostasis and antioxidation, has the health-care effects of resisting inflammation, softening blood vessels, reducing blood pressure and the like, and has a certain promotion effect on human health.
(3) Improves the traditional fresh-keeping storage process of caviar, does not add any inorganic salt, is more beneficial to human health, and conforms to the big health concept of contemporary society.
Drawings
FIG. 1 shows (a) natural tea tree essential oil (b) natural tea tree essential oil microparticle solution (TEO-NPs).
FIG. 2 is a graph showing the change in the number of colonies of the sturgeon caviar obtained in examples 2 to 5 of the present invention and a control group.
FIG. 3 is a comparison of the antioxidant properties of the preservatives of examples 2 to 5 of the present invention and the control group.
FIG. 4 is a comparative graph of sensory evaluation of products of examples 2 to 5 of the present invention.
Detailed Description
The invention is further described with reference to specific examples.
Example 1
The preparation method of the natural essential oil nanoliposome (EO-NPs-Lps) preservative comprises the following steps:
adding 4mL of natural tea Tree Essential Oil (TEO) into a glass sample bottle, magnetically stirring at 1200rpm, heating at 160 ℃ for 0.5h, stopping heating, continuing stirring, and naturally cooling to room temperature; filtering with PVDF (polyvinylidene fluoride) microporous membrane with pore diameter of 0.45 μm, collecting filtrate to obtain natural tea tree essential oil microparticle solution (TEO-NPs) containing nano-nanoparticles, and storing at 4 deg.C for use.
Preparing natural tea tree essential oil nanoliposomes (TEO-NPs-Lps): dissolving the above 36mg natural tea tree essential oil microparticle solution (TEO-NPs) in 12mL ethanol (96%), mixing well with 60mg lecithin, stirring well at room temperature under magnetic force, mixing well, and storing overnight at 4 deg.C in refrigerator. Performing rotary evaporation at the temperature of 60 ℃ under reduced pressure until a thin uniform dry film is formed at the bottom of the round-bottom flask; dispersing the liposome in 10mL deionized water, wherein the microjet pressure is 120Mpa, the microjet frequency is 2 times, so as to obtain a monolayer stable liposome (lipospheres) meeting the particle size requirement, collecting the product (EO-NPs-Lps), and storing at 4 ℃ for later use.
Example 2
Fully and uniformly mixing the natural essential oil nanoliposome (EO-NPs-Lps) preservative with the unprocessed fresh sturgeon caviar, putting the natural essential oil nanoliposome preservative with the concentration of 0.5 wt% in the sturgeon caviar into a packaging bag, and carrying out vacuum packaging or modified atmosphere packaging at the refrigeration temperature of 4 ℃.
(1) The samples were taken at different times and used for the determination of the microbial content. The storage period of the product obtained by the method reaches 30-90 days. The obtained caviar has no strong fishy smell, and the change curve of colony number is shown in figure 2.
(2) The DPPH free radical eliminating capability test of the preservative comprises the following steps: 0.005g of the above-mentioned antistaling agent is dissolved in a 100mL volumetric flask with ultrapure water. Accurately weighing 0.0080g DPPH to 100mL brown volumetric flask by a precision balance, dissolving with absolute ethyl alcohol, and fixing the volume to a scale mark to obtain 2.0 × 10-4Storing the mol/L DPPH test solution in dark, newly preparing and standing overnight for use, and fully shaking before use to ensure that the upper part and the lower part are uniform. The absorbance A at 517nm was measured by adding 2mL of DPPH and 1mL of ultrapure water to the cuvetteoThe absorbance value of the white DPPH solution without the addition of the active substance is obtained. Accurately transferring DPPH and a solvent into a cuvette by using a pipette, adding a corresponding volume of sample liquid to be detected, and measuring the DPPH absorbance value after reacting for 25 min. Reading the absorbance value, denoted Ai。
The clearance EC is calculated using the following formula:
clearance (EC) ═ 1-Ai/Ao)×100%
The DPPH clearance rate of the obtained compound preservative is shown in figure 3.
(3) The sample in (1) above was left at 4 ℃ for 6 days, and then subjected to sensory evaluation. Caviar was used for sensory evaluation, and 20 persons constituted a panel, and scored separately from elasticity, color, smell, taste, fullness of caviar and made a comprehensive evaluation, with a maximum score of 9, a minimum score of 0, and an average comprehensive score of 4.5, which was regarded as unacceptable hereinafter. The sensory evaluation results of each index of caviar are shown in figure 4.
Example 3
Fully and uniformly mixing the natural essential oil nanoliposome (EO-NPs-Lps) preservative with the unprocessed fresh sturgeon caviar, putting the natural essential oil nanoliposome preservative with the concentration of 1 wt% in the sturgeon caviar into a packaging bag, and carrying out vacuum packaging or modified atmosphere packaging at the refrigeration temperature of 4 ℃.
(1) The samples were taken at different times and used for the determination of the microbial content. The storage period of the product obtained by the method reaches 45-140 days. The obtained caviar has no strong fishy smell, and the change curve of colony number is shown in figure 2.
(2) The DPPH free radical eliminating capability test of the preservative comprises the following steps: 0.01g of the preservative was dissolved in a 100mL volumetric flask with ultrapure water. Accurately weighing 0.0080g DPPH to 100mL brown volumetric flask by a precision balance, dissolving with absolute ethyl alcohol, and fixing the volume to a scale mark to obtain 2.0 × 10-4Storing the mol/L DPPH test solution in dark, newly preparing and standing overnight for use, and fully shaking before use to ensure that the upper part and the lower part are uniform. The absorbance A at 517nm was measured by adding 2mL of DPPH and 1mL of ultrapure water to the cuvetteoThe absorbance value of the white DPPH solution without the addition of the active substance is obtained. Accurately transferring DPPH and a solvent into a cuvette by using a pipette, adding a corresponding volume of sample liquid to be detected, and measuring the DPPH absorbance value after reacting for 25 min. Reading the absorbance value, denoted Ai。
The clearance EC is calculated using the following formula:
clearance (EC) ═ 1-Ai/Ao)×100%
The DPPH clearance rate of the obtained compound preservative is shown in figure 3.
(3) The sample in (1) above was left at 4 ℃ for 6 days, and then subjected to sensory evaluation. Caviar was used for sensory evaluation, and 20 persons constituted a panel, and scored separately from elasticity, color, smell, taste, fullness of caviar and made a comprehensive evaluation, with a maximum score of 9, a minimum score of 0, and an average comprehensive score of 4.5, which was regarded as unacceptable hereinafter. The sensory evaluation results of each index of caviar are shown in figure 4.
Example 4
Fully and uniformly mixing the natural essential oil nanoliposome (EO-NPs-Lps) preservative with the unprocessed fresh sturgeon caviar, putting the natural essential oil nanoliposome preservative with the concentration of 1.5 wt% in the sturgeon caviar into a packaging bag, and carrying out vacuum packaging or modified atmosphere packaging at the refrigeration temperature of 4 ℃.
(1) The samples were taken at different times and used for the determination of the microbial content. The storage period of the product obtained by the method reaches 90-140 days. The obtained caviar has no strong fishy smell, and the change curve of colony number is shown in figure 2.
(2) The DPPH free radical eliminating capability test of the preservative comprises the following steps: 0.015g of the preservative was dissolved in a 100mL volumetric flask with ultrapure water. Accurately weighing 0.0080g DPPH to 100mL brown volumetric flask by a precision balance, dissolving with absolute ethyl alcohol, and fixing the volume to a scale mark to obtain 2.0 × 10-4Storing the mol/L DPPH test solution in dark, newly preparing and standing overnight for use, and fully shaking before use to ensure that the upper part and the lower part are uniform. The absorbance A at 517nm was measured by adding 2mL of DPPH and 1mL of ultrapure water to the cuvetteoThe absorbance value of the white DPPH solution without the addition of the active substance is obtained. Accurately transferring DPPH and a solvent into a cuvette by using a pipette, adding a corresponding volume of sample liquid to be detected, and measuring the DPPH absorbance value after reacting for 25 min. Reading the absorbance value, denoted Ai。
The clearance EC is calculated using the following formula:
clearance (EC) ═ 1-Ai/Ao)×100%
The DPPH clearance rate of the obtained compound preservative is shown in figure 3.
(3) The sample in (1) above was left at 4 ℃ for 6 days, and then subjected to sensory evaluation. Caviar was used for sensory evaluation, and 20 persons constituted a panel, and scored separately from elasticity, color, smell, taste, fullness of caviar and made a comprehensive evaluation, with a maximum score of 9, a minimum score of 0, and an average comprehensive score of 4.5, which was regarded as unacceptable hereinafter. The sensory evaluation results of each index of caviar are shown in figure 4.
Example 5
Fully and uniformly mixing the natural essential oil nanoliposome (EO-NPs-Lps) preservative with the unprocessed fresh sturgeon caviar, putting the natural essential oil nanoliposome preservative with the concentration of 2 wt% in the sturgeon caviar into a packaging bag, and carrying out vacuum packaging or modified atmosphere packaging at the refrigeration temperature of 4 ℃.
(1) The samples were taken at different times and used for the determination of the microbial content. The storage period of the product obtained by the method reaches 80-145 days. The obtained caviar has no strong fishy smell, and the change curve of colony number is shown in figure 2.
(2) The DPPH free radical eliminating capability test of the preservative comprises the following steps: 0.02g of the above-mentioned antistaling agent is dissolved in a 100mL volumetric flask with ultrapure water. Accurately weighing 0.0080g DPPH to 100mL brown volumetric flask by a precision balance, dissolving with absolute ethyl alcohol, and fixing the volume to a scale mark to obtain 2.0 × 10-4Storing the mol/L DPPH test solution in dark, newly preparing and standing overnight for use, and fully shaking before use to ensure that the upper part and the lower part are uniform. The absorbance A at 517nm was measured by adding 2mL of DPPH and 1mL of ultrapure water to the cuvetteoThe absorbance value of the white DPPH solution without the addition of the active substance is obtained. Accurately transferring DPPH and a solvent into a cuvette by using a pipette, adding a corresponding volume of sample liquid to be detected, and measuring the DPPH absorbance value after reacting for 25 min. Reading the absorbance value, denoted Ai。
The clearance EC is calculated using the following formula:
clearance (EC) ═ rate(1-Ai/Ao)×100%
The DPPH clearance rate of the obtained compound preservative is shown in figure 3.
(3) The sample in (1) above was left at 4 ℃ for 6 days, and then subjected to sensory evaluation. Caviar was used for sensory evaluation, and 20 persons constituted a panel, and scored separately from elasticity, color, smell, taste, fullness of caviar and made a comprehensive evaluation, with a maximum score of 9, a minimum score of 0, and an average comprehensive score of 4.5, which was regarded as unacceptable hereinafter. The sensory evaluation results of each index of caviar are shown in figure 4.
Comparative example
(1) Adding 6 wt% of NaCl into fresh caviar, mixing well, placing into a packaging bag, vacuum packaging or modified atmosphere packaging, and refrigerating at 4 deg.C. Used as a blank control group for microorganism experiments.
(2) Adding 6 wt% NaCl into fresh caviar, mixing, and placing into packaging bag at refrigeration temperature of 4 deg.C. Used as a blank control group for sensory evaluation experiments.
(3) The control group for DPPH clearance test is a sample group added with an equal amount of NaCl.
Claims (6)
1. The application of the natural essential oil nanoliposome preservative in the storage of sturgeon caviar is characterized in that the preparation method of the natural essential oil nanoliposome preservative comprises the following steps:
(1) preparing natural essential oil microparticle liquid: adding natural plant essential oil into a sample bottle, magnetically stirring, heating at high temperature, stirring for a period of time, stopping heating, continuing stirring, and naturally cooling to room temperature; filtering with polyvinylidene fluoride resin microporous membrane with pore diameter of 0.45 μm, and collecting filtrate to obtain natural essential oil microparticle solution containing nanoparticles;
(2) preparing a natural essential oil nano liposome preservative: dissolving the natural essential oil microparticle solution in ethanol, fully mixing with lecithin, stirring at room temperature by magnetic force, fully mixing and dissolving the two, and storing at 4 ℃ for 12-24 h; heating the system, decompressing and removing the solvent, and forming a thin uniform dry film at the bottom of the container; dispersing the membrane in deionized water, carrying out dynamic ultrahigh pressure micro-jet treatment to obtain a stable single-layer liposome meeting the particle size requirement, and freeze-drying to obtain the natural essential oil nanoliposome preservative.
2. The use of the natural essential oil nanoliposome preservative in sturgeon caviar storage according to claim 1, wherein the natural plant essential oil is one of the group consisting of peppermint oil, tea tree essential oil, thyme essential oil, cinnamon essential oil, ginger essential oil, fennel essential oil, clove oil, cardamom essential oil and combinations thereof.
3. The application of the natural essential oil nanoliposome preservative in the storage of sturgeon caviar according to claim 2 or 3, wherein in the preparation method of the natural essential oil microparticle liquid, the heating temperature is 160-180 ℃, the heating time is 25-30 min, and the rotating speed of a stirrer is 1000-1500 rpm.
4. The application of the natural essential oil nanoliposome preservative in the storage of sturgeon caviar according to claim 2 or 3, wherein in the preparation of the natural essential oil nanoliposome, the mass ratio of ethanol to natural essential oil microparticle solution and lecithin is 14: 20-40: 60-80 parts; the homogenizing condition is that the microjet pressure is 100-.
5. The application of the natural essential oil nanoliposome preservative in the storage of the sturgeon caviar according to claim 1, wherein the method for applying the preservative in the preservation of the sturgeon caviar is as follows: (1) adding: adding a natural essential oil nanoliposome preservative into unprocessed fresh caviar, and fully mixing the materials, (2) filling the caviar into a vacuum packaging bag, and carrying out vacuum heat sealing packaging by using an inclined vacuum packaging machine with the frequency of 50Hz, wherein the power of the inclined vacuum packaging machine is 2-3 KW, and the vacuum degree is 0.1-0.2 MPa.
6. The application of the natural essential oil nanoliposome preservative in the storage of the sturgeon caviar according to claim 5, wherein in the step (1), the content of the natural essential oil nanoliposome preservative in the sturgeon caviar is 0.5-2 wt%.
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