CN115590059A - Preparation method and application of antibacterial Pickering emulsion - Google Patents
Preparation method and application of antibacterial Pickering emulsion Download PDFInfo
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- CN115590059A CN115590059A CN202211345506.7A CN202211345506A CN115590059A CN 115590059 A CN115590059 A CN 115590059A CN 202211345506 A CN202211345506 A CN 202211345506A CN 115590059 A CN115590059 A CN 115590059A
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- pickering emulsion
- zein
- thymol
- pectin
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Images
Classifications
-
- 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
- A23B4/20—Organic compounds; Microorganisms; Enzymes
-
- 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 a preparation method and application of an antibacterial Pickering emulsion. The invention firstly utilizes an anti-solvent anti-precipitation method to prepare the zein-pectin composite nano particles loaded with thymol, and the nano particles have uniform shape and size and certain bacteriostatic effect. Secondly, in order to improve the antibacterial effect, thymol and star anise essential oil are combined, and the star anise essential oil is stabilized by using the thymol-loaded zein-pectin composite nanoparticles to prepare the oil-in-water Pickering emulsion. The invention optimizes the preparation process and obtains the optimal parameters, and the prepared Pickering emulsion has small droplet size, uniform distribution and long-term stability. And finally, applying the prepared Pickering emulsion to the snakehead fish fillets, so that the shelf life of the snakehead fish fillets can be prolonged remarkably.
Description
Technical Field
The invention belongs to food science and engineering, and particularly relates to a preparation method of an antibacterial Pickering emulsion and application of the antibacterial Pickering emulsion in snakehead fish fillets.
Background
Snakeheads (Channa argus), commonly called snakeheads, are common high-quality freshwater fishes, have high protein content, low cholesterol and rich fatty acid and various amino acids, have high edible value, have the medicinal values of clearing away heat and toxic materials, tonifying spleen and benefiting stomach and the like, and are so called as 'fish treasure'. At present, snakeheads on the market are mainly sold fresh and alive. The snakehead fish has delicious taste, low price and rich nutrition, and is deeply loved by consumers. With the transformation of consumption concepts of young people, fresh conditioning fish products are gradually replacing the traditional fresh selling mode. Because the life rhythm of the young generation is faster, the convenient and fast conditioning product is gradually favored, if the live fish is slaughtered and then put into a supermarket, the live fish is not sterilized, the cold storage and preservation time is short, and the sales radius is extremely short. Generally, the shelf life of the snakehead fish from a fishery to a dining table of a consumer needs at least more than 3 days, and in addition, the snakehead fish is extremely easy to decay and deteriorate in the links of transportation, processing and the like due to the characteristics of a large amount of bacteria adhered to the surface and the body of the snakehead fish after being killed, the enzyme activity in the body is high and the like, so that the sale range of products is limited, the economic value is reduced, and the problem of developing a preservation technology is urgently needed to solve. According to statistics, the spoilage loss rate of aquatic products in China in the storage and transportation process is up to 15 percent and far higher than that of aquatic products in developed countries by about 5 percent. In the past, people often utilize chemical preservatives to control the putrefaction of food, and with the high importance of people on physical health and food safety, the development and application of biological preservatives become hot spots of research in the field of aquatic product preservation.
Many researches show that the spice essential oil has good antibacterial effect on putrefying bacteria in food and can be used as a novel food fresh-keeping preservative. Essential oil is a generic name of volatile flavor-containing substances extracted from aromatic plants, and has been pursued for its excellent antibacterial and antioxidant properties, wherein Star Anise Essential Oil (SAEO) is one of the effective components of plant star anise, and has not only medicinal and nutritional values, but also a series of food-borne spoilage bacteria. However, when SAEO is exposed to light, oxygen or heat, it evaporates or decomposes rapidly, limiting its use in the preservation of food products. In addition, essential oils, when added to vegetables and fruits, cause color and odor changes. However, if SAEO is emulsified to overcome its susceptibility, for example, hao et al combine peppermint oil with resveratrol to make Pickering emulsions which not only enhance bacterial inhibition but also increase its antioxidant properties. The combination of two or more agents will be more effective than a single agent used alone under the combined action, and thus the combined use of multiple antibacterial agents has become an important approach to improve antibacterial efficiency and overcome the resistance of antibacterial agents. Thymol (2-isopropyl-5-methylphenol) is a natural antibacterial agent and can inhibit escherichia coli, bacillus subtilis, staphylococcus aureus and the like, so that thymol has a certain application value in food and medicines. However, thymol is easily degraded, has a certain volatility, and is very low in water solubility, thus resulting in low bioavailability. Therefore, the development of a carrier can not only improve antibacterial activity but also overcome limitations.
The results of the effect of the compound preservative on the storage quality of the weever by the radiation in the published article of meat research of white Chan in the prior art (2021, 35 (06): 50-56) show that the weever slices treated by the combination of the compound preservative and the radiation effectively inhibit the growth and the propagation of microorganisms, delay the reduction of the muscle protein quality in the storage process of the weever and prolong the shelf life of the weever slices. However, the irradiation treatment also accelerates the lipid oxidation, and the protein and lipid content of the weever slices have a tendency to decrease.
The result of the effect of the vacuum impregnation of the biological preservative on the protein characteristics of tilapia stored at ice temperature in the article published by Liu rock in Guangdong university of oceans (2022, 42 (02): 88-94) shows that the vacuum impregnation and the treatment of the biological preservative inhibit the enhancement of the denaturation of myogenin protein, effectively prolong the storage period of tilapia and delay the putrefactive process of fish. However, the vacuum storage method has strict technical requirements and high cost, and cannot be generally applied.
The result of the application Yu in the publication of 'food industry' article 'influence of biological preservative on the storage quality of mackerel slices processed through blue spot processing' (2017, 38 (04): 174-177) shows that the pH, volatile basic nitrogen, microorganisms and histamine of the mackerel slices processed through the biological preservatives nisin and natamycin are all superior to those of the blank samples, so that the storage period is prolonged by 1-2 days, but the preservative is strictly used according to the national standard limit standard, and no harmful ingredients are generated during the heat treatment of food.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the problems in the prior art, the invention provides a preparation method of an antibacterial Pickering emulsion, the stable and antibacterial Pickering emulsion is prepared and applied to snakehead fish fillets, the problem that the existing snakehead fish fillets are short in shelf life is effectively solved, and the sale range of the snakehead fish fillets is expanded.
The invention also provides application of the antibacterial Pickering emulsion.
The technical scheme is as follows: in order to achieve the purpose, the preparation method of the antibacterial Pickering emulsion comprises the following steps:
(1) Adding zein into ethanol, stirring for dissolving, adding thymol, stirring for dissolving completely, adding the above liquid dropwise into deionized water, vacuum rotary steaming, removing ethanol, and adding deionized water;
(2) Adding pectin into deionized water, heating and stirring until the pectin is fully dissolved, cooling and storing at low temperature;
(3) Dropwise adding the liquid obtained in the step (1) into the pectin solution obtained in the step (2) to obtain a final nano particle suspension system;
(4) And adding the oil phase into the nanoparticle suspension, and emulsifying by using a high-speed shearing machine to obtain the antibacterial Pickering emulsion.
Wherein, 0.01-0.02g/mL zein solution is prepared in the step (1), the zein solution is stirred and dissolved, thymol is added, and the ratio of the thymol to the zein is 5-10.
Preferably, the zein solution of 0.02g/mL is prepared in the step (1), stirred and dissolved, and then thymol is added, wherein the ratio of the thymol to the zein is 10. The method comprises the following steps of (1) taking the liquid, dropwise adding the liquid into deionized water, wherein the volume ratio of the liquid to the deionized water is 1.
Preferably, the liquid in the step (1) is dropwise added into deionized water, and the volume ratio of the liquid to the deionized water is 1.
Wherein the pH value of the deionized water used in the step (1) is 3-5.
Preferably, the deionized water used in step (1) has a pH of 4.
Wherein, the pectin in the step (2) is added into deionized water, and the concentration of the pectin solution is 0.0015-0.02g/mL.
Preferably, the pectin in step (2) is added to deionized water to give a pectin solution concentration of 0.0015g/mL.
And (2) dropwise adding the liquid obtained in the step (1) into the pectin solution obtained in the step (2), wherein the volume ratio of the liquid to the pectin solution is (4).
Preferably, in the step (3), the liquid obtained in the step (1) is dropwise added into the pectin solution in the step (2), and the volume ratio of the liquid to the pectin solution is 4. And (4) freeze-drying the prepared nanoparticle suspension for 48 hours by using a freeze-drying agent in the step (3), and storing for later use.
Wherein, after the oil phase in the step (4) is added into the nanoparticle suspension, the concentration of the zein is measured by adopting a Lowry method, and the percent of the zein concentration in the nanoparticles is 0.5-2.5 percent.
Wherein the oil phase in the step (4) is star anise essential oil, and the mass ratio of the oil phase in the whole system is 10-60%.
The antibacterial Pickering emulsion prepared by the preparation method disclosed by the invention is applied to the fresh-keeping of snakehead fish fillets.
The snakehead fish fillets are placed in Pickering emulsion to be soaked for 2-3h, placed in a sterile packaging bag, and the change of physical and chemical indexes is observed within tens of days at 4 ℃.
Preferably, the present invention comprises: (1) Preparing a Zein thymol solution, namely adding 0.2g of Zein into 10mL of ethanol with the mass fraction of 85%, stirring and dissolving for half an hour, then adding thymol, wherein the mass ratio of the thymol to the Zein is 10, stirring and fully dissolving, absorbing 2.5mL of the liquid, dropwise adding into 10mL of deionized water, performing vacuum rotary evaporation to remove ethanol, performing rotary evaporation under the condition of-0.1Mpa and at the temperature of 40 ℃ for 30 minutes, and adding deionized water to supplement the original volume.
(2) Preparing pectin solution, weighing 0.6g of pectin, adding into 400mL of deionized water, wherein the pectin concentration is about 0.15%, stirring at 70 ℃ for 30 minutes until the pectin is fully dissolved, rapidly cooling for 1h, and storing in a refrigerator.
(3) Preparing zein-pectin nanoparticles, putting 15.625mL of pectin solution into a beaker, and dropwise adding 12.5mL of liquid into the pectin solution to obtain a final solution system.
(4) Adding the star anise essential oil into the nanoparticle suspension, and emulsifying by using a high-speed shearing machine.
Wherein, the pH of the used deionized water is 4, the volume ratio of the zein thymol solution to water is 1.
And the concentration of the zein is measured by adopting a Lowry method, the concentration of the zein is 0.5-2.5 percent, the oil phase of the Pickering emulsion adopts the aniseed essential oil, the mass ratio of the oil phase is 10-60 percent, and the preparation method is high-speed shearing dispersion. In addition, thymol and star anise essential oil are both food grade. The rotational speed of the shear dispersion was 12000rmp, and the dispersion time was 3min. The emulsion did not delaminate on standing for 24h and remained stable for 1 month.
Soaking snakehead fish fillets in sterile water, a thymol aqueous solution, a nano particle suspension and a Pickering emulsion for 2h, taking out, placing in a sterile packaging bag, and observing the change of physical and chemical indexes within 14 days at 4 ℃.
Wherein the concentrations of thymol, the thymol-loaded zein-pectin nano particles and the Pickering emulsion are all 0.5mg/mL. Changes in the total number of colonies, volatile basic nitrogen, thiobarbituric acid value and pH were observed at 4 ℃ for 14 days. The Pickering emulsion prepared by the invention is uniform and fine, has good stability, is not easy to delaminate, has antibacterial activity, and effectively delays the putrefaction and deterioration speed of the snakehead fish fillets soaked in the Pickering emulsion.
Compared with the prior researches, the natural nuisanceless plant preservative (thymol and star anise essential oil) is selected, and the bioavailability of the thymol and the star anise essential oil is greatly improved by using the packaging and emulsifying methods, so that the hydrophilicity is enhanced.
The star anise essential oil not only has medicinal and nutritional values, but also can inhibit a series of food-borne pathogenic bacteria and putrefying bacteria. However, when exposed to light, oxygen or heat, the star anise oil evaporates or decomposes rapidly, which greatly limits its use in food processing. When essential oils are introduced to preserve any vegetables and fruits, their color and odor must change. The invention emulsifies the star anise essential oil to effectively overcome the susceptibility. Thymol, while effective in inhibiting the growth of spoilage bacteria, is easily degraded, volatile, and poorly water soluble, resulting in low bioavailability. The prepared Pickering emulsion not only has better anti-aggregation stability than the traditional surfactant, but also has the characteristic of sustained release of bioactivity, and in addition, the Pickering emulsion also has the characteristics of good biocompatibility, low cytotoxicity and capability of encapsulating active ingredients. According to the invention, the zein-pectin composite nanoparticles loaded with thymol are prepared firstly, then the zein-pectin composite nanoparticles are used for stabilizing the Pickering emulsion of the aniseed oil, and the Pickering emulsion is applied to snakehead fish fillets, so that the shelf life of the fillets is obviously prolonged by 5 days. In conclusion, the Pickering emulsion prepared by the method is extremely innovative and can play a great role in practical application.
In the invention, the thymol-loaded zein-pectin composite nanoparticles are prepared, are uniformly dispersed and have no aggregation phenomenon, and are then used for preparing the anise essential oil Pickering emulsion. Secondly, the preparation method and conditions of the aniseed essential oil Pickering emulsion are optimized, and the microstructure, the particle size potential and the laser confocal scanning microscope (CLSM) are used for characterization, and the optimal preparation conditions are determined by using 2.5% of ZTNPs and 50% of oil phase. And the prepared Pickering emulsion is applied to snakehead fish fillets, so that the shelf life of the snakehead fish fillets is prolonged.
The invention selects the common natural preservatives thymol and anise essential oil in food to prepare the antibacterial Pickering emulsion for keeping the snakehead fish fresh. The invention also provides a preparation method of the stable and antibacterial Pickering emulsion, and provides a potential application for preparing the Pickering emulsion by using the zein-pectin composite nanoparticles as antibacterial carriers.
The invention firstly utilizes an anti-solvent anti-precipitation method to prepare the zein-pectin composite nano particles loaded with thymol, and the nano particles have uniform shape and size and certain bacteriostatic effect. Secondly, in order to improve the antibacterial effect, thymol and star anise essential oil are combined, and the star anise essential oil is stabilized by utilizing the zein-pectin composite nanoparticles loaded with the thymol to prepare the oil-in-water Pickering emulsion. The preparation method optimizes the preparation process and obtains the optimal parameters, and the prepared Pickering emulsion has small droplet size, uniform distribution and long-term stability. Finally, the prepared Pickering emulsion is applied to the snakehead fish fillets, so that the shelf life of the snakehead fish fillets can be prolonged remarkably.
The stable and bacteriostatic Pickering emulsion prepared by the invention has good stability and antibacterial property, is applied to snakehead fish fillets, and prolongs the shelf life of the snakehead fish fillets.
Has the advantages that: compared with the prior art, the invention has the following advantages:
1. the preparation method is novel, the prepared antibacterial emulsion breaks through the low bioavailability of the traditional biological preservative, and the bioavailability of the biological preservative is improved by a zein-pectin packaging mode.
2. The invention solves the problems of volatile oil and easy decomposition of essential oil, and adopts an emulsification method to reduce susceptibility. The zein-pectin composite nanoparticles loaded with thymol are used for stabilizing the star anise essential oil Pickering emulsion, and the thymol and the star anise essential oil are combined to improve the antibacterial effect.
3. The prepared star anise essential oil Pickering emulsion is applied to the snakehead fish fillets, so that the shelf life of the snakehead fish fillets is prolonged, the preparation steps of the emulsion are simple and easy to realize, the raw materials are all natural and healthy, other surfactants are not required to be added, and the cost is low.
Drawings
FIG. 1 shows the particle size potential and microstructure of Pickering emulsion prepared at different protein concentrations according to the present invention (scale bar 5 μm).
FIG. 2 shows the particle size potential and microstructure (scale bar 5 μm) of Pickering emulsion prepared according to different oil phase ratios (0.5% -2.5%) of the present invention.
FIG. 3 is a CLSM micrograph (scale bar 10 μm) of Pickering emulsions prepared with different oil phase ratios (10% to 60%) according to the present invention.
FIG. 4 is a graph showing the change in particle size potential of Pickering emulsion prepared according to the invention over different days of storage.
FIG. 5 is a CLSM micrograph (scale bar 10 μm) of Pickering emulsion prepared according to the invention on different days of storage.
FIG. 6 shows the colony count (TVC), thiobarbituric acid number (TBA), volatile basic nitrogen (TVBN) and pH change of the Pickering emulsion prepared by the invention applied to snakehead fillets, and the changes are compared with untreated fillets, the treatment of thymol aqueous solution and the fillets treated by the thymol-loaded zein-pectin composite nanoparticles.
FIG. 7 is a flow chart of the preparation of Pickering emulsion of the present invention.
Detailed Description
The experimental methods described in the examples are all conventional methods unless otherwise specified; the reagents and materials are commercially available, unless otherwise specified.
Among them, thymol (Thymol, ≧ 98%), zein (Zein, > 95%) and Pectin (Pectin, > 65%) are commercially available from Michelin, inc. (Shanghai, china); star Anise Essential Oil (SAEO) was purchased from hessen botanical flavors limited (jiang west, china).
Example 1
The flow chart of the preparation of Pickering emulsion in the present invention is shown in FIG. 7.
(1) Adding 0.2g of Zein (Zein) into 10mL of 85% ethanol, stirring to dissolve for half an hour, adding thymol, wherein the mass ratio of the thymol to the Zein is 10.
(2) 0.6g of pectin is weighed into 400mL of deionized water, stirred at 70 ℃ for 30 minutes until fully dissolved, rapidly cooled for 1 hour, and stored in a refrigerator at 4 ℃.
(3) Preparing zein-pectin nano particles: and (3) putting 15.625mL of pectin solution into a beaker, and dropwise adding 12.5mL of liquid obtained in the step (1) into the pectin solution and uniformly mixing to obtain a final nanoparticle suspension solution system.
(4) Adding star anise essential oil into the nanoparticle suspension, wherein the mass ratio of the star anise essential oil in the system is 50% (namely in the whole system of the star anise essential oil and the nanoparticle suspension), and emulsifying by using a high-speed shearing machine, wherein the rotating speed of the shearing machine for dispersing is 12000rmp, and the dispersing time is 3min. The emulsion did not delaminate on standing for 24h and remained stable for 1 month.
Example 2
The embodiment relates to the influence of protein concentration on the stability of Pickering emulsion, and the zein concentration in the nanoparticles has great influence on the stability of the Pickering emulsion by using the thymol-loaded zein-pectin composite nanoparticles to stabilize the anise essential oil.
According to the preparation method of example 1, using zein as a raw material, a thymol-zein solution is prepared first, then a pectin stock solution is prepared, a nanoparticle suspension is prepared by an anti-solvent precipitation method, the concentration of nanoparticles is concentrated by rotary evaporation, and the concentration of zein is measured by a Lowry method, wherein the fixed amount is the proportion by mass of the star anise essential oil, and the variable is the proportion of the concentration of zein (0.5%, 1%, 1.5%,2%,2.5% g/mL). Adding oleum Anisi Stellati into the water phase nanoparticle suspension, 12000rmp, and shearing and dispersing for 3min to obtain emulsion. The particle size and zeta potential of the Pickering emulsion were determined with a nanoparticle size potentiometer. The microstructure of the Pickering emulsion was observed at room temperature with an optical microscope. A20. Mu.L sample of the diluted emulsion was dropped onto the slide, covered with a cover slip, and ensured that there were no air bubbles between the cover slip and the slide. The prepared sample is observed under a microscope, and a representative picture is found and photographed by a camera.
As can be seen from fig. 1a, as the concentration of zein, i.e. the concentration of nanoparticles, increases, the size of the emulsion droplets gradually decreases. This is probably because the area covered by the oil-water interface is increased, which promotes the formation of smaller particles during homogenization. And the absolute value of zeta potential also increased with increasing concentration, indicating that the higher the zein concentration, the more stable the resulting emulsion. And the difference between the potential and the particle size of the last three groups becomes small, which shows that when the concentration of the zein reaches the concentration required by the oil-water interface stability, the concentration is about 1.5%, and the droplet size of the Pickering emulsion also becomes stable. When more particles are adsorbed on the oil-water distribution interface, a thick and stable interface layer can be formed. When the zein concentration was 1.5%,2%,2.5%, the change in the particle size of the Pickering emulsion droplets was not large, probably because the nanoparticle concentration had reached the concentration of the stable oil-water two phase, and a stable interface layer had formed. The absolute value of the ZETA potential (ZETA potential) also increases with increasing concentration, indicating that the greater the concentration, the more stable the emulsion obtained. As can be seen from fig. 1b, pickering emulsions stabilized with different concentrations of zein or nanoparticles can form uniform spheres, and the lower the concentration, the larger the droplet size formed, consistent with the results obtained from the particle size potential. The liquid drops of Pickering emulsion prepared from low-concentration nanoparticles can also generate aggregation and flocculation phenomena, and when the concentration is increased continuously, the phenomenon can be obviously relieved. When the concentration is increased to 2.5%, the emulsion particle size is minimal and no aggregate flocculation is optimal.
Example 3
This example relates to the effect of the oil phase mass ratio on the stability of Pickering emulsion, and the oil phase ratio has a great effect on the stability of Pickering emulsion by stabilizing anise essential oil with thymol-loaded zein-pectin composite nanoparticles.
According to the preparation method of the embodiment 1, the zein is used as a raw material, the thymol-zein solution is prepared firstly, then the pectin stock solution is prepared, and the nanoparticle suspension is prepared by an anti-solvent precipitation method. The nanoparticle concentration (i.e. zein concentration was 2.5%) was fixed, and the variables were the oil phase ratios (10%, 20%, 30%, 40%,50%, 60%). Adding oleum Anisi Stellati, 12000rmp, and shearing and dispersing for 3min to obtain emulsion. The particle size and zeta potential of the Pickering emulsion were determined with a nanoparticle size potentiometer. The microstructure of the Pickering emulsion was observed at room temperature with an optical microscope. A20. Mu.L sample of the diluted emulsion was dropped onto the slide, covered with a cover slip, and ensured that there were no air bubbles between the cover slip and the slide. The prepared sample is observed under a microscope, and a representative picture is found and photographed by a camera.
From the analysis of the particle size results, the droplet size gradually increased with increasing proportion of the oil phase (fig. 2 a). In fig. 2b, the results of the optical microscope show that the droplet particle size increases significantly with increasing proportion of the oil phase. The particle size and microstructure indicate that the oil phase ratio has a significant effect on the Pickering emulsion. When the oil phase mass ratio is 10% or more and 20% or less, the droplet size is small but relatively dispersed, and it is found from the above experimental results that the formation of the Pickering emulsion may be insufficient because of the tendency to delaminate. When the oil phase mass ratio is 30-50%, due to the increase of the interface area, more ZTNPs are adsorbed on the surface, the entanglement among particles is reduced, the electrostatic repulsive force among liquid drops is increased, and the aggregation and flocculation phenomena are avoided. However, the oil phase increases, the mass concentration of ZNTPs per interfacial film decreases, and emulsification needs to be completed by decreasing the specific surface area when subjected to high-speed shearing, and thus the particle size tends to increase. However, when the oil phase mass ratio is 60%, the absorption rate of the interface particles is lowered, the thickness of the interface film is reduced, and the potential space resistance is reduced, so that oil droplets are agglomerated. The zeta potential showed a tendency to decrease first and then increase, but the absolute value of the zeta potential was the highest at 50% mass of the oil phase, indicating that the Pickering emulsion was the most stable in this oil phase.
Example 4
This example relates to the effect of storage time on the stability of Pickering emulsions, and the results of examples 2 and 3 above gave the most stable emulsions with the best formulation and the storage stability of the Pickering emulsions was investigated.
According to the preparation method of the embodiment 1, the zein is used as a raw material, the thymol-zein solution is prepared firstly, then the pectin stock solution is prepared, and the nanoparticle suspension is prepared by an anti-solvent precipitation method. The concentration of zein in the nanoparticle suspension is determined to be 2.5% by rotary evaporation and concentration, the mass proportion of an oil phase is determined to be 50%, and star anise essential oil is added into the aqueous phase nanoparticle suspension immediately, and the mixture is cut and dispersed for 3min to prepare the emulsion. Nanoparticle concentration and oil phase ratio were fixed, with the variables being storage time (1, 3, 7, 15 and 30 days). The particle size and zeta potential of the Pickering emulsion were determined with a nanometer particle size potentiometer.
As shown in fig. 3, the Pickering emulsion formed using a 2.5% concentration of zein and a 50% oil phase changed during storage over 30 days. The particle size of the emulsion droplets is analyzed, and the distribution of the droplet sizes is expanded along with the prolonging of the storage time. The particle size remained essentially unchanged on days 1, 3 and 7. After day 15, the emulsion began to separate, so the particle size increased, probably due to aggregation of some colloidal particles, or density change between the oil and water phases, causing separation. However, from the zeta potential, the zeta potential of the emulsion was still large after 30 days of storage. Therefore, this Pickering emulsion has good stabilizing potential.
Example 5
This example relates to the observation of the microstructure of the Pickering emulsion prepared in example 3 using different concentrations of oil phase using a laser confocal microscope (CLSM). First, pickering emulsion was stained with a mixed fluorescent dye solution consisting of 1mg/mL nile red and 1mg/mL FITC. Nile red stains the oil droplets red, while FITC stains the protein nanoparticles green. And then, a microstructure of the Pickering emulsion is imaged by a laser confocal scanning microscope (CLSM) and an FV1000 type 60-time objective lens, wherein the excitation wavelength of Nile red is 488nm, and the excitation wavelength of FITC is 561nm.
As shown in fig. 4, CLSM can be used to analyze the microstructure of Pickering emulsions and determine whether protein flocculation or aggregation, etc. From fig. 4, it is clear that the red-dyed oil phase and the green-dyed protein particles show that the oil droplet surface is adsorbed by the nanoparticles, and the emulsion is also demonstrated to be a Pickering emulsion. Very large droplets were seen when the oil phase was 10%,20%, 30% and was not a uniform and dispersed sphere, nor was there flocculation, indicating that its emulsifying capacity was low and no stable Pickering emulsion was formed, which is also similar to the results observed for particle size potential. With the increasing of the star anise essential oil, the size of the emulsion liquid drop is reduced. When the oil phase accounts for 40% and 50% of the mass ratio, the emulsion droplets are uniform in size and shape and do not aggregate or flocculate. Further, the absolute value of zeta potential of the emulsion was the largest at an oil phase mass ratio of 50%, which also indicates that the Pickering emulsion at this oil phase mass ratio was the most stable. When the mass ratio of the oil phase is increased to 60%, the morphology of the droplets becomes uneven, the droplets become large, and aggregation and flocculation occur. The optimum proportion of oil phase is therefore 50%.
As shown in fig. 5, the morphological characteristics of the emulsion after 15 and 30 days of standing were observed by CLSM to verify the stability of the Pickering emulsion. At day 15 and day 30, it can clearly be seen that the oil phase is encapsulated within the nanoparticles and forms a network, probably because a stable oil-water interface layer has formed. However, some aggregation of droplets occurred in the Pickering emulsion on day 30 compared to day 15, but no oil phase precipitated, resulting in the same particle size as measured above. The results of these experiments show that the Pickering emulsion produced in this way has good storage properties, which provides a reasonable basis for the use of the emulsion in antimicrobial systems.
Example 6
The embodiment relates to the fresh-keeping effect of the prepared Pickering emulsion on snakehead fillets. Putting snakehead fish fillets into sterile water, a thymol aqueous solution, a nano particle suspension and a Pickering emulsion, wherein the preparation method comprises the steps of weighing a proper amount of thymol particles and freeze-dried powder (the nano particle suspension or the Pickering emulsion) to be dissolved in the water, controlling the concentration to be 0.5mg/mL, then putting the fillets into the water to be soaked for 2-3h, taking out the fillets to be put into a sterile packaging bag, and observing the change of physical and chemical indexes within 14 days at 4 ℃.
Determination of total number of colonies (TVC): under the aseptic condition, 10.00g of snakehead fish fillets are placed in an aseptic cooking bag, and 90mL of aseptic normal saline is poured into the cooking bag. Placing the steamed bag on a slapping type homogenizer, beating for 60s, standing, taking 1.0mL of supernatant with a pipette, adding into a test tube containing 9.0mL of sterile physiological saline, performing gradient dilution by 10 times, taking appropriate concentration, and determining colony count (TVC) in fish meat by reference to GB4789.2-2016 method. Determination of thiobarbituric acid number (TBA): weighing 10.00g of minced snakehead fish fillets, adding 25mL of deionized water, fully homogenizing at a high speed, adding 25.0mL of 5% (m/V) trichloroacetic acid, uniformly stirring by using a glass rod, and standing for 30min. After filtering through filter paper, 5.00mL of supernatant is mixed with 5.00mL of 0.02mol/L thiobarbituric acid solution, the mixture is placed into a constant-temperature water bath to react for 30min (90 ℃), cold water is used for cooling to room temperature, trichloroacetic acid is used for replacing the supernatant as a control, and the absorbance of a sample at 532nm is measured. The thiobarbituric acid value (TBA) of the fillet sample was calculated from the malondialdehyde standard curve and the result was expressed as malondialdehyde mg/kg of sample. Measurement of pH: weighing 5.00g of minced fish, adding 45.0mL of deionized water, fully homogenizing at a high speed, standing for 30min, and measuring the pH value of the homogenate. Determination of volatile basic nitrogen (TVBN): weighing 5.00g of minced snakehead fish fillets and 0.50g of magnesium oxide, adding into a distillation tube, adding 30.0mL of 2% (m/V) boric acid, and then dropwise adding 5-8 drops of a mixed indicator. Distillation was carried out using a semi-automatic Kjeldahl apparatus, and the distillate was titrated with 0.01mol/L hydrochloric acid, and the result was expressed as mgN/100g of sample.
As shown in fig. 6a, growth and propagation of microorganisms can lead to spoilage of fish. The total number of colonies of the fresh fillets is 3.5log CFU/g, and the fillets are in first-grade freshness. At the beginning, the colony count of the treated snakehead fish fillets is also slightly reduced probably because the star anise essential oil and the thymol release sterilization. The acceptable TVC of the fillets was 7logCFU/g, it can be seen from the figure that the untreated fillets reached the threshold value on the fifth day, but the treated fillets reached the threshold value for a prolonged period of time, with Pickering's emulsion being the best effect, for a period of approximately 5 days. As shown in FIG. 6b, the unsaturated fatty acids in the fillet undergo oxidation reaction in the presence of oxygen to form ketones, aldehydes, etc. Wherein malondialdehyde forms a red complex with thiobarbituric acid, and thus measurement of malondialdehyde content can indicate the degree of oxidation of fat. The acceptable TBA of the fillet is 1.1mgMDA/kg, and the figure shows that the fillet treated by Pickering emulsion has strong oxidation resistance and can inhibit fat oxidation. As shown in fig. 6c, TVBN will accumulate in the fish meat over time, which will affect the quality of the fish meat. The TVBN value of qualified fish meat is below 30 mg. During the whole refrigeration process, the TVBN of the fillets showed a tendency to increase, and the TVBN value treated with Pickering emulsion was significantly lower than that of the samples untreated at the same time. The essential oil and thymol can inhibit the growth of microorganisms and delay the decomposition of protein. As shown in FIG. 6d, during the storage of the fillets, the pH of the fillets is increased due to the decomposition of macromolecular proteins, small molecular peptides and amino acids into alkaline compounds by microbial metabolism, and the treated fillets can delay the generation of alkaline nitrogenous substances in vivo and have little pH change. This is also the same as the above result. Therefore, the invention has the effect of preserving the snakehead fish fillets, and can prolong the growth of microorganisms, fat oxidation and the like, thereby prolonging the shelf life of the snakehead fish fillets.
Claims (10)
1. The preparation method of the antibacterial Pickering emulsion is characterized by comprising the following steps:
(1) Adding zein into ethanol, stirring for dissolving, adding thymol, stirring for dissolving completely, adding the above liquid dropwise into deionized water, vacuum rotary steaming, removing ethanol, and adding deionized water;
(2) Adding pectin into deionized water, heating and stirring until the pectin is fully dissolved, cooling and storing at low temperature;
(3) Dropwise adding the liquid obtained in the step (1) into the pectin solution obtained in the step (2) to obtain a final nano particle suspension system;
(4) And adding the oil phase into the nanoparticle suspension, and emulsifying by using a high-speed shearing machine to obtain the antibacterial Pickering emulsion.
2. The preparation method according to claim 1, wherein in the step (1), 0.01-0.02g/mL of zein solution is preferably prepared, the zein solution is stirred and dissolved, thymol is added, and the mass ratio of the thymol to the zein is 5-10.
3. The preparation method according to claim 1, wherein the liquid in the step (1) is dropwise added into deionized water, and the volume ratio of the liquid to the deionized water is 1.
4. The method according to claim 1, wherein the deionized water used in step (1) has a pH of 3 to 5.
5. The method of claim 1, wherein in step (2), the pectin is added to deionized water to give a pectin solution having a concentration of 0.0015-0.02g/mL.
6. The preparation method according to claim 1, wherein the liquid obtained in step (1) is added dropwise into the pectin solution in step (2) in step (3), and the volume ratio of the liquid to the pectin solution is 4.
7. The method of claim 1, wherein the oil phase of step (4) is added to the nanoparticle suspension and the zein concentration is measured by Lowry method to obtain a zein concentration in the nanoparticles of 0.5% to 2.5% g/mL.
8. The preparation method according to claim 1, wherein the oil phase in step (4) is star anise essential oil, and the mass ratio of the oil phase in the whole system is 10-60%.
9. An application of the antibacterial Pickering emulsion prepared by the preparation method in the fresh-keeping of snakehead fish fillets.
10. The use as claimed in claim 9, wherein the snakehead fillets are soaked in Pickering emulsion for 2-3h, and then placed in a sterile packaging bag, and the change of physicochemical index is observed at 4 ℃ for tens of days.
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| CN113956500A (en) * | 2021-10-14 | 2022-01-21 | 江南大学 | Zein composite particles, carrying system, preparation method and application |
| CN113940400A (en) * | 2021-10-25 | 2022-01-18 | 广东省农业科学院蚕业与农产品加工研究所 | Nano thymol with strong antibacterial activity and preparation method and application thereof |
| CN114948903A (en) * | 2022-06-06 | 2022-08-30 | 盐城工业职业技术学院 | Preparation method of thymol-loaded zein-Arabic gum-chitosan hydrochloride composite nanoparticles |
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| CN116195745A (en) * | 2023-03-30 | 2023-06-02 | 盐城工业职业技术学院 | Preparation method of pekrin emulsion loaded with eugenol |
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