CN115069180B - Secondary cross-linking type plant essential oil microcapsule as well as preparation method and application thereof - Google Patents
Secondary cross-linking type plant essential oil microcapsule as well as preparation method and application thereof Download PDFInfo
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- CN115069180B CN115069180B CN202210851350.3A CN202210851350A CN115069180B CN 115069180 B CN115069180 B CN 115069180B CN 202210851350 A CN202210851350 A CN 202210851350A CN 115069180 B CN115069180 B CN 115069180B
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
-
- 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 belongs to the technical field of microcapsule material preparation, and particularly relates to a secondary cross-linking type plant essential oil microcapsule, and a preparation method and application thereof. According to the preparation method of the secondary crosslinking type plant essential oil microcapsule, the aldehyde-based soybean polysaccharide and epsilon-polylysine are used as composite wall materials, and the secondary crosslinking type plant essential oil microcapsule and antibacterial plant essential oil can play a synergistic antibacterial role. The plant essential oil is fixed and embedded by adopting a secondary chemical crosslinking technology to form microcapsules, so that the volatility of the plant essential oil can be effectively reduced, the stability of the plant essential oil is improved, and particularly the slow release and antibacterial effects of the plant essential oil are enhanced. The method provided by the invention enlarges the antibacterial activity and the application range of the plant essential oil, and has a good application prospect in the preparation and application fields of antibacterial microcapsules.
Description
Technical Field
The invention belongs to the technical field of microcapsule material preparation, and particularly relates to a cross-linked plant essential oil microcapsule, and a preparation method and application thereof.
Background
The plant essential oil is volatile oily liquid substance with strong fragrance extracted from aromatic plant, and mainly comprises alcohol, ether, aldehyde, ketone, and ester aromatic compounds. At present, common plant essential oils such as rosemary essential oil, lavender essential oil, lemon essential oil and the like have been verified to have a spectrum antibacterial function. In recent years, with the scientific and technological progress and the enhancement of the concept of health and environmental protection, people put higher requirements on food preservation. Compared with the common chemical synthetic preservatives such as benzoic acid, potassium sorbate and the like (with potential toxic and side effects and even teratogenic carcinogenic risks), the plant essential oil type preservatives are more and more widely concerned due to the advantages of safety, no toxicity, environmental protection and good bacteriostatic activity.
However, most bacteriostatic plant essential oils are sensitive to air, light and temperature and are volatile, so that the application of the bacteriostatic plant essential oils in the aspect of food preservatives is greatly limited. The microcapsule technology is a technology in which a micro container is constructed by using a natural or synthetic polymer as a wall material and a small solid, liquid, or gas as a core material by means of emulsification, polymerization, complex aggregation, or the like, and an active ingredient is coated and used. The essential oil microcapsule prepared from the plant essential oil can effectively protect the active substances of the essential oil from the influence of external conditions such as light, heat, oxidation and the like, reduce the release rate of the volatile core essential oil and greatly improve the application value of the plant essential oil. Therefore, the microcapsule technology of plant essential oil has become a research focus in recent years.
The patent application with application publication number CN111359552A discloses a self-crosslinking essential oil microcapsule and a preparation method thereof, plant essential oil is used as a capsule core, a polyelectrolyte macromolecular substance (chitosan) with positive charge is used as an inner wall material, a main monomer and a self-crosslinking monomer are used as outer wall materials, and the slow release effect of the essential oil is improved through a crosslinking grafting reaction between the wall materials. The invention patent application with application publication number CN109046192A discloses a preparation method of chitosan nano microcapsule of plant essential oil, which uses sodium tripolyphosphate as a cross-linking agent to be cross-linked with chitosan to form a coating of the plant essential oil, thereby improving the stability of the essential oil and expanding the application of the essential oil.
At present, in the prior art, when the plant essential oil is subjected to microcapsule coating modification, attention is paid to how to improve the stability of the essential oil, and the problem of how to further improve the bacteriostatic effect of the essential oil is not considered. In the existing application market, the requirements of food fresh-keeping materials not only require good self-stability, but also often require strong bacteriostatic ability and long slow-release effect, thereby meeting the requirements of food fresh-keeping with higher requirements. Therefore, how to solve the problems is of great significance to fully exerting the economic value of the plant essential oil and expanding the application of the plant essential oil.
Disclosure of Invention
In order to solve the above problems, the first aspect of the present invention provides a method for preparing a secondary cross-linking type plant essential oil microcapsule, which has mild conditions and easy operation, and the microcapsule prepared by the method has good encapsulation efficiency and stability, and strong bacteriostatic and sustained release effects.
The second aspect of the invention provides a secondary crosslinking type plant essential oil microcapsule which has high stability, good bacteriostatic and slow-release effects and better application value in the field of food preservation.
In a third aspect of the invention, the invention provides an application of a secondary crosslinking type plant essential oil microcapsule.
In order to realize the purpose, the technical scheme of the preparation method of the secondary crosslinking type plant essential oil microcapsule is as follows:
a preparation method of a secondary cross-linking type plant essential oil microcapsule comprises the following steps:
1) Dissolving aldehyde soybean polysaccharide in water to obtain an aldehyde soybean polysaccharide solution with the concentration of 4-6 mg/mL;
2) Adding soybean lecithin and sodium alginate into the aldehyde soybean polysaccharide solution, mechanically stirring uniformly, then adding plant essential oil, and homogenizing and emulsifying at a high speed of 10000 to 12000r/min for 30 to 40min to obtain mixed emulsion;
3) Adding an aqueous solution of epsilon-polylysine into the mixed emulsion obtained in the step 2), performing crosslinking reaction for 2 to 3 hours at the temperature of 20 to 30 ℃ under the condition of mechanical stirring, and then adding a glutaraldehyde solution for continuous crosslinking;
4) Centrifuging, washing, freezing and drying after crosslinking to obtain secondary crosslinking type plant essential oil microcapsules;
wherein, the addition amount of the aldehyde group soybean polysaccharide solution is (4 to 6 g): (1 to 2g): 0.10 to 0.12mL per 100 mL; the mass ratio of the aldehyde soybean polysaccharide to the epsilon-polylysine is 1 (2 to 4).
In the preparation method of the secondary crosslinking plant essential oil microcapsule, the wall material of the microcapsule is selected to play a role in fixing and stabilizing the plant essential oil, and the bacteriostatic action of the plant essential oil needs to be enhanced, so that the food fresh-keeping application range of the essential oil is expanded.
Based on the purposes, the invention simultaneously uses the soybean polysaccharide and the epsilon-polylysine in the essential oil coating wall material to achieve better coating and bacteriostasis effects. The soybean polysaccharide is a natural polysaccharide derived from bean dregs, has the characteristics of degradability, no toxicity and no harm, is rich in dietary fiber, and has certain antibacterial and antioxidant properties. In addition, the epsilon-polylysine is a natural antiseptic bacteriostatic agent which is formed by peptide bond connection between alpha-carboxyl and epsilon-amino of lysine, has good bacteriostatic activity on most gram-negative bacteria, positive bacteria and fungi, can be biodegraded, and is nontoxic and harmless to human bodies.
Based on the wall material raw materials, in order to realize effective fixation and stable coating of the wall material on plant essential oil, on one hand, the chemically modified aldehydized soybean polysaccharide is adopted, the aldehyde group in the soybean polysaccharide and the amino group in the epsilon-polylysine are utilized to form a typical Schiff base reaction, so that a stable chemically crosslinked composite wall material is formed, the composite wall material takes the biological activities of the soybean polysaccharide and the epsilon-polylysine into account, the effective load of the essential oil can be realized, and the synergistic improvement of the microcapsule stability and the antibacterial activity can be realized. On the other hand, in order to make the capsule wall material exert a stable coating effect, it is necessary to ensure that the crosslinking system has good emulsibility and stability, and to prevent the microspheres from agglomerating during embedding. Based on the situation, the soybean lecithin and the sodium alginate are used as the composite emulsifier, wherein the soybean lecithin is a phospholipid byproduct in the process of refining the soybean oil, and belongs to homologous plant raw materials with soybean polysaccharide, the biocompatibility of the soybean lecithin and the soybean polysaccharide is better, the soybean lecithin is used as a main emulsifier, and the sodium alginate is used as an auxiliary emulsifier, so that uniform and fine emulsified liquid drops can be obtained, a stable microenvironment is provided for embedding plant essential oil in a wall material, the stability of a fine emulsion and a subsequent crosslinking process can be maintained by reducing an interface between oil and water phases, and the coating stability of the obtained microcapsule is improved.
In addition, the invention finds that the crosslinking process of the soybean polysaccharide and the epsilon-polylysine can realize the effective embedding of the plant essential oil, but the intermolecular crosslinking degree is low, so that the slow release effect of the microcapsule is still not ideal. Therefore, in order to improve the stability of the microcapsule, regulate and control the release speed of the core material, the essential oil microcapsule with more excellent performance is prepared. According to the invention, glutaraldehyde is further introduced to carry out secondary crosslinking on the composite system, so that the structural stability of the essential oil microcapsule is further improved, better controlled release and sustained release effects are given to the microcapsule, and the application range of the plant essential oil in the field of food preservation is further expanded.
Further preferred embodiments of the present invention will be described below. In order not to affect the use quality of the aldehyde-based soybean polysaccharide, in step 1), the aldehyde-based soybean polysaccharide is preferably obtained by oxidizing water-soluble soybean polysaccharide with sodium periodate.
Sodium periodate is used as a modifying reagent, hydroxyl sites in polysaccharide molecules can be selectively broken to generate corresponding polysaccharide aldehyde, and the water-soluble soybean polysaccharide is subjected to aldehyde modification to realize controllable chemical modification, so that functional groups are diversified. In the process of preparing the aldehydic soybean polysaccharide by the sodium periodate, the aldehydic degree can influence the coating stability of the microcapsule and the controlled release performance of the product to a certain degree, the sodium periodate is adopted to carry out oxidation treatment on the water-soluble soybean polysaccharide, and the preferable technical scheme is as follows: stirring and dissolving water-soluble soybean polysaccharide in 1% (v/v) acetic acid solution, preparing water-soluble soybean polysaccharide solution with the concentration of 0.01g/mL, then adding equal volume of sodium periodate solution with the concentration of 0.015g/mL, reacting for 2-3h at room temperature in a dark place after mixing, then adding ethylene glycol to terminate the reaction, filtering, and drying in vacuum to obtain the aldehyde-group soybean polysaccharide.
The plant essential oil is a core material of the microcapsule, the type of the plant essential oil is not particularly limited, and the plant essential oil with the bacteriostatic effect can be conventionally adopted according to bacteriostatic requirements. As a further preferable scheme, the plant essential oil is one of rosemary essential oil, lavender essential oil and lemon essential oil.
Preferably, in the step 2), the rotation speed of mechanical stirring is 50 to 80r/min. After soybean lecithin and sodium alginate are added into the aldehyde soybean polysaccharide solution, the mixed solution is stirred uniformly by adopting a mechanical stirring mode, and then plant essential oil is added, so that the dispersion, emulsification and embedding effects of the plant essential oil can be effectively ensured.
The crosslinking stage is a process for obtaining a stable embedded particle dispersion, in order to promote the chemical crosslinking process of the aldehyde soybean polysaccharide and the epsilon-polylysine and realize the embedding of the essential oil, the crosslinking process needs to be carried out at a certain stirring speed, and preferably, in the step 3), the rotation speed of mechanical stirring is 200 to 300r/min.
And (3) carrying out secondary crosslinking by using glutaraldehyde to improve the coating stability and the sustained release effect of the microcapsule, wherein preferably, in the step 3), the mass fraction of the glutaraldehyde solution is 2-4%, and the volume is 2-3mL. More preferably, the temperature of the glutaraldehyde crosslinking reaction is 45 to 55 ℃ and the time is 4 to 6 hours.
The secondary cross-linking type plant essential oil microcapsule is prepared by the preparation method.
The invention relates to an application of a secondary cross-linking type plant essential oil microcapsule in food preservation.
According to the invention, the aldehyde soybean polysaccharide and epsilon-polylysine are used as composite wall materials, and can play a synergistic bacteriostatic role with the antibacterial plant essential oil. The plant essential oil is fixedly embedded by adopting a secondary chemical crosslinking technology to form the microcapsule, so that the volatility of the plant essential oil can be effectively reduced, the stability of the plant essential oil is improved, particularly the slow release and bacteriostatic effects of the plant essential oil are enhanced, the antibacterial activity and the application range of the plant essential oil are enlarged, and meanwhile, a theoretical basis and a technical support can be provided for the commercial production of the green and safe bacteriostatic microcapsule.
Drawings
Fig. 1 is a graph showing the sustained-release effect of essential oil microcapsules prepared in example 1 of the present invention and a comparative example.
Detailed Description
The following further describes embodiments of the present invention with reference to specific examples. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples and test examples, the raw materials used in the respective examples were commercially available unless otherwise specified. In the following examples, the water-soluble soybean polysaccharides used were obtained from Shandong Riche Biotech Co., ltd; epsilon-polylysine is from New Yinxing bioengineering, inc. of Zhejiang; rosemary essential oil was obtained from Guangzhou Hengxin spices, inc.
In the following examples, the plant essential oil is rosemary essential oil, and the technical effects of the present invention are illustrated by taking rosemary essential oil as an example. In the following examples, the aldehyde soybean polysaccharide used was prepared by the following method: stirring and dissolving water-soluble soybean polysaccharide in 1% (v/v) acetic acid solution, preparing 0.01g/mL water-soluble soybean polysaccharide solution, then adding equal volume of 0.015g/mL sodium periodate aqueous solution, mixing, reacting at room temperature in a dark place for 3h, then adding ethylene glycol to terminate the reaction, decompressing and filtering, dissolving by using deionized water, precipitating by using ethanol again, filtering, and then vacuum-drying the product at 50 ℃ to obtain the aldehyde-group soybean polysaccharide.
Example 1
The preparation of the secondary cross-linking type plant essential oil microcapsule of the embodiment comprises the following specific steps:
1) Weighing 0.5g of aldehyde-based soybean polysaccharide, and completely dissolving the aldehyde-based soybean polysaccharide in 100mL of deionized water to obtain an aldehyde-based soybean polysaccharide solution with the concentration of 5 mg/mL;
2) Adding 5g of soybean lecithin and 2g of sodium alginate into the aldehyde soybean polysaccharide solution, mechanically stirring for 20min at the rotating speed of 60r/min, uniformly mixing, adding 0.10mL of rosemary essential oil, and homogenizing and emulsifying at high speed for 30min at the rotating speed of 11000r/min at room temperature to obtain uniform mixed emulsion;
3) Adding 50mL of epsilon-polylysine aqueous solution with the concentration of 0.03g/mL into the mixed emulsion obtained in the step 2), carrying out crosslinking reaction for 3h under the mechanical stirring condition of 250r/min at 30 ℃, then adding 3mL of glutaraldehyde solution with the mass fraction of 3%, and carrying out secondary crosslinking for 5h at 50 ℃.
4) And after crosslinking, centrifuging for 10min at the rotating speed of 10000r/min by using a centrifugal machine, washing by using deionized water, and freeze-drying to obtain the secondary crosslinking type plant essential oil microcapsule.
Example 2
The preparation method of the secondary cross-linking type plant essential oil microcapsule of the embodiment comprises the following specific steps:
1) Weighing 0.6g of aldehyde-based soybean polysaccharide, and completely dissolving the aldehyde-based soybean polysaccharide in 100mL of deionized water to obtain an aldehyde-based soybean polysaccharide solution with the concentration of 6 mg/mL;
2) Adding 6g of soybean lecithin and 1g of sodium alginate into the aldehyde soybean polysaccharide solution, mechanically stirring for 20min at the rotating speed of 50r/min, adding 0.12mL of rosemary essential oil after uniform mixing, and homogenizing and emulsifying at high speed at the rotating speed of 10000r/min for 40min at room temperature to obtain uniform mixed emulsion;
3) Adding 50mL of epsilon-polylysine aqueous solution with the concentration of 0.024g/mL into the mixed emulsion obtained in the step 2), carrying out crosslinking reaction for 2h under the mechanical stirring condition of 300r/min at 30 ℃, then adding 3mL of glutaraldehyde solution with the mass fraction of 3%, and carrying out secondary crosslinking for 6h at 45 ℃.
4) And after crosslinking, centrifuging for 10min at 10000r/min by using a centrifuge, washing by using deionized water, and freeze-drying to obtain the secondary crosslinking type plant essential oil microcapsule.
Example 3
The preparation of the secondary cross-linking type plant essential oil microcapsule of the embodiment comprises the following specific steps:
1) Weighing 0.4g of aldehyde-based soybean polysaccharide, and completely dissolving the aldehyde-based soybean polysaccharide in 100mL of deionized water to obtain an aldehyde-based soybean polysaccharide solution with the concentration of 4 mg/mL;
2) Adding 4g of soybean lecithin and 2g of sodium alginate into the aldehyde soybean polysaccharide solution, mechanically stirring for 20min at the rotating speed of 60r/min, adding 0.10mL of rosemary essential oil after uniformly mixing, and homogenizing and emulsifying at high speed at the rotating speed of 12000r/min for 30min at room temperature to obtain uniform mixed emulsion;
3) Adding 50mL of epsilon-polylysine aqueous solution with the concentration of 0.032g/mL into the mixed emulsion obtained in the step 2), carrying out crosslinking reaction for 3h under the mechanical stirring condition of 80r/min at 25 ℃, then adding 3mL of glutaraldehyde solution with the mass fraction of 3%, and carrying out secondary crosslinking for 5h at 55 ℃.
4) And after crosslinking, centrifuging for 10min at the rotating speed of 10000r/min by using a centrifugal machine, washing by using deionized water, and freeze-drying to obtain the secondary crosslinking type plant essential oil microcapsule.
Comparative example 1
The preparation of plant essential oil microcapsules of this comparative example, which is largely similar to example 1, differs mainly only in that: in step 2), the emulsifier combination of tween-80 (5 g) and glycerol (2 g) which is common in the field is adopted to replace the combination of the soybean lecithin and the sodium alginate.
Comparative example 2
The preparation of plant essential oil microcapsules of this comparative example, which is largely similar to example 1, differs mainly only in that: in the step 3), the common gelatin raw material in the prior art is adopted to replace epsilon-polylysine to carry out crosslinking with the aldehyde soybean polysaccharide, and other steps are the same.
Comparative example 3
The preparation of plant essential oil microcapsules of this comparative example is largely similar to that of example 1, and the main differences are only that: the step 3) is specifically as follows: 50mL of an aqueous solution of epsilon-polylysine with the concentration of 0.03g/mL is added into the mixed emulsion obtained in the step 2), and crosslinking reaction is carried out for 8 hours under the mechanical stirring condition of 30 ℃ and 250 r/min.
Experimental example 1 encapsulation efficiency measurement
The experimental method for determining the encapsulation efficiency is as follows: precisely weighing the microcapsules prepared in the examples 1 to 3 and the comparative examples 1 to 3, respectively, putting 0.1g of microcapsule sample into round bottom flasks filled with zeolite, adding 200mL of deionized water, connecting a volatile oil tester, heating to boil, stopping heating until the oil amount is not increased any more, and obtaining the weight of the volatile oil in the microcapsules according to a formula: encapsulation ratio (%) = (mass of essential oil in microcapsule/total amount of essential oil added at the time of preparation) × 100%, and the encapsulation ratio was calculated and the result was taken as an average of two parallel tests. The results are shown in Table 1.
TABLE 1 encapsulation efficiency test results of essential oil microcapsules obtained from different experimental groups
From the results in Table 1, it can be seen that the encapsulation efficiency is closely related to the emulsifier, the wall material and the crosslinking process. Under the condition that epsilon-polylysine is adopted to be crosslinked with the aldehyde soybean polysaccharide, if soybean lecithin and sodium alginate are adopted as the emulsifier and secondary crosslinking is carried out, the composite effect and the interaction degree of the wall material can be effectively improved, so that the embedding effect of the plant essential oil is improved.
Experimental example 2 measurement of sustained Release Performance
Taking rosemary essential oil with the same quality as a control group, uniformly paving the rosemary essential oil microcapsule and the essential oil microcapsules of the examples 1 and the comparative examples 1 to 3 on a culture dish, placing the culture dish in a room temperature environment, sampling for 10 days, 30 days and 60 days, measuring the quality of the essential oil in the microcapsules according to the method of the experimental example 1, and then according to a formula: the release rate of essential oil (%) = (the reduction amount of essential oil in the microcapsule/the amount of essential oil originally in the microcapsule) × 100%, the release rate of essential oil in example 1 and comparative examples 1 to 3 was calculated, the release rate of essential oil in the control group was the percentage of the ratio of the reduction amount of essential oil to the initial amount of essential oil, and the results were averaged in two parallel tests. The results are shown in FIG. 1.
As can be seen from FIG. 1, with the increase of the number of days of storage, both the essential oil control group and the microcapsule group contained plant essential oil were gradually released, and the release rate was gradually increased. After the plant essential oil microcapsule is stored for 60 days, the loss rate of the plant essential oil microcapsule is only 19.7 percent, while the loss rates of the plant essential oil microcapsule not embedded and the essential oil microcapsules of comparative examples 1 to 3 respectively reach 46.8 percent, 25.1 percent, 23.7 percent and 32.6 percent, which shows that the secondary cross-linking essential oil microcapsule of epsilon-polylysine and aldehyde soybean polysaccharide can effectively protect essential oil from the influence of the external environment, thereby improving the long-term action stability of the essential oil.
Experimental example 3 measurement of bacteriostatic Activity
And diluting the essential oil of the control group and the essential oil microcapsules of the examples 1 and the comparative examples 1 to 3 by adopting a proper amount of beef peptone culture medium to obtain the same concentration. Escherichia coli, staphylococcus and mould are taken as investigation strains, beef peptone culture medium is adopted to dilute the bacteria to proper concentration, 200 mu L of the bacteria liquid is dipped by a sterilized cotton swab and coated on the surface of a plate, the plate is continuously rotated to enable the bacteria liquid to be uniform, then diluted essential oil or microcapsule preparation is dipped by a drug sensitive paper sheet and clings to the middle of the plate culture medium inoculated with the bacteria liquid, the plate culture medium is marked and placed into a 37 ℃ incubator for culturing for 24 and 72 hours, the diameter of a bacteriostatic ring is measured and recorded by a cross method, the average value of two tests is taken for the diameter of the bacteriostatic ring, and the results are shown in tables 2 and 3.
TABLE 2 antibacterial Effect of different experimental groups after 24h
TABLE 3 bacteriostatic Effect of different experimental groups after 72h
As can be seen from tables 2 and 3, the diameters of the inhibition zones of the essential oil on different strains are reduced along with the prolongation of the inhibition time, and the inhibition effect is weakened. However, compared with the control group essential oil and the comparative example microcapsule, the plant essential oil microcapsule provided by the invention can obviously increase the diameter of the inhibition zone of escherichia coli, staphylococcus and mould, so that the plant essential oil microcapsule provided by the invention has stronger antibacterial activity to different strains, and after being coated by the cross-linked compound, the plant essential oil can be promoted to exert longer antibacterial performance.
Therefore, the preparation method of the secondary crosslinking plant essential oil microcapsule can expand the antibacterial activity and the sustained-release performance of the plant essential oil, and has wide application prospect in the fields of preparation and application of green and safe bacteriostatic microcapsules for food preservation.
Claims (6)
1. The preparation method of the secondary cross-linking type plant essential oil microcapsule is characterized by comprising the following steps:
1) Dissolving aldehyde soybean polysaccharide in water to obtain an aldehyde soybean polysaccharide solution with the concentration of 4-6 mg/mL;
2) Adding soybean lecithin and sodium alginate into the aldehyde soybean polysaccharide solution, mechanically stirring uniformly, then adding plant essential oil, and homogenizing and emulsifying at a high speed of 10000 to 12000r/min for 30 to 40min to obtain mixed emulsion;
3) Adding an aqueous solution of epsilon-polylysine into the mixed emulsion obtained in the step 2), performing crosslinking reaction for 2 to 3 hours at the temperature of 20 to 30 ℃ under the condition of mechanical stirring, and then adding a glutaraldehyde solution for continuous crosslinking;
4) Centrifuging, washing, freezing and drying after crosslinking to obtain secondary crosslinking type plant essential oil microcapsules;
wherein, the addition amount of the aldehyde group soybean polysaccharide solution is (4 to 6 g): (1 to 2g): 0.10 to 0.12mL per 100 mL; the mass ratio of the aldehyde soybean polysaccharide to the epsilon-polylysine is 1 (2 to 4);
in the step 1), the aldehyde-based soybean polysaccharide is obtained by oxidizing water-soluble soybean polysaccharide by using sodium periodate; sodium periodate is adopted to carry out oxidation treatment on water-soluble soybean polysaccharide, and the specific process is as follows: stirring and dissolving water-soluble soybean polysaccharide in 1% v/v acetic acid solution, preparing 0.01g/mL water-soluble soybean polysaccharide solution, then adding an equal volume of 0.015g/mL sodium periodate aqueous solution, mixing, reacting at room temperature in a dark place for 2-3 h, then adding ethylene glycol to terminate the reaction, filtering, and drying in vacuum to obtain aldehyde-group soybean polysaccharide;
in the step 3), the mass fraction of the glutaraldehyde solution is 2% -4%, and the volume is 2-3mL; the temperature of glutaraldehyde crosslinking reaction is 45 to 55 ℃, and the time is 4 to 6 hours.
2. The method for preparing a secondary cross-linking type plant essential oil microcapsule according to claim 1, wherein in the step 2), the plant essential oil is one of rosemary essential oil, lavender essential oil and lemon essential oil.
3. The preparation method of the secondary cross-linking plant essential oil microcapsule as claimed in claim 1, wherein in the step 2), the rotation speed of mechanical stirring is 50 to 80r/min.
4. The method for preparing the secondary cross-linking type plant essential oil microcapsule according to claim 1, wherein in the step 3), the rotation speed of mechanical stirring is 200 to 300r/min.
5. A secondary crosslinking type plant essential oil microcapsule, which is characterized by being prepared by the preparation method according to any one of claims 1 to 4.
6. Use of the secondary cross-linking plant essential oil microcapsule according to claim 5 for food preservation.
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| PCT/CN2022/139847 WO2024016581A1 (en) | 2022-07-20 | 2022-12-19 | Twice-cross-linked plant essential oil microcapsule, and preparation method therefor and use thereof |
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