CN113729037A - Plant fungus antibacterial agent, antibacterial film and preparation method thereof - Google Patents

Plant fungus antibacterial agent, antibacterial film and preparation method thereof Download PDF

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CN113729037A
CN113729037A CN202111146271.4A CN202111146271A CN113729037A CN 113729037 A CN113729037 A CN 113729037A CN 202111146271 A CN202111146271 A CN 202111146271A CN 113729037 A CN113729037 A CN 113729037A
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hydrotalcite
essential oil
oil
antibacterial agent
plant fungus
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CN113729037B (en
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王卓
侯欣慧
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/08—Magnoliopsida [dicotyledons]
    • A01N65/22—Lamiaceae or Labiatae [Mint family], e.g. thyme, rosemary, skullcap, selfheal, lavender, perilla, pennyroyal, peppermint or spearmint
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
    • C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
    • C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
    • C08K5/0058—Biocides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The invention relates to the field of antibacterial materials, and discloses a plant fungus antibacterial agent and an antibacterial film containing the same. The plant fungus antibacterial agent contains an essential oil-hydrotalcite nanosheet composite material, and the mass ratio of the hydrotalcite nanosheet to the essential oil to the surfactant in the composite material is 0.5-3: 3-10: 1.5-5. During preparation, firstly, dissolving essential oil in an aqueous solution containing a surfactant, and preparing the stable essential oil nano emulsion with the concentration of 8-28 mg/mL through high-pressure homogenization; and mixing the essential oil nano emulsion and the hydrotalcite nano sheets, stirring at normal temperature, centrifugally washing, and then suspending in deionized water to obtain a stable aqueous dispersion colloidal solution of the essential oil-hydrotalcite nano sheet composite material, namely the plant fungus antibacterial agent. The plant fungus antibacterial agent provided by the invention is green, safe and pollution-free to the environment, good in biocompatibility, simple in preparation method and stable in property, and the problems of plant fungus diseases and stored grain/feed mildew caused by plant fungi can be effectively solved by utilizing the plant fungus antibacterial agent to prepare the antifungal film.

Description

Plant fungus antibacterial agent, antibacterial film and preparation method thereof
Technical Field
The invention relates to the field of antibacterial materials, in particular to a plant fungus antibacterial agent and an antibacterial film containing the same.
Background
Plant fungal diseases caused by plant fungi and stored grain/feed mildew have been a major factor that limits the yield and quality of agricultural products. Taking the problem of grain storage as an example, with the increasing population of the world, the demand of agricultural products is increasing day by day, and the grain storage mildew caused by plant fungi causes huge economic loss. The grains are rich in various nutrient substances capable of enabling fungi to grow, and under the condition of a proper growth environment, the fungi can decompose the nutrient substances in the grains to cause the grains to go bad and rot, so that abnormal conditions such as discoloration, peculiar smell, heating, mildew and the like occur to the grains, and the quality of the grains is irretrievably deteriorated. Furthermore, fungal infestation can also produce mycotoxins which are strongly toxic and carcinogenic.
In the prevention and treatment work of plant fungal diseases and stored grain/feed mildew, the application of chemical pesticides and the addition of mildew inhibitors are the most widely applied and low-cost methods. At present, the chemical pesticides which are effective for plant fungal diseases caused by different fungi comprise carbendazim and thiophanate which take benzimidazole medicines as active ingredients, and tebuconazole and triadimefon which take triazole medicines as active ingredients; the mildew preventive used widely includes propionate, sorbate, benzoate, sodium diacetate and the like. However, these chemical pesticides and antifungal agents have problems in practical use, such as pungent odor, environmental damage, susceptibility to plant fungi, susceptibility to mold deterioration, and susceptibility to environmental impact.
Therefore, it is very necessary to develop a novel inorganic environment-friendly plant fungus antibacterial agent having a stronger and more stable control effect on plant fungal diseases and stored grain/feed mold.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a plant fungus antibacterial agent, an antibacterial film and a preparation method thereof.
In order to realize the purpose of the invention, the technical scheme of the invention is as follows:
in a first aspect, the invention provides a plant fungus antibacterial agent, which contains an essential oil-hydrotalcite nanosheet composite material, wherein the mass ratio of hydrotalcite nanosheets, essential oil and a surfactant in the essential oil-hydrotalcite nanosheet composite material is 0.5-3: 3-10: 1.5-5.
Further, the hydrotalcite nanosheet is a single-layer hydrotalcite nanosheet, the particle size is 40-60 nm, and the thickness is 1.5-2.5 nm; the hydrotalcite nano-sheet is selected from one or more of magnesium aluminum hydrotalcite, nickel aluminum hydrotalcite, zinc aluminum hydrotalcite, cobalt iron hydrotalcite, nickel iron hydrotalcite, zinc magnesium aluminum hydrotalcite, nickel zinc aluminum hydrotalcite and cobalt magnesium aluminum hydrotalcite nano-sheet.
Further, the essential oil is selected from one or more of origanum oil, cinnamon oil, clove oil, litsea cubeba oil, rose geranium oil, peppermint oil, patchouli oil, thyme oil, nutmeg oil, basil oil and mustard oil.
Further, the surfactant is selected from one or more of Tween type surfactant, lecithin, bovine serum albumin, span type surfactant and polyether surfactant.
Further, the particle size of the essential oil-hydrotalcite nanosheet composite material is 80-100 nm.
In a second aspect, the present invention provides a method for preparing the plant fungus antibacterial agent, comprising the following steps:
(1) dissolving essential oil in an aqueous solution containing a surfactant, and preparing a stable essential oil nano emulsion with the concentration of 8-28 mg/mL through high-pressure homogenization;
(2) and mixing the essential oil nano emulsion and the hydrotalcite nanosheet colloidal solution, stirring at normal temperature, centrifugally washing, and then suspending in deionized water to obtain a stable aqueous dispersion colloidal solution of the essential oil-hydrotalcite nanosheet composite material, namely the plant fungus antibacterial agent.
Preferably, in the essential oil-hydrotalcite nanosheet composite material, the mass ratio of the hydrotalcite nanosheets, the essential oil and the surfactant is 1:3: 3. Under the condition, the prepared water dispersible colloidal solution of the essential oil-hydrotalcite nano-sheet nano composite material has the best antibacterial effect. When the proportion of the essential oil is increased, the loading capacity of the essential oil is increased, and at the moment, the supporting effect of the hydrotalcite nano-sheets on the essential oil is reduced; when the proportion of essential oil is reduced, the effective inhibitory concentration of the plant fungus antibacterial agent is increased.
In a third aspect, the present invention provides a plant fungus antibacterial film containing the aforementioned plant fungus antibacterial agent of the present invention.
The content of the essential oil-hydrotalcite nanosheet composite material in the plant fungus antibacterial film is 0.40 mg/mL.
In a fourth aspect, the present invention provides a method for preparing the plant fungus antibacterial film, comprising the following steps:
(1) adding the plant fungus antibacterial agent into a polyvinyl alcohol solution, and adding a plasticizer to prepare a film forming solution;
(2) and standing the film forming solution until bubbles completely overflow, forming a film by adopting a tape casting method, and balancing in a dryer after uncovering the film to obtain the film.
Further, the plasticizer is glycerin.
Further, the volume using ratio of the plant fungus antibacterial agent to the polyvinyl alcohol solution to the plasticizer is 2:50: 0.5.
The concentration of the polyvinyl alcohol solution is preferably 50 mg/mL.
Further, standing the film-forming solution at room temperature for a period of time until bubbles completely overflow, forming a film on a glass plate by adopting a tape casting method, and balancing in a drier at 25 ℃ for 48 hours after film uncovering to obtain the film containing the plant fungus antibacterial agent.
The hydrotalcite is layered double hydroxide, and the single-layer hydrotalcite can be used as a carrier with excellent properties due to the advantages of increased specific surface area, increased dispersity in water and the like.
The "essential oil" according to the invention is an aromatic oily liquid obtained by hydro-distillation from plant material (whole tissue or seeds), usually a mixture of several components, such as active substances containing phenols, flavonoids, etc., having antibacterial properties.
The raw materials or reagents involved in the invention are all common commercial products, and the operations involved are all routine operations in the field unless otherwise specified.
The above-described preferred conditions may be combined with each other to obtain a specific embodiment, in accordance with common knowledge in the art.
The invention has the beneficial effects that:
the plant fungus antibacterial agent based on the essential oil and single-layer hydrotalcite nanocomposite provided by the invention can obviously improve the antifungal activity and the antibacterial stability of the essential oil and can obviously inhibit the growth of fungi at a lower concentration. In addition, the nano composite material can effectively improve the thermal stability of the essential oil. The plant fungus antibacterial agent is green, safe and pollution-free to the environment, good in biocompatibility, simple in preparation method and stable in property, and the problems of plant fungus diseases and stored grain/feed mildew caused by plant fungi can be effectively solved by utilizing the plant fungus antibacterial agent to prepare the antifungal film.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 is a schematic diagram of the process for preparing the plant fungal antimicrobial agent of the present invention;
FIG. 2 is a Zeta potential diagram of LDH, OEO and OEO/LDH;
FIG. 3 is an FTIR profile for LDH, OEO and OEO/LDH; wherein, (a) OEO/LDH, (b) LDH, (c) OEO;
FIG. 4 is a film sample of the antibacterial film of plant fungi;
FIG. 5 shows the growth inhibition rate of LDH, OEO and OEO/LDH with different concentrations on Fusarium graminearum;
FIG. 6 shows the growth inhibition rate of LDH, OEO and OEO/LDH with different concentrations on Aspergillus flavus;
FIG. 7 shows the growth inhibition rate of different concentrations of LDH, OEO and OEO/LDH on Fusarium moniliforme.
FIG. 8 is a graph showing the percentage reduction in the antibacterial effect of 0.08mg/mL OEO and OEO/LDH treated at 90 ℃ on Fusarium graminearum, Aspergillus flavus and Fusarium moniliforme compared to the percentage reduction in the antibacterial effect of OEO and OEO/LDH treated at 25 ℃.
FIG. 9 shows the inhibition of Fusarium graminearum by PVA membranes containing different concentrations of OEO, OEO/LDH.
FIG. 10 shows the inhibition of Fusarium moniliforme by PVA membranes containing different concentrations of OEO, OEO/LDH.
FIG. 11 shows the inhibition of Aspergillus flavus by PVA membranes containing different concentrations of OEO, OEO/LDH.
Detailed Description
In order that the above objects, features and advantages of the present invention may be more clearly understood, a solution of the present invention will be further described below. It should be noted that the embodiments of the present invention and features of the embodiments may be combined with each other without conflict.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those described herein; it is to be understood that the embodiments described in this specification are only some embodiments of the invention, and not all embodiments.
Preferred embodiments of the present invention will be described in detail with reference to the following examples. It is to be understood that the following examples are given for illustrative purposes only and are not intended to limit the scope of the present invention. Various modifications and alterations of this invention will become apparent to those skilled in the art without departing from the spirit and scope of this invention.
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Example 1: preparation of oregano oil/cobalt aluminum hydrotalcite nanosheet (OEO/LDH)
0.1764g of Co (NO)3)2·6H2O，0.1125g Al(NO3)3·9H2Dissolving O in 20mL of water to obtain solution A, dissolving 0.1173g of NaOH in 20mL of water to obtain solution B, and dissolving 0.04g of NaNO in 20mL of water35mL of formamide was dissolved in 15mL of water to prepare solution C.
And (3) rapidly and simultaneously adding the solution A and the solution B into the solution C in a water bath at the temperature of 80 ℃, and stirring for 20 min. Washing with deionized water, centrifuging for 3 times, and suspending in deionized water to obtain a colloidal solution of single-layer cobalt aluminum hydrotalcite nanosheet (LDH) which can be stably dispersed in water. The particle size of the single-layer cobalt-aluminum hydrotalcite nanosheet is 40-60 nm, and the thickness of the single-layer cobalt-aluminum hydrotalcite nanosheet is about 2 nm.
Dissolving oregano oil (OEO) in 1% Tween-80 aqueous solution, and homogenizing to obtain 10mg/mL oregano oil nanoemulsion.
Mixing the oregano oil nanoemulsion and the hydrotalcite nanosheet colloidal solution according to the mass ratio of 1:1, stirring at normal temperature for 12 hours, centrifugally washing, then suspending in deionized water, and fixing the volume to obtain the aqueous dispersion colloidal solution of OEO/LDH with the mass concentration of 25 mg/mL.
And centrifuging the prepared OEO/LDH water dispersible colloid solution, taking a supernatant to obtain OEO/LDH, and measuring and calculating by using an ultraviolet-visible spectrophotometer, wherein in the OEO/LDH obtained in the embodiment, the mass ratio of the oregano oil to the single-layer cobalt-aluminum hydrotalcite nanosheet to the tween-80 is 1:3: 3.
And (3) detecting the LDH, the OEO and the OEO/LDH by Zeta potential and FTIR, and evaluating the successful combination of the essential oil and the hydrotalcite nano-sheets. Zeta potential is shown in FIG. 2 and FTIR profile is shown in FIG. 3. As can be seen from FIG. 2, the Zeta potential of OEO/LDH decreased from 33.07mV to 21.16mV compared to LDH due to the loading of OEO. As can be seen from FIG. 3, characteristic peaks (809.53,2867.63, 2925.26 cm) of OEO-1) Characteristic peaks of tween-80 (2958.19, 1735.57, 1114.65 cm)-1) And LCharacteristic peak of DH (426.19 cm)-1) Both can be observed in FIG. 3(c), which means that OEO was successfully loaded onto LDH nanoplates with the aid of tween-80.
Example 2: preparation of origanum oil/cobalt aluminum hydrotalcite nanosheet (OEO/LDH) film
10g of polyvinyl alcohol (PVA) is weighed in 200mL of deionized water, heated to 95 ℃ until the PVA is dissolved, 1.985mL of glycerol is added as a plasticizer, and the oregano oil/cobalt aluminum hydrotalcite nanosheet (OEO/LDH) and the oregano oil (OEO) prepared in example 1 are respectively diluted to certain concentrations by the film forming solution. Standing the film-forming solution at room temperature for a period of time until bubbles completely overflow, forming a film on a glass plate with the specification of 20cm multiplied by 20cm by adopting a tape casting method, drying at 25 ℃ for 48h, and balancing in a drier at 25 ℃ for 48h after the film is uncovered to obtain films respectively containing OEO and OEO/LDH and having mass concentrations of 0, 0.1, 0.2, 0.3, 0.4 and 0.5 mg/mL. The film sample is shown in figure 4.
Example 3: growth rate method for detecting antifungal activity of OEO/LDH on fusarium graminearum, aspergillus flavus and fusarium moniliforme
Respectively diluting and plating the first generation strains of fusarium graminearum, aspergillus flavus and fusarium moniliforme on a flat plate, and carrying out primary culture on a potato glucose agar (PDA) culture medium. Culturing at 25 deg.C for 5 days, taking hypha with diameter of 5mm from edge position of the culture medium at central position of blank PDA culture medium, and culturing at 29 deg.C for 5 days to obtain twice-passaged Fusarium graminearum, Aspergillus flavus and Fusarium moniliforme.
Origanum oil (OEO), cobalt aluminum hydrotalcite nanosheets (LDH) prepared in example 1, and origanum oil/cobalt aluminum hydrotalcite nanosheets (OEO/LDH) prepared in example 1 were diluted with PDA medium to make antibacterial medium with concentration gradients of 0.02, 0.04, 0.06, 0.08, 0.10, 0.12mg/mL, respectively. And (3) taking fusarium graminearum, aspergillus flavus and fusarium moniliforme hyphae which are subcultured for 2 times at 5mm in the center of the culture medium, culturing for 84h at 28 ℃, and measuring the growth diameter change of the fusarium graminearum, aspergillus flavus and fusarium moniliforme hyphae.
FIG. 5 shows the growth inhibition rate of different concentrations of LDH, OEO and OEO/LDH on Fusarium graminearum, when the OEO concentration is 0.06mg/mL, the inhibition rate of OEO/LDH is already > 90%, and the inhibition rate of pure OEO is only about 70%.
FIG. 6 shows the growth inhibition rate of different concentrations of LDH, OEO and OEO/LDH on Aspergillus flavus, when the OEO concentration is 0.06mg/mL, the inhibition rate of OEO/LDH is about 40%, and the inhibition rate of pure OEO is about 30%.
FIG. 7 shows the inhibition rate of different concentrations of LDH, OEO and OEO/LDH on the growth of Fusarium moniliforme, when the concentration of OEO is 0.06mg/mL, the inhibition rate of OEO/LDH is about 90%, and the inhibition rate of pure OEO is about 70%.
Example 4: detection of thermal stability of OEO/LDH
The OEO, OEO/LDH prepared in example 1 was treated at 25 deg.C, 50 deg.C, 90 deg.C, 120 deg.C for 1h, respectively. Then, the culture medium was diluted with PDA medium to prepare an antibacterial medium having a concentration of 0.08 mg/mL. And (3) taking fusarium graminearum, aspergillus flavus and fusarium moniliforme hyphae which are subcultured for 2 times at 5mm in the center of the culture medium, culturing for 84h at 28 ℃, and measuring the growth diameter change of the fusarium graminearum, aspergillus flavus and fusarium moniliforme hyphae.
FIG. 8 shows the percent reduction in the antibacterial effect of 90 ℃ treated OEO and OEO/LDH versus 25 ℃ treated OEO and OEO/LDH on Fusarium graminearum, Aspergillus flavus, and Fusarium moniliforme. For fusarium graminearum, the OEO antibacterial effect is reduced by about 14%, and the OEO/LDH is reduced by about 2%; for aspergillus flavus, the OEO antibacterial effect is reduced by about 10%, and the OEO/LDH is reduced by about 6%; for fusarium moniliforme, the OEO antibacterial effect is reduced by about 16%, and the OEO/LDH is reduced by about 9%.
Example 5: detection of antibacterial Activity of PVA Membrane containing OEO/LDH
PVA films containing OEO and OEO/CoAl-LDH UNs were made into square pockets with sides of 4 cm. The wheat is soaked in the spore water solution containing 105 spores/mL overnight, taken out and dried. 3g of the above wheat was put into an inlet bag and cultured at 29 ℃ for 15 days. The wheat was removed from the pocket, placed in 50mL of sterile water containing sterile glass beads, and shaken at 29 ℃ for 1 h. The supernatant was diluted 100 times and applied to a plate. The plate was incubated at 29 ℃ for 3 days, and spore germination was observed.
FIG. 9 shows the inhibition of Fusarium graminearum spores by PVA membranes containing OEO and OEO/LDH. The results show that the PVA membrane pair containing OEO/LDH almost completely inhibited fungal growth at 0.4 mg/mL. The PVA film containing OEO cannot be completely inhibited at the same concentration.
FIG. 10 shows the inhibition rate of Fusarium moniliforme spores by PVA membranes containing OEO and OEO/LDH. The results show that the PVA membrane pair containing OEO/LDH almost completely inhibited fungal growth at 0.4 mg/mL. The PVA film containing OEO cannot be completely inhibited at the same concentration.
FIG. 11 shows the inhibition of Aspergillus flavus spores by PVA membranes containing OEO and OEO/LDH. The results show that the PVA membrane pair containing OEO/LDH almost completely inhibited fungal growth at 0.4 mg/mL. The PVA film containing OEO cannot be completely inhibited at the same concentration.
Example 6
This example differs from example 1 in that peppermint oil was used in place of oregano oil.
Example 7
The present embodiment is different from embodiment 1 in that a zinc-aluminum hydrotalcite nanosheet is used to replace a cobalt-aluminum hydrotalcite nanosheet therein.
Example 8
This example differs from example 1 in that tween-20 was used in place of tween-80.
Comparative example 1
This comparative example differs from example 1 in that no surfactant was added as an emulsifier during compounding. After stirring, centrifuging and other procedures in the same process, all essential oil is remained in the supernatant, and cannot be successfully compounded with the hydrotalcite nanosheets.
The foregoing are merely exemplary embodiments of the present invention, which enable those skilled in the art to understand or practice the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (10)

1. The plant fungus antibacterial agent is characterized by comprising an essential oil-hydrotalcite nanosheet composite material, wherein the mass ratio of hydrotalcite nanosheets, essential oil and a surfactant in the essential oil-hydrotalcite nanosheet composite material is 0.5-3: 3-10: 1.5-5.
2. The plant fungus antibacterial agent according to claim 1, wherein the hydrotalcite nanosheets are single-layer hydrotalcite nanosheets, having a particle size of 40-60 nm and a thickness of 1.5-2.5 nm; the hydrotalcite nano-sheet is selected from one or more of magnesium aluminum hydrotalcite, nickel aluminum hydrotalcite, zinc aluminum hydrotalcite, cobalt iron hydrotalcite, nickel iron hydrotalcite, zinc magnesium aluminum hydrotalcite, nickel zinc aluminum hydrotalcite and cobalt magnesium aluminum hydrotalcite nano-sheet.
3. The plant fungus antibacterial agent according to claim 1, wherein said essential oil is selected from one or more of oregano oil, cinnamon oil, clove oil, litsea cubeba oil, rose geranium oil, peppermint oil, patchouli oil, thyme oil, nutmeg oil, basil oil and mustard oil.
4. The plant fungus antibacterial agent according to claim 1, wherein the surfactant is one or more selected from the group consisting of tween-type surfactants, lecithin, bovine serum albumin, span-type surfactants, and polyether-type surfactants.
5. A plant fungus antibacterial agent according to any one of claims 1 to 4, wherein the particle size of the essential oil-hydrotalcite nanosheet composite is 80 to 100 nm.
6. A process for the preparation of a plant fungal antimicrobial according to any of claims 1 to 5, comprising the steps of:
(1) dissolving essential oil in an aqueous solution containing a surfactant, and preparing a stable essential oil nano emulsion with the concentration of 8-28 mg/mL through high-pressure homogenization;
(2) and mixing the essential oil nano emulsion and the hydrotalcite nanosheet colloidal solution, stirring at normal temperature, centrifugally washing, and then suspending in deionized water to obtain a stable aqueous dispersion colloidal solution of the essential oil-hydrotalcite nanosheet composite material, namely the plant fungus antibacterial agent.
7. The preparation method according to claim 6, wherein in the essential oil-hydrotalcite nanosheet composite material, the mass ratio of hydrotalcite nanosheet to essential oil to surfactant is 1:3: 3.
8. A plant fungus antibacterial film characterized by comprising the plant fungus antibacterial agent according to any one of claims 1 to 5.
9. The plant fungus antibacterial film according to claim 8, wherein the content of the essential oil-hydrotalcite nanosheet composite in the plant fungus antibacterial film is 0.40 mg/mL.
10. A method for preparing a plant fungus antibacterial film according to claim 8 or 9, characterized by comprising the steps of:
(1) adding the plant fungus antibacterial agent into a polyvinyl alcohol solution, and adding a plasticizer to prepare a film forming solution;
(2) and standing the film forming solution until bubbles completely overflow, forming a film by adopting a tape casting method, and balancing in a dryer after uncovering the film to obtain the film.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101909734A (en) * 2008-01-09 2010-12-08 阿克佐诺贝尔股份有限公司 Stable emulsion and process for preparing the same
CN102613176A (en) * 2012-03-06 2012-08-01 苏州百馥生化科技有限公司 Mildewproof spray
CN107082896A (en) * 2017-05-02 2017-08-22 上海海洋大学 A kind of intelligence colour developing antibacterial oxidation resistanct fresh-keeping method for manufacturing thin film

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101909734A (en) * 2008-01-09 2010-12-08 阿克佐诺贝尔股份有限公司 Stable emulsion and process for preparing the same
CN102613176A (en) * 2012-03-06 2012-08-01 苏州百馥生化科技有限公司 Mildewproof spray
CN107082896A (en) * 2017-05-02 2017-08-22 上海海洋大学 A kind of intelligence colour developing antibacterial oxidation resistanct fresh-keeping method for manufacturing thin film

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
ANDREA VELLUTI: "Initial screening for inhibitory activity of essential oils on growth of Fusarium verticillioides, F. proliferatum and F. graminearum on maize-based agar media", 《FOOD MICROBIOLOGY》 *
郑德，黄锐: "《热稳定剂的生产应用及进展》", 30 June 2011, 国防工业出版社 *

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