CN116406662B - Plant source mixed microemulsion and preparation method and application thereof - Google Patents
Plant source mixed microemulsion and preparation method and application thereof Download PDFInfo
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- CN116406662B CN116406662B CN202310394362.2A CN202310394362A CN116406662B CN 116406662 B CN116406662 B CN 116406662B CN 202310394362 A CN202310394362 A CN 202310394362A CN 116406662 B CN116406662 B CN 116406662B
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- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 123
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000593 microemulsion method Methods 0.000 title description 2
- 241000196324 Embryophyta Species 0.000 claims abstract description 34
- 239000004094 surface-active agent Substances 0.000 claims abstract description 31
- 239000004064 cosurfactant Substances 0.000 claims abstract description 27
- 235000008708 Morus alba Nutrition 0.000 claims abstract description 23
- 239000010634 clove oil Substances 0.000 claims abstract description 22
- 240000000249 Morus alba Species 0.000 claims abstract description 20
- 239000003921 oil Substances 0.000 claims abstract description 20
- 239000010676 star anise oil Substances 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims abstract description 16
- 229920000053 polysorbate 80 Polymers 0.000 claims abstract description 16
- 241000221662 Sclerotinia Species 0.000 claims abstract description 15
- 229920001214 Polysorbate 60 Polymers 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 10
- 241000218231 Moraceae Species 0.000 claims description 3
- 230000002265 prevention Effects 0.000 claims description 3
- 239000000575 pesticide Substances 0.000 abstract description 5
- 239000012071 phase Substances 0.000 description 19
- 238000010587 phase diagram Methods 0.000 description 17
- 239000000341 volatile oil Substances 0.000 description 15
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 13
- 239000002245 particle Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 150000002500 ions Chemical class 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- 239000000523 sample Substances 0.000 description 7
- 229920001213 Polysorbate 20 Polymers 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 239000000975 dye Substances 0.000 description 6
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- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 6
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000001045 blue dye Substances 0.000 description 5
- 238000004945 emulsification Methods 0.000 description 5
- 239000000839 emulsion Substances 0.000 description 5
- 235000011187 glycerol Nutrition 0.000 description 5
- 229960000907 methylthioninium chloride Drugs 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 240000007232 Illicium verum Species 0.000 description 4
- 235000008227 Illicium verum Nutrition 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 238000004817 gas chromatography Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
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- 201000010099 disease Diseases 0.000 description 3
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000011835 investigation Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 241000186146 Brevibacterium Species 0.000 description 2
- 208000033962 Fontaine progeroid syndrome Diseases 0.000 description 2
- 241000233866 Fungi Species 0.000 description 2
- 244000223014 Syzygium aromaticum Species 0.000 description 2
- 235000016639 Syzygium aromaticum Nutrition 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- FAMPSKZZVDUYOS-UHFFFAOYSA-N alpha-Caryophyllene Natural products CC1=CCC(C)(C)C=CCC(C)=CCC1 FAMPSKZZVDUYOS-UHFFFAOYSA-N 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 239000003899 bactericide agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 239000012470 diluted sample Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 238000003306 harvesting Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
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- 238000004949 mass spectrometry Methods 0.000 description 2
- 229960004063 propylene glycol Drugs 0.000 description 2
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- NPNUFJAVOOONJE-ZIAGYGMSSA-N β-(E)-Caryophyllene Chemical compound C1CC(C)=CCCC(=C)[C@H]2CC(C)(C)[C@@H]21 NPNUFJAVOOONJE-ZIAGYGMSSA-N 0.000 description 2
- FAMPSKZZVDUYOS-OWEBEESNSA-N (1e,4z,8e)-2,6,6,9-tetramethylcycloundeca-1,4,8-triene Chemical compound C\C1=C/CC(C)(C)\C=C/C\C(C)=C\CC1 FAMPSKZZVDUYOS-OWEBEESNSA-N 0.000 description 1
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- NVEQFIOZRFFVFW-UHFFFAOYSA-N 9-epi-beta-caryophyllene oxide Natural products C=C1CCC2OC2(C)CCC2C(C)(C)CC21 NVEQFIOZRFFVFW-UHFFFAOYSA-N 0.000 description 1
- 241001127714 Amomum Species 0.000 description 1
- 241000209134 Arundinaria Species 0.000 description 1
- 241001530056 Athelia rolfsii Species 0.000 description 1
- NPBVQXIMTZKSBA-UHFFFAOYSA-N Chavibetol Natural products COC1=CC=C(CC=C)C=C1O NPBVQXIMTZKSBA-UHFFFAOYSA-N 0.000 description 1
- 239000005770 Eugenol Substances 0.000 description 1
- 241000251953 Leucotrichia Species 0.000 description 1
- 241000322338 Loeseliastrum Species 0.000 description 1
- UVMRYBDEERADNV-UHFFFAOYSA-N Pseudoeugenol Natural products COC1=CC(C(C)=C)=CC=C1O UVMRYBDEERADNV-UHFFFAOYSA-N 0.000 description 1
- 239000010617 anise oil Substances 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- NPNUFJAVOOONJE-UHFFFAOYSA-N beta-cariophyllene Natural products C1CC(C)=CCCC(=C)C2CC(C)(C)C21 NPNUFJAVOOONJE-UHFFFAOYSA-N 0.000 description 1
- 229940117948 caryophyllene Drugs 0.000 description 1
- NPNUFJAVOOONJE-UONOGXRCSA-N caryophyllene Natural products C1CC(C)=CCCC(=C)[C@@H]2CC(C)(C)[C@@H]21 NPNUFJAVOOONJE-UONOGXRCSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
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- JBTHDAVBDKKSRW-UHFFFAOYSA-N chembl1552233 Chemical compound CC1=CC(C)=CC=C1N=NC1=C(O)C=CC2=CC=CC=C12 JBTHDAVBDKKSRW-UHFFFAOYSA-N 0.000 description 1
- 210000001072 colon Anatomy 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000004495 emulsifiable concentrate Substances 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229960002217 eugenol Drugs 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- QBNFBHXQESNSNP-UHFFFAOYSA-N humulene Natural products CC1=CC=CC(C)(C)CC=C(/C)CCC1 QBNFBHXQESNSNP-UHFFFAOYSA-N 0.000 description 1
- 230000001969 hypertrophic effect Effects 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000010494 opalescence Effects 0.000 description 1
- 230000003071 parasitic effect Effects 0.000 description 1
- 244000052769 pathogen Species 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000000361 pesticidal effect Effects 0.000 description 1
- 239000003090 pesticide formulation Substances 0.000 description 1
- 229920000136 polysorbate Polymers 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
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- 239000000725 suspension Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- RUVINXPYWBROJD-ONEGZZNKSA-N trans-anethole Chemical compound COC1=CC=C(\C=C\C)C=C1 RUVINXPYWBROJD-ONEGZZNKSA-N 0.000 description 1
Classifications
-
- 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
- A01N25/30—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 characterised by the surfactants
-
- 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
- A01N25/02—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 liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- 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
- 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]
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P3/00—Fungicides
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Plant Pathology (AREA)
- Environmental Sciences (AREA)
- Wood Science & Technology (AREA)
- Agronomy & Crop Science (AREA)
- Dentistry (AREA)
- Mycology (AREA)
- Pest Control & Pesticides (AREA)
- Microbiology (AREA)
- Chemical & Material Sciences (AREA)
- Biotechnology (AREA)
- Toxicology (AREA)
- Dispersion Chemistry (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Medicinal Preparation (AREA)
Abstract
The invention relates to the technical field of pesticide preparation, and particularly discloses a plant source mixed microemulsion, a preparation method and application thereof, wherein the mixed microemulsion is obtained by mixing a surfactant and a cosurfactant according to a mass ratio of 3:1, the surfactant is Tween-80 or Tween-60, the cosurfactant is absolute ethyl alcohol, and then the mixed microemulsion and an oil phase are mixed according to a mass ratio of 8-18:2 to obtain the plant source mixed microemulsion, wherein the oil phase is formed by mixing clove oil and star anise oil; the plant source mixed microemulsion prepared by the invention can effectively prevent and treat the mulberry sclerotinia.
Description
Technical Field
The invention relates to the technical field of pesticide preparation, in particular to a plant source mixed microemulsion, and a preparation method and application thereof.
Background
Microemulsions (microemulsions) are thermodynamically stable systems that are transparent or translucent in appearance, small and uniform in particle size, and are spontaneously formed by mixing an oil phase, an aqueous phase, a surfactant, and a cosurfactant in a certain ratio (Paul and Moulik, 1997). The microemulsion has low surface tension, can be spread rapidly after being sprayed on plant leaves, can form liquid crystal phase after water is evaporated, and can firmly adhere pesticides on leaf surfaces, so that the pesticide utilization rate is greatly improved. In addition, the microemulsion has very low surface tension, so that the resistance of capillaries in the epidermal tissue of the leaf blade can be overcome, the active ingredients can more easily permeate into the leaf blade, and the pesticide effect of the pesticide formulation can be improved.
Plant essential oils as natural effective substances extracted from plants, excellent antibacterial ability of many plant essential oils has been confirmed. Because of the characteristics of high efficiency, low toxicity, environmental friendliness and the like, the compound is often used as an active ingredient of a medicament, but because the compound is unstable in property, is easy to volatilize and is difficult to dissolve in water, the application range of the plant essential oil is limited. In order to increase the stability of the plant essential oil as a plant source bactericide, the plant essential oil can be prepared into a microemulsion form, so that the service life and the bactericidal effect of the plant source bactericide are prolonged.
The mulberry sclerotinia is generally three types, namely, the mulberry hypertrophic sclerotinia, the mulberry shrinking sclerotinia and the mulberry small-particle sclerotinia, and the pathogens are in turn sclerotinia leucotrichia, bai Jing cane fungus and calico. The disease mainly infects female flowers, green fruits and young shoots and tender buds of early-growing mulberry. Spores invade female flowers and are parasitic in the mulberry, so that a large amount of hyphae are generated, pulp is swollen, and the mulberry is milky white. The disease has strong disease condition, high epidemic frequency, easy expansion of infection and characteristic of outbreak in successive years, has great harm to the mulberry, especially the mulberry for fruit, and can seriously lead to no harvest of mulberry particles if not timely controlled, thus bringing huge economic loss to mulberry farmers. At present, the prevention and treatment effect on the mulberry sclerotinia is poor, and the normal harvest of the mulberry field is seriously influenced.
Disclosure of Invention
The invention provides a plant source mixed microemulsion capable of preventing and treating mulberries sclerotinia, and a preparation method and application thereof.
The invention provides a preparation method of a plant source mixed microemulsion, which is characterized by comprising the following steps:
s1, mixing a surfactant and a cosurfactant according to a mass ratio of 3:1 to obtain a mixed microemulsion;
the surfactant is Tween-80 or Tween-60;
the cosurfactant is absolute ethyl alcohol;
s2, mixing the mixed microemulsion with the oil phase according to a mass ratio of 8-18:2 to obtain a plant source mixed microemulsion;
the oil phase is formed by mixing clove oil and star anise oil.
Further, in S1, the surfactant is Tween-80.
Further, in S2, the mass ratio of the mixed microemulsion to the oil phase is 8:2.
Further, in S2, the mixed essential oil is formed by mixing clove oil and star anise oil according to a mass ratio of 2:1.
The invention also provides the plant source mixed microemulsion prepared by the method.
The invention also provides application of the plant source mixed microemulsion in preventing and treating the sclerotinia rot of mulberry.
Further, the mulberry sclerotinia is caused by sclerotium rolfsii.
Compared with the prior art, the invention has the beneficial effects that:
1. in the plant source mixed microemulsion prepared by the invention, tween-80 is used as a surfactant, the area of the formed microemulsion is obviously larger than that of Tween-60, and the emulsification effect is best; when the cosurfactant is absolute ethyl alcohol, the cosurfactant can be mutually dissolved with two plant essential oils (clove oil and star anise oil) at the same time, which indicates that the absolute ethyl alcohol can better reduce interfacial tension when being used as the cosurfactant, adjust the viscosity of the system, be beneficial to the formation of microemulsion intervals and meet the conditions for preparing mixed microemulsion.
2. The oil phase in the plant source mixed microemulsion is obtained by mixing clove oil and star anise oil according to the mass ratio of 2:1, and compared with the single use of the clove oil or the star anise oil, the oil phase prepared by mixing the clove oil and the star anise oil according to the mass ratio of 2:1 has the best control effect on the mulberry sclerotinia and plays a role in adding 1 to more than 2.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing chemical analysis of clove oil and star anise oil;
wherein, figure A is the total ion chromatogram of clove oil;
panel B is the total ion chromatogram of star anise oil.
FIG. 2 is a pseudo-ternary phase diagram of a microemulsion of Tween-80 (A), tween-60 (B), tween-20 (C);
wherein, the image A is a microemulsion pseudo ternary phase diagram of Tween-80;
FIG. B is a microemulsion pseudo-ternary phase diagram of Tween-60;
and the diagram C is a microemulsion pseudo-ternary phase diagram of Tween-20.
FIG. 3 is a pseudo-ternary phase diagram of microemulsions of different Km values;
wherein, the graph A is a microemulsion pseudo-ternary phase graph with Km value of 1:1;
FIG. B is a pseudo-ternary phase diagram of the microemulsion with the Km value of 2:1;
FIG. C is a pseudo-ternary phase diagram of the microemulsion with the Km value of 3:1;
and the graph D is a microemulsion pseudo-ternary phase diagram with the Km value of 4:1.
FIG. 4 is an external view of a clove microemulsion, an star anise microemulsion and a mixed microemulsion;
wherein, the appearance patterns of the clove microemulsion, the star anise microemulsion and the mixed microemulsion are sequentially shown from left to right.
Detailed Description
The following detailed description of specific embodiments of the invention is, but it should be understood that the invention is not limited to specific embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The experimental methods described in the examples of the present invention are conventional methods unless otherwise specified, and materials, reagents, etc. used in the examples described below are commercially available.
Example 1: a plant source mixed microemulsion and its preparation method and application are provided.
1. Material
1. Test materials
The main reagent comprises: star anise oil, clove oil (Shanghai derived leaf biology Co., ltd.); tween-80, tween-60, tween-20 (Colon Chemicals Co., ltd.); absolute ethanol, ethylene glycol, glycerol.
2. Experimental method
1. GC-MS analysis of essential oil components
(1) Star anise oil gas chromatography conditions:
an Shimadzu GCMS-QP2010 gas chromatograph-mass spectrometer is adopted; chromatographic column: rtx-5ms (30 m. Times.0.25 mm. Times.0.25 um); the temperature of the sample inlet is 250 ℃; carrier gas: helium (He); column flow rate: 1mL/min; sample injection amount is 0.2 mu L; the split ratio is 10:1; programming temperature: the initial column temperature was 60℃and maintained at 1min, and 5℃/min was raised to 240℃and maintained for 5min.
Star anise oil mass spectrometry conditions:
electron bombardment (EI) ion source, ionization energy: 70eV; ion source temperature: 230 ℃; interface temperature: 250 ℃; four-stage bar temperature: 150 ℃; mass scan range: 30-500 amu; searching a spectrum library: NIST08, the percentage content of each component was finally calculated using the peak area.
Clove oil gas chromatography conditions:
an Shimadzu GCMS-QP2010 gas chromatograph-mass spectrometer is adopted; chromatographic column: rtx-5ms (30 m. Times.0.25 mm. Times.0.25 um); the temperature of the sample inlet is 270 ℃; carrier gas: helium (He); column flow rate: 1mL/min; the sample injection amount is 1 mu L; the split ratio is 40:1; programming temperature: the initial column temperature was 70℃and maintained at 1min, and 5℃/min was raised to 190℃and maintained for 15min.
(2) Clove oil mass spectrometry conditions:
electron bombardment (EI) ion source, ionization energy: 70eV; ion source temperature: 230 ℃; interface temperature: 230 ℃; four-stage bar temperature: 150 ℃; mass scan range: 35-500 amu; searching a spectrum library: NIST08, the percentage content of each component was finally calculated using the peak area.
2. Preparation and optimization of plant source mixed microemulsion
In the process of preparing the plant source mixed microemulsion, the ratio of the components is the mass ratio.
(1) Preliminary screening of cosurfactants
1.0g of plant essential oil (clove oil and star anise oil) is respectively added into 5mL of EP pipe with scales, 3.0g of alternative reagent (absolute ethyl alcohol, 1, 2-propylene glycol, glycerol and glycerin) is respectively added into the EP pipe, the mixture is vibrated and evenly mixed by a high-speed vortex vibration instrument, and then the mixture is stood for observing the mixing condition, so that the proper cosurfactant is selected.
(2) Drawing of microemulsion pseudo-ternary phase diagram
Firstly fixing the ratio of an oil phase to a surfactant, then dropwise adding a water phase into the system to calculate the content of each component, and drawing a pseudo ternary phase diagram: according to the basic prescription of the screened microemulsion, mixing the surfactant and cosurfactant according to a certain mass ratio (Km) to prepare the mixed microemulsion (S) mix ). Uniformly mixing by using a magnetic stirrer, and mixing according to the mass ratio of the plant source mixed microemulsion to the oil phase of 9:1,8:2,7:3,6:4,5:5,4:6,3:7,2:8 and 1:9. Distilled water was then gradually added dropwise to the oil phase with stirring. And (5) observing the moment that the liquid system changes from clear to turbid or from turbid to clear in the dripping process by naked eyes, recording the water adding quantity of the critical point, and determining the limit of the micro-emulsion area.
The pseudo-ternary phase diagram is drawn by using Origin2021 software according to the mass percentage of each component at the critical point according to the three vertexes of the water phase, the oil phase and the mixed microemulsion (Smix) as the pseudo-ternary phase diagram.
(3) Selection of surfactants
And respectively preparing mixed microemulsions with Km=3:1 ratio by using Tween-80, tween-60 and Tween-20 as surfactants and cosurfactants (absolute ethyl alcohol), and drawing a pseudo-ternary phase diagram of the microemulsions by referring to the method.
(4) Selection of surfactant to cosurfactant ratio (Km)
Tween-80 is used as a surfactant, and absolute ethyl alcohol is used as a cosurfactant. Mixing according to a certain mass ratio (Km=4:1, 3:1,2:1, 1:1), and drawing a microemulsion pseudo-ternary phase diagram according to the method.
3. Basic property investigation of microemulsion
(1) Microemulsion appearance and type identification
After the microemulsion is prepared, whether the microemulsion developed according to the prescription is uniform, clear and still transparent or nearly transparent stable liquid system after diluted by distilled water is observed by naked eyes according to the standard. And the method can not be layered or demulsified and the like, and is regarded as qualified.
Identification of the microemulsion type by staining: two micro-emulsion samples with the same volume are sucked into a test tube, one drop of Sudan red IV dye solution and one drop of methylene blue dye solution are respectively dripped into the test tube, and the diffusion speed of the two dyes is observed. If the diffusion speed of the methylene blue dye in the microemulsion is greater than that of the Sudan IV dye, the prepared microemulsion is of O/W type, and if the diffusion speed of the Sudan IV dye is greater than that of the methylene blue dye, the prepared microemulsion is of W/O type.
(2) Particle size and distribution investigation of microemulsions
The particle size and distribution of the microemulsions were determined using a NanoBrook Omni nanosize analyzer. To avoid multiple scattering affecting the observations, the emulsions were each diluted 50-fold with water and then assayed.
4. Microemulsion stability detection
(1) Microemulsion stability detection
Emulsion stability detection is carried out by referring to a test method specified by the national standard of pesticide emulsifiable concentrates. Diluting a sample to be tested by using 342mg/L standard hard water, standing for 30min at 20 ℃, observing the appearance condition of the diluted sample, and if the diluted sample can be kept in a transparent state, has no solid sediment or oily suspension, and can be mixed with water under the condition of any proportion, judging that the emulsion is in a stable state.
(2) Microemulsion centrifugation stability detection
And (3) placing a proper amount of the microemulsion into a 2.5mL centrifuge tube, centrifuging at 4000r/min for 20min, and observing the color and appearance change of the microemulsion.
3. Analysis of results
1. Chemical composition analysis of clove oil and star anise oil
The components of oleum Caryophylli and oleum Anisi Stellati were analyzed by GC-MS technique, and the total ion chromatogram is shown in figure 1. The gas chromatography of clove oil totally detects 5 volatile components (figure 1, figure A), and the main components and the content are shown in table 1. The highest content of the components is three substances of eugenol (85.54%), caryophyllene (11.96%) and alpha-caryophyllene (2.34%), which account for 99.84% of the total amount. The volatile components 2 were detected by gas chromatography of star anise (see table 2), wherein the highest compound was trans-anethole (panel B of fig. 1) and found to be 99.98% of the total content.
TABLE 1 essential components of clove oil
TABLE 2 essential ingredients of Anise oil
2. Preparation and optimization of essential oil microemulsion
(1) Preliminary screening of cosurfactants
The cosurfactant in the microemulsion reduces the liquid level tension by adjusting the HLB value of the surfactant, thus forming the liquid level curvature required by the spherical molecules of the microemulsion, improving the interface fluidity and greatly improving the emulsification efficiency. The preferred test results of the present test using absolute ethanol, 1, 2-propanediol, glycerol, and glycerin as cosurfactants are shown in table 3. The results show that only the absolute ethyl alcohol can be mutually dissolved with two plant essential oils (clove oil and star anise oil) at the same time, so that the absolute ethyl alcohol can better reduce interfacial tension when being used as a cosurfactant, adjust the viscosity of a system, contribute to the formation of a microemulsion interval and meet the conditions for preparing mixed microemulsions. Absolute ethanol is therefore chosen as cosurfactant.
TABLE 3 dissolution of essential oils in solvents
(2) Selection of surfactants
Surfactants are one of the substances constituting the microemulsion, and promote the formation of the microemulsion by lowering the interfacial tension. Tween series surfactants are widely applied to the industrial fields of foods, cosmetics, medicines and the like due to the advantages of safety, small irritation, low price, remarkable emulsifying effect and the like. The test selects Tween-80, tween-60 and Tween-20 as study objects to select the better surfactant. The oil phase is prepared from mixed essential oil of star anise (mass ratio=2:1), and the cosurfactant is prepared from absolute ethanol. According to the above method, when km=3:1, a pseudo ternary phase diagram of the different surfactant microemulsions can be made (fig. 2). As can be seen from FIG. 2, tween-20 was unable to form effective areas of microemulsion in the system (panel C of FIG. 2), while Tween-80 formed areas of microemulsion that were larger than Tween-60 (panels A and B of FIG. 2). Therefore, tween-80 with the best emulsification effect is selected as the surfactant.
(3) Selection of surfactant to cosurfactant ratio (Km)
The ratio (Km) of surfactant to cosurfactant is critical to the preparation of the emulsion system, and in different emulsion systems, km values are also different, and the effect of microemulsion formation can be affected by the difference in Km ratio. According to the test, tween-80 with good emulsification effect is selected as a surfactant, absolute ethyl alcohol is used as a cosurfactant, the two surfactants are mixed according to the Km ratio of 1:1, 2:1, 3:1 and 4:1, a pseudo-ternary phase diagram of the microemulsion is drawn, and the influence of different Km values on the formation area of the microemulsion is examined.
As shown in fig. 3, as the Km ratio increases gradually, the area of the micro-emulsion region increases gradually, and the area of the micro-emulsion region reaches a maximum value by km=3:1, and then the area of the micro-emulsion region decreases. Indicating that the higher the surfactant ratio, the better the ability to form microemulsions in the presence of a certain amount of cosurfactant. And when Km exceeds 3:1, the area of the formed microemulsion decreases, probably due to the lack of co-emulsification of the co-surfactant at higher concentrations of surfactant, resulting in a decrease in the ability of the system to form a microemulsion. So km=3:1 is determined as the optimal Km value.
(4) Mixed microemulsion optimization
In the process of constructing a pseudo ternary phase diagram of the mixed microemulsion, the surfactant is Tween-80, the cosurfactant is absolute ethyl alcohol, and the ratio Km=3:1. When mixing microemulsions S mix : when the ratio of the oil phase is 9:1,8:2 and 7:3, the prepared mixed microemulsion is clear and transparent microemulsion, and when the ratio is lower than 7:3, the microemulsion system is unstable and turbidity is easy to generate. The essential oil microemulsion with the ratio of 9:1 to 8:2 has good stability, still presents a clear and transparent state after dilution, and shows good dilutability. Due to the consideration of the drug loading of the microemulsion, smix is finally selected: oil phase = 8:2 as the final mixed microemulsion formulation. The oil phase is selected from single star anise oil or clove oil, and in view of the prevention and treatment effect on the mulberry sclerotinia, the clove oil is preferred: the star anise oil is used as an oil phase according to the mass ratio of 2:1, the cup fungus of mulberry purchased from China center for type culture collection is selected, the collection number is CCTCC AF 2014019, and the bacteriostasis effect is shown in table 4.
TABLE 4 inhibition of Amomum star oil and clove oil formulations against Brevibacterium katsumadai
"ten" means bacterial growth and "one" means aseptic growth; MIC (MIC) A MIC (MIC) B MIC values of star anise oil and clove oil for Brevibacterium katsumadai are shown, respectively.
3. Determination of basic Properties of Mixed microemulsions
(1) Mixed microemulsion appearance and type identification
The microemulsion prepared according to the formula is shown in figure 4, and the prepared microemulsion is clear and transparent and has light blue opalescence. Meanwhile, after methylene blue dye and Sudan IV dye are added into the microemulsion in a dropwise manner, the diffusion speed of the methylene blue dye in the microemulsion is obviously higher than that of the Sudan IV dye, so that the microemulsion prepared by the test can be judged to belong to O/W type microemulsion.
(2) Particle size and distribution investigation of mixed microemulsions
The average particle diameters and distribution of the three microemulsions were measured by a laser particle sizer, and the results are shown in table 5. The particle size of the three essential oil microemulsions is smaller than 100nm, the dispersion degree of the particle size distribution is small, and the definition of the microemulsions is met.
TABLE 5 particle size and distribution of microemulsions
(2) Microemulsion stability detection
The microemulsion is diluted 10 times and 100 times, and the diluted microemulsion still presents a clear and transparent state and shows good dilutability.
(3) Microemulsion stability detection
After the tested sample is centrifuged for 20min under the condition of 4000r/min, the sample is sampled and observed, the appearance of all the samples is transparent and uniform, no layering phenomenon occurs, and the result shows that the microemulsion has better stability.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (5)
1. The preparation method of the plant source mixed microemulsion is characterized by comprising the following steps:
s1, mixing a surfactant and a cosurfactant according to a mass ratio of 3:1 to obtain a mixed microemulsion;
the surfactant is Tween-80 or Tween-60;
the cosurfactant is absolute ethyl alcohol;
s2, mixing the mixed microemulsion with an oil phase according to a mass ratio of 9:1 or 8:2 to obtain a plant source mixed microemulsion;
the oil phase is formed by mixing clove oil and star anise oil according to the mass ratio of 2:1.
2. The method for preparing a plant-derived mixed microemulsion according to claim 1, wherein in S1, said surfactant is Tween-80.
3. A plant-derived hybrid microemulsion prepared by the preparation method of claims 1-2.
4. Use of the plant-derived mixed microemulsion of claim 3 in the prevention and treatment of mulberry sclerotinia.
5. The use of a plant-derived mixed microemulsion according to claim 4 for the control of mulberries sclerotinia, wherein said mulberries sclerotinia is caused by sclerotiorum.
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