CN119014403B - A nano pesticide preparation and its application - Google Patents
A nano pesticide preparation and its application Download PDFInfo
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- CN119014403B CN119014403B CN202411514081.7A CN202411514081A CN119014403B CN 119014403 B CN119014403 B CN 119014403B CN 202411514081 A CN202411514081 A CN 202411514081A CN 119014403 B CN119014403 B CN 119014403B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000575 pesticide Substances 0.000 title abstract description 48
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000000839 emulsion Substances 0.000 claims abstract description 25
- 239000012074 organic phase Substances 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229920001577 copolymer Polymers 0.000 claims abstract description 16
- 239000008346 aqueous phase Substances 0.000 claims abstract description 15
- 229920001213 Polysorbate 20 Polymers 0.000 claims abstract description 12
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims abstract description 12
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims abstract description 12
- 239000005457 ice water Substances 0.000 claims abstract description 10
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 10
- 244000068988 Glycine max Species 0.000 claims abstract description 9
- 235000010469 Glycine max Nutrition 0.000 claims abstract description 9
- 241000221662 Sclerotinia Species 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 7
- 239000005878 Azadirachtin Substances 0.000 claims abstract 5
- VEHPJKVTJQSSKL-UHFFFAOYSA-N azadirachtin Natural products O1C2(C)C(C3(C=COC3O3)O)CC3C21C1(C)C(O)C(OCC2(OC(C)=O)C(CC3OC(=O)C(C)=CC)OC(C)=O)C2C32COC(C(=O)OC)(O)C12 VEHPJKVTJQSSKL-UHFFFAOYSA-N 0.000 claims abstract 5
- FTNJWQUOZFUQQJ-IRYYUVNJSA-N azadirachtin A Natural products C([C@@H]([C@]1(C=CO[C@H]1O1)O)[C@]2(C)O3)[C@H]1[C@]23[C@]1(C)[C@H](O)[C@H](OC[C@@]2([C@@H](C[C@@H]3OC(=O)C(\C)=C/C)OC(C)=O)C(=O)OC)[C@@H]2[C@]32CO[C@@](C(=O)OC)(O)[C@@H]12 FTNJWQUOZFUQQJ-IRYYUVNJSA-N 0.000 claims abstract 5
- FTNJWQUOZFUQQJ-NDAWSKJSSA-N azadirachtin A Chemical compound C([C@@H]([C@]1(C=CO[C@H]1O1)O)[C@]2(C)O3)[C@H]1[C@]23[C@]1(C)[C@H](O)[C@H](OC[C@@]2([C@@H](C[C@@H]3OC(=O)C(\C)=C\C)OC(C)=O)C(=O)OC)[C@@H]2[C@]32CO[C@@](C(=O)OC)(O)[C@@H]12 FTNJWQUOZFUQQJ-NDAWSKJSSA-N 0.000 claims abstract 5
- 241000221696 Sclerotinia sclerotiorum Species 0.000 claims description 14
- 201000010099 disease Diseases 0.000 claims description 5
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 claims description 5
- 239000003112 inhibitor Substances 0.000 claims description 2
- IMOLAGKJZFODRK-UHFFFAOYSA-N 2-phenylprop-2-enamide Chemical compound NC(=O)C(=C)C1=CC=CC=C1 IMOLAGKJZFODRK-UHFFFAOYSA-N 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 8
- 230000004071 biological effect Effects 0.000 abstract description 6
- 239000002105 nanoparticle Substances 0.000 description 22
- 240000000233 Melia azedarach Species 0.000 description 18
- 241000196324 Embryophyta Species 0.000 description 16
- 239000003090 pesticide formulation Substances 0.000 description 15
- 239000000284 extract Substances 0.000 description 14
- 239000003264 margarine Substances 0.000 description 12
- 235000013310 margarine Nutrition 0.000 description 12
- 239000004480 active ingredient Substances 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 10
- 235000013399 edible fruits Nutrition 0.000 description 9
- 239000012071 phase Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000003814 drug Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 230000000844 anti-bacterial effect Effects 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 238000001704 evaporation Methods 0.000 description 7
- 239000003960 organic solvent Substances 0.000 description 7
- 239000002245 particle Substances 0.000 description 7
- 239000008363 phosphate buffer Substances 0.000 description 7
- 239000004094 surface-active agent Substances 0.000 description 7
- NAHTXVIXCMUDLF-RFNFAWMESA-N toosendanin Chemical compound C=1([C@H]2[C@]3(C)[C@@H](OC(C)=O)C(=O)[C@H]4[C@@]([C@@]53O[C@@H]5C2)(C)[C@H](O)C[C@H]2[C@@]3(C)[C@H](O)OC[C@]24[C@@H](O)C[C@H]3OC(=O)C)C=COC=1 NAHTXVIXCMUDLF-RFNFAWMESA-N 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- NAHTXVIXCMUDLF-DUJPAFNYSA-N Toosendanin Natural products O=C(O[C@H]1C(=O)[C@H]2[C@@](C)([C@H](O)C[C@H]3[C@@]4(C)[C@H](O)OC[C@@]23[C@@H](O)C[C@H]4OC(=O)C)[C@@]23[C@]1(C)[C@H](c1cocc1)C[C@H]2O3)C NAHTXVIXCMUDLF-DUJPAFNYSA-N 0.000 description 6
- 239000008488 toosendanin Substances 0.000 description 6
- RYNDYESLUKWOEE-UHFFFAOYSA-N 2-benzylprop-2-enoic acid Chemical compound OC(=O)C(=C)CC1=CC=CC=C1 RYNDYESLUKWOEE-UHFFFAOYSA-N 0.000 description 5
- RIOXQFHNBCKOKP-UHFFFAOYSA-N benomyl Chemical compound C1=CC=C2N(C(=O)NCCCC)C(NC(=O)OC)=NC2=C1 RIOXQFHNBCKOKP-UHFFFAOYSA-N 0.000 description 5
- MITFXPHMIHQXPI-UHFFFAOYSA-N benzoxaprofen Natural products N=1C2=CC(C(C(O)=O)C)=CC=C2OC=1C1=CC=C(Cl)C=C1 MITFXPHMIHQXPI-UHFFFAOYSA-N 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 230000001988 toxicity Effects 0.000 description 5
- 231100000419 toxicity Toxicity 0.000 description 5
- 241000233866 Fungi Species 0.000 description 4
- 241000607479 Yersinia pestis Species 0.000 description 4
- XDROKJSWHURZGO-UHFFFAOYSA-N angelicin Chemical compound C1=C2OC=CC2=C2OC(=O)C=CC2=C1 XDROKJSWHURZGO-UHFFFAOYSA-N 0.000 description 4
- 241000238631 Hexapoda Species 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007709 nanocrystallization Methods 0.000 description 3
- 230000002265 prevention Effects 0.000 description 3
- 230000001954 sterilising effect Effects 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- 239000005592 Penoxsulam Substances 0.000 description 2
- SYJGKVOENHZYMQ-UHFFFAOYSA-N Penoxsulam Chemical compound N1=C2C(OC)=CN=C(OC)N2N=C1NS(=O)(=O)C1=C(OCC(F)F)C=CC=C1C(F)(F)F SYJGKVOENHZYMQ-UHFFFAOYSA-N 0.000 description 2
- 239000003899 bactericide agent Substances 0.000 description 2
- 210000000170 cell membrane Anatomy 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001493 electron microscopy Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- WBYWAXJHAXSJNI-UHFFFAOYSA-N methyl p-hydroxycinnamate Natural products OC(=O)C=CC1=CC=CC=C1 WBYWAXJHAXSJNI-UHFFFAOYSA-N 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000006272 natural pesticide Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000001782 photodegradation Methods 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- MLMVLVJMKDPYBM-UHFFFAOYSA-N pseudoisopsoralene Natural products C1=C2C=COC2=C2OC(=O)C=CC2=C1 MLMVLVJMKDPYBM-UHFFFAOYSA-N 0.000 description 2
- ZCCUUQDIBDJBTK-UHFFFAOYSA-N psoralen Chemical compound C1=C2OC(=O)C=CC2=CC2=C1OC=C2 ZCCUUQDIBDJBTK-UHFFFAOYSA-N 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- WBYWAXJHAXSJNI-VOTSOKGWSA-N trans-cinnamic acid Chemical compound OC(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-N 0.000 description 2
- 230000001018 virulence Effects 0.000 description 2
- VXGRJERITKFWPL-UHFFFAOYSA-N 4',5'-Dihydropsoralen Natural products C1=C2OC(=O)C=CC2=CC2=C1OCC2 VXGRJERITKFWPL-UHFFFAOYSA-N 0.000 description 1
- LFYJSSARVMHQJB-UHFFFAOYSA-N Backuchiol Natural products CC(C)=CCCC(C)(C=C)C=CC1=CC=C(O)C=C1 LFYJSSARVMHQJB-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000222120 Candida <Saccharomycetales> Species 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 208000030852 Parasitic disease Diseases 0.000 description 1
- 239000005814 Pencycuron Substances 0.000 description 1
- 241001446509 Psoralea Species 0.000 description 1
- 241000235006 Torulaspora Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000008485 antagonism Effects 0.000 description 1
- LFYJSSARVMHQJB-GOSISDBHSA-N bakuchinol Natural products CC(C)=CCC[C@@](C)(C=C)C=CC1=CC=C(O)C=C1 LFYJSSARVMHQJB-GOSISDBHSA-N 0.000 description 1
- LFYJSSARVMHQJB-QIXNEVBVSA-N bakuchiol Chemical compound CC(C)=CCC[C@@](C)(C=C)\C=C\C1=CC=C(O)C=C1 LFYJSSARVMHQJB-QIXNEVBVSA-N 0.000 description 1
- 229940117895 bakuchiol Drugs 0.000 description 1
- KXXXNMZPAJTCQY-UHFFFAOYSA-N bakuchiol Natural products CC(C)CCCC(C)(C=C)C=Cc1ccc(O)cc1 KXXXNMZPAJTCQY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- -1 benzyl acrylic ketone Chemical class 0.000 description 1
- 238000004166 bioassay Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003640 drug residue Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 230000000749 insecticidal effect Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000002539 nanocarrier Substances 0.000 description 1
- 150000007523 nucleic acids Chemical class 0.000 description 1
- 102000039446 nucleic acids Human genes 0.000 description 1
- 108020004707 nucleic acids Proteins 0.000 description 1
- OGYFATSSENRIKG-UHFFFAOYSA-N pencycuron Chemical compound C1=CC(Cl)=CC=C1CN(C(=O)NC=1C=CC=CC=1)C1CCCC1 OGYFATSSENRIKG-UHFFFAOYSA-N 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 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
- A01N25/26—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 in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
-
- 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
- A01N25/10—Macromolecular compounds
-
- 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
- A01N35/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
- A01N35/04—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical containing aldehyde or keto groups, or thio analogues thereof, directly attached to an aromatic ring system, e.g. acetophenone; Derivatives thereof, e.g. acetals
-
- 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Plant Pathology (AREA)
- Environmental Sciences (AREA)
- Zoology (AREA)
- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Nanotechnology (AREA)
- Toxicology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Physics & Mathematics (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Pharmacology & Pharmacy (AREA)
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- General Engineering & Computer Science (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
本发明公开了一种纳米农药制剂及其应用，属于农药的技术领域。所述纳米农药制剂由以下方法制备而成：将苦楝素和苯丙烯菌酮加入乙醇中，而后加入聚乳酸‑羟基乙酸共聚物，搅拌均匀，得到有机相；将Tween 20溶于水中，得到水相；在冰水浴条件下，将有机相逐滴加入水相中，高速搅拌30‑45min，得到乳液，旋蒸去除乙醇，洗涤，冷冻干燥，得到纳米农药制剂。本发明通过纳米化将苦楝素和苯丙烯菌酮有效结合，显著提高了苦楝素和苯丙烯菌酮的生物活性和利用率，减少农药的用量，提高了对大豆菌核病的防治效果。
The invention discloses a nano pesticide preparation and its application, and belongs to the technical field of pesticides. The nano pesticide preparation is prepared by the following method: adding azadirachtin and fenpropicyclopentyl to ethanol, and then adding polylactic acid-glycolic acid copolymer, stirring evenly, and obtaining an organic phase; dissolving Tween 20 in water to obtain an aqueous phase; under ice-water bath conditions, the organic phase is added dropwise to the aqueous phase, and stirred at high speed for 30-45min to obtain an emulsion, and ethanol is removed by rotary evaporation, washed, and freeze-dried to obtain a nano pesticide preparation. The present invention effectively combines azadirachtin and fenpropicyclopentyl through nano-ization, significantly improves the biological activity and utilization rate of azadirachtin and fenpropicyclopentyl, reduces the dosage of pesticides, and improves the control effect of soybean sclerotinia.
Description
Technical Field
The invention relates to the technical field of pesticides, in particular to a nano pesticide preparation and application thereof.
Background
The pesticide plays an important role in preventing and controlling crop diseases, insect pests and grass damage, and can ensure the normal growth of crops, improve the yield and the like. Chemical pesticides are mainly used in the market at present, but the long-term use of the chemical pesticides inevitably causes pressure on the environment, damages natural balance and causes serious threat to human health and life. In addition, some pests have developed resistance to chemical pesticides over long periods of time, which not only does not achieve the control objective but even makes some pests more rampant.
The plant bactericide comprises plant itself with antibacterial ability or antibacterial active ingredient obtained from plant, and can be made into pesticide. Compared with chemical pesticides, the botanical pesticide has the characteristics of easy degradation, safety to non-target organisms, difficult generation of resistance to harmful organisms, special action mode, multiple development ways, multiple types and the like. Fructus Psoraleae is annual herb, and fructus Psoraleae seed is rich in effective active ingredients such as isopsoralen, psoralen and bakuchiol. The benomyl is a pesticide name of isopsoralen, is an effective antibacterial active ingredient extracted from psoralea seed of leguminous plants, is a novel plant source bactericide which is newly and independently created and developed in China, has the characteristics of broad-spectrum sterilization, immunity induction resistance, growth promotion and the like, meets the requirements of green prevention and control, is green, and is environment-friendly and free of residues. Chinaberry is widely used in traditional agriculture in India, southeast Asia, africa, etc. in ancient times, i.e. for the treatment of digestive tract parasitic diseases, and its leaves, seeds, bark and fruits are often used as natural pesticides to control plant diseases and insect pests. The active ingredients in the chinaberry mainly comprise chinaberry extract, chinaberry acid, chinaberry ketone and the like, and the compounds have multiple biological activities, especially the chinaberry extract has outstanding insecticidal and antibacterial aspects.
In the prior art, although the chinaberry extract and the benpropenone respectively show remarkable biological activities, such as broad-spectrum sterilization, disease inhibition, insect expelling and the like, no pesticide product is available for compounding the chinaberry extract and the benpropenone. In addition, most of plant-derived pesticides are easy to photodegradation, non-biological oxidation or loss through volatilization, and compared with chemical pesticides, the plant-derived pesticides have the defects of poor stability and easy decomposition, so that the application of the plant-derived pesticides in production is restricted. Nanotechnology is widely applied to various disciplines as one of the key technologies in the 21 st century, and along with the continuous development of nanotechnology, the development of nano preparation is also receiving more and more attention from students at home and abroad. The nano medicine carrying system developed based on nano carrier can change the medicine releasing rate, change medicine administration path and lower medicine toxic side effect, so that the medicine utilization rate is raised. Therefore, the combination of the nano technology and the plant pesticide has important significance for improving the stability of the plant pesticide, enhancing the biological activity and prolonging the lasting period.
Disclosure of Invention
Aiming at the prior art, the invention aims to provide a nano pesticide preparation and application thereof.
In order to achieve the above purpose, the invention adopts the following technical scheme:
In a first aspect of the present invention, there is provided a nano pesticide formulation prepared by the method of:
(1) Adding the chinaberry fruit extract and the fenpropione into ethanol, then adding polylactic acid-glycolic acid copolymer (PLGA), and uniformly stirring to obtain an organic phase;
(2) Dissolving Tween 20 in water to obtain a water phase;
(3) Under the ice water bath condition, the organic phase is added into the water phase drop by drop, the mixture is stirred for 30 to 45 minutes at high speed to obtain emulsion, ethanol is removed by rotary evaporation, and the emulsion is washed and freeze-dried to obtain the nano pesticide preparation.
Preferably, in the step (1), the ratio of the addition amount of the toosendanin, the pencycuron and the ethanol is (1-10) mg to 1mg (15-25) mL.
Preferably, in the step (1), the ratio of the addition amount of the polylactic acid-glycolic acid copolymer (PLGA) to ethanol is (5-27.5) mg (15-25) mL.
Preferably, in the step (2), the mass concentration of Tween 20 in the aqueous phase is 0.2% -1%.
Preferably, in step (3), the volume ratio of the organic phase to the aqueous phase is 1 (3-10).
Preferably, in the step (3), the dropping speed is 1-2 mL/min and the stirring speed is 1000-1500rpm.
In a second aspect of the invention, there is provided the use of a nano pesticide formulation as described above in the preparation of a sclerotinia inhibitor.
In a third aspect of the present invention, there is provided the use of the above-described nano-pesticide formulation for the preparation of a product for controlling sclerotinia rot of soybean, said sclerotinia rot being caused by sclerotinia sclerotiorum.
The invention has the beneficial effects that:
1. The invention combines the chinaberry extract and the penoxsulam effectively through nanocrystallization, which obviously improves the biological activity and the utilization rate of the chinaberry extract and the penoxsulam extract, reduces the dosage of pesticides and improves the prevention and treatment effect on soybean sclerotinia.
2. The invention combines the margarine and the benpropenone which are plant source natural pesticides, wherein the margarine and the benpropenone inhibit fungi mainly through the ways of interfering the cell membrane, the enzyme activity, the propagation process and the like of the fungi, the benpropenone acts through inhibiting the electron transfer chain, damaging the cell membrane and inhibiting the synthesis of nucleic acid, and after the combination, the two ways of action are different, and can jointly act on a plurality of metabolic links of the fungi, thereby obviously improving the sterilization effect on the fungi.
3. According to the invention, through nanocrystallization, the high specific surface area of the nano particles can enable the effective components to be more uniformly distributed in a target area, so that the loss and the residue of the medicine are reduced, the polylactic acid-glycolic acid copolymer (PLGA) is used as a carrier, the polylactic acid-glycolic acid copolymer (PLGA) has good biodegradability, can not cause persistent chemical pollution in soil, meets the requirements of environmental protection in modern agriculture, and meanwhile, the nano pesticide coated by the polylactic acid-glycolic acid copolymer (PLGA) can slowly release the effective components, so that the duration of the preparation is prolonged, the frequent medicine application requirement is reduced, and the labor cost of farmers is reduced.
Drawings
FIG. 1 is a photograph of the nano pesticide formulation prepared in example 2 at a resolution of 400 nm by electron microscopy;
FIG. 2 is a photograph of the nano pesticide formulation prepared in example 2 at a resolution of 4 μm by electron microscopy.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the application. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
As described in the background art, the plant-derived pesticide has the characteristics of easy degradation, safety to non-target organisms, difficult generation of resistance to harmful organisms, special action mode, multiple development ways, multiple types and the like compared with the chemical pesticide, but the plant-derived pesticide is easy to photodegradation, non-biological oxidation or loss through volatilization, and compared with the chemical pesticide, the plant-derived pesticide has the defects of poor stability and easy decomposition, so that the application of the plant-derived pesticide in production is restricted.
Based on the advantages of the botanical pesticide and the nano technology, the invention provides a nano pesticide preparation, which not only remarkably improves the bioactivity and the utilization rate of the chinaberry fruit and the fenpropidone, but also effectively solves the problems of poor stability and easy degradation of the botanical pesticide, the preparation has prolonged efficacy, enhanced stability, reduced drug residue and environmental pollution, meets the requirements of green, environment-friendly and sustainable development of modern agriculture, and has obvious effect and potential proved by the application in preventing and treating soybean sclerotinia, thereby having wide application prospect.
In order to enable those skilled in the art to more clearly understand the technical scheme of the present application, the technical scheme of the present application will be described in detail with reference to specific embodiments.
The test materials used in the examples of the present invention are all conventional in the art and are commercially available.
The strain number of the sclerotinia sclerotiorum (Sclerotinia sclerotiorum) used in the invention is CGMCC 3.7083, and the sclerotinia sclerotiorum is purchased from the common microorganism center of China Committee for culture Collection of microorganisms.
The polylactic acid-glycolic acid copolymer (PLGA) used in the present invention is purchased from Shandong Xinfu industries, inc., and has a product model number of B6029-1.
The margarine used in the invention is purchased from Hubei Weissen chemical reagent Co., ltd., CAS number 58812-37-6, and the content of the effective components is 95%.
The phenylacrylic acid mycoketone used in the invention is purchased from Shenyang homoauspicious biological pesticide Co., ltd, CAS accession number is 20784-50-3, and the mass fraction of the phenylacrylic acid mycoketone is 1.5%.
Example 1 preparation of nano pesticide formulation:
(1) Weighing 1mg of chinaberry fruit extract and 1mg of benzyl acrylic acid mycoketone, adding into 20mL of ethanol, adding 5mg of polylactic acid-glycolic acid copolymer (PLGA), and stirring at normal temperature until the solution is uniform to obtain an organic phase;
(2) 0.5g Tween 20 was dissolved in 100mL deionized water to give a water phase;
(3) Dropwise adding an organic phase into an aqueous phase at a speed of 1.5mL/min under ice water bath conditions, stirring at a speed of 1200rpm for 40 minutes to form an emulsion, transferring the emulsion into a rotary evaporator, slowly evaporating ethanol at 30 ℃ through rotary evaporation until the organic solvent is completely volatilized, and gradually wrapping the margarine and the fenpropione by PLGA along with the volatilization of the ethanol to form nano pesticide particles;
(4) The emulsion was ultracentrifuged using an ultracentrifuge (13000 rpm,20 minutes, 4 ℃) to separate nanoparticles, and the nanoparticles were washed twice using 100 mL phosphate buffer (PBS, pH 7.4) to remove unencapsulated active ingredients and residual surfactant, and the separated nanoparticles were freeze-dried to obtain a nano pesticide formulation.
Example 2 preparation of nano pesticide formulation:
(1) Weighing 5mg of chinaberry fruit extract and 1mg of benzyl acrylic acid mycoketone, adding into 20mL of ethanol, adding 15mg of polylactic acid-glycolic acid copolymer (PLGA), and stirring at normal temperature until the solution is uniform to obtain an organic phase;
(2) 0.5g Tween 20 was dissolved in 100mL deionized water to give a water phase;
(3) Dropwise adding an organic phase into an aqueous phase at a speed of 1.5mL/min under ice water bath conditions, stirring at a speed of 1200rpm for 40 minutes to form an emulsion, transferring the emulsion into a rotary evaporator, slowly evaporating ethanol at 30 ℃ through rotary evaporation until the organic solvent is completely volatilized, and gradually wrapping the margarine and the fenpropione by PLGA along with the volatilization of the ethanol to form nano pesticide particles;
(4) The emulsion was ultracentrifuged using an ultracentrifuge (13000 rpm,20 minutes, 4 ℃) to separate nanoparticles, and the nanoparticles were washed twice using 100 mL phosphate buffer (PBS, pH 7.4) to remove unencapsulated active ingredients and residual surfactant, and the separated nanoparticles were freeze-dried to obtain a nano pesticide formulation.
Example 3 preparation of nano pesticide formulation:
(1) Weighing 10mg of margarine and 1mg of benzyl acrylic ketone, adding into 20mL of ethanol, adding 27.5mg of polylactic acid-glycolic acid copolymer (PLGA), and stirring at normal temperature until the solution is uniform to obtain an organic phase;
(2) 0.5g Tween 20 was dissolved in 100mL deionized water to give a water phase;
(3) Dropwise adding an organic phase into an aqueous phase at a speed of 1.5mL/min under ice water bath conditions, stirring at a speed of 1200rpm for 40 minutes to form an emulsion, transferring the emulsion into a rotary evaporator, slowly evaporating ethanol at 30 ℃ through rotary evaporation until the organic solvent is completely volatilized, and gradually wrapping the margarine and the fenpropione by PLGA along with the volatilization of the ethanol to form nano pesticide particles;
(4) The emulsion was ultracentrifuged using an ultracentrifuge (13000 rpm,20 minutes, 4 ℃) to separate nanoparticles, and the nanoparticles were washed twice using 100 mL phosphate buffer (PBS, pH 7.4) to remove unencapsulated active ingredients and residual surfactant, and the separated nanoparticles were freeze-dried to obtain a nano pesticide formulation.
Comparative example 1:
(1) Weighing 6mg of margarine, adding into 20mL of ethanol, adding 1mg of polylactic acid-glycolic acid copolymer (PLGA), and stirring at normal temperature until the solution is uniform to obtain an organic phase;
(2) 0.5g Tween 20 was dissolved in 100mL deionized water to give a water phase;
(3) Dropwise adding an organic phase into an aqueous phase at a speed of 1.5mL/min under ice water bath conditions, stirring at a speed of 1200rpm for 40 minutes to form an emulsion, transferring the emulsion into a rotary evaporator, slowly evaporating ethanol at 30 ℃ through rotary evaporation until the organic solvent is completely volatilized, and gradually wrapping the margarine and the fenpropione by PLGA along with the volatilization of the ethanol to form nano pesticide particles;
(4) The emulsion was ultracentrifuged using an ultracentrifuge (13000 rpm,20 minutes, 4 ℃) to separate nanoparticles, and the nanoparticles were washed twice using 100 mL phosphate buffer (PBS, pH 7.4) to remove unencapsulated active ingredients and residual surfactant, and the separated nanoparticles were freeze-dried to obtain a nano pesticide formulation.
Comparative example 2:
(1) Weighing 6mg of benomyl, adding the benomyl into 20mL of ethanol, adding 1mg of polylactic acid-glycolic acid copolymer (PLGA), and stirring the mixture at normal temperature until the solution is uniform to obtain an organic phase;
(2) 0.5g Tween 20 was dissolved in 100mL deionized water to give a water phase;
(3) Dropwise adding an organic phase into an aqueous phase at a speed of 1.5mL/min under ice water bath conditions, stirring at a speed of 1200rpm for 40 minutes to form an emulsion, transferring the emulsion into a rotary evaporator, slowly evaporating ethanol at 30 ℃ through rotary evaporation until the organic solvent is completely volatilized, and gradually wrapping the margarine and the fenpropione by PLGA along with the volatilization of the ethanol to form nano pesticide particles;
(4) The emulsion was ultracentrifuged using an ultracentrifuge (13000 rpm,20 minutes, 4 ℃) to separate nanoparticles, and the nanoparticles were washed twice using 100 mL phosphate buffer (PBS, pH 7.4) to remove unencapsulated active ingredients and residual surfactant, and the separated nanoparticles were freeze-dried to obtain a nano pesticide formulation.
Comparative example 3:
(1) Weighing 1mg of chinaberry fruit extract and 5mg of benzyl acrylic acid mycoketone, adding the chinaberry fruit extract and the benzyl acrylic acid mycoketone into 20mL of ethanol, adding 15mg of polylactic acid-glycolic acid copolymer (PLGA), and stirring the mixture at normal temperature until the solution is uniform to obtain an organic phase;
(2) 0.5g Tween 20 was dissolved in 100mL deionized water to give a water phase;
(3) Dropwise adding an organic phase into an aqueous phase at a speed of 1.5mL/min under ice water bath conditions, stirring at a speed of 1200rpm for 40 minutes to form an emulsion, transferring the emulsion into a rotary evaporator, slowly evaporating ethanol at 30 ℃ through rotary evaporation until the organic solvent is completely volatilized, and gradually wrapping the margarine and the fenpropione by PLGA along with the volatilization of the ethanol to form nano pesticide particles;
(4) The emulsion was ultracentrifuged using an ultracentrifuge (13000 rpm,20 minutes, 4 ℃) to separate nanoparticles, and the nanoparticles were washed twice using 100 mL phosphate buffer (PBS, pH 7.4) to remove unencapsulated active ingredients and residual surfactant, and the separated nanoparticles were freeze-dried to obtain a nano pesticide formulation.
Comparative example 4:
(1) Weighing 15mg of chinaberry fruit extract and 1mg of benzyl acrylic acid mycoketone, adding into 20mL of ethanol, adding 40mg of polylactic acid-glycolic acid copolymer (PLGA), and stirring at normal temperature until the solution is uniform to obtain an organic phase;
(2) 0.5g Tween 20 was dissolved in 100mL deionized water to give a water phase;
(3) Dropwise adding an organic phase into an aqueous phase at a speed of 1.5mL/min under ice water bath conditions, stirring at a speed of 1200rpm for 40 minutes to form an emulsion, transferring the emulsion into a rotary evaporator, slowly evaporating ethanol at 30 ℃ through rotary evaporation until the organic solvent is completely volatilized, and gradually wrapping the margarine and the fenpropione by PLGA along with the volatilization of the ethanol to form nano pesticide particles;
(4) The emulsion was ultracentrifuged using an ultracentrifuge (13000 rpm,20 minutes, 4 ℃) to separate nanoparticles, and the nanoparticles were washed twice using 100 mL phosphate buffer (PBS, pH 7.4) to remove unencapsulated active ingredients and residual surfactant, and the separated nanoparticles were freeze-dried to obtain a nano pesticide formulation.
Comparative example 5:
The chinaberry fruit extract and the benpropenone are mixed according to the mass ratio of 5:1 to be used as pesticide preparations.
Test example Toosendan and Phenylketone were mixed and tested for indoor virulence of Nuclear bacteria:
1. The strain to be tested is sclerotinia sclerotiorum (Sclerotinia sclerotiorum).
2. The test method comprises the following steps:
2.1 measurement was performed by the growth rate method of the medicated medium, referring to the "laboratory biological assay guidelines for pesticides NY/T1156.2-2006".
The pesticide preparations prepared in examples 1-3 and comparative examples 1-5 were prepared as mother liquor with an equal concentration gradient, the drug to be tested was added to PDA medium at about 45℃and mixed well, and poured into petri dishes with diameter of 9 cm to prepare a medicated plate, and an equal amount of dimethyl sulfoxide was added as a control. The sclerotinia sclerotiorum (Sclerotinia sclerotiorum) cakes cultured for 3 days are picked up by a puncher with the inner diameter of 5mm and placed in the center of a flat plate, and are subjected to dark culture in a culture box with the temperature of 25+/-1 ℃ and each treatment is repeated for 3 times. And when the colony of the control group grows to be close to the edge of the culture dish, measuring the diameter of the colony by a crisscross method, and calculating the bacteriostasis rate.
Antibacterial ratio= (control colony diameter-treated colony diameter)/control colony diameter x 100%.
The inhibition rate of the different concentration agents on the growth of the sclerotinia sclerotiorum (Sclerotinia sclerotiorum) hyphae of the soybean sclerotinia sclerotiorum is calculated, data analysis is carried out, and a regression equation and EC 50 are calculated.
2.2 Co-toxicity coefficients (CTCs) of the blends were then calculated according to the grand cloud Pei method. The effect of the blending is analyzed by the co-toxicity coefficient. The co-toxicity coefficient (CTC) is calculated as follows:
toxicity Index (TI) = (EC 50 of standard agent/EC 50 of test agent) ×100;
Mix observed virulence index (ATI) = (EC 50 of standard dose/EC 50 of mixed dose) ×100;
The mixed agent Theoretical Toxicity Index (TTI) =the toxicity index of agent a x the percentage of agent a in the mixed agent+the toxicity index of agent B x the percentage of agent B in the mixed agent;
co-toxicity coefficient (CTC) = (ATI/TTI) ×100;
according to the division standard of co-toxicity coefficient (CTC), CTC is less than or equal to 80 and is antagonism, CTC 80 is additive, CTC is greater than or equal to 120 and is synergistic.
TABLE 1 results of indoor toxicity measurements of Torulopsis with Torulaspora
As can be seen from the results in Table 1, the toosendanin and the benomyl are mixed, the co-toxicity coefficient (CTC) of the toosendanin and the benomyl is greater than 120 in the range of 1-10:1, the synergistic effect is obvious, the active on sclerotinia sclerotiorum of soybean sclerotiorum is very high, and the optimal ratio is 5:1. In addition, in comparative example 5 and example 2, the ratio of the toosendanin to the fenpropione is 5:1, but the synergy of example 2 is stronger and EC 50 is lower than that of comparative example 5, which shows that the synergy between the toosendanin and the fenpropione is enhanced through nanocrystallization, the biological activity and the utilization rate of the toosendanin and the fenpropione are obviously improved, the dosage of pesticides is reduced, and the prevention and treatment effect on soybean sclerotinia is improved.
The above description is only of the preferred embodiments of the present application and is not intended to limit the present application, but various modifications and variations can be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the protection scope of the present application.
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