Insecticide composition containing biogenic insecticide and application thereof

By compounding the compound of formula I with spinosad or ethyl spinetoram, an insecticidal composition is formed, which solves the problem of pest resistance caused by chemical insecticides and achieves efficient and low-cost pest control, especially with significant effects on Lepidoptera and Thysanoptera pests.

CN119032952BActive Publication Date: 2025-09-12QINGDAO KYX CHEMICAL CO LTD
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Patent Information

Application Number
CN202411162609.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-08-23
Publication Date
2025-09-12
Estimated Expiration
2044-08-23

AI Technical Summary

Technical Problem

The continued use of chemical pesticides in the existing technology has led to a prominent problem of pest resistance, and there is a lack of effective pesticide combination solutions to improve control effects and reduce costs.

Method used

The compound of formula I is rationally compounded with the biogenic insecticide spinosad or ethyl spinetoram to form an insecticidal composition, and the compounds with different mechanisms of action are used to enhance the insecticidal effect at a certain mass ratio, and auxiliary ingredients allowed in pesticides are added to form various preparations.

Benefits of technology

It significantly improves the control effect of agricultural, horticultural and forestry pests, delays the occurrence and development of pest resistance, reduces the amount of pesticide used, is low in cost and has little impact on the environment.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention belongs to the field of pesticide control technology and discloses an insecticidal composition containing a biogenic insecticide and its use. The active ingredients of the insecticidal composition include a compound of Formula I and a biogenic insecticide. The compound of Formula I has the following structure: #imgabs0# The biogenic insecticide is either spinetoram or spinosad, and the mass ratio of the compound of Formula I to the biogenic insecticide is 1:30 to 32:1. The insecticidal composition of the present invention has excellent insecticidal efficacy, multiple mechanisms of action and sites, and can effectively delay the development and progression of insecticide resistance in pests. It is also low-cost and has significant economic benefits.
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Description

Technical Field

[0001] The invention belongs to the technical field of pesticide killing technology and discloses an insecticide composition containing a biogenic insecticide and application thereof. Background Art

[0002] Spinetoram is a macrolide biogenic insecticide developed in recent years by Dow AgroSciences of the United States. It mainly acts on nicotinic acetylcholine receptors and γ-aminobutyric acid receptors in the insect nervous system, rendering the insect insensitive to excitatory or inhibitory signal transmission, leading to death.

[0003] Spinosad, also known as spinosad, is a biopesticide purified from actinomycete metabolites. It rapidly paralyzes and incapacitates pests, ultimately killing them. It has both stomach and contact effects, with the stomach poison being the primary agent. It is used to control pests such as diamondback moth, beet armyworm, and thrips on vegetables and cotton, with low toxicity and rapid insecticide efficacy.

[0004] The compound of Formula I is an allosteric modulator of γ-aminobutyric acid (GABA)-gated chloride channels, belonging to IRAC group 30. It has a unique mechanism of action and exhibits no cross-resistance with other insecticides. The structure of the compound of Formula I is shown below:

[0005]

[0006] In the actual process of agricultural production, chemical control is still the most effective means of controlling pests, but due to the continuous and large-scale use of chemical pesticides, the problem of pest resistance is constantly prominent. In view of the above problems, the rational compounding of agents with different insecticide mechanisms can be selected, which can not only improve drug efficacy and reduce costs, but also be one of the important methods for overcoming the development of pest resistance. Therefore, the inventors have explored the combined effects of the compound of formula I and the biogenic insecticide spinosad or ethyl spinetoram on various types of pests, aiming to provide a theoretical basis for reducing the amount of agent used for controlling pests and improving the control effect. However, there is currently no report on the control of pests by the compound of formula I and spinosad or ethyl spinetoram. Summary of the Invention

[0007] To address the aforementioned problems in the prior art, the present invention provides an insecticidal composition containing a biogenic insecticide and its use. This insecticidal composition has excellent control effects against a variety of agricultural, horticultural, and forestry pests. The composition has multiple mechanisms of action and sites of action, effectively delaying the development and progression of insecticide resistance. It also offers low cost and significant economic benefits.

[0008] To achieve the above objectives, the present invention adopts the following technical solution: an insecticide composition containing a biogenic insecticide and its application, wherein the active ingredient of the insecticide composition comprises a compound of formula I and a biogenic insecticide, and the structure of the compound of formula I is as follows: The biogenic insecticide is any one of spinosad or ethyl spinosad, and the mass ratio of the compound of formula I to the biogenic insecticide is 1:30 to 32:1, such as 1:30, 1:27, 1:26, 1:25, 1:24, 1:22, 1:20, 1:18, 1:17, 1:15, 1:12, 1:10, 1:9, 1:6, 1:5, 1:3, 1:1, 3:2, 2:1, 5:2, 3:1, 5:1, 6:1, 7:1, 10:1, 12:1, 15:1, 16:1, 18:1, 20:1, 24:1, 25:1, 32:1 or any value therebetween;

[0009] Furthermore, the biogenic insecticide is spinetoram, and the mass ratio of the compound of formula I to spinetoram is 1:26 to 24:1, such as 1:26, 1:24, 1:22, 1:18, 1:17, 1:10, 1:12, 1:6, 1:5, 1:1, 2:1, 5:2, 6:1, 7:1, 10:1, 12:1, 16:1, 18:1, 20:1, 24:1 or any value therebetween;

[0010] Furthermore, the biogenic insecticide is spinetoram, and the mass ratio of the compound of formula I to spinetoram is 1:24 to 20:1, such as 1:24, 1:22, 1:18, 1:17, 1:10, 1:12, 1:6, 1:5, 1:1, 2:1, 5:2, 6:1, 7:1, 10:1, 12:1, 16:1, 18:1, 20:1 or any value therebetween;

[0011] Furthermore, the biogenic insecticide is spinetoram, and the mass ratio of the compound of formula I to spinetoram is 1:22 to 18:1, such as 1:22, 1:18, 1:17, 1:10, 1:12, 1:6, 1:5, 1:1, 2:1, 5:2, 6:1, 7:1, 10:1, 12:1, 16:1, 18:1 or any value therebetween;

[0012] Furthermore, the biogenic insecticide is spinosad, and the mass ratio of the compound of formula I to spinosad is 1:27 to 32:1, such as 1:27, 1:25, 1:20, 1:18, 1:15, 1:10, 1:9, 1:5, 1:3, 3:2, 3:1, 5:1, 6:1, 10:1, 12:1, 15:1, 18:1, 20:1, 24:1, 25:1, 32:1 or any value therebetween;

[0013] Furthermore, the biogenic insecticide is spinosad, and the mass ratio of the compound of formula I to spinosad is 1:20 to 25:1, such as 1:20, 1:18, 1:15, 1:10, 1:9, 1:5, 1:3, 3:2, 3:1, 5:1, 6:1, 10:1, 12:1, 15:1, 18:1, 20:1, 24:1, 25:1 or any value therebetween;

[0014] Furthermore, the biogenic insecticide is spinosad, and the mass ratio of the compound of formula I to spinosad is 1:18 to 24:1, such as 1:18, 1:15, 1:10, 1:9, 1:5, 1:3, 3:2, 3:1, 5:1, 6:1, 10:1, 12:1, 15:1, 18:1, 20:1, 24:1 or any value therebetween;

[0015] Furthermore, the total weight of the insecticide composition is 100 wt%, and the compound of formula I and the biogenic insecticide account for 0.01% to 80% of the total weight of the insecticide composition;

[0016] Furthermore, the insecticide composition contains, in addition to the active ingredient, auxiliary ingredients permitted in pesticides, wherein the auxiliary ingredients are selected from one or more of a wetting agent, a dispersant, an emulsifier, a thickener, a disintegrant, an antifreeze agent, a defoaming agent, a solvent, a preservative, a stabilizer, a synergist or a carrier;

[0017] The wetting agent is selected from one or more of alkylbenzene sulfonate, alkylnaphthalene sulfonate, lignin sulfonate, sodium lauryl sulfate, sodium dioctyl sulfosuccinate, α-olefin sulfonate, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol ethoxylate, fatty alcohol ethoxylate, fatty alcohol polyoxyethylene ether sodium sulfate, silkworm feces, soapberry powder, soapberry powder, SOPA, detergent, emulsifier 2000 series and wetting penetrant F; and / or

[0018] The dispersant is selected from one or more of lignin sulfonate, alkylnaphthalene sulfonate formaldehyde condensate, naphthalene sulfonate, tristyrylphenol ethoxylate phosphate, fatty alcohol ethoxylate, alkylphenol polyoxyethylene ether, alkylphenol polyoxyethylene ether methyl ether condensate sulfate, fatty amine polyoxyethylene ether, glycerol fatty acid ester polyoxyethylene ether, polycarboxylates, polyacrylic acids, phosphates, EO-PO block copolymers and EO-PO graft copolymers; and / or

[0019] The emulsifier is selected from one or more of calcium dodecylbenzenesulfonate, alkylphenol formaldehyde resin polyoxyethylene ether, phenylethylphenol polyoxyethylene polyoxypropylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, styrylphenol polyoxyethylene ether, castor oil polyoxyethylene ether and alkylphenol ether phosphate; and / or

[0020] The thickener is selected from one or more of xanthan gum, organobentonite, gum arabic, sodium alginate, magnesium aluminum silicate, carboxymethyl cellulose and white carbon black; and / or

[0021] The disintegrant is selected from one or more of sodium sulfate, ammonium sulfate, aluminum chloride, sodium chloride, ammonium chloride, bentonite, glucose, sucrose, starch, cellulose, urea, sodium carbonate, sodium bicarbonate, citric acid and tartaric acid; and / or

[0022] The antifreeze agent is selected from one or more of alcohols, alcohol ethers, chlorinated hydrocarbons and inorganic salts; and / or

[0023] Defoaming agent selected from C 10 -C 20 Saturated fatty acid compounds, silicone oil, silicone compounds, C8-C 10 One or more of fatty alcohols; and / or

[0024] The solvent is selected from one or more of benzene, toluene, xylene, durene, methanol, ethanol, isopropanol, n-butanol, dimethyl sulfoxide, dimethylformamide, cyclohexanone, alkylene carbonate, diesel, solvent oil, vegetable oil, vegetable oil derivatives and water; and / or

[0025] The preservative is selected from one or more of propionic acid, sodium propionic acid, sorbic acid, sodium sorbic acid, potassium sorbic acid, benzoic acid, sodium benzoic acid, sodium p-hydroxybenzoic acid, methyl p-hydroxybenzoate, kasone and 1,2-benzisothiazolin-3-one; and / or

[0026] The stabilizer is selected from one or more of disodium hydrogen phosphate, oxalic acid, succinic acid, adipic acid, borax, 2,6-di-tert-butyl-p-cresol, triethanolamine oleate, epoxidized vegetable oil, kaolin, bentonite, attapulgite, white carbon black, talc, montmorillonite and starch; and / or

[0027] Synergists are selected from synergist, piperonyl butoxide; and / or

[0028] The carrier is selected from one or more of ammonium salts, ground natural minerals, ground artificial minerals, silicates, resins, waxes, solid fertilizers, water, organic solvents, mineral oils, vegetable oils and vegetable oil derivatives;

[0029] Furthermore, the insecticide composition is prepared into a pesticide formulation, which is a solid formulation or a liquid formulation;

[0030] Furthermore, the solid preparation includes powders, granules, pellets, tablets, strips, wettable powders, oil-dispersible powders, emulsion powders, water-dispersible granules, emulsion granules, water-dispersible tablets, soluble powders, soluble tablets or soluble granules;

[0031] The liquid preparations include soluble solutions, soluble gels, oils, film-spreading oils, emulsifiable concentrates, latexes, dispersible solutions, ointments, aqueous emulsions, oil emulsions, microemulsions, lipid suspensions, microcapsule suspensions, oil suspensions, dispersible oil suspensions, suspoemulsions, microcapsule suspension-suspension concentrates, microcapsule suspension-water emulsions, or microcapsule suspension-suspoemulsions;

[0032] Furthermore, the solid preparation is a water-dispersible granule or a wettable powder; the liquid preparation is a suspension, a microemulsion, a dispersible oil suspension or an aqueous emulsion;

[0033] The present invention also discloses the use of the insecticide composition for preventing and controlling agricultural, horticultural or forestry pests.

[0034] Furthermore, the pests are Lepidoptera pests and Thysanoptera pests;

[0035] Furthermore, the Lepidoptera includes, but is not limited to, Plutellaxylostella, diamondback moth, Polychrosis viteana (grapeberry moth), Prays endocarpa, Prays oleae (olive moth), Pseudaletia spp. (snoctuids), Pseudaletia unipunctata (armyworm), Pseudoplusia includes (soybean looper), Rachiplusia nu, Scirpophaga incertulas, Sesamia spp. (stemborers), Sesamia inferens (pink rice stem borer), Sesamia nonagrioides), Setora nitens, Sitotroga cerealella (Angoumois grain moth), Sparganothis pilleriana, Spodoptera spp. (snooper moths), Spodoptera exigua (beet armyworm), Spodoptera fugiperda (fall armyworm), Adoxophyes spp., Adoxophyes orana, Agrotis spp.(cutworm), Agrotis ipsilon (black cutworm), Alabama argillacea, Amorbia cuneana, Amyelosis transitella (navel orangeworm), Anarsia lineatella (peach twig borer), Anomissa bulifera (jute looper), Anticarsia gemma talis (velvet bean pelleter), Archips argyrospila (fruittree leafroller), Archips rosana (rose leaf roller), Argyrotaenia spp. (tortricidmoths), Argyrotaenia citrana, Autographa gamma, Bonagota cranaodes, Borbo cinnara), Caloptilia spp. (leaf miners), Capuareticulana, Carposina niponensis (peach fruit moth), Chilospp., Chlumetia transversa (mango shoot borer), Choristoneura rosaceana (obliquebanded leafroller), Chrysodeixis spp., Cnaphalocerus medinalis (grass leafroller), Colias spp., Conpomorpha cramerella, Cossus cossus, Crambus spp.) (Sod webworms), Cydia funebrana (plum fruit moth), Cydia molesta (oriental fruit moth), Cydia nignicana (pea moth), Cydia pomonella, Darna diducta, Diaphania spp. (stem borers), Diatraea spp. (stalk borers), Diatraea saccharalis (sugarcane borer), Diatraea graniosella (southwester cornborer), Earias spp. (cotton bollworms), Earias spp. (Egyptian bollworms). insulata (Egyptian bollworm), Earias vitella (rough northern bollworm), Ecdytopophaaurantianum, Elasmopalpus lignosellus (lesser cornstalk borer), Ephestia spp. (flour moths), Ephestia cautella (almond moth), Ephestia elutella (tobbaco moth), Ephestia kuehniella (Mediterranean flour moth), Epimeces spp., Epinotia aporema, Erionota thrax (banana skipper), Eupoecilia ambiguella, Euxoa auxiliaris (army cutworm), Feltia spp., Gortyna spp.(stemborers), Grapholita molesta (oriental fruit moth), Hedylepta indicate, bean leaf webber, Helicoverpas pp. (spotworms), Helicoverpa paarmigera, Helicoverpa zea, Heliothis spp. (spotworms), Heliothis virescens, tobacco budworm, Hellula undalis (cabbage webworm), Indarbela spp., root borers, Keiferia lycopersicella, (tomato pinworm), Leucinodes orbonalis (eggplant fruit borer). borer), Leucoptera malifoliella, Lithocollectis spp., Lobesia botrana (grape fruit moth), Loxagrotis spp. (southworm), Loxagrotis albicosta (western bean cutworm), Lymantria dispar (gypsy moth), Lyonetia clerkella (apple leaf miner), Mahasena corbetti (oil palm bagworm), Malacosoma spp.(tent caterpillars), Mamestra brassicae (cabbage armyworm), Maruca testulalis, Metisa plana, Mythimna unipuncta (true armyworm), Neoleucinodes elegantalis (small tomato borer), Operophthera brumata (winter moth), Ostrinia nubilalis (European corn borer), Pandemis cerasana, common currant tortrix, Pandemis heparana (brown apple tortrix), Papilio demodocus, Pectinophora gossypiella (pink bollworm), Peridroma species ( spp. (cutworm), Peridroma saucia (variegated cutworm), Perileucoptera coffeella (white coffee leafminer), Phthorimaea operculella (potato tuber moth), Phyllocnisitis citrella, Phyllonorycter spp. (leafminers), Pieris rapae (imported cabbageworm), Plathypena scabra, Plodia interpunctella (Indian mealmoth), Spodoptera oridania (southern armyworm), Synanthedon spp.) (root borers), Thecla basilides, Thermisiagemmatalis, Tineola bisselliella (webbing clothes moth), Trichoplusia ni (rape worm), Tuta absoluta, Yponomeuta spp., Zeuzera coffeae (red branch borer), and Zeuzera pyrina (leopard moth).

[0036] The Thysanoptera pests include, but are not limited to, Frankliniella occidentalis, Thrips spp., Scirtothrips dorsalis, Stenchaetothrips biformis, Frankliniella intonsta, Thrips palmi, Anaphothrips obscurus, Neohydatothrips samayunkur, Dendrothrips minowai, Haplothrips aculeatus, Frankliniella tenuicornis, and Thrips hawaiiensis.

[0037] In particular, the insecticide composition of the present invention has excellent control effects on diamondback moth, beet armyworm, rice leaf roller, thrips, bean pod borer, etc.

[0038] Furthermore, the insecticide composition or its formulation is applied to the pests to be controlled or the medium in which they grow.

[0039] In order to obtain the desired insecticidal effect, the dosage of the insecticidal composition varies depending on various factors, such as the crop to be protected, the type of pest, the degree of infection, climatic conditions, application site, application method, dosage form used, etc.

[0040] The beneficial effects of the present invention are as follows:

[0041] 1) The insecticidal composition of the present invention rationally combines compounds with different mechanisms of action, and under certain mass ratios, has a significant synergistic effect on pests and an excellent insecticidal effect;

[0042] 2) The insecticidal composition of the present invention has excellent control effects on Lepidoptera and Thysanoptera in agriculture, horticulture and forestry;

[0043] 3) The insecticide composition of the present invention reduces the amount of pesticides used, has low cost, high economic benefits, and little impact on the environment, and can effectively delay the occurrence and development of pesticide resistance in pests. DETAILED DESCRIPTION

[0044] In order to make the technical solutions, objectives and advantages of the present invention more clearly understood, the present invention is described with reference to the following specific embodiments. However, the present invention can be implemented in various forms and should not be limited to the embodiments described herein.

[0045] Preparation example:

[0046] Preparation Example 1: 21% Formula I Compound·Spinetoram Water Dispersible Granules (1:6)

[0047] Formula composition: 3% compound of formula I, 18% spinetoram, 10% sodium lignin sulfonate, 5% sodium salt of polycarboxylate, 2% sodium lauryl sulfate, 12% ammonium sulfate, and starch makes up the balance;

[0048] Preparation method: According to the formula ratio, the active ingredient is added to the carrier, and the surfactant and other functional additives are added thereto, mixed, and after air flow grinding, 10-25% water is added, and then the mixture is kneaded, granulated, dried, and sieved to obtain a water-dispersible granule product; or the pulverized powder is sprayed with water in a boiling granulator, granulated, dried, and then sieved to obtain the product.

[0049] Preparation Example 2: 18% Formula I compound·Spinetoram wettable powder (2:1)

[0050] Formula composition: 12% compound of formula I, 6% spinetoram, 5% sodium lignin sulfonate, 5% formaldehyde condensate of sodium methylnaphthalene sulfonate, 2.5% pulverized powder BX, 10% white carbon black, and kaolin to make up the balance;

[0051] Preparation method: According to the formula ratio, the active ingredients, dispersants, wetting agents and fillers are mixed, uniformly stirred in a stirring kettle, and pulverized and mixed uniformly multiple times in a jet mill to prepare the wettable powder of the composition of the present invention.

[0052] Preparation Example 3: 17.5% Formula I Compound·Spinetoram Suspension Concentrate (5:2)

[0053] Formula composition: 12.5% ​​compound of formula I, 5% ethyl spinosad, 2% Guerbet alcohol polyoxyethylene ether, 3% triphenylphenol polyoxyethylene ether, 3% arylphenol polyoxyethylene ether phosphate, 1% tristyrylphenol ethoxylate phosphate, 1% sodium alkylnaphthalene sulfonate, 1.5% magnesium aluminum silicate, 0.1% carboxyethyl cellulose, 0.5% potassium benzoate, 5% ethylene glycol, 0.5% silicone oil, and deionized water to make up the balance;

[0054] Preparation method: According to the formula ratio, the active ingredients, surfactants and other functional additives are placed in a reactor in sequence, water is added and mixed evenly, and the suspension product is obtained by high-speed shearing, wet sand grinding, and finally homogenization filtration.

[0055] Preparation Example 4: 1.1% Formula I Compound·Spinetoram Microemulsion (10:1)

[0056] Formula composition: 1% compound of formula I, 0.1% ethyl spinosad, 30% cyclohexanone, 10% castor oil polyoxyethylene ether, 1% calcium dodecylbenzenesulfonate, 4% sodium octylphenol polyoxyethylene ether sulfonate, 5% styrylphenol polyoxyethylene ether, 2% styrylphenol polyoxyethylene ether phosphate, 0.05% silicone defoamer, and deionized water to make up the balance;

[0057] Preparation method: According to the formula ratio, the active ingredient is completely dissolved in the solvent, and then emulsified to prepare the oil phase. The dispersant, deionized water, etc. are stirred evenly to prepare the water phase; the oil phase is added to the water phase and stirred evenly, and high-speed shearing is performed until the particle size meets the requirements. After adding the defoaming agent, stir evenly to obtain the microemulsion product.

[0058] Preparation Example 5: 1.95% Formula I compound·Spinetoram aqueous emulsion (1:12)

[0059] Formula composition: 0.15%% compound of formula I, 1.8% ethyl spinosad, 28% cyclohexanone, 4% alkyl aryl polyoxyethylene ether polyoxypropylene ether, 1% fatty alcohol polyoxyethylene ether phosphate, 4% glycerol, 0.01% silicone defoamer, and deionized water to make up the balance;

[0060] Preparation method: After completely dissolving the active ingredient in the solvent according to the formula ratio, add the emulsifier to form the oil phase; stir the dispersant, antifreeze, deionized water, etc. to form the water phase; add the oil phase to the water phase and stir evenly, shear at high speed until the particle size meets the requirements, add the defoaming agent and stir evenly to obtain the water emulsion product.

[0061] Preparation Example 6: 25% Formula I Compound·Spinosad Water Dispersible Granules (3:2)

[0062] Formula composition: 15% compound of formula I, 10% spinosad, 5% sodium dioctyl sulfosuccinate, 3% sodium alkyl polyoxyethylene ether sulfonate, 2% flaking powder BX, 10% naphthalenesulfonate formaldehyde condensate, 10% ammonium sulfate, and kaolin makes up the balance;

[0063] Preparation method: Same as Preparation Example 1.

[0064] Preparation Example 7: 20% Formula I compound·Spinosad wettable powder (1:9)

[0065] Formula composition: 10% compound of formula I, 20% spinosad, 5% tea saponin, 6% sodium alkylnaphthalene sulfonate, 3% styrenated phenol polyoxyethylene ether sulfate, 2% sodium lauryl sulfate, 10% attapulgite, and kaolin makes up the balance;

[0066] Preparation method: Same as Preparation Example 2.

[0067] Preparation Example 8: 26% Formula I Compound·Spinosad Suspension (12:1)

[0068] Formula composition: 24% compound of formula I, 2% spinosad, 3% sorbitan oleate polyoxyethylene ether, 1% naphthalenesulfonate formaldehyde condensate, 4% fatty alcohol polyoxyethylene ether phosphate, 3% fatty alcohol polyoxyethylene ether, 0.25% xanthan gum, 1% magnesium aluminum silicate, 5% ethylene glycol, 0.1% sodium sorbate, 0.5% silicone oil, and deionized water to make up the balance;

[0069] Preparation method: Same as Preparation Example 3.

[0070] Preparation Example 9: 2% Formula I Compound·Spinosad Microemulsion (3:1)

[0071] Formula composition: 1.5% compound of formula I, 0.5% spinosad, 10% xylene, 25% cyclohexanone, 12% tristyrylphenol polyoxyethylene ether, 4% EO-PO block copolymer, 2% alkylphenol polyoxyethylene ether methyl ether condensate sodium sulfate, 5% propylene glycol, 0.05% silicone defoamer, and deionized water to make up the balance;

[0072] Preparation method: same as Preparation Example 4.

[0073] Preparation Example 10: 1.2% Formula I Compound·Spinosad Emulsion in Water (5:1)

[0074] Formula composition: 1% compound of formula I, 0.2% spinosad, 6% phenethylphenol polyoxyethylene polyoxypropylene ether, 1% alkylphenol polyoxyethylene ether phosphate, 20% cyclohexanone, 0.25% xanthan gum, 4% propylene glycol, 1% urea, 0.25% potassium benzisothiazolinone, 0.05% silicone defoamer, and deionized water to make up the balance;

[0075] Preparation method: Same as Preparation Example 5.

[0076] Indoor biological activity assay

[0077] Example 1: Indoor bioactivity test on lepidopteran pest bean pod borer

[0078] Test basis: The test refers to NY / T-1154.14-2008 "Guidelines for Indoor Biological Testing of Pesticides - Insecticides Part 14: Leaf Dipping Method".

[0079] Test target: 3rd instar larvae of pod borer.

[0080] Test agents: compound of formula I, spinetoram, and spinosad original drug.

[0081] Test Method: Based on the results of the preliminary test, the above raw drugs were dissolved in appropriate solvents and then diluted with 0.1% Tween 80 aqueous solution to an appropriate concentration gradient. A treatment without the drug (containing all organic solvents and emulsifiers) served as a blank control. Third-instar larvae of uniform size were immersed in the different concentrations of the drug for 10 seconds, removed, dried on absorbent paper, and placed in 24-well insect culture plates. The insect culture plates were placed in an incubator at a temperature of (28±1)°C, a relative humidity of (70±1)%, and a photoperiod of L:D = 14h:10h for breeding.

[0082] Experimental investigation: 48 hours after treatment, the number of dead larvae in each treatment was counted. The insect bodies were lightly touched with a small brush or tweezers. Individuals that could not coordinate movement or whose bodies differed greatly from those of the control were considered dead.

[0083] Calculation method:

[0084] Based on the survey data, calculate the mortality rate of each treatment. Calculate as follows:

[0085]

[0086] Where:

[0087] P——mortality rate, in percentage (%);

[0088] K——indicates the number of dead insects, the unit is head;

[0089] N——represents the total number of insects processed, in heads.

[0090]

[0091] Where:

[0092] P1——adjusted mortality rate, in percentage (%);

[0093] P t——Treatment mortality rate, expressed in percentage (%);

[0094] P0 - blank control mortality rate, in percentage (%).

[0095] If the control mortality rate is less than 5%, no correction is required; if the control mortality rate is between 5% and 20%, correction should be made according to the correction mortality formula; if the control mortality rate is greater than 20%, the test needs to be repeated.

[0096] The DPS statistical analysis system was used to analyze the toxicity regression equation, correlation coefficient and LC 50 The activity of the test agent on the biological test material is evaluated by the value.

[0097] The co-toxicity coefficient (CTC value) of the mixture is calculated as follows:

[0098]

[0099] Where:

[0100] ATI - measured toxicity index of mixture;

[0101] S——LC of standard pesticide 50 , the unit is milligrams per liter (mg / L);

[0102] M——LC of the mixture 50 , the unit is milligrams per liter (mg / L).

[0103] TTI=TI A ×P A +TI B ×P B

[0104] Where:

[0105] TTI – Theoretical Toxicity Index of Mixtures;

[0106] TI A ——Agent toxicity index;

[0107] P A ——The percentage of agent A in the mixture, in percentage (%);

[0108] TI B ——Toxicity index of agent B;

[0109] P B ——The percentage of agent B in the mixture, in percentage (%).

[0110]

[0111] Where:

[0112] CTC – Co-toxicity coefficient;

[0113] ATI - measured toxicity index of mixture;

[0114] TTI - Theoretical Toxicity Index of Mixture.

[0115] A co-toxicity coefficient (CTC) of 120 or higher indicates a synergistic effect; a co-toxicity coefficient (CTC) of 80 or lower indicates an antagonistic effect; and a co-toxicity coefficient (CTC) of 80 or lower indicates an additive effect.

[0116] The indoor test results are shown in the table below:

[0117] Table 1 Results of indoor biological activity test of compound of formula I combined with spinetoram against bean pod borer

[0118]

[0119] Table 2 Indoor biological activity test results of compound of formula I combined with spinosad against Plutella xylostella

[0120]

[0121] From the test results in Tables 1 and 2, it can be seen that the compound of formula I combined with spinetoram or spinosad showed good activity against C.

[0122] The mass ratio of the compound of formula I to ethyl spinetoram is 1:26-24:1, and the co-toxicity coefficient to bean pod borer is greater than 120, showing a synergistic effect; the mass ratio of the two is 1:22-24:1, and the co-toxicity coefficient to bean pod borer is greater than 130, and the synergistic effect is obvious; the mass ratio of the two is 1:18-16:1, and the co-toxicity coefficient to bean pod borer is greater than 140, and the synergistic effect is significant; and the mass ratio of the two is 32:1, and the co-toxicity coefficient is less than 120, showing an additive effect.

[0123] The mass ratio of the compound of formula I to spinosad is 1:20-25:1, and the co-toxicity coefficient to bean pod borer is greater than 120, showing a synergistic effect; the mass ratio of the two is 1:15-20:1, and the co-toxicity coefficient to bean pod borer is greater than 130, and the synergistic effect is obvious; the mass ratio of the two is 1:10-15:1, and the co-toxicity coefficient to bean pod borer is greater than 140, and the synergistic effect is significant; and the mass ratio of the two is 1:25, which shows an additive effect.

[0124] Example 2: Indoor biological activity test on Thysanoptera pests

[0125] Test target: Common giant thrips [Megalurothrips usitatus (Bagnall)] adults.

[0126] Test agents: compound of formula I, spinetoram, and spinosad original drug.

[0127] Preparation of drugs: After dissolving the above drugs in appropriate solvents, dilute them to appropriate concentrations with water containing 0.1% Tween-80. Use the treatment without drugs (containing all organic solvents and emulsifiers) as a blank control.

[0128] Test Method: The leaf tube pellicle method was used. Each concentration of the test solution was filled to the brim with a 4mL centrifuge tube. The tubes were shaken upside down several times, then the solution was discarded. The tubes were opened and placed on a shelf to dry before use. Several small holes were made in the bottom and cap of the centrifuge tubes using a sterile needle. The pore size was determined to prevent thrips from escaping. Fresh cowpea pods were cut into approximately 1.5cm segments with scissors and immersed in each concentration of the solution for 10 seconds. The treated cowpea pods were placed on absorbent paper to air dry, then placed in centrifuge tubes. Twenty adult cowpea thrips were aspirated using an insect aspirator, and the tubes were capped. The centrifuge tubes were then placed in a climate chamber at (26±1)°C, relative humidity (65±5)%, and a light intensity setting of 14h:10h. Mortality was assessed after 48 hours by gently touching the insects with the tip of a brush. Any insects that did not move were considered dead. Each tube constituted a single replicate, with four replicates per concentration.

[0129] Calculation method:

[0130] Based on the survey data, calculate the mortality rate of each treatment. Calculate as follows:

[0131]

[0132] Where:

[0133] P——mortality rate, in percentage (%);

[0134] K——indicates the number of dead insects, the unit is head;

[0135] N——represents the total number of insects processed, in heads.

[0136]

[0137] Where:

[0138] P1——adjusted mortality rate, in percentage (%);

[0139] P t ——Treatment mortality rate, expressed in percentage (%);

[0140] P0 - blank control mortality rate, in percentage (%).

[0141] If the control mortality rate is less than 5%, no correction is required; if the control mortality rate is between 5% and 20%, correction should be made according to the correction mortality formula; if the control mortality rate is greater than 20%, the test needs to be repeated.

[0142] The DPS statistical analysis system was used to analyze the toxicity regression equation, correlation coefficient and LC 50 The activity of the test agent on the biological test material is evaluated by the value.

[0143] The co-toxicity coefficient (CTC value) of the mixture is calculated as follows:

[0144]

[0145] Where:

[0146] ATI - measured toxicity index of mixture;

[0147] S——LC of standard pesticide 50 , the unit is milligrams per liter (mg / L);

[0148] M——LC of the mixture 50 , the unit is milligrams per liter (mg / L).

[0149] TTI=TI A ×P A +TI B ×P B

[0150] Where:

[0151] TTI – Theoretical Toxicity Index of Mixtures;

[0152] TI A ——Agent toxicity index;

[0153] P A ——The percentage of agent A in the mixture, in percentage (%);

[0154] TI B ——Toxicity index of agent B;

[0155] P B ——The percentage of agent B in the mixture, in percentage (%).

[0156]

[0157] Where:

[0158] CTC – Co-toxicity coefficient;

[0159] ATI - measured toxicity index of mixture;

[0160] TTI - Theoretical Toxicity Index of Mixture.

[0161] A co-toxicity coefficient (CTC) of ≥120 indicates a synergistic effect; a CTC of ≤80 indicates an antagonistic effect; and a CTC of 80 < CTC <120 indicates an additive effect. The results of the laboratory test are shown in the table below:

[0162] Table 3 Indoor biological activity test results of the compound of formula I combined with spinetoram against common thrips

[0163]

[0164]

[0165] Table 4 Indoor biological activity test results of the compound of formula I combined with spinosad against common thrips

[0166]

[0167] From the test results in the above tables (see Tables 3-4), it can be seen that compounding the compound of formula I with spinetoram or spinosad in an appropriate mass ratio has a certain synergistic effect on thrips.

[0168] When the compound of formula I is compounded with ethyl spinetoram at a mass ratio of 1:24 to 20:1, the co-toxicity coefficient is greater than 120, and a synergistic effect is shown on thrips; when the mass ratio of the compound of formula I to ethyl spinetoram is 1:17 to 18:1, the co-toxicity coefficient is greater than 130, and a significant synergistic effect on thrips is observed; when the mass ratio of the compound of formula I to ethyl spinetoram is 1:10 to 18:1, the co-toxicity coefficient is greater than 140, and a significant synergistic effect on thrips is observed.

[0169] When the mass ratio of the compound of formula I and spinosad is 1:27 to 32:1, the co-toxicity coefficient is greater than 120, and a synergistic effect is shown on thrips; when the mass ratio of the compound of formula I and spinosad is 1:18 to 18:1, the co-toxicity coefficient is greater than 130, and a significant synergistic effect is shown; when the mass ratio of the compound of formula I and spinosad is 1:18 to 12:1, the co-toxicity coefficient is greater than 140, and a significant synergistic effect is shown.

[0170] Field efficacy trials

[0171] Example 3: Control of Cowpea Pod Borer in the Field

[0172] The test site was a cowpea field in Shuixi Village, Lincheng Town, Shanghang County, Fujian Province. The pod borer had occurred seriously in the test site over the years. The soil was sandy loam with medium fertility.

[0173] Experimental design: The experiment was conducted in 8 treatments, each treatment was repeated 4 times, and there were 32 plots in total. Each plot was 20m2 in area. 2The experimental plots were arranged in random blocks.

[0174] Application method: The first application was conducted on April 10, 2024, and the second application was conducted 7 days later. Conventional spraying was performed using a Linong Jacto HD400 sprayer, spraying the cowpeas evenly from top to bottom. Five cowpea plants with sufficient larvae were randomly selected at five fixed points in each plot, for a total of 25 marked plants. The number of larvae on the flowers, pods, petioles, and leaves of the marked plants was surveyed (excluding larvae injected into pods, which were manually removed) as the pre-application baseline. Three and seven days after the final application, the flowers, pods, petioles, young stems, and pods of the marked plants were surveyed (larvae in pods were counted based on the number of holes bored into them). The population reduction rate and control efficacy were calculated.

[0175] The calculation formula is as follows:

[0176]

[0177] The results of the field efficacy test are shown below:

[0178] Table 5 Field efficacy test on control of cowpea pod borer

[0179]

[0180] Impact on cowpea and other organisms: During the field trial, no pesticide damage occurred in any treatment group, and no adverse effects were found on the surrounding environment and other beneficial organisms in the test area, indicating that the test agents were safe for cowpea growth at the doses provided.

[0181] Three days after application of the different agents, the results are shown in Table 7. The control efficacy of 18% Formula I compound·spinetosad wettable powder (2:1), 1.2% Formula I compound·spinetosad emulsion in water (5:1), 25% Formula I compound·spinetosad water dispersible granules (3:2), and 1.95% Formula I compound·spinetosad emulsion in water (1:12) were 93.27%, 88.93%, 90.97%, and 86.93%, respectively, demonstrating the good rapid-acting properties of the insecticidal compositions of the present invention. Seven days after application, the highest control efficacy of 18% Formula I compound·spinetosad wettable powder (2:1) was 97.28%. The four combination treatments exhibited good long-lasting efficacy compared to the single-agent control.

[0182] Example 4: Control of cowpea thrips in the field

[0183] The experimental site is located in the cowpea field of Dongqiaojia Village, Jinzhuang Town, Sishui County, Jining City, Shandong Province. The experimental site has a flat terrain, medium soil fertility, and convenient irrigation and drainage.

[0184] Experimental design: The experiment set up 6 treatments, including 5 chemical treatments and 1 water control. Each treatment was repeated 4 times, and each plot was 25m2.2 The plots are randomly arranged in groups, and isolation zones are set up between the plots.

[0185] Test Method: The pesticide was applied on April 5, 2024, using a backpack electric sprayer to evenly spray the plant leaves until no drips remained. The base insect population was assessed before application, and efficacy was assessed 3 and 7 days after application. Samples were collected at five locations per plot, with two cowpea plants surveyed at each location. Two flowers per plant were marked, and the number of live insects on all 20 flowers was counted. The insect population reduction rate and control efficacy were calculated.

[0186] Calculation method of prevention effect:

[0187]

[0188] Field efficacy test results:

[0189] Table 6 Field efficacy test on control of cowpea thrips

[0190]

[0191] Safety investigation: During the field trial, no pesticide damage occurred in any treatment group, and no adverse effects were found on the surrounding environment and other beneficial organisms in the test area, indicating that the test agents were safe for cowpea growth at the doses provided.

[0192] The results showed (see Table 6) that the control effects of different agents varied greatly. 3 and 7 days after application, the fast-acting and long-lasting effects of 2% Formula I compound·spinosad microemulsion (3:1) and 17.5% Formula I compound·spinosad suspension (5:2) in controlling thrips were significantly better than those of other agents.

[0193] In summary, through indoor toxicity assays and field efficacy tests, it can be seen that the insecticidal composition of the present invention has a good control effect on Lepidoptera, Thysanoptera and Coleoptera pests, is safe for target crops, has significant control effects, and is superior to a single agent in delaying the development of drug resistance and prolonging the lasting effect.

[0194] Although the present application describes specific embodiments in detail by way of example, the disclosure of the present application may adopt various modifications and alternative forms. However, it should be understood that the disclosure of the present application is not limited to the specific forms disclosed. On the contrary, the disclosure of the present application covers all modifications, equivalents and alternative forms within the scope of the disclosure of the present application, and the scope of the present application is limited by the appended claims and their legal equivalents.

Claims

1. An insecticide composition containing a biogenic insecticide, characterized in that: The active ingredients of the insecticide composition include a compound of formula I and a biogenic insecticide. The structure of the compound of formula I is as follows: (Formula I), the biogenic insecticide is spinosad, and the mass ratio of the compound of Formula I to spinosad is 1:27~32:

1.

2. The insecticidal composition according to claim 1, characterized in that The mass ratio of the compound of formula I to spinosad is 1:20 to 25:

1.

3. The insecticidal composition according to claim 2, characterized in that The mass ratio of the compound of formula I to spinosad is 1:18~24:

1.

4. The insecticidal composition according to claim 1, characterized in that The total weight of the insecticide composition is 100 wt %, and the total weight of the compound of formula I and the biogenic insecticide accounts for 0.01% to 80% of the total weight of the insecticide composition.

5. The insecticidal composition according to claim 1, characterized in that In addition to the active ingredients, the insecticide composition also contains auxiliary ingredients allowed in pesticides, and the auxiliary ingredients are selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoaming agents, solvents, preservatives, stabilizers, synergists or carriers.

6. The insecticidal composition according to claim 1, characterized in that The insecticide composition is prepared into a formulation form permitted by pesticides, and the formulation form is a solid preparation or a liquid preparation.

7. The insecticidal composition according to claim 6, characterized in that The solid preparation is a water-dispersible granule or a wettable powder; the liquid preparation is a suspension, a microemulsion, a dispersible oil suspension or an aqueous emulsion.

8. Use of the insecticidal composition according to any one of claims 1 to 7 for controlling agricultural, horticultural or forestry pests.

9. The use according to claim 8, characterized in that The insecticidal composition according to any one of claims 1 to 7 is applied to pests to be controlled or to the medium in which they grow.

Citation Information

Patent Citations

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    CN117800929A