Insecticidal composition and application thereof

Abstract

The invention belongs to the field of pesticides, and relates to an insecticidal composition. Effective components of the insecticidal composition comprise an active component A and an active component B, the active component A is a compound shown as a formula (I), the active component B is any one of Indazapyraxamet and Nicofluprole, and the mass ratio of the active component A to the active component B is (1: 50)-(34: 1). The insecticidal composition has the advantages of synergism, resistance delay and the like, and is used for preventing and treating resistant pests.

Description

[0001] This invention application is a divisional application of application number 2024112473550, application date 20240906, and invention title "An insecticidal composition and its application". Technical Field

[0002] This invention belongs to the field of pesticide and insecticide technology, specifically relating to an insecticidal composition and its application. Background Technology

[0003] Flupyroxystrobin is a methoxyacrylate insecticide with high activity against dipteran pests such as fruit flies, leaf miners, leaf miners, and leek gnats, as well as thrips. Its chemical name is (2E)-3-methoxy-2-(2-{[4-(trifluoromethyl)pyridin-2-yl]oxy}phenyl)prop-2-enoic acid methyl ester, and its chemical structural formula is:

[0004]

[0005] Indazapyroxamet is a pyridine-containing amide insecticide developed by FMC Corporation for the control of Thysanoptera or Hemiptera pests such as western flower thrips, potato leafhoppers, aphids, and whiteflies. Its chemical name is N-(1-methylcyclopropyl)-2-(3-pyridyl)-2H-benzopyrazole-4-carboxamide, and its chemical structural formula is:

[0006]

[0007] Nicofluprole is a nicotinamide compound with broad-spectrum insecticidal activity, exhibiting excellent insecticidal activity against lepidopteran, hemiptera, and mites. Its chemical name is 2-chloro-N-cyclopropyl-5-(1-(2,6-dichloro-4-(perfluoropropane-2-yl)phenyl)-1H-pyrazol-4-yl)-N-methylnicotinamide, and its chemical structural formula is as follows:

[0008]

[0009] In agricultural production, long-term, continuous, and high-dose use of single-variety or single-mode chemical insecticides can easily lead to problems such as insecticide resistance and the evolution of resistance in pests. The rational combination or mixing of insecticides has advantages such as reducing pesticide dosage, improving control efficacy, and delaying the occurrence and development of insecticide resistance, making it one of the most effective methods to solve these problems. By mixing compound (I) with Flupyroxystrobin, Indazapyroxamet, and Nicofluprole, it is possible to achieve rapid and comprehensive control of different pests, broaden the control spectrum, improve pesticide efficacy, and reduce the development of insecticide resistance. Currently, no reports have been found regarding this aspect. Summary of the Invention

[0010] The purpose of this invention is to provide an insecticidal composition that has a synergistic effect, reduces resistance, and has low usage cost.

[0011] To achieve the above objectives, the technical solution adopted by the present invention is as follows: an insecticidal composition comprising active ingredient A and active ingredient B, wherein active ingredient A is a compound of formula (I) with the following structural formula:

[0012] The active ingredient B is any one of Flupyroxystrobin, Indazapyroxamet, and Nicofluprole;

[0013] Furthermore, the mass ratio of active ingredient A to active ingredient B is 1:50 to 34:1;

[0014] Furthermore, the mass ratio of active ingredient A to active ingredient B is 1:24 to 28:1;

[0015] Furthermore, the mass ratio of the compound of formula (I) to Flupyroxystrobin is 1:27 to 27:1, such as 1:27, 1:18, 1:9, 2:3, 3:2, 9:2, 18:1, 27:1 or any value between these values;

[0016] Furthermore, the mass ratio of the compound of formula (I) to Flupyroxystrobin is 1:18 to 27:1;

[0017] Furthermore, the mass ratio of the compound of formula (I) to Flupyroxystrobin is 1:18, 1:9, 2:3, 3:2, 9:2, 18:1, or 27:1;

[0018] Furthermore, the mass ratio of the compound of formula (I) to Indazapyroxamet is 1:50 to 30:1, such as 1:50, 1:32, 1:22, 1:16, 1:11, 1:10, 1:6, 2:11, 2:5, 5:2, 10:3, 11:2, 17:1, 18:1, 24:1, 30:1 or any value between these values;

[0019] Furthermore, the mass ratio of the compound of formula (Ⅰ) to Indazapyroxamet is 1:32 to 24:1;

[0020] Furthermore, the mass ratio of the compound of formula (I) to Indazapyroxamet is 1:32, 1:22, 1:16, 1:11, 1:10, 1:6, 2:11, 2:5, 5:2, 10:3, 11:2, 17:1, 18:1, 24:1;

[0021] Furthermore, the mass ratio of the compound of formula (I) to Nicofluprole is 1:24 to 34:1, such as 1:24, 1:14, 1:8, 2:3, 7:1, 14:3, 28:1, 34:1 or any value between these values;

[0022] Furthermore, the mass ratio of the compound of formula (I) to Nicofluprole is 1:24 to 28:1;

[0023] Furthermore, the mass ratio of the compound of formula (I) to Nicofluprole is 1:24, 1:14, 1:8, 2:3, 7:1, 14:3, or 28:1;

[0024] Furthermore, based on a total mass of 100 wt% of the insecticidal composition, the sum of the contents of active ingredient A and active ingredient B in the insecticidal composition is 0.5% to 90%.

[0025] Furthermore, based on a total mass of 100 wt% of the insecticidal composition, the sum of the contents of active ingredient A and active ingredient B in the insecticidal composition is 1% to 85%.

[0026] Furthermore, the sum of the contents of active ingredient A and active ingredient B in the insecticidal composition is 1% to 85%;

[0027] Furthermore, in addition to the active ingredient, the insecticidal composition also includes agriculturally acceptable auxiliary ingredients, which are selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoamers, solvents, preservatives, stabilizers, synergists or carriers.

[0028] Furthermore, the insecticidal composition further includes an adjuvant selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoamers, solvents, preservatives, stabilizers, synergists, and carriers;

[0029] The wetting agent is selected from one or more of the following: alkylbenzene sulfonates, alkylnaphthalene sulfonates, lignin sulfonates, sodium dodecyl sulfate, sodium dioctyl succinate sulfonate, α-olefin sulfonates, alkylphenol polyoxyethylene ethers, castor oil polyoxyethylene ethers, alkylphenol ethoxylates, fatty alcohol ethoxylates, sodium fatty alcohol polyoxyethylene ether sulfate, silkworm excrement, soapberry powder, soapberry powder, SOPA, detergents, emulsifiers 2000 series, and wetting and penetrating agents F; and / or

[0030] The dispersant is selected from one or more of the following: lignin sulfonates, alkyl naphthalene sulfonates formaldehyde condensates, naphthalene sulfonates, tristyrylphenol ethoxylate phosphates, fatty alcohol ethoxylates, alkylphenol polyoxyethylene ethers, alkylphenol polyoxyethylene ether methyl ether condensates sulfates, fatty amine polyoxyethylene ethers, glycerol fatty acid ester polyoxyethylene ethers, polycarboxylates, polyacrylic acids, phosphates, EO-PO block copolymers, and EO-PO graft copolymers; and / or

[0031] The emulsifier is selected from one or more of the following: calcium dodecylbenzenesulfonate, alkylphenol formaldehyde resin polyoxyethylene ether, phenethylphenol polyoxyethylene polyoxypropylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, styrene-phenol polyoxyethylene ether, castor oil polyoxyethylene ether, and alkylphenol ether phosphate; and / or

[0032] The thickener is selected from one or more of xanthan gum, organobentonite, gum arabic, sodium alginate, magnesium aluminum silicate, carboxymethyl cellulose, and silica; and / or

[0033] 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

[0034] Antifreeze is selected from one or more of alcohols, alcohol ethers, chlorinated hydrocarbons, and inorganic salts; and / or

[0035] Defoamer selected from C 10 -C 20 Saturated fatty acid compounds, silicone oil, silicone compounds, C8-C 10 One or more of the fatty alcohols; and / or

[0036] The solvent is selected from one or more of benzene, toluene, xylene, mesitylene, methanol, ethanol, isopropanol, n-butanol, dimethyl sulfoxide, dimethylformamide, cyclohexanone, hydrocarbon carbonates, diesel oil, solvent oil, vegetable oil, vegetable oil derivatives, and water; and / or

[0037] The preservative is selected from one or more of propionic acid, sodium propionate, sorbic acid, sodium sorbate, potassium sorbate, benzoic acid, sodium benzoate, sodium p-hydroxybenzoate, methyl p-hydroxybenzoate, Kathon, and 1,2-benzisothiazolin-3-one; and / or

[0038] The stabilizer is selected from one or more of the following: 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, silica, talc, montmorillonite, and starch; and / or

[0039] Synergists are selected from synergistic phosphorus, synergistic ether; and / or

[0040] The carrier is selected from one or more of the following: ammonium salts, ground natural minerals, ground artificial minerals, silicates, resins, waxes, solid fertilizers, water, organic solvents, mineral oils, vegetable oils, and vegetable oil derivatives.

[0041] Furthermore, the insecticidal composition can be prepared into an agriculturally permissible formulation, wherein the formulation is selected from solid and / or liquid formulations;

[0042] Furthermore, the solid dosage forms include powders, granules, balls, tablets, strips, wettable powders, oil-dispersible powders, emulsion powders, water-dispersible granules, emulsion granules, water-dispersible tablets, soluble powders, soluble tablets, or soluble granules;

[0043] Furthermore, the liquid formulation includes soluble agents, colloids, oils, spreading oils, emulsions, latexes, dispersible liquids, ointments, water emulsions, oil emulsions, microemulsions, lipids, suspensions, microcapsule suspensions, oil suspensions, dispersible oil suspensions, suspensions, microcapsule suspension-suspensions, microcapsule suspension-water emulsions, or microcapsule suspension-suspension emulsions;

[0044] Furthermore, the solid dosage form is selected from wettable powders and water-dispersible granules; the liquid dosage form is selected from emulsifiable concentrates, water-in-oil emulsions, microemulsions, suspensions, suspension emulsions, and dispersible oil suspensions.

[0045] Furthermore, the solid dosage form is selected from wettable powders and water-dispersible granules; the liquid dosage form is selected from emulsifiable concentrates and suspension concentrates.

[0046] Application of the insecticidal composition of the present invention in the control of agricultural and forestry pests and sanitary pests;

[0047] The insecticidal composition of the present invention can be used to control pests on fruit trees, vegetables, ornamental plants, tea, cotton, and cereal crops;

[0048] Furthermore, the aforementioned agricultural and forestry pests and sanitary pests are Lepidoptera and Thysanoptera pests;

[0049] Furthermore, the aforementioned Lepidoptera pests include: *Adoxophyes spp.*, *Adoxophyes orana*, *Agrotis spp.* (root cutter), *Agrotis ipsilon* (black cutworm), *Alabamaargillacea* (cotton leafworm), *Amorbia cuneana*, *Amyelosis transitella* (navel orange moth), *Anacamptodes defectaria*, *Anarsia lineatella* (peach twig borer), *Anomis sabulifera* (jute looper), *Anticarsia gemma ta lis*, *Archips argyrospila* (fruittree leafroller), and *Archips* (rose leafroller). *Argyrotaenia spp.* (rose leaf roller), *Argyrotaenia citrana* (orange tortrix), *Autographa gamma*, *Bonagota cranaodes*, *Borbo cinnara* (rice leaf folder), *Bucculatrix thurberiella* (cotton leafperforator), *Caloptilia spp.* (leaf miners), *Ca pua reticulana*, *Carposina niponensis* (peach fruit moth), *Chilo spp.*, *Chlumetia transversa* (mango shoot borer), *Choristoneurarosaceana* (obliquebanded rose leaf roller) Leafroller), and species of the genus Chrysodeixis spp.The following species are listed: *Cnaphalocerus medinalis* (grass leafroller), *Colias* spp., *Conpomorpha cramerella*, *Cossus cossus* (carpenter moth), *Crambus* spp. (soil webworms), *Cydiafunebrana* (plum fruit moth), *Cydia molesta* (oriental fruit moth), *Cydia nignicana* (pea moth), *Cydiapomonella* (codling moth), *Darna diducta*, and *Diaphania* spp. (stem borer). *Diatraea* spp. (stalk borers), *Diatraeas accharalis* (sugarcane borer), *Diatraea graniosella* (southwester corn borer), *Earias* spp. (cotton bollworm), *Earias insulata* (Egyptian cotton bollworm), *Earias vitella* (rough northern bollworm), *Ecdytopopha aurantianum*, *Elasmopalpus lignosellus* (lesser cornstalk borer), *Epiphysias postruttana* (light brown apple moth), *Ephestia* spp. (flour moths), *Ephestia* cautella (almond moth), Tobacco moth (Ephestia elutella), Mediterranean flour moth (Ephestia kuehniella), and species of the genus Epimeces (Epimeces spp.).), Epinotia aporema, Erionotathrax (banana skipper), Eupoecilia ambiguella (grape leafroller), Euxoa auxiliaris (army cutworm), Feltia spp. (root cutter), Gortyna spp. (stemborers), Grapholitamolesta (oriental fruit moth), Hedylepta indicate (bean leaf webber), Helicoverpa sp p. (noctus), Helicoverpa armigera, Helicoverpa zea, Heliothis spp., Heliothis virescens, cabbage webworm (Hellula undalis), root borers (Indarbela spp.), tomato codling moth (Keiferia lycopersicella), eggplant orbonalis, spiny leafminer (Leucoptera malifoliella), slender moth (Lithocollectis spp.), grape fruit moth (Lobesia botrana), western bean cutworm (Loxagrotis spp.), gypsy moth (Lymantria dispar), apple leaf miner (Lyonetia clerkella), and oil palm bagworm (Mahasena corbetti). bagworm), tent caterpillar (Malacosoma spp.)(tent caterpillars), cabbage armyworm (Mamestra brassicae), bean pod borer (Maruca testulalis), bagworm (Metisa plana), true armyworm (Mythimna unipuncta), elegantalis (Neoleucinodes elegantalis), depunctalis (Nymphula depunctalis), winter inchworm (Operophtherabrumata), European corn borer (Ostrinia nubilalis), Oxydiavesulia, common currant tortrix (Pandemis cerasana), brown apple tortrix (Pandemis heparana), African swallowtail butterfly (Papilio demodocus), pink bollworm (Pectinophora gossypiella). The following species are listed: bollworm, Peridroma saucia (variegated cutworm), Perileucoptera coffeella (white coffee leafminer), Phthorimaea operculella (potato tuber moth), Phylloocnisitis citrella (citrus leafminer), Phyllonorycter spp. (leek moth), Pieris rapae (cabbage white butterfly), Plathapena scabra (alfalfa green armyworm), Plodia interpunctella (Indian grain moth), Plutellaxylostella (diamondback moth), Polychrosis viteana (grape leafroller), Prays endocarpa (citrus fruit borer), and Prays endocarpa (olive borer). oleae (olive moth), species of the genus Pseudaletia (Pseudaletia spp.).(Noctus), Spodoptera litura Fabricius, Pseudaletia unipunctata (armyworm), Pseudoplusia includes (soybean noctus), Rachiplusia nu, Chilo suppressalis (Walker), Scirpophaga incertulas, Sesamia spp. (stem borers), Sesamia inferens (pink rice stem borer), Spodoptera frugiperda (JESmmith), Sesamia nonagrioides, Setora nitens, Sitotroga cerealella (Angoumois grain moth), Sparganothispilleriana, Spodoptera spp.), beet armyworm (Spodoptera exigua), fall armyworm (Spodoptera fugiperda), southern armyworm (Spodoptera oridania), Synanthedon spp., Thecla basilides, Thermisia gemmatalis, clothes moth (Tineola bisselliella), cabbage white butterfly (Trichoplusia ni), cabbage white butterfly (Pierisrapae Linne), tomato leafminer (Tuta absoluta);

[0050] Furthermore, the aforementioned Thysanoptera pests include: palm thrips (Thrips palmiKarny), tobacco thrips (Thrips tabaci), brown tobacco thrips (Frankliniella fusca), alfalfa flower thrips (Frankliniella occidentalis), western flower thrips (Frankliniella shultzei), corn thrips (Frankliniella williamsi), greenhouse thrips (Heliothrips haemorrhaidalis), greenhouse thrips (Rhiphiphorothrips cruentatus), spp. of the genus *Scirtothrips*, citrus thrips (*Scirtothrips citri*), and yellow tea thrips (*Scirtothrips*). dorsalis (yellow tea thrips), Taeniothrips rhopalantennalis, and Thripsspp.;

[0051] Furthermore, the lepidopteran pests mentioned are cabbage caterpillar, diamondback moth, beet armyworm, cotton bollworm, two-spotted cutworm, rice stem borer, and cotton bollworm;

[0052] Furthermore, the aforementioned Thysanoptera pests are western flower thrips, tobacco thrips, palm thrips, and watermelon thrips;

[0053] The present invention also provides a method of using the insecticidal composition as described above, specifically applying an effective dose to the pest that needs to be controlled or to the medium in which it grows.

[0054] The insecticidal composition of the present invention has the following beneficial effects:

[0055] 1) The insecticidal composition of the present invention exhibits a synergistic effect within a certain ratio range, resulting in significant control efficacy;

[0056] 2) The insecticidal composition of the present invention can delay the development of pesticide resistance in pests, is environmentally friendly, can reduce the amount of pesticides used, and reduce the cost of pest control. Detailed Implementation

[0057] The present invention will be further described below with reference to the embodiments. The percentages in the embodiments are all weight percentages, but the present invention is not limited thereto.

[0058] The compositions of the present invention can be provided in formulation form. They can be formulated as suspensions, emulsifiable concentrates, water-dispersible granules, water-emulsions, granules, wettable powders, dispersible oil suspensions, etc., as needed. The content of the active ingredient in the compositions of the present invention depends on the application rate when used alone, as well as on the mixing ratio and the degree of synergistic effect. The optimal range of active ingredient content varies depending on the formulation type of the composition.

[0059] Formulation preparation examples

[0060] Example 1:

[0061] 25% Formula (I) compound·flupyroxystrobin suspension (15+10)

[0062] Formula: 15% compound of formula (I), 10% flupyroxystrobin,

[0063] 4% fatty alcohol polyoxyethylene ether phosphate, 2% sodium lignosulfonate, 2.5% alkyl aryl polyoxyethylene ether polyoxypropylene ether, 1% magnesium aluminum silicate, 0.2% xanthan gum, 0.5% methyl paraben, 5% ethylene glycol, 0.5% silicone defoamer, deionized water to make up the balance;

[0064] Preparation method: Add the active ingredient to the wetting and dispersing agent and defoamer, use zirconia beads, and wet pulverize with a sand mill to D. 90 (90% of the particles have a particle size) <10μm to obtain a pulverized slurry. Thickener, antifreeze, preservative, etc. are added to the pulverized slurry and mixed evenly. Deionized water is added to make up to 100%, and the mixture is sheared at high speed to prepare the suspension formulation of the composition of the present invention.

[0065] Example 2:

[0066] 28% Formula (I) Compound · indazapyroxamet Suspension (8+20)

[0067] Formula: 8% compound of formula (I), 20% indazapyroxamet,

[0068] 2% sodium lignosulfonate, 2.5% alkyl aryl polyoxyethylene ether polyoxypropylene ether, 4% alkylphenol polyoxyethylene ether phosphate, 1% magnesium aluminum silicate, 0.2% xanthan gum, 0.5% methyl paraben, 5% ethylene glycol, 0.5% silicone defoamer, deionized water to make up the balance;

[0069] Preparation method: Same as in Example 1.

[0070] Example 3:

[0071] 20% Formula (I) Compound · Nicofluprole Suspension (8+12)

[0072] Formula: 8% compound of formula (I), 12% nicofluprole,

[0073] 4.2% styrene-phenol ethoxylated phosphate, 2.5% sodium lignosulfonate, 2.5% alkyl aryl polyoxyethylene ether polyoxypropylene ether, 1% magnesium aluminum silicate, 0.3% xanthan gum, 0.5% sodium sorbate, 5% ethylene glycol, 0.5% silicone defoamer, deionized water to make up the balance;

[0074] Preparation method: Same as in Example 1.

[0075] Example 4:

[0076] 45% Formula (I) compound·flupyroxystrobin water-dispersible granules (25+20)

[0077] Formula: 25% compound of formula (I), 20% flupyroxystrobin,

[0078] 2% sodium lignosulfonate, 6% sodium polycarboxylate, 5% naphthalene sulfonate formaldehyde condensate, 3.5% sodium dodecyl sulfate, 5% silica, 2% bentonite, and kaolin to make up the balance;

[0079] Preparation method: According to the formula ratio, the active ingredients are added to the carrier, and surfactants and other functional additives are added thereto. After mixing, the mixture is pulverized by air jet and then an appropriate amount of water is added. After kneading, granulation, drying and sieving, the water-dispersible granule formulation of the composition of the present invention can be prepared.

[0080] Example 5:

[0081] 50% Formula (I) compound · indazapyroxamet water-dispersible granules (37.5+22.5)

[0082] Formula: 37.5% compound of formula (I), 22.5% indazapyroxamet,

[0083] 6% sodium polycarboxylate, 2.5% sodium lignosulfonate, 6% naphthalene sulfonate formaldehyde condensate, 3.5% sodium dodecyl sulfate, 3% ammonium sulfate, 4% silica, 2% bentonite, and kaolin to make up the balance;

[0084] Preparation method: Same as in Example 4.

[0085] Example 6:

[0086] 1.4% Formula (I) compound · indazapyroxamet water emulsion (1+0.4)

[0087] Formula: 1% compound of formula (I), 0.4% indazapyroxamet,

[0088] 12% Trimethylbenzene, 10% Cyclohexanone, 1% Calcium Dodecylbenzenesulfonate, 1% Sodium Fatty Alcohol Polyoxyethylene Ether Sulfate, 6.5% EO / PO Block Copolymer, 5% Glycerol, 1.5% Glycerin, 0.1% Silicone Defoamer, 0.2% Xanthan Gum, 0.1% Sodium Benzoate, Deionized Water to make up the balance;

[0089] Preparation method: According to the formulation ratio in the example, the active ingredient is dissolved in the solvent and an emulsifier is added to form a homogeneous oil phase. Deionized water and antifreeze are mixed together to form a homogeneous aqueous phase. Under high-speed shearing, the aqueous phase is added to the oil phase to form a well-dispersed water-emulsion formulation.

[0090] Example 7:

[0091] 5.2% Formula (I) compound nicofluprole water emulsion (3.2+2)

[0092] Formulation: 3.2% compound of formula (I), 2% nicofluprole,

[0093] 15% Cyclohexanone, 12% Trimethylbenzene, 1% Styrene-phenol ethoxylated phosphate, 6% EO / PO block copolymer, 5% Glycerol, 2% Glycerin, 0.1% Silicone defoamer, 0.1% Xanthan gum, 0.1% Sodium benzoate, deionized water to make up the balance;

[0094] Preparation method: Same as in Example 6.

[0095] Example 8:

[0096] 20% Formula (I) Compound · Nicofluprole Dispersible Oil Suspension (8+12)

[0097] Formula: 8% compound of formula (I), 12% nicofluprole,

[0098] 2.5% fatty alcohol polyoxyethylene ether, 15% castor oil polyoxyethylene ether, 0.3% organic bentonite, 0.2% organosilicon defoamer, 2% succinate sulfonate, and soybean oil to make up the balance;

[0099] Preparation method: According to the formula ratio, the active ingredients, surfactants and other functional additives are placed in the reaction vessel in sequence, mixed with oil until uniform, and then subjected to high-speed shearing, wet sand milling and finally homogenized filtration to prepare the dispersible oil suspension formulation of the composition of the present invention.

[0100] Indoor bioactivity assay

[0101] Refer to agricultural industry standards:

[0102] "Guidelines for Indoor Bioassay Testing of Pesticides - Insecticides Part 6: Immersion Method" (NY / T 1154.6-2006);

[0103] "Guidelines for Indoor Bioassay Testing of Pesticides - Insecticides Part 14: Leaf Dipping Method" (NY / T 1154.14-2008);

[0104] "Guidelines for Indoor Bioassay Testing of Pesticides - Part 7: Determination of Combined Effects of Mixtures" (NY / T1154.7-2006), etc.

[0105] Specific indoor toxicity tests:

[0106] 1) Lepidoptera larvae: A combination of leaf soaking and insect soaking method;

[0107] Test insect age: A sensitive population that has been raised indoors for multiple generations was selected, and healthy, consistent second-instar lepidopteran larvae were selected.

[0108] Use tweezers to soak fresh cabbage slices in the solution for 10 seconds, then remove them and let the solution air dry naturally. Place the cabbage slices in a petri dish lined with moisturizing filter paper. Place 16 second-instar lepidopteran larvae in the solution for 5 seconds, then use filter paper to absorb the excess solution. Place the test insects in a petri dish with leaves soaked at the appropriate concentration.

[0109] Each treatment was repeated four times, with a blank treatment serving as a control. The treated insects were then reared in an AI-controlled culture room at 26±1℃, with a light duration of L:D = 16h:8h and a relative humidity of 60%.

[0110] Investigation method: The mortality of test insects was investigated 48 hours after the treatment with the agent. The criteria for judging the mortality of test insects were obvious shrinkage of the insect body or inability to crawl normally when pierced by a needle. The number of dead insects was recorded.

[0111] 2) Adult Thysanoptera: Glass rolling tube method;

[0112] Test insect age: A sensitive population that has been raised indoors for multiple generations was selected, and healthy, uniform female adult tsioptera were selected.

[0113] After rolling the glass tube evenly with 250ul of medicine, use a punch to cut the cabbage leaves into 1.5cm diameter round pieces. Use tweezers to immerse the fresh cabbage pieces in the medicine for 10 seconds, then remove them and let the medicine air dry naturally. Place the cabbage pieces in the glass tube, and suck 20 adult female Thysanoptera into the glass tube using an insect suction device. Seal the tube with 200-mesh gauze.

[0114] Each treatment was repeated four times, with a blank treatment serving as a control. The treated insects were then reared in an AI-controlled culture room at 26±1℃, with a light duration of L:D = 16h:8h and a relative humidity of 60%.

[0115] Investigation method: The mortality of test insects was investigated 48 hours after the treatment with the agent. The criterion for judging the mortality of test insects was that they could not crawl normally when pricked with a needle. The number of dead insects was recorded.

[0116] Data statistics and analysis:

[0117] Based on the survey data, calculate the adjusted mortality rate for each treatment. Use the following formula to calculate the mortality rate, and round the results to two decimal places:

[0118]

[0119] In the formula:

[0120] P – Mortality rate, expressed as a percentage (%);

[0121] K represents the number of dead insects, in heads;

[0122] N represents the total number of insects treated, in units of heads.

[0123]

[0124] In the formula:

[0125] P1 – Corrected mortality rate, in percentage (%);

[0126] P t —The mortality rate is expressed as a percentage (%).

[0127] P0 – Mortality rate in the blank control group, expressed as a percentage (%).

[0128] If the control mortality rate is <5%, no correction is needed; if the control mortality rate is between 5% and 20%, correction should be made according to formula (2); if the control mortality rate is >20%, the experiment needs to be repeated.

[0129] The data was processed using probability value analysis. The DPS statistical analysis system can be used to analyze the data and determine the toxicity regression line and LC. 50 The values, their 95% confidence limits, and correlation coefficients r are used to evaluate the activity of the test reagent on the biological sample.

[0130] The co-toxicity coefficient (CTC value) of the mixture is calculated using the following formula:

[0131]

[0132] In the formula:

[0133] ATI – Actual Measured Toxicity Index of Mixtures;

[0134] S – LC50 of standard insecticides 50 The unit is milligrams per liter (mg / L);

[0135] M – LC of the mixture 50 The unit is milligrams per liter (mg / L).

[0136] TTI = TI A *P A +TI B *P B

[0137] In the formula:

[0138] TTI – Theoretical Toxicity Index of Mixtures;

[0139] TI A —A. Toxicity index of drug A;

[0140] P A —Percentage content of drug A in the mixture, expressed as percentage (%);

[0141] TI B —Toxicity index of drug B;

[0142] P B —Percentage content of agent B in the mixture, expressed as percentage (%).

[0143]

[0144] In the formula:

[0145] CTC – Cotoxicity Coefficient;

[0146] ATI – Actual Measured Toxicity Index of Mixtures;

[0147] TTI – Theoretical Toxicity Index of Mixtures.

[0148] The co-toxicity coefficient of the compound is ≥120, which shows a synergistic effect; CTC≤80 shows an antagonistic effect; and 80<CTC<120 shows an additive effect.

[0149] Experimental results:

[0150] Combined toxicity of mixed pesticides against cabbage caterpillars:

[0151] The results in Tables 1 and 2 show that the compound of formula (Ⅰ) combined with Indazapyroxamet and Nicofluprole has a good synergistic effect on cabbage caterpillars, and under a certain mass ratio, it shows a significant synergistic effect.

[0152] When the mass ratio of compound (I) to Indazapyroxamet is 1:32 to 30:1, the co-toxicity coefficient of the control efficacy against cabbage caterpillar is greater than 80, showing an additive or synergistic effect; when the mass ratio of compound (I) to Indazapyroxamet is 1:32 to 18:1, the co-toxicity coefficient of the control efficacy against cabbage caterpillar is greater than 120, showing a synergistic effect.

[0153] Table 1 shows the toxicity test results of compound (I) and different ratios of Indazapyroxamet against cabbage caterpillars.

[0154]

[0155] When the mass ratio of compound (I) to Nicofluprole is 1:24 to 34:1, the co-toxicity coefficient of the control efficacy against cabbage caterpillar is greater than 80, indicating an additive or synergistic effect; when the mass ratio of compound (I) to Nicofluprole is 1:24 to 28:1, the co-toxicity coefficient of the control efficacy against cabbage caterpillar is greater than 120, indicating a synergistic effect.

[0156] Table 2 shows the toxicity test results of compound (I) and different ratios of Nicofluprole against cabbage caterpillars.

[0157]

[0158]

[0159] Combined toxicity of mixed pesticides against tobacco thrips:

[0160] The results in Tables 3 and 4 show that the compound of formula (Ⅰ) combined with Flupyroxystrobin and Indazapyroxamet has a good synergistic effect on tobacco thrips, and under a certain mass ratio, it shows a significant synergistic effect.

[0161] When the mass ratio of compound (I) to Flupyroxystrobin is 1:27 to 27:1, the co-toxicity coefficient of the control efficacy against tobacco thrips is greater than 80, indicating an additive or synergistic effect; when the mass ratio of compound (I) to Flupyroxystrobin is 1:18 to 27:1, the co-toxicity coefficient of the control efficacy against tobacco thrips is greater than 120, indicating a synergistic effect.

[0162] Table 3 shows the toxicity test results of compound (I) and different ratios of Flupyroxystrobin to thrips.

[0163]

[0164] When the mass ratio of compound (I) to Indazapyroxamet is 1:50 to 24:1, the co-toxicity coefficient of the control efficacy against tobacco thrips is greater than 80, showing an additive or synergistic effect; when the mass ratio of compound (I) to Indazapyroxamet is 1:22 to 24:1, the co-toxicity coefficient of the control efficacy against tobacco thrips is greater than 120, showing a synergistic effect.

[0165] Table 4 shows the toxicity test results of compound (I) and different ratios of Indazapyroxamet to thrips.

[0166]

[0167] Field efficacy examples

[0168] Field Trial 1

[0169] Experimental crop: Leeks (Dajingou);

[0170] Conditions of the experimental field: moderate fertility, convenient irrigation and drainage, and sandy soil.

[0171] Experimental target: Leek thrips;

[0172] Test location: Qiantianbutou Village, Haiyang City, Yantai City;

[0173] Test date: November 8, 2022;

[0174] Application method: In the experimental field, manual application of pesticides was carried out using a backpack electric sprayer according to the design plan. First, the whole plant was sprayed, and then the back of the leaves was sprayed with more attention. The spraying machine was a 3WBS-16 backpack electric sprayer, and the spray volume was 30L / mu.

[0175] Experimental environment: All experimental plots were cultivated under uniform conditions, with the same level of fertilizer and water management, and the soil was clay loam with good water and fertilizer conditions;

[0176] Test reagents:

[0177] Table 5 Field Trial Design and Pesticide Dosage

[0178]

[0179] Experimental method: Apply the pesticide once at the initial stage of thrips infestation in leeks (when small white spots appear on the leaves).

[0180] Cell size and duplication: randomized block arrangement, cell size 25m² 2 Each treatment was repeated 4 times.

[0181] Survey method: Five random sampling points were taken in each plot. The thrips were tapped three times at each random sampling point (5 clumps (20 plants)). The number of thrips shaken into the white porcelain plate was counted. The initial insect population was investigated before the pesticide was applied, and the number of residual insects was investigated 1 day and 7 days after the pesticide was applied.

[0182] Calculation formulas and data analysis:

[0183]

[0184] Results of field efficacy trials:

[0185] Table 6 shows the field control efficacy of various pesticides against leek thrips. The table indicates that, one day after application, 25% compound (I)·flupyroxystrobin suspension (15+10) and 28% compound (I)·indazapyroxamet suspension (8+20) exhibited better rapid efficacy against leek thrips, with an effective dosage of 10 g ai / hm. 2 The control efficacy was 87.35% and 86.19% respectively. With increasing time, 7 days after application, the control efficacy of 25% compound (I)·flupyroxystrobin suspension (15+10) and 28% compound (I)·indazapyroxamet suspension (8+20) against leek thrips increased. The effective ingredient dosage was 10g ai / hm. 2 The efficacy of the two drugs was 92.27% and 91.44% respectively, which was significantly higher than the control drug with a longer duration of action.

[0186] Table 6. Field control efficacy of different treatments against thrips on leeks

[0187]

[0188] Note: The above data on insect population size and control efficacy are the average of four replicates, and the values ​​are rounded to two decimal places. Different letters after the control efficacy data in the same column indicate significant differences (P < 0.05).

[0189] Field Trial 2

[0190] Experimental crop: Chinese cabbage (Green Show);

[0191] Experimental target: cabbage caterpillar;

[0192] Experimental site: Chinese cabbage planting experimental field in Lijia Village, Zhucheng District, Weifang City, Shandong Province;

[0193] Test date: October 6, 2022;

[0194] Application method: In the experimental field, manual application of pesticides was carried out using a backpack electric sprayer according to the design plan. First, the whole plant was sprayed, and then the back of the leaves was sprayed with more attention.

[0195] Experimental environment: The terrain was flat, the soil was loam with moderate fertility, and the cultivation conditions in all experimental plots were uniform and consistent. The same level of fertilizer and water management was adopted, and the water and fertilizer conditions were relatively good. The soil was clay loam.

[0196] Test reagents:

[0197] Table 7 Field Trial Design and Pesticide Dosage

[0198]

[0199] Experimental method: Apply the pesticide once during the peak occurrence period of cabbage caterpillars (mostly in the 2nd to 4th instar).

[0200] Cell size and duplication: randomized block arrangement, cell size 20m² 2 Each treatment was repeated 4 times.

[0201] Survey method: Five random sampling points were taken in each area, and four plants were fixed at each point with a tag. The number of cabbage caterpillars on all Chinese cabbage plants was investigated. The initial number of caterpillars was investigated before the application of pesticides, and the number of residual caterpillars was investigated 3 days and 7 days after the application of pesticides.

[0202] Calculation formulas and data analysis:

[0203]

[0204] Field efficacy test results: The field control effects of each pesticide on cabbage caterpillar are shown in Table 8. The table shows that 3 days after application, 1.4% compound (I)·indazapyroxamet emulsion (1+0.4%) and 20% compound (I)·nicofluprole dispersible oil suspension (8+12%) exhibited better rapid efficacy against cabbage caterpillar, with an effective ingredient dosage of 15 g a.i / hm. 2 The control efficacy was 84.17% and 85.28% respectively. With the increase of time, 7 days after application, the control efficacy of 1.4% compound (I)·indazapyroxamet water emulsion (1+0.4) and 20% compound (I)·nicofluprole dispersible oil suspension (8+12) against cabbage caterpillar increased. The effective ingredient dosage was 15g ai / hm. 2 The efficacy of the two drugs was 89.63% and 90.20% respectively, which was significantly higher than that of the control drug and had a longer duration of action.

[0205] Table 8. Field control efficacy of different treatments against cabbage caterpillars in Chinese cabbage.

[0206]

[0207] Note: The above data on insect population size and control efficacy are the average of four replicates, and the values ​​are rounded to two decimal places. Different letters after the control efficacy data in the same column indicate significant differences (P < 0.05).

[0208] Safety: During the trial period and later observations, the Chinese cabbage grew normally and no obvious phytotoxicity was observed.

[0209] The insecticidal composition or formulation obtained by this invention exhibits significant control efficacy, superior to single-agent formulations in delaying the development of resistance and prolonging pesticide retention. Furthermore, no phytotoxicity was observed in the experiments with the compounded formulation, indicating that the improved synergistic effect of the obtained insecticidal composition or formulation can reduce production and usage costs while ensuring crop safety.

[0210] Although the present invention has been described in detail above with general description and specific embodiments, some modifications or improvements can be made to it based on the present invention, which will be obvious to those skilled in the art. Therefore, all such modifications or improvements made without departing from the spirit of the present invention are within the scope of protection claimed by the present invention.

Claims

1. An insecticidal composition, characterized in that, It contains active ingredient A and active ingredient B. Active ingredient A is a compound of formula (Ⅰ), with the following structural formula: The active ingredient B is either Indazapyroxamet or Nicofluprole, and the mass ratio of active ingredient A to active ingredient B is 1:50 to 34:

1.

2. The insecticidal composition according to claim 1, characterized in that: The mass ratio of the compound of formula (I) to Indazapyroxamet is 1:50 to 30:1; the mass ratio of the compound of formula (I) to Nicofluprole is 1:24 to 34:

1.

3. The insecticidal composition according to claim 3, characterized in that: The mass ratio of the compound of formula (I) to Indazapyroxamet is 1:32 to 24:1; the mass ratio of the compound of formula (I) to Nicofluprole is 1:24 to 28:

1.

4. The insecticidal composition according to claim 1, characterized in that: Based on a total mass of 100 wt% of the insecticidal composition, the sum of the contents of active ingredient A and active ingredient B in the insecticidal composition is 0.5% to 90%.

5. The insecticidal composition according to claim 4, characterized in that: The sum of the contents of active ingredient A and active ingredient B in the insecticidal composition is 1% to 85%.

6. The insecticidal composition according to claim 1, characterized in that: In addition to the active ingredient, the insecticidal composition also includes agriculturally acceptable auxiliary ingredients selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoamers, solvents, preservatives, stabilizers, synergists, or carriers.

7. The insecticidal composition according to claim 6, characterized in that: The insecticidal composition is prepared into an agriculturally permissible formulation, wherein the formulation is selected from solid formulations and / or liquid formulations; the solid formulation is selected from wettable powders and water-dispersible granules; and the liquid formulation is selected from emulsifiable concentrates, water-in-oil emulsions, microemulsions, suspensions, suspension emulsions, and dispersible oil suspensions.

8. The use of the insecticidal composition according to any one of claims 1-7 in the control of agricultural and forestry pests and sanitary pests.

9. The application according to claim 8, characterized in that: The agricultural and forestry pests and sanitary pests mentioned are Lepidoptera and Thysanoptera pests; The Lepidoptera pests mentioned are cabbage caterpillar, diamondback moth, beet armyworm, cotton bollworm, two-spotted cutworm, rice stem borer, and cotton bollworm. The Thysanoptera pests mentioned are western flower thrips, tobacco thrips, palm thrips, and watermelon thrips.

10. The application according to claim 8, characterized in that: The insecticidal composition is applied in an effective dose to the pest that needs to be controlled or to the medium in which it grows.

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