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 in a formula (I), the active component B is any one of Dampropyridaz, Oxazosulfyl and Flometoquin, and the mass ratio of the active component A to the active component B is (1: 42)-(32: 1). The insecticidal composition has the advantages of synergism, resistance delay and the like, and is used for preventing and treating resistant pests.

Description

Technical Field

[0001] The invention belongs to the technical field of pesticides and insecticides, and specifically relates to an insecticide composition and application thereof. Background Art

[0002] Dimpropyridaz is a pyrazole carboxamide insecticide, which has good control effects on aphids, whiteflies, thrips, leafhoppers and diamondback moths of Lepidoptera, Coleoptera, Diptera and Hemiptera. It contains a racemic body with a chiral center and has a novel chemical structure. It can be used for pest control of crops such as cotton, vegetables and fruits. Its chemical name is: N-ethyl-5-methyl-1-(3-methylbutan-2-yl)-N-pyridazin-4-ylpyrazole-4-carboxamide, and its chemical structure is:

[0003]

[0004] Oxazosulfyl is a benzoxazole insecticide with a broad insecticidal spectrum and high activity against pests of Diptera, Lepidoptera, Coleoptera, Hemiptera, etc. Its chemical name is: 2-(3-ethylsulfonylpyridin-2-yl)-5-(trifluoromethylsulfonyl)-1,3-benzoxazole, and its chemical structure is:

[0005]

[0006] Flometoquin is a novel quinoline insecticide, an inhibitor of the complex III of the mitochondrial electron transport chain of insects. It has excellent control effects on thysanoptera pests (thrips), whiteflies, gall mites and lepidoptera pests, and has a fast killing speed and a long lasting effect. Chemical name: [2-ethyl-3,7-dimethyl-6-[4-(trifluoromethoxy)phenoxy]quinolin-4-yl] methyl carbonate, its chemical structure is:

[0007]

[0008] In the actual process of agricultural production, the most common problem in pest control is the development of pest resistance. Compounding of ingredients of different varieties is a very common method for controlling resistant pests. In most cases, the compounding effect of pesticides is an additive effect, and there are very few compounds that truly have a synergistic effect, especially those with very obvious synergistic effects and high co-toxicity coefficients. Therefore, screening new pesticide compositions to meet the screening requirements of obvious synergistic effects and high co-toxicity coefficients is of great significance for delaying the resistance of crop pests and improving the control effect. The present invention has found through a large number of experiments that compounding the compound of formula (I) with Dimpropyridaz, Oxazosulfyl, and Flometoquin in a certain mass ratio shows a significant synergistic effect. No reports on this have been found so far. Summary of the invention

[0009] The invention aims to provide an insecticide composition which has synergistic effect, reduces resistance and has low use cost.

[0010] To achieve the above object, the technical solution adopted by the present invention is: an insecticide composition, comprising active ingredient A and active ingredient B, wherein active ingredient A is a compound of formula (I), and the structural formula is as follows:

[0011] The active ingredient B is any one of Dimpropyridaz, Oxazosulfyl and Flometoquin;

[0012] Furthermore, the mass ratio of the active ingredient A to the active ingredient B is 1:42 to 32:1;

[0013] Furthermore, the mass ratio of the active ingredient A to the active ingredient B is 1:42 to 30:1;

[0014] Further, the mass ratio of the compound of formula (I) to Dimpropyridaz is 1:32 to 30:1, such as 1:32, 1:28, 1:14, 1:6, 2:3, 3:2, 6:1, 15:1, 30:1 or any value between the above values;

[0015] Furthermore, the mass ratio of the compound of formula (I) to Dimpropyridaz is 1:28 to 30:1.

[0016] Furthermore, the mass ratio of the compound of formula (I) to Dimpropyridaz is 1:28, 1:14, 1:6, 2:3, 3:2, 6:1, 15:1, 30:1;

[0017] Further, the mass ratio of the compound of formula (I) to Oxazosulfyl is 1:42 to 32:1, such as 1:42, 1:17, 1:8, 1:4, 9:2, 18:1, 32:1 or any value between the above values;

[0018] Furthermore, the mass ratio of the compound of formula (I) to Oxazosulfyl is 1:17 to 18:1.

[0019] Furthermore, the mass ratio of the compound of formula (I) to Oxazosulfyl is 1:17, 1:8, 1:4, 9:2, 18:1;

[0020] Further, the mass ratio of the compound of formula (I) to Flometoquin is 1:32 to 32:1, such as 1:32, 1:16, 1:8, 2:3, 4:1, 8:1, 16:1, 32:1 or any value between the above values;

[0021] Furthermore, the mass ratio of the compound of formula (I) to Flometoquin is 1:32 to 16:1;

[0022] Furthermore, the mass ratio of the compound of formula (I) to Flometoquin is 1:32, 1:16, 1:8, 2:3, 4:1, 8:1, 16:1;

[0023] Furthermore, based on the total mass of the insecticide composition being 100 wt%, the sum of the contents of the active ingredient A and the active ingredient B in the insecticide composition is 0.5% to 90%;

[0024] Furthermore, the sum of the contents of the active ingredient A and the active ingredient B in the insecticide composition is 1% to 85%;

[0025] Furthermore, the insecticide composition includes agriculturally acceptable auxiliary ingredients in addition to the active ingredients, and the auxiliary ingredients are selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoamers, solvents, preservatives, stabilizers, synergists or carriers;

[0026] The wetting agent is selected from one or more of alkylbenzene sulfonate, alkylnaphthalene sulfonate, lignin sulfonate, sodium dodecyl sulfate, sodium dioctyl succinate sulfonate, alpha olefin sulfonate, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol ethoxylate, fatty alcohol ethoxylate, fatty alcohol polyoxyethylene ether sodium sulfate, silkworm feces, saponin powder, soapberry powder, SOPA, detergent, emulsifier 2000 series and wetting penetrant F; and / or

[0027] 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 acid, phosphates, EO-PO block copolymers and EO-PO graft copolymers; and / or

[0028] The emulsifier is selected from one or more of calcium dodecylbenzene sulfonate, 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

[0029] 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

[0030] 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

[0031] The antifreeze agent is selected from one or more of alcohols, alcohol ethers, chlorinated hydrocarbons and inorganic salts; and / or

[0032] The defoamer is selected from C 10 -C 20 Saturated fatty acid compounds, silicone oil, silicone compounds, C 8 -C 10 One or more of fatty alcohols; and / or

[0033] 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

[0034] 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

[0035] 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

[0036] The synergist is selected from synergist phosphite, synergist ether; and / or

[0037] 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.

[0038] Furthermore, the insecticide composition can be prepared into an agriculturally acceptable formulation, and the formulation is selected from a solid formulation and / or a liquid formulation;

[0039] 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;

[0040] Further, the liquid preparation includes a soluble solution, a soluble gel, an oil, a film-spreading oil, an emulsifiable concentrate, a latex, a dispersible liquid, an ointment, an aqueous emulsion, an oil emulsion, a microemulsion, a fat, a suspension, a microcapsule suspension, an oil suspension, a dispersible oil suspension, a suspoemulsion, a microcapsule suspension-suspension, a microcapsule suspension-water emulsion or a microcapsule suspension-suspoemulsion;

[0041] Furthermore, the solid preparation is selected from wettable powders and water dispersible granules; the liquid preparation is selected from emulsifiable concentrates, aqueous emulsions, microemulsions, suspensions, suspoemulsions, and dispersible oil suspensions;

[0042] Furthermore, the solid preparation is selected from wettable powders and water dispersible granules; the liquid preparation is selected from emulsifiable concentrates and suspensions;

[0043] Application of the insecticide composition of the present invention in preventing and controlling agricultural and forestry pests and sanitary pests;

[0044] The insecticide composition of the present invention can be used to control pests on fruit trees, vegetables, ornamental plants, tea, cotton, and cereal crops;

[0045] Furthermore, the agricultural and forestry pests and sanitary pests are Lepidoptera, Thysanoptera, and Hemiptera pests;

[0046] Further, the Lepidoptera pests include: Adoxophyes spp., Adoxophyes orana, Agrotis spp. (cutworms), Agrotis ipsilon (black cutworm), Alabamaargillacea (cotton leafworm), Amorbia cuneana, Amyelosis transitella (navel orangeworm), Anacamptodes defectaria, Anarsia lineatella (peach twig borer), Anomis sabulifera (jute looper), Anticarsia g emma talis, Archips argyrospila (fruittreeleafroller), Archips rose leafroller, rosana(rose leaf roller), Argyrotaenia spp.(tortricid moths), Argyrotaenia citrana(orange tortrix), Autographa gamma, Bonagota cranaodes, Borbo cinnara(rice leaf folder), Bucculatrix thurberiella(cotton leaf perforator), Caloptilia spp.(leaf miners), Capua reticulana, Carposina niponensis(peach fruit moth), Chilo spp., Chlumetia transversa(mango shoot borer), Choristoneura rosaceana(obliquebanded leaf roller), leafroller)), Chrysodeixis spp.), Cnaphalocerus medinalis (grass leafroller), Colias spp., Conpomorpha cramerella, Cossus cossus (carpenter moth), Crambus spp. (sod webworms), Cydia funebrana (plum fruit moth), Cydia molesta (oriental fruit moth), Cydia nignicana (pea moth), Cydia pomonella (codling moth), Darna diducta, Diaphania spp. (stem borer), borers), Diatraea spp. (stalk borers), Diatraea spp. (sugarcane borer), Diatraea graniosella (southwester corn borer), Earias spp. (bollworms), Earias insulata (Egyptian 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 pink moth.

[0047] Ephestia elutella (tobbaco moth), Ephestiakuehniella (Mediterranean flour moth), Epimeces spp., Epinotia aporema, Erionota thrax (banana skipper), Eupoecilia ambiguella (grape berry moth), Euxoa auxiliaris (army cutworm), Feltia spp. (cutworms), Gortyna spp. (stemblerers), Grapholita molesta (oriental fruit moth), Hedylepta indicate (bean leaf roller), leafwebber), Helicoverpa sp p. (southworm), Helicover paarmigera, Helicoverpa zea, Heliothis spp., Heliothis virescens, Hellula undalis (cabbage webworm), Indarbela spp. (root borers), Keiferia lycopersicella, Leucinodes orbonalis, Leucoptera malifoliella, Lithocollectis spp., Lobesia botrana (grape fruit moth), Loxagrotis spp.), 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 (bean pod borer), Metisa plana, Mythimna unipuncta (true armyworm), Neoleucinodes elegantalis, Nymphula depunctalis, Operophtherabrumata, Ostrinia nubilalis (European corn borer), Oxydia vesulia, Pandemis cerasana (common currant tortrix), Pandemis heparana (brown apple tortrix), Papilio demodocus, Pectinophora gossypiella (pink bollworm), Peridroma spp. (cutworm), Peridroma saucia (variegated cutworm), Perileucoptera coffeella (white coffee leafminer), Phthorimaea operculella (potato tuber moth), Phyllocnisitis citrella, Phyllonorycter spp.), Pieris rapae, Plathypena scabra, Plodia interpunctella, Plutellaxylostella (diamondback moth), Polychrosis viteana (grapeberry moth), Prays endocarpa, Prays oleae (olive moth), Pseudaletia spp. (spot moth), Spodoptera litura Fabricius, Pseudaletia unipunctata (armyworm), Pseudoplusia includes (, 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), Sparganothis pilleriana, Spodoptera spp., Spodoptera exigua, Spodoptera fugiperda, Spodoptera oridania (southern armyworm), Synanthedon spp.), Thecla basilides, Thermisia gemmatalis, Tineola bisselliella (webbing clothesmoth), Trichoplusia ni (cabbage worm), Pierisrapae Linne (cabbage worm), Tuta absoluta;.

[0048] Further, the Thysanoptera pests include: Thrips palmiKarny, Thrips tabaci, Frankliniella fusca (tobacco thrips), Frankliniella occidentalis, (western flower thrips), Frankliniella shultzei, Frankliniella williamsi (cornthrips), Heliothrips haemorrhaidalis, greenhouse thrips, Riphiphorothrips cruentatus, Scirtothrips spp., Scirtothrips citri (citrus thrips), Scirtothrips citri (citrus thrips), and Scirtothrips occidentalis. dorsalis) (yellow tea thrips), Taeniothrips rhopalantennalis, and Thrips spp.;

[0049] Further, the Hemiptera pests include: Lygus spp., Eurygastermaura, Nezaraviridula, Piezodorus guildingi, Leptocorisavaricornis, Cimex lectularius, Cimex hemipterus, Aphis spp., Myzus Persicae, Rhopalosiphum spp., Dysaphis plantaginea, Toxoptera spp., Aphis craccivora Koch, Macrosiphum euphorbiae, Aulacorthum solani, Sitobionavenae, Metopolophium dirhodum, Schizaphis graminum), Brachycolus noxius, Nephotettix spp.), Nilaparvatalugens, Sogatella furcifera, Laodelphax striatellus, Aleurothrixus floccosus, Quadraspidiotusperniciosus, Unaspisyanonenses, Ceroplastes rubens, Aonidiella aurantii, Aleurocanthus spiniferus (Quaintance), Dialeurodes citri (Ashmead), Bemisa tabaci (Gennadius), Trialeurodes vaporariotum (Westwood), Dialeuroropora photiniana, Siphoninus phillyreae (Haliday), Aleurolobus marlatti (Quaintance), Parabemisia myricae (Kuwana), Aleuroclava psidii Singh, Aleuroclava guyavae (Takahashi), Aleuroclava aucubae (Kuwana), Crenidoresum turpiniae (Takahashi);

[0050] Furthermore, the lepidopteran pests are cabbage worm, diamondback moth, beet armyworm, Spodoptera litura, Spodoptera litura, two-spotted armyworm, striped stem borer, and cotton bollworm;

[0051] Furthermore, the Thysanoptera pests are western flower thrips, tobacco thrips, palm thrips, and watermelon thrips;

[0052] Furthermore, the hemiptera pests are whitefly, greenhouse whitefly, rice planthopper, and aphid;

[0053] The present invention also provides a method for using the insecticidal composition as described above, specifically applying an effective dose to the pests to be controlled or the medium in which they grow.

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

[0055] 1) The insecticide composition of the present invention rationally compounds agents with different action mechanisms, has excellent control effects on Lepidoptera, Hemiptera, and Thysanoptera pests, has good rapidity, long lasting effect, and exhibits synergistic effects within a certain ratio range;

[0056] 2) The insecticide composition of the present invention has the advantages of reducing the amount of pesticide used, delaying the occurrence and development of pest resistance and drug resistance, etc. DETAILED DESCRIPTION

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

[0058] The composition of the present invention can be provided in the form of a preparation. It can be prepared into a suspension, emulsifiable concentrate, water dispersible granules, aqueous emulsion, granules, wettable powder, dispersible oil suspension, etc. as needed. The content of the active ingredient in the composition of the present invention depends on the application amount when used alone, and also depends on the mixing ratio and the degree of synergistic effect. The optimal range of the active ingredient content varies according to the type of preparation of the composition.

[0059] Preparation Example

[0060] Embodiment 1:

[0061] 24% compound of formula (I)·dimpropyridaz suspension (14+10)

[0062] Formula: 14% compound of formula (I), 10% dimpropyridaz,

[0063] 1.5% sodium lignin sulfonate, 2% fatty alcohol polyoxyethylene ether, 4% styrene phenol polyoxyethylene ether sulfate, 2.5% alkyl aryl polyoxyethylene ether polyoxypropylene ether, 1% magnesium aluminum silicate, 0.2% xanthan gum, 0.5% sodium sorbate, 5% glycerol, 0.5% organosilicon defoamer, and deionized water to make up the balance;

[0064] Preparation method: Add active ingredients to the wetting dispersant and defoamer, use zirconium beads, and wet grind with a sand mill to D 90 (90% of the particle size) <10 μm, and a pulverized slurry is obtained. A thickener, antifreeze agent, preservative, etc. are added to the pulverized slurry and mixed evenly, and deionized water is added to 100%, and high-speed shearing is performed evenly to prepare a suspension preparation of the composition of the present invention.

[0065] Embodiment 2:

[0066] 20% compound of formula (I)·flometoquin suspension (8+12)

[0067] Formula: 8% compound of formula (I), 12% flometoquin,

[0068] 5% styrene phenol polyoxyethylene ether sulfate, 1.5% sodium lignin sulfonate, 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% organosilicon defoamer, and deionized water to make up the balance;

[0069] Preparation method: Same as Example 1.

[0070] Embodiment 3:

[0071] 60% compound of formula (I)·dimpropyridaz wettable powder (36+24)

[0072] Formula: 36% compound of formula (I), 24% dimpropyridaz,

[0073] 3% tea saponin, 7.5% naphthalenesulfonate formaldehyde condensate, 6% sodium alginate, 5% light calcium carbonate, 4% starch, and kaolin make up the balance;

[0074] Preparation method: Active ingredients, dispersants, wetting agents and fillers are mixed according to the formula ratio, uniformly stirred in a stirring kettle, and pulverized and mixed uniformly for multiple times by a jet mill to prepare a wettable powder preparation of the composition of the present invention.

[0075] Embodiment 4:

[0076] 20% compound of formula (I)·dimpropyridaz dispersible oil suspension (12+8)

[0077] Formula: 12% compound of formula (I), 8% dimpropyridaz,

[0078] 1% naphthalenesulfonate condensate, 12% castor oil polyoxyethylene ether, 3% fatty alcohol polyoxyethylene ether, 2.5% calcium dodecylbenzene sulfonate, 0.2% organosilicon defoamer, 0.3% organobentonite, and soybean oil to make up the balance;

[0079] Preparation method: according to the formula ratio, the active ingredients, surfactants and other functional additives are placed in a reaction kettle in sequence, oil is added and mixed evenly, and the dispersible oil suspension preparation of the composition of the present invention can be prepared by high-speed shearing, wet sand grinding, and finally homogenization filtration.

[0080] Embodiment 5:

[0081] 23% compound of formula (I) ·flometoquin dispersible oil suspension (8+15)

[0082] Formula: 8% compound of formula (I), 15% flometoquin,

[0083] 1.5% naphthalenesulfonate condensate, 13% castor oil polyoxyethylene ether, 3.4% fatty alcohol polyoxyethylene ether, 2% calcium dodecylbenzene sulfonate, 0.2% organosilicon defoamer, 0.2% organobentonite, 5% peanut oil, soybean oil to make up the balance;

[0084] Preparation method: Same as Example 4.

[0085] Embodiment 6:

[0086] 44% Compound of formula (I)·oxazosulfyl water dispersible granules (8+36)

[0087] Formula: 8% compound of formula (I), 36% oxazosulfyl,

[0088] 6% sodium polycarboxylate, 2.5% sodium lignin sulfonate, 6% naphthalene sulfonate formaldehyde condensate, 3.5% sodium lauryl sulfate, 4% white carbon black, 2% starch, 1.5% bentonite, kaolin makes up the balance;

[0089] Preparation method: According to the formula ratio, the active ingredient is added to the carrier, and a surfactant and other functional additives are added thereto, mixed, and after air flow pulverization, appropriate water is added, and then kneading, granulation, drying, and sieving can be made into a water-dispersible granule preparation of the composition of the present invention.

[0090] Embodiment 7:

[0091] 1.5% formula (Ⅰ) compound · oxazosulfyl granules (0.3+1.2)

[0092] Formula: 0.3% compound of formula (I) 1.2% oxazosulfyl,

[0093] 1.5% sodium polycarboxylate, 3% sodium lignin sulfonate, 2.5% naphthalene sulfonate formaldehyde condensate, 2% polyvinyl alcohol, and diatomaceous earth particles make up the balance;

[0094] Preparation method: adopt coating granulation method, mix the original drug, dispersant and auxiliary agent evenly to form mother powder, add the mother powder and carrier into coating granulator and stir, add the prepared binder aqueous solution while stirring, mix well and then discharge, dry and sieve to prepare the granule preparation of the composition of the present invention.

[0095] Embodiment 8:

[0096] 8% compound of formula (I)·flometoquin emulsifiable concentrate (3+5)

[0097] Formula: 3% compound of formula (I), 5% flometoquin,

[0098] 20% propylene carbonate, 5% styrylphenol polyoxyethylene ether, 7% castor oil polyoxyethylene ether, 2% calcium dodecylbenzene sulfonate, 10% N,N-dimethylformamide, 2% peanut oil, 22.5% cyclohexanone, and methyl oleate make up the balance;

[0099] Preparation method: firstly add the active ingredient into the solvent and completely dissolve it, then add the emulsifier and the like and stir evenly to form a uniform and transparent oily liquid, and then fill it to prepare the emulsifiable concentrate preparation of the composition of the present invention.

[0100] Indoor biological activity assay

[0101] Refer to agricultural industry standards:

[0102] "Guidelines for Indoor Bioassay Tests of Pesticides - Pesticides Part 6: Insect Dipping Method" (NY / T 1154.6-2006);

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

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

[0105] Specific indoor toxicity test:

[0106] 1) Hemiptera adults: spray method;

[0107] Test insect age: healthy adults with consistent growth and development;

[0108] Drug preparation: The test drug was dissolved in acetone and prepared into 5 series of concentrations using 0.1% Tween 80 aqueous solution.

[0109] Test treatment: Use an insect sucker to select at least 15 test insects of the same physiological state and place them in a culture dish. Then place the culture dish on the bottom plate of a potter spray tower for quantitative spraying. The spraying volume is 1mL. After the liquid settles for 1 minute, take out the test insects.

[0110] Each treatment was repeated 4 times, and the blank treatment was used as the control. The treated test insects were placed in an artificial intelligence culture room at 25±1°C, a light period of L:D=16h:8h, and a relative humidity of 65%±5% for breeding.

[0111] Investigation method: Investigate the mortality of test insects 48 hours after treatment with pesticides. The criterion for judging the death of test insects is that they cannot crawl normally after being pricked with a needle. Record the total number of insects and the number of dead insects respectively.

[0112] 2) Lepidoptera larvae: a combination of leaf and insect dipping;

[0113] Test insect age: Use sensitive populations raised indoors for multiple generations, and select healthy and uniform second-instar Lepidoptera larvae.

[0114] Use tweezers to place fresh cabbage slices in the drug solution and immerse them for 10 seconds, then take them out. After the drug solution dries naturally, place the cabbage slices in a culture dish lined with moisturizing filter paper. Place 16 second-instar lepidopteran larvae in the drug solution for 5 seconds, absorb the excess drug solution with filter paper, and place the test insects in a culture dish with leaves immersed in the corresponding concentration.

[0115] Each treatment was repeated 4 times, and the blank treatment was used as the control. The treated test insects were placed in an artificial intelligence culture room at 26±1°C, a light period of L:D=16h:8h, and a relative humidity of 60% for breeding.

[0116] Investigation method: Investigate the mortality of test insects 48 hours after treatment with pesticides. The criterion for judging the death of test insects is obvious shrinkage of the insect body or inability to crawl normally after being pricked with a needle. Record the number of dead insects.

[0117] 3) Thysanoptera adults: glass roller tube method;

[0118] Test insect age: Use sensitive populations raised indoors for multiple generations, and select healthy and uniform female adults of the order Thysanoptera.

[0119] After the glass tube is evenly rolled with 250ul of the drug solution, the cabbage leaves are punched into 1.5cm diameter discs with a hole puncher. Then, fresh cabbage slices are placed in the drug solution with tweezers and immersed for 10s before being taken out. After the drug solution is naturally dried, the cabbage slices are placed in a glass tube. 20 female adults of Thysanoptera are sucked into the glass tube with an insect sucker and the tube is sealed with a 200-mesh gauze.

[0120] Each treatment was repeated 4 times, and the blank treatment was used as the control. The treated test insects were placed in an artificial intelligence culture room at 26±1°C, a light period of L:D=16h:8h, and a relative humidity of 60% for breeding.

[0121] Investigation method: Investigate the mortality of test insects 48 hours after treatment with pesticides. The criterion for judging the death of test insects is that they cannot crawl normally after being pricked with a needle. Record the number of dead insects.

[0122] Data statistics and analysis:

[0123] According to the survey data, the adjusted mortality rate of each treatment was calculated using the following formula, with the results retained to two decimal places:

[0124]

[0125] Where:

[0126] P——mortality rate, in percentage (%);

[0127] K——indicates the number of dead insects, in units of heads;

[0128] N——represents the total number of insects treated, in heads.

[0129]

[0130] Where:

[0131] P 1 ——Adjusted mortality rate, expressed as percentage (%);

[0132] P t ——Treatment mortality rate, expressed as percentage (%);

[0133] P 0 ——Blank control mortality rate, in percentage (%).

[0134] 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 formula (2); if the control mortality rate is greater than 20%, the test needs to be repeated.

[0135] The data can be processed by probability value analysis. The DPS statistical analysis system can be used to calculate the toxicity regression line, LC 50 The activity of the test agent on the biological test material was evaluated by using the value, 95% confidence limit and correlation coefficient r.

[0136] The co-toxicity coefficient (CTC value) of the mixture is calculated as follows:

[0137]

[0138] Where:

[0139] ATI——Actual Toxicity Index of Mixture;

[0140] S——LC of standard pesticide 50 , the unit is milligrams per liter (mg / L);

[0141] M——LC of the mixture 50 , the unit is milligrams per liter (mg / L).

[0142] TTI=TI A *P A +TI B *P B

[0143] Where:

[0144] TTI – Theoretical Toxicity Index of Mixtures;

[0145] TI A ——A: toxicity index of the agent;

[0146] P A ——The percentage of agent A in the mixture, in percentage (%);

[0147] TI B ——Toxicity index of agent B;

[0148] P B ——The percentage of agent B in the mixture, in percentage (%).

[0149]

[0150] Where:

[0151] CTC – Co-toxicity coefficient;

[0152] ATI——Actual Toxicity Index of Mixture;

[0153] TTI - Theoretical Toxicity Index of Mixture.

[0154] The co-toxicity coefficient of the combination CTC≥120 shows a synergistic effect; CTC≤80 shows an antagonistic effect; 80<CTC<120 shows an additive effect.

[0155] Test results:

[0156] Combined toxicity of mixed pesticides to rice planthoppers:

[0157] The results in Table 1 show that the LC of the compound of formula (I) against rice planthoppers 50 The LC value of Oxazosulfyl to rice planthoppers is 7.1989 mg / L. 50 It is 60.2938mg / L.

[0158] The compound of formula (I) and Oxazosulfyl mixed have a good combined effect on rice planthoppers, and show obvious synergistic effect at a certain mass ratio. When the mass ratio of the compound of formula (I) to Oxazosulfyl is 1:42 to 32:1, the co-toxicity coefficient of the rice planthopper prevention effect is greater than 120, showing a synergistic effect.

[0159] Table 1 Toxicity test results of different ratios of compound of formula (I) and Oxazosulfyl to rice planthoppers

[0160]

[0161] Combined toxicity of mixed pesticides to Plutella xylostella:

[0162] The results in Table 2 show that the LC of the compound of formula (I) against Plutella xylostella50 The LC of Dimpropyridaz to Plutella xylostella is 6.6352. 50 It is 2.0422mg / L.

[0163] The compound of formula (I) and Dimpropyridaz have a good combined effect on diamondback moth, and show obvious synergistic effect at a certain mass ratio. When the mass ratio of the compound of formula (I) to Dimpropyridaz is 1:28 to 30:1, the co-toxicity coefficient of the protective effect on diamondback moth is greater than 120, showing a synergistic effect.

[0164] Table 2 Toxicity test results of different ratios of the compound of formula (I) and Dimpropyridaz to Plutella xylostella

[0165]

[0166]

[0167] Combined toxicity of mixed pesticides to Thrips tabaci:

[0168] The results in Table 3 show that the LC of the compound of formula (I) against Thrips tabaci 50 The LC value of Flometoquin to Thrips tabaci is 9.1862 mg / L. 50 It is 7.6891mg / L.

[0169] The compound of formula (I) and Flometoquin have a good combined effect on Thrips tabaci, and show obvious synergistic effect at a certain mass ratio. When the mass ratio of the compound of formula (I) to Flometoquin is 1:32 to 32:1, the co-toxicity coefficient of the control effect on Thrips tabaci is greater than 80, showing an additive or synergistic effect; when the mass ratio of the compound of formula (I) to Flometoquin is 1:32 to 16:1, the co-toxicity coefficient of the control effect on Thrips tabaci is greater than 120, showing a synergistic effect.

[0170] Table 3 Toxicity test results of different ratios of the compound of formula (I) and Flometoquin against Thrips tabaci

[0171]

[0172] Field trial 1

[0173] Test crops and targets: Rice (Wuyou Rice No. 2), rice planthopper;

[0174] Experimental location: rice planting fields in Wangtaiping Village, Taiping Street, Hedong District, Linyi City, Shandong Province;

[0175] Spraying equipment: 3WBS-16 backpack electric sprayer, first spray the water control plot, then spray the test drug plot. When spraying, the nozzle should be pointed downward, and the liquid should be sprayed to the base of the rice stem as much as possible; the liquid volume is 450L / hm 2 ; The blank group used clear water as a control.

[0176] Trial date: August 19, 2022;

[0177] Experimental environment: The cultivation conditions of all experimental plots were uniform and consistent, and the same fertilizer and water management level was adopted. The rice grew well, and no agricultural operations such as fertilization, drainage and irrigation were carried out during the experiment;

[0178] Test drug:

[0179] Table 4 Field test design and dosage

[0180]

[0181] Plot area and replication: randomized block arrangement, 25m per plot 2 , each treatment was repeated 4 times.

[0182] Survey method: Randomly sample 5 points in each plot, with 2 clumps at each point. Use a 20×33cm white porcelain plate as a carrier. Put a small amount of water in the plate and pat the rice clumps 4 times each time. Count the number of rice planthoppers (including nymphs and adults) in the plate. Investigate the number of remaining insects in each plot 3d and 10d after spraying.

[0183] Calculation formula and data analysis:

[0184]

[0185] Field efficacy test results:

[0186] The field control effects of various agents on rice planthoppers in rice fields are shown in Table 5. It can be seen from the table that 3 days after the application, 44% formula (Ⅰ) compound·oxazosulfyl water dispersible granules (8+36) showed good rapid effect, and its control effect was 89.07%; 10 days after the application, the mixed preparation of 44% formula (Ⅰ) compound·oxazosulfyl water dispersible granules (8+36) also showed good lasting effect, and the control effect was above 90%, which was significantly higher than the control single agent.

[0187] Table 5 Field test design and dosage

[0188]

[0189] Note: The above efficacy data are the average of 4 repetitions, and the values ​​are rounded to two decimal places.

[0190] Safety: The test agent treatment did not cause any phytotoxicity or other adverse effects on rice compared with the blank control area. The occurrence of rice planthoppers is sudden, and the current production mainly relies on chemical control to control the occurrence of rice planthoppers. In summary, the compound of formula (I) mixed with Oxazosulfyl has a good control effect on rice planthoppers.

[0191] Field trial 2

[0192] Experimental crops: Cabbage (Brassica oleracea L.);

[0193] Test target: Diamondback moth;

[0194] Experimental location: Cruciferous vegetable planting experimental field in Pingdu, Qingdao, Shandong Province;

[0195] Trial date: July 8, 2022;

[0196] Application method: Use a backpack electric sprayer in the test field to apply pesticides manually according to the designed plan. First spray the whole plant, and then focus on spraying the back of the leaves.

[0197] Experimental environment: All experimental plots had uniform cultivation conditions, the same fertilizer and water management level, good water and fertilizer conditions, and sticky loam;

[0198] Test drug:

[0199] Table 6 Field test design and dosage

[0200]

[0201] Test method: Apply the pesticide once during the peak period of diamondback moth (mostly 2nd to 4th instar).

[0202] Plot size and repetition: random block arrangement, plot size 30m 2 , each treatment was repeated 4 times.

[0203] Survey method: Randomly sample five points in each plot, hang a sign on 4 cabbages at each point, investigate the number of diamondback moths on all cabbages, investigate the base number of insects before applying pesticides, and investigate the number of remaining insects 1d and 7d after applying pesticides.

[0204] Calculation formula and data analysis:

[0205]

[0206] Field efficacy test results:

[0207] Safety to crops: Cabbage in each treatment area grew normally, no pesticide damage was observed, and no adverse effects on non-target organisms were found.

[0208] Effect on the control of diamondback moth: As can be seen from Table 7, one day after the application, all the tested agents can effectively control the occurrence of diamondback moth. Among them, the 24% formula (Ⅰ) compound·dimpropyridaz suspension (14+10) has a very good control effect, and the dosage of the active ingredient is 15g ai / hm 2 At 14:00 p.m., the prevention effect was 88.94%, with good rapid effect; 7 days after application, the prevention effect was 90.83%, with good lasting effect.

[0209] Table 7 Field control effects of different treatment agents on Plutella xylostella

[0210]

[0211] Note: The above insect population base and control efficacy data are the average of 4 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).

[0212] Field trial 3

[0213] Experimental crops: Chinese chives (Dajingou);

[0214] Conditions of the experimental field: medium fertility, convenient irrigation and drainage, and sandy soil.

[0215] Test target: Leek thrips;

[0216] Test location: Qiantianbutou Village, Haiyang City, Yantai City;

[0217] Trial date: November 15, 2022;

[0218] Application method: In the test field, a backpack electric sprayer was used to apply pesticides manually according to the design plan. The whole plant was sprayed first, and then the back of the leaves was sprayed. The application machine was a 3WBS-16 backpack electric sprayer with a spray volume of 450L / hm 2 .

[0219] Experimental environment: All experimental plots had uniform cultivation conditions, the same fertilizer and water management level, good water and fertilizer conditions, and sticky loam;

[0220] Test drug:

[0221] Table 8 Field test design and dosage

[0222]

[0223] Test method: Apply the pesticide once at the early stage of leek thrips infestation (small white spots appear on the leaves).

[0224] Plot size and repetition: random block arrangement, plot size 25m 2 , each treatment was repeated 4 times.

[0225] Survey method: Randomly sample five points in each plot, use the clapping method, randomly survey 5 clumps (20 plants) at each point, clap them together 3 times, count the number of thrips shaken into the white porcelain plate, investigate the insect base number before applying the pesticide, and investigate the number of residual insects 1d and 7d after applying the pesticide.

[0226] Calculation formula and data analysis:

[0227]

[0228] Field efficacy test results:

[0229] The field control effects of each agent on leek thrips are shown in Table 9. It can be seen from the table that 1 day after the application, 8% formula (Ⅰ) compound·flometoquin emulsifiable concentrate (3+5) showed good quick-acting effect on leek thrips, and the dosage of the active ingredient was 20g ai / hm 2 The control effect was 89.07% at 14:00 p.m.; with the increase of time, 7 days after application, the control effect of 8% compound (Ⅰ)·flometoquin emulsifiable concentrate (3+5) on leek thrips increased, and the dosage of active ingredient was 10 g ai / hm 2 The protective efficacy was 93.62%, which was significantly higher than the control single-dose and had a longer duration of effect.

[0230] Table 9 Field control effect of different treatment agents on the control of tobacco thrips in chives

[0231]

[0232] Note: The above insect population base and control efficacy data are the average of 4 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).

[0233] The insecticide composition or the preparation obtained by compounding the present invention has significant control effect, and is superior to a single agent in delaying the generation of drug resistance and prolonging drug retention. In addition, no compound agent was found to cause phytotoxicity to crops in the test, indicating that the insecticide composition or preparation obtained can reduce production costs and use costs and is safe for crops when the insecticide synergistic synergy is improved.

[0234] Although the present invention has been described in detail above with general descriptions and specific implementation schemes, it is obvious to those skilled in the art that some modifications or improvements can be made on the basis of the present invention. Therefore, these 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: The active ingredient A and the active ingredient B are included, wherein the active ingredient A is a compound of formula (I) with the following structural formula: The active ingredient B is any one of Dimpropyridaz, Oxazosulfyl and Flometoquin.

2. The insecticidal composition according to claim 1, characterized in that: The mass ratio of the active ingredient A to the active ingredient B is 1:42 to 32:1; Preferably, the mass ratio of the active ingredient A to the active ingredient B is 1:42 to 30:

1.

3. The insecticidal composition according to claim 1, characterized in that: The mass ratio of the compound of formula (I) to Dimpropyridaz is 1:32 to 30:1, the mass ratio of the compound of formula (I) to Oxazosulfyl is 1:42 to 32:1, and the mass ratio of the compound of formula (I) to Flometoquin is 1:32 to 32:

1.

4. The insecticidal composition according to claim 1, characterized in that: The mass ratio of the compound of formula (I) to Dimpropyridaz is 1:28-30:1, the mass ratio of the compound of formula (I) to Oxazosulfyl is 1:17-18:1, and the mass ratio of the compound of formula (I) to Flometoquin is 1:32-16:

1.

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

6. The insecticidal composition according to claim 1, characterized in that: In addition to the active ingredients, the insecticide 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.

7. The insecticidal composition according to claim 6, characterized in that: The insecticide composition is prepared into a formulation form permitted in agriculture, and the formulation form is selected from a solid formulation and / or a liquid formulation; Preferably, the solid preparation is selected from wettable powders and water-dispersible granules; the liquid preparation is selected from emulsifiable concentrates, aqueous emulsions, microemulsions, suspensions, suspoemulsions, and dispersible oil suspensions.

8. Use of the insecticide composition according to any one of claims 1 to 7 in preventing and controlling agricultural and forestry pests and sanitary pests.

9. The use according to claim 8, characterized in that: The agricultural and forestry pests and sanitary pests are Lepidoptera, Thysanoptera and Hemiptera pests; Preferably, the lepidopteran pests are cabbage worm, diamondback moth, beet armyworm, Spodoptera litura, Spodoptera litura, two-spotted armyworm, striped stem borer, and cotton bollworm; The thysanoptera pests are western flower thrips, tobacco thrips, palm thrips, and watermelon thrips; The hemiptera pests are whitefly, greenhouse whitefly, rice planthopper and aphid.

10. The insecticidal composition according to claim 1, characterized in that: The insecticide composition is applied to the pests to be controlled or the medium where they grow in an effective dose.

Images