An insecticidal composition containing bis(triflufenoxuron) and its application

Abstract

This invention belongs to the field of pesticides and insecticides, specifically relating to an insecticidal composition containing bis(triflufenoxuron) and its application. The insecticidal composition includes active ingredient A and active ingredient B. Active ingredient A is bis(triflufenoxuron), and active ingredient B is any one of dinotefuran, spinosad, flonicamid, and acetamiprid. The mass ratio of active ingredient A to active ingredient B is 1:30 to 25:1. The insecticidal composition of this invention has advantages such as synergistic effects and reduced resistance. This insecticidal composition can be used to control agricultural, forestry, and horticultural pests.

Description

[0001] This invention application is a divisional application of application number 202111303461.2, filed on November 5, 2021, entitled "An insecticidal composition containing bis(triflufenicol) and its application therein". Technical Field

[0002] This invention belongs to the field of pesticides and insecticides, specifically relating to an insecticidal composition containing bis(triflufenoxuron) and its application. Background Technology

[0003] Bis(trifluorourea) is a highly effective insect growth regulator screened from benzoylurea derivatives. Its chemical name is 1-[(2-fluoro-3,5-bis(trifluoromethyl)phenyl)-3-(2,6-difluorobenzoyl)]urea. Benzoylurea derivatives (BPUS) are a class of insect growth regulators (IGRs) that inhibit chitin synthesis in insects and have stomach poison effects. They exhibit high specificity, are very effective against larval insects, degrade rapidly in the environment, and have low toxicity to mammals. The chemical structural formula is:

[0004]

[0005] Spinosad is a biological insecticide extracted directly from the fermentation broth of the actinomycete *Saccharopolyspora spinosa*, a secondary metabolite produced during fermentation. It acts as an allosteric modulator of the nicotinic acetylcholine receptor (nAChR)—binding site I—affecting insect neural activity. Allosteric activation of this receptor (different from binding site II in group 32) causes hyperexcitability of the insect nervous system. In addition to the main components A and D, it also contains B, C, E, F, H, and J. Spinosad is a first-generation insecticide, primarily used to control lepidopteran and thalassopteran pests.

[0006] Dinotefuran is a competitive regulator of nicotinic acetylcholine receptors (nAChRs) and acts on the insect nervous system. It binds to the acetylcholine site on its receptor, causing a range of symptoms in insects, from hyperexcitability to lethargy and paralysis. Acetylcholine is the main excitatory neurotransmitter in the insect central nervous system. Dinotefuran is a third-generation neonicotinoid insecticide that is rapidly absorbed by plants and widely distributed within them.

[0007] Flunicamid is a novel, low-toxicity pyridine amide insecticide developed and produced by Ishihara Sangyo Co., Ltd. of Japan. It has contact, systemic, and penetrating effects and exhibits good neurotoxicity and antifeedant activity against piercing-sucking pests such as aphids. Its antifeedant activity is irreversible.

[0008] Nitenpyram is a neonicotinoid insecticide that primarily acts on the insect nervous system, blocking nerve activity through synaptic receptors. Nitenpyram exhibits excellent systemic and penetrating activity, allowing it to be absorbed and translocated by plant tissues. It is characterized by high efficacy, low toxicity, and long-lasting effect against piercing-sucking pests.

[0009] In the actual process of agricultural production, the development of pesticide resistance in pests has become an increasingly urgent problem, and formulating appropriate resistance control measures is an important part of integrated pest management. Developing a new pesticide is relatively time-consuming and costly, and pesticides are being phased out at an increasingly rapid pace due to pest resistance. Therefore, selecting the best pesticides without cross-resistance for combination to effectively prevent the development of pesticide resistance in agricultural pest control is crucial. Through the inventors' experimental research, it was found that combining bismuth subtilis with spinosad, dinotefuran, flonicamid, and acetamiprid produces a good synergistic effect on pests, reduces pesticide resistance, decreases pesticide dosage, lowers pesticide residues on crops, and mitigates environmental pollution. Summary of the Invention

[0010] The purpose of this invention is to provide an insecticidal composition containing bis(triflufenoxuron) that has synergistic effects, low cost of use, and good control efficacy.

[0011] To achieve the above objectives, the present invention discloses an insecticidal composition containing bis(triflufenican) and its application. The insecticidal composition includes active ingredient A and active ingredient B. Active ingredient A is bis(triflufenican), and active ingredient B is any one of dinotefuran, spinosad, flonicamid, and acetamiprid. The mass ratio of active ingredient A to active ingredient B is 1:30 to 25:1.

[0012] Furthermore, the mass ratio of bis(triflufenican) to spinosad is 1:10 to 25:1;

[0013] Furthermore, the mass ratio of bis(triflufenican) to spinosad is 1:10 to 6:1;

[0014] Furthermore, the mass ratio of bis(triflufenican) to spinosad is 1:10, 1:8, 1:3, 2:5, 3:1, or 6:1.

[0015] Furthermore, the mass ratio of bis(triflufenican) to dinotefuran is 1:15 to 10:1;

[0016] Furthermore, the mass ratio of bis(triflufenican) to dinotefuran is 2:9 to 10:1;

[0017] Furthermore, the mass ratio of bis(triflufenican) to dinotefuran is 2:9, 3:4, 5:1, or 10:1;

[0018] Furthermore, the mass ratio of bis(triflufenican) to flonicamid is 1:25 to 10:1;

[0019] Furthermore, the mass ratio of bis(triflufenican) to flonicamid is 2:15 to 7:1;

[0020] Furthermore, the mass ratio of bis(triflufenican) to flonicamid is 2:15, 1:8, 3:2, 1:3, or 7:1;

[0021] Furthermore, the mass ratio of bis(triflufenican) to acetamiprid is 1:10 to 7:1;

[0022] Furthermore, the mass ratio of bis(triflufenican) to acetamiprid is 1:7 to 7:1;

[0023] Furthermore, the mass ratio of bis(triflufenican) to acetamiprid is 1:7, 1:3, 2:5, 5:1, or 7:1.

[0024] Furthermore, the content of active ingredient A and active ingredient B in the insecticidal composition is 1-80 wt%, preferably 2-60 wt%.

[0025] Furthermore, the insecticidal composition, in addition to the active ingredient, also includes an adjuvant, which is selected from one or more of the following: wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoamers, solvents, stabilizers, penetrants, and carriers.

[0026] Furthermore, the wetting agent is selected from one or more of the following: sodium dodecyl sulfate, sodium dodecylbenzene sulfonate, pull-opening powder BX, wetting and penetrating agent F, soapberry powder, silkworm excrement, or soapberry powder;

[0027] Furthermore, the dispersant is selected from one or more of the following: polycarboxylate, lignin sulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, calcium alkylbenzene sulfonate, sodium naphthalene sulfonate formaldehyde condensate, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty acid polyoxyethylene ether, or glycerol fatty acid ester polyoxyethylene ether.

[0028] Furthermore, the emulsifier is selected from one or a mixture of multiple of the following: calcium alkylbenzene sulfonate, OP series phosphate esters (nonylphenol polyoxyethylene ether phosphate ester), phenylphenol polyoxyethylene ether phosphate ester, styrene polyoxyethylene ether ammonium sulfate, alkyl biphenyl ether magnesium disulfonate, triethanolamine salt, benzyl dimethylphenol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, phenethylphenol formaldehyde resin polyoxyethylene ether, phenethylphenol polyoxyethylene polypropylene ether, ethylene oxide-propylene oxide block copolymer, OP series (nonylphenol polyoxyethylene ether), castor oil polyoxyethylene ether, alkyl aryl polyoxyethylene polyoxypropylene ether, sorbitan monostearate, dehydrated sorbitan fatty acid ester polyoxyethylene ether, or fatty alcohol polyoxyethylene ether.

[0029] Furthermore, the thickener is selected from one or more of xanthan gum, polyvinyl alcohol, bentonite, carboxymethyl cellulose, or magnesium aluminum silicate;

[0030] Furthermore, the disintegrant is selected from one or more of the following: bentonite, urea, ammonium sulfate, aluminum chloride, low-substituted hydroxypropyl cellulose, lactose, citric acid, succinic acid, or sodium bicarbonate;

[0031] Furthermore, the antifreeze is selected from one or more of ethylene glycol, propylene glycol, glycerol, or urea, or a mixture thereof;

[0032] Furthermore, the defoamer is selected from one or more of the following: silicone oil, silicone compounds, C10-C20 saturated fatty acid compounds, or C8-C10 fatty alcohol compounds;

[0033] Further, the solvent is selected from one or more of the following: N,N-dimethylformamide, cyclohexanone, butyl ether, xylene, dimethyl sulfoxide, methanol, ethylene glycol, ethanol, propanol, butanol, trimethylcyclohexanone, N-octylpyrrolidone, toluene, ethanolamine, triethanolamine, isopropylamine, N-methylpyrrolidone, diethylene glycol, ethylene glycol methyl ether, ethyl acetate, or acetonitrile.

[0034] Furthermore, the stabilizer is selected from one or more of the following: epoxidized soybean oil, epichlorohydrin, BHT, ethyl acetate, and triphenyl phosphate;

[0035] Furthermore, the penetrant is selected from one or more of penetrant JFC, penetrant T, azone, or organosilicon;

[0036] Furthermore, the carrier is one, two, or three of the solvent or filler, and the water is preferably deionized water;

[0037] Furthermore, the filler is selected from one or more of the following: kaolin, diatomaceous earth, bentonite, attapulgite, silica, starch, or light calcium carbonate.

[0038] All of the above substances are commercially available.

[0039] This insecticidal composition can be prepared into any agriculturally acceptable formulation as needed, wherein the formulation is selected from any of the following: powder, granules, soluble powder, soluble granules, soluble tablets, water-dispersible granules, wettable powder, water-dispersible tablets, dispersible liquid, emulsifiable concentrate, water-emulsion, microemulsion, suspension concentrate, suspension emulsion, and soluble concentrate.

[0040] Furthermore, the dosage form of the formulation is selected from suspension concentrates, emulsifiable concentrates, water-dispersible particles, and dispersible oil suspensions;

[0041] Furthermore, the suspension preparation method of the present invention is as follows: according to the formula ratio, the active ingredients, surfactants and other functional additives are placed in the reaction vessel in sequence, water is added and mixed evenly, and then subjected to high-speed shearing, wet sand milling, and finally homogenized filtration to obtain the suspension product.

[0042] The preparation method of the emulsifiable concentrate is as follows: according to the formula ratio, the measured active ingredients, solvents and cosolvents are added to the mixing tank and stirred to dissolve them. Then, the emulsifier is added, and the remaining solvent is used to make up the balance. The mixture is stirred evenly in the mixing tank and filtered to obtain the emulsifiable concentrate.

[0043] The method for preparing the water-dispersible granules is as follows: 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 milling, and 10-25% water is added. Then, the mixture is kneaded, granulated, dried, and sieved to obtain the water-dispersible granule product; or the pulverized powder is sprayed with water, granulated, dried in a fluidized bed granulator, and then sieved to obtain the product.

[0044] The preparation method of the dispersible oil suspension is as follows: according to the formula ratio, the active ingredients, surfactants and other functional additives are placed in the reaction vessel in sequence, mixed evenly with oil, subjected to high-speed shearing, wet sand milling, and finally homogenized filtration to obtain the dispersible oil suspension product.

[0045] Application of an insecticidal composition containing bis(triflufenoxuron) in the control of agricultural, forestry and horticultural pests.

[0046] Furthermore, the pests mentioned are Lepidoptera and Hemiptera pests;

[0047] 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 worm), *Anacamptodes defectaria*, *Anarsia lineatella* (peach twig borer), *Anomis sabulifera* (jute looper), *Anticarsiag emmatalis*, *Archips argyrospila* (fruittree leafroller), and *Archips rosana* (rose leafroller). The following are listed as examples of leaf rollers: *Argyrotaenia spp.* (tortricid moths), *Argyrotaenia citrana* (orange tortrix), *Autographa gamma*, *Bonagota cranaodes*, *Borbo cinnara* (rice leaf folder), *Bucculatrix thurberiella* (cotton leafperforator), *Caloptilia spp.* (leaf miners), *Capua reticulana*, *Carposina niponensis* (peach fruit moth), *Chilo spp.*, *Chlumetia transversa* (mango shoot borer), *Choristoneurarosaceana* (obliquebanded leafroller), and *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), armyworm (Mythimna separate (Walker)), elegantalis (Neoleucinodes elegantalis), three-spotted water moth (Nymphuladepunctalis), winter inchworm (Operophthera brumata), European corn borer (Ostrinia nubilalis), Oxydia vesulia, common currant tortrix (Pandemis cerasana), brown apple tortrix (Pandemis heparana), African swallowtail butterfly (Papilio demodocus), red bollworm (Pectinophora) *Phyllopyella gossypiella* (pinkbollworm), *Peridroma* spp. (root cutter), *Peridroma saucia* (variegated cutworm), *Perileucoptera coffeella* (white coffee leafminer), *Phthorimaea operculella* (potatotuber moth), *Phyllocnisitis citrella* (citrus leafminer), and *Phyllonorycters* pp.The following species are listed: cabbage white butterfly (Pieris rapae), alfalfa green armyworm (Plathypena scabra), Indian grain moth (Plodiainterpunctella), diamondback moth (Plutella xylostella), grape leafroller (Polychrosis viteana), citrus nut moth (Prays endocarpa), olive moth (Prays oleae), noctuid moth (Pseudaletia spp.), armyworm (Pseudaletia unipunctata), soybean noctuid moth (Pseudoplusia includes), inchworm (Rachiplusia nu), rice stem borer (Chilo suppressalis (Walker), rice stem borer (Scirpophaga incertulas), and stem borer (Sesamia). spp. (stemborers), pink rice stem borer (Sesamia inferens), nonagrioides, setora nitens, grain moth (Angoumois grain moth), grape pill roller (Sparganothis pilleriana), Spodoptera spp., beet armyworm (Spodoptera exigua), fall armyworm (Spodoptera fugiperda), southern armyworm (Spodoptera oridania), Synanthedon spp., Thecla basilides, Thermisia gemmatalis, clothes moth (Tineola bisselliella), powdery spot moth (Trichoplusia) (Cabbage caterpillar), tomato leafminer (Tutaabsoluta);

[0048] The aforementioned Hemiptera pests include: green stink bugs (Acrosternum hilare), chinch bugs (Blissus leucopterus), potato blind bugs (Calocoris norvegicus), green stink bugs (Acrosternum hilare), chinch bugs (Blissus leucopterus), potato blind bugs (Calocoris norvegicus), aphids, scales, whiteflies, leafhoppers, pea aphids (Acrythosiphon pisum), aphids (Adelges spp.), cabbage whiteflies (Aleurodes proletella), and spiral whiteflies (Aleurodicus). * *Aleurothrixus floccosus* (woolly whitefly), *Aluacaspis* spp., *Aonidiella aurantii*, *Aphis* spp., *Aphis gossypii* (cotton aphid), *Aphis pomi*, *Aulacorthum solani* (foxglove aphid), *Bemisia* spp. (whitefly), *Trialeurodea vaporirum (Westwood)*, *Bemisia argentifolii*, *Bemisia tabaci* (sweet potato whitefly), *Brachycolus noxius*, *Brachycorynella asparagi* (asparagus aphid), *Brevennia* rehi, cabbage aphid (Brevicoryne brassicae), wax scale (Ceroplastes spp.), red wax scale (Ceroplastes rubens) (red wax scale), snow shield scale (Chionaspis spp.), round shield scale (Chrysomphalus spp.).The following aphids are listed: *Dysaphis plantaginea* (red apple aphid), *Empoasca spp.*, *Eriosoma lanigerum*, *Icerya purchasi* (cottony cushion scale), *Idioscopus nitidulus* (mango leafhopper), *Laodelphax striatellus*, *Lepidosaphes spp.*, *Macrosiphum spp.*, *Macrosiphumeuphorbiae*, *Macrosiphum granarium*, *Macrosiphum rosae* (rose aphid), *Macrosteles quadrilineatus* (aster leafhopper), *Mahanarva frimbiolata*, and *Metopolophium*. * *dirhodum*, *Mictis longicornis*, *Myzus spp.*, *Myzus persicae* (green peach aphid), *Nephotettix spp.*, *Nephotettix cinctipes* (green leafhopper), *Nilaparvata lugens*, *Parlatoria pergandii*, *Peregrinus maidis* (corndelphacid), *Philaenus spp.*, *Phylloxera vitifoliae* (grape phylloxera), *Physokermes piceae* (spruce bud scale), *Planococcus spp.* (mealyptus), *Pseudococcus* spp.(Mealybug), Pseudococcus brevipes (pine apple mealybug), Quadraspidiotus perniciosus (San Jose scale), Rhopalosiphum spp., Rhopalosiphum maida (corn leaf aphid), Rhapalosiphum padi (oat bird-cherry aphid), Saissetias pp., Saissetia oleae, Schizaphis graminum (green bug), Sitobion avenae (English grain aphid), Sogatellafurcifera, Therioaphis spp.), *Toumeyella* spp., *Trialeurodes* spp., *Trialeurodes vaporariorum*;

[0049] Furthermore, the Lepidoptera pests include diamondback moth, beet armyworm, cotton bollworm, rice stem borer, armyworm, cotton bollworm, and cabbage caterpillar; the Hemiptera pests include whitefly, rice planthopper, and aphid.

[0050] An insecticidal composition containing bis(triflufenoxuron) is applied in an effective dose to pests that need to be controlled or their growth media.

[0051] The advantages of this invention are:

[0052] (1) When bis(triflufenoxam) is combined with any one of spinosad, dinotefuran, flonicamid, or acetamiprid, it has a significant synergistic effect within a certain range.

[0053] (2) Reduce the amount of pesticides used, reduce pesticide residues on crops, and mitigate environmental pollution;

[0054] (3) This insecticidal composition has broadened the insecticidal spectrum and has a good control effect on a variety of pests. Detailed Implementation

[0055] To make the technical solutions, objectives, and advantages of this invention clearer, the invention is illustrated by the following specific embodiments. However, this invention can be implemented in various forms and should not be limited to the embodiments described herein. The invention has been described in detail below with general descriptions and specific embodiments. However, modifications or improvements can be made to this invention, which will be obvious to those skilled in the art. All equivalent transformations made based on the technical solutions of this application fall within the protection scope of this invention.

[0056] Formulation preparation examples:

[0057] Example 1: 28% diflubenzuron·spinosad suspension (2:5)

[0058] Formula: By weight percentage, 8% bis(triflufenican), 20% spinosad, 1% isotridecyl alcohol polyoxyethylene ether, 1% naphthalene sulfonate formaldehyde condensate, 3% styrene-phenol polyoxyethylene ether phosphate, 2% alkyl aryl polyoxyethylene ether polyoxypropylene ether, 0.2% xanthan gum, 1% magnesium aluminum silicate, 5% propylene glycol, 0.2% potassium benzoate, 0.5% silicone oil, deionized water to make up the balance.

[0059] Preparation method: According to the formula ratio, the active ingredients, surfactants and other functional additives are placed in the reaction vessel in sequence, water is added and mixed evenly, and then subjected to high-speed shearing, wet sand milling and finally homogenization filtration to obtain the suspension product.

[0060] Example 2: 20% diflubenzuron·spinosad suspension (3:1)

[0061] Formula: By weight percentage, 15% diflubenzuron, 5% spinosad, 3% alkylphenol polyoxyethylene ether, 4% alkylphenol polyoxyethylene ether phosphate, 1% sodium polycarboxylate, 0.25% xanthan gum, 5% glycerol, 0.1% sodium benzoate, 0.5% silicone oil, with deionized water to make up the balance.

[0062] Preparation method: Same as in Example 1.

[0063] Example 3: 18% diflubenzuron·spinosad suspension (1:8)

[0064] Formula: By weight percentage, 2% trifluralin, 16% spinosad, 1% succinate sulfonate, 3% styrene-phenol polyoxyethylene ether sulfate, 2% alkyl aryl polyoxyethylene ether polyoxypropylene ether, 1% lignin sulfonate, 1.5% magnesium aluminum silicate, 0.1% carboxyethyl cellulose, 0.1% xanthan gum, 1% sodium sorbate, 5% ethylene glycol, 0.5% silicone oil, deionized water to make up the balance.

[0065] Preparation method: Same as in Example 1.

[0066] Example 4: 20% diflubenzuron·spinosad water-dispersible granules (1:3)

[0067] Formula: By weight percentage, 5% diflubenzuron, 15% spinosad, 10% lignin sulfonate, 4% sodium dodecylbenzene sulfonate, 5% silica, 30% starch, and kaolin to make up the balance.

[0068] Preparation method: According to the formulation ratio in the example, the active ingredient is added to the carrier, and surfactants and other functional additives are added thereto. After mixing, the mixture is pulverized by air jet and 10-25% water is added. Then, the mixture is kneaded, granulated, dried and sieved to obtain the water-dispersible granule product.

[0069] Example 5:

[0070] 30% Spinosad·Triflufenoxam water-dispersible granules (1:2)

[0071] Formula: By weight percentage, 10% diflubenzuron, 20% spinosad, 8% sodium lignosulfonate, 2.5% BX (a type of lignosulfonate), 1.5% sodium dodecylbenzenesulfonate, 5% ammonium sulfate, and kaolin to make up the balance.

[0072] Preparation method: Same as in Example 4.

[0073] Example 6: 35% diflubenzuron·spinosad water-dispersible granules (6:1)

[0074] Formula: By weight percentage, 30% diflubenzuron, 5% spinosad, 8% naphthalene sulfonate formaldehyde condensate, 2% sodium polycarboxylate, 3% BX (a type of acetic acid powder), and kaolin to make up the balance.

[0075] Preparation method: Same as in Example 4.

[0076] Example 7: 21% diflubenzuron·fipronil suspension (3:4)

[0077] Formula: By weight percentage, 9% bis(triflufenican), 12% dinotefuran, 1% sodium dodecyl sulfate, 1% naphthalene sulfonate formaldehyde condensate, 3% styrene-phenol polyoxyethylene ether phosphate, 0.2% xanthan gum, 1% magnesium aluminum silicate, 4% propylene glycol, 0.01% benzisothiazolinone potassium, 0.5% silicone oil, deionized water to make up the balance.

[0078] Preparation method: Same as in Example 1.

[0079] Example 8: 20% diflubenzuron·fipronil suspension concentrate (1:3)

[0080] Formula: By weight percentage, 5% bis(triflufenican), 15% dinotefuran, 0.5% alkylphenol polyoxyethylene ether, 4% alkylphenol polyoxyethylene ether phosphate, 1% sodium lignosulfonate, 0.25% xanthan gum, 5% glycerol, 0.1% sodium benzoate, 0.5% silicone oil, with deionized water to make up the balance.

[0081] Preparation method: Same as in Example 1.

[0082] Example 9: 30% diflubenzuron·fipronil suspension (1:2)

[0083] Formula: By weight percentage, 10% bis(triflufenican), 20% dinotefuran, 1% fatty alcohol polyoxyethylene ether, 3% alkyl aryl polyoxyethylene ether polyoxypropylene ether, 2% styrene-phenol polyoxyethylene ether sulfate, 1% sodium polycarboxylate, 1.5% magnesium aluminum silicate, 0.1% carboxyethyl cellulose, 1% sodium sorbate, 5% ethylene glycol, 0.5% silicone oil, and deionized water to make up the balance.

[0084] Preparation method: Same as in Example 1.

[0085] Example 10: 20% diflubenzuron·fipronil water-dispersible granules (1:3)

[0086] Formula: By weight percentage, 5% diflubenzuron, 15% diflubenzuron, 10% lignin sulfonate, 4% sodium dodecylbenzene sulfonate, 2% sodium dodecyl sulfate, 5% silica, 30% starch, and kaolin to make up the balance.

[0087] Preparation method: Same as in Example 4.

[0088] Example 11: 30% diflubenzuron·fipronil water-dispersible granules (1:2)

[0089] Formula: By weight percentage, 10% diflubenzuron, 20% difenoconazole, 8% sodium lignosulfonate, 2.5% bleaching powder BX, 1.5% sodium dodecylbenzenesulfonate, 5% white sugar, and kaolin to make up the balance.

[0090] Preparation method: Same as in Example 4.

[0091] Example 12: 40% diflubenzuron·fipronil water-dispersible granules (1:3)

[0092] Formula: By weight percentage, 10% bis(triflufenican), 30% dinotefuran, 8% naphthalenesulfonate formaldehyde condensate, 2% sodium polycarboxylate, 2% sodium dodecyl sulfate, 10% ammonium sulfate, and starch to make up the balance.

[0093] Preparation method: Same as in Example 4.

[0094] Example 13: 24% Diflubenzuron·Fentanyl Dispersible Oil Suspension (1:5)

[0095] Formula: By weight percentage, 4% bis(triflufenican), 20% dinotefuran, 2% lignin sulfonate, 14% alkyl aryl polyoxyethylene polyoxypropylene ether, 3% fatty alcohol polyoxyethylene ether, 2% calcium dodecylbenzene sulfonate, 1% silica, 1% organobentonite, 20% 200# solvent oil, and methyl oleate to make up the balance.

[0096] Preparation method: According to the formula ratio, the active ingredients, surfactants and other functional additives are placed in the reaction vessel in sequence, oil is added and mixed evenly, and then subjected to high-speed shearing, wet sand milling and finally homogenization filtration to obtain the dispersible oil suspension product.

[0097] Example 14: 20% Diflubenzuron·Fipronil dispersible oil suspension (1:3)

[0098] Formula: By weight percentage, 5% diflubenzuron, 15% difenoconazole, 4% alkylphenol polyoxyethylene ether, 12% castor oil polyoxyethylene ether, 1% calcium dodecylbenzene sulfonate, 1% sodium polycarboxylate, 1% naphthalene sulfonate formaldehyde condensate, and soybean oil to make up the balance.

[0099] Preparation method: Same as in Example 13.

[0100] Example 15: 15% Diflubenzuron·Fentanyl Dispersible Oil Suspension (1:2)

[0101] Formula: By weight percentage, 5% diflubenzuron, 10% diflubenzuron, 1% fatty alcohol polyoxyethylene ether, 15% polyoxyethylene dehydrated sorbitan monooleate, 2% calcium dodecylbenzene sulfonate, 2% succinate sulfonate, 1.5% magnesium aluminum silicate, 1% Tesco 869, corn oil to make up the balance.

[0102] Preparation method: Same as in Example 13.

[0103] Example 16: 30% diflubenzuron·fipronil EC (5:1)

[0104] Formula: By weight percentage, 25% bis(triflufenican), 5% dinotefuran, 15% DMF, 14% styrene-phenol polyoxyethylene ether, 2% calcium dodecylbenzenesulfonate, 20% propylene carbonate, and xylene to make up the balance.

[0105] Preparation method: According to the formula ratio, add the measured active ingredients, solvent and co-solvent into the mixing tank and stir to dissolve them. Then add the emulsifier, and use the remaining solvent to make up the balance. Stir evenly in the mixing tank, and filter to obtain the emulsifiable oil.

[0106] Example 17: 18% diflubenzuron·fipronil EC (2:1)

[0107] Formula: By weight percentage, 12% bis(triflufenican), 6% dinotefuran, 20% N-methylpyrrolidone, 14% alkylphenol polyoxyethylene ether, 2% calcium dodecylbenzenesulfonate, 10% DMF, and methyl oleate to make up the balance.

[0108] Preparation method: Same as in preparation example 16.

[0109] Example 18: 10% diflubenzuron·fipronil EC (1:1)

[0110] Formula: 5% bis(triflufenican), 5% dinotefuran, 15% EO / PO block copolymer, 15% acetophenone, 10% N-octylpyrrolidone, 1% calcium dodecylbenzenesulfonate, and the balance is made up with tricresylbenzene.

[0111] Preparation method: Same as in preparation example 16.

[0112] Example 19: 24% bis(triflufenican)·fluoxetine suspension concentrate (1:5)

[0113] Formula: By weight percentage, 4% trifluralin, 20% flonicamid, 1% fatty alcohol polyoxyethylene ether, 1% sodium polycarboxylate, 3% styrene-phenol polyoxyethylene ether sulfate, 2% alkyl aryl polyoxyethylene ether polyoxypropylene ether, 0.5% magnesium aluminum silicate, 0.20% xanthan gum, 4% propylene glycol, 0.2% potassium benzoate, 0.5% silicone oil, deionized water to make up the balance.

[0114] Preparation method: Same as in Example 1.

[0115] Example 20: 20% bis(triflufenican)·fluoxetine suspension concentrate (1:3)

[0116] Formula: By weight percentage, 5% trifluralin, 15% flonicamid, 1% isomeric alcohol polyoxyethylene ether, 4% alkylphenol polyoxyethylene ether phosphate, 1% lignin sulfonate, 2% alkyl aryl polyoxyethylene ether polyoxypropylene ether, 0.25% xanthan gum, 5% glycerol, 0.1% sodium benzoate, 0.5% silicone oil, with deionized water to make up the balance.

[0117] Preparation method: Same as in Example 1.

[0118] Example 21: 25% bis(triflufenican)·fluoxetine suspension concentrate (3:2)

[0119] Formula: By weight percentage, 15% trifluralin, 10% flonicamid, 1% fatty alcohol polyoxyethylene ether, 2% alkyl aryl polyoxyethylene ether polyoxypropylene ether, 1% naphthalene sulfonate formaldehyde condensate, 4% styrene phenol polyoxyethylene ether phosphate, 1.5% magnesium aluminum silicate, 0.1% carboxyethyl cellulose, 1% sodium sorbate, 5% ethylene glycol, 0.5% silicone oil, deionized water to make up the balance.

[0120] Preparation method: Same as in Example 1.

[0121] Example 22: 25% bis(triflufenoxam)·fluoxetine water-dispersible granules (2:3)

[0122] Formula: By weight percentage, 10% bis(triflufenican), 15% flufenoxuron, 10% lignin sulfonate, 4% sodium dodecylbenzene sulfonate, 2% sodium dodecyl sulfate, 30% starch, and kaolin to make up the balance.

[0123] Preparation method: Same as in Example 4.

[0124] Example 23: 30% bis(triflufenoxam)·fluoxetine water-dispersible granules (1:2)

[0125] Formula: By weight percentage, 10% bis(triflufenican), 20% flonicamid, 8% sodium lignosulfonate, 3% naphthalenesulfonate formaldehyde condensate, 2.5% pyrrolidone BX, 1.5% sodium dodecylbenzenesulfonate, 10% ammonium sulfate, and kaolin to make up the balance.

[0126] Preparation method: Same as in Example 4.

[0127] Example 24: 40% bis(triflufenoxam)·fluoxetine water-dispersible granules (1:3)

[0128] Formula: By weight percentage, 10% bis(triflufenican), 30% flonicamid, 10% naphthalenesulfonate formaldehyde condensate, 2% sodium polycarboxylate, 4% sodium dodecyl sulfate, with light calcium carbonate to make up the balance.

[0129] Preparation method: Same as in Example 4.

[0130] Example 25: 27% Diflubenzuron·Fluoxane Dispersible Oil Suspension (1:8)

[0131] Formula: By weight percentage, 3% bis(triflufenican), 24% flonicamid, 1% naphthalenesulfonate formaldehyde condensate, 12% alkylaryl polyoxyethylene polyoxypropylene ether, 3% fatty alcohol polyoxyethylene ether, 2% calcium dodecylbenzenesulfonate, 1% silica, 1% organobentonite, and methyl oleate to make up the balance.

[0132] Preparation method: Same as in Example 13.

[0133] Example 26: 20% Diflubenzuron·Fluoxane Dispersible Oil Suspension (1:3)

[0134] Formula: By weight percentage, 5% bis(triflufenican), 15% flonicamid, 4% alkylphenol polyoxyethylene ether, 10% castor oil polyoxyethylene ether, 1% calcium dodecylbenzene sulfonate, 1% sodium polycarboxylate, and soybean oil to make up the balance.

[0135] Preparation method: Same as in Example 13.

[0136] Example 27: 15% Diflubenzuron·Fluoxane Dispersible Oil Suspension (1:2)

[0137] Formula: By weight percentage, 5% trifluralin, 10% flonicamid, 1% fatty alcohol polyoxyethylene ether, 14% polyoxyethylene dehydrated sorbitan monooleate, 2% calcium dodecylbenzene sulfonate, 1% succinate sulfonate, 1.5% magnesium aluminum silicate, 1% Tesco 869, corn oil to make up the balance.

[0138] Preparation method: Same as in Example 13.

[0139] Example 28: 20% bis(triflufenoxam)·flufenoxam EC (3:1)

[0140] Formula: By weight percentage, 15% bis(triflufenican), 5% flonicamid, 10% dimethyl sulfoxide, 13% styrene-phenol polyoxyethylene ether, 2% calcium dodecylbenzenesulfonate, 20% propylene carbonate, and xylene to make up the balance.

[0141] Preparation method: Same as in Example 16.

[0142] Example 29: 18% bis(triflufenoxam)·flufenoxam EC (2:1)

[0143] Formula: By weight percentage, 12% bis(triflufenican), 6% flonicamid, 20% propylene glycol methyl ether, 15% alkylphenol polyoxyethylene ether, 2% calcium dodecylbenzenesulfonate, 10% DMF, and methyl oleate to make up the balance.

[0144] Preparation method: Same as in preparation example 16.

[0145] Example 30: 10% bis(triflufenoxam)·fluoxetine emulsifiable concentrate (1:1)

[0146] Formula: By weight percentage, 5% bis(triflufenican), 5% flonicamid, 15% EO / PO block copolymer, 15% acetophenone, 10% propylene glycol methyl ether, 1% calcium dodecylbenzenesulfonate, and 100% tricresylbenzene.

[0147] Preparation method: Same as in preparation example 16.

[0148] Example 31: 20% diflubenzuron·acetamiprid water-dispersible granules (1:3)

[0149] Formula: By weight percentage, 5% bis(triflufenican), 15% acetamiprid, 10% dispersant NNO, 2% sodium dodecyl sulfate, 4% sodium dodecylbenzene sulfonate, 30% starch, and light calcium carbonate to make up the balance.

[0150] Preparation method: Same as in Example 4.

[0151] Example 32: 30% diflubenzuron·acetamiprid water-dispersible granules (1:2)

[0152] Formula: By weight percentage, 10% bis(triflufenican), 20% acetamiprid, 10% sodium lignosulfonate, 2.5% bleaching powder BX, 1.5% sodium dodecylbenzenesulfonate, 10% glucose, and starch to make up the balance.

[0153] Preparation method: Same as in Example 4.

[0154] Example 33: 40% diflubenzuron·acetamiprid water-dispersible granules (1:3)

[0155] Formula: By weight percentage, 10% bis(triflufenican), 30% acetamiprid, 4% naphthalenesulfonate formaldehyde condensate, 10% sodium polycarboxylate, 2% sodium dodecyl sulfate, 5% silica, and kaolin to make up the balance.

[0156] Preparation method: Same as in Example 4.

[0157] Example 34: 14% diflubenzuron·acetamiprid EC (2:5)

[0158] Formula: By weight percentage, 4% bis(triflufenican), 10% acetamiprid, 15% EO / PO block copolymer, 10% dimethyl sulfoxide, 10% propylene glycol methyl ether, 1% calcium dodecylbenzenesulfonate, and 100% thallium benzene.

[0159] Preparation method: Same as in Example 16.

[0160] Example 35: 18% bispyribac-methyl·acetamiprid EC (5:1)

[0161] Formula: By weight percentage, 15% bis(triflufenican), 3% acetamiprid, 30% acetophenone, 10% castor oil polyoxyethylene ether, 5% fatty alcohol polyoxyethylene ether, 2% calcium dodecylbenzenesulfonate, and methyl oleate to make up 100%.

[0162] Preparation method: Same as in Example 16.

[0163] Example 36: 15% diflubenzuron·acetamiprid EC (1:2)

[0164] Formula: By weight percentage, 5% bis(triflufenican), 10% acetamiprid, 30% propylene carbonate, 10% polyoxyethylene sorbitan monooleate, 5% isotridecyl polyoxyethylene ether, 1% calcium dodecylbenzenesulfonate, and pine resin-based vegetable oil to make up 100%.

[0165] Preparation method: Same as in Example 16.

[0166] Indoor bioactivity assay

[0167] Indoor test 1: Combined toxicity of trifluralin and spinosad mixture on rice stem borer and armyworm

[0168] Experimental method: Leaf dipping method;

[0169] Test reagents: 94.7% diflubenzuron technical grade (provided by the Group's R&D Center), 92% spinosad technical grade (provided by Qilu Pharmaceutical (Inner Mongolia) Co., Ltd.).

[0170] Experimental targets and age groups: early third instar of the rice stem borer (Chilo suppressalis (Walker)) and early third instar of the armyworm (Mythimna separata (Walker)). The insects used in the experiment were populations that were continuously bred and raised indoors by the research and development center.

[0171] The larvae were fed fresh water chestnut segments. Rearing conditions: a constant temperature rearing room of 25±1℃, relative humidity of 65%±5%, and light intensity L:D = 14:10h.

[0172] Assay method: Single-agent stock solutions were prepared separately, and five formulations were designed based on the purpose of mixing and the activity of the agents. Five series of mass concentrations were prepared for each single agent and each formulation mixture using a proportional method. Each treatment consisted of 20 test insects, with four replicates. The insects were placed in a constant temperature rearing room at 25±1℃, with a relative humidity of 65%±5% and a light intensity of L:D = 14:10h.

[0173] The examples refer to NY / T 1154.7-2006 "Guidelines for Indoor Bioassay of Pesticides - Insecticides - Part 7: Determination of Combined Effects of Mixtures" and NY / T 1154.14-2008 "Guidelines for Indoor Bioassay of Pesticides - Insecticides - Part 14: Leaf Dipping Method".

[0174] Data statistics and analysis:

[0175] The mortality of the test insects was checked 72 hours after treatment, and the total number of insects and the number of dead insects were recorded. The corrected mortality rate for each treatment was calculated based on the survey data. The calculations were performed using formulas (1) and (2), and the results were rounded to two decimal places.

[0176]

[0177] In the formula:

[0178] P – Mortality rate, expressed as a percentage (%);

[0179] K represents the number of dead insects, in heads;

[0180] N represents the total number of insects treated, in units of heads.

[0181]

[0182] In the formula:

[0183] P1 – Corrected mortality rate, in percentage (%);

[0184] P t —The mortality rate is expressed as a percentage (%).

[0185] P0 – Mortality rate in the blank control group, expressed as a percentage (%).

[0186] 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.

[0187] The data was processed using probability value analysis. The IBM SPSS Statistics 20 statistical analysis system can be used to analyze the data and determine the toxicity regression line and LC-value. 50 Values, their 95% confidence limits, and correlation coefficient R 2 To evaluate the activity of the test reagent on biological materials.

[0188] The co-toxicity coefficient (CTC value) of the mixture is calculated according to formulas (3), (4), and (5):

[0189]

[0190] In the formula:

[0191] ATI – Actual Measured Toxicity Index of Mixtures;

[0192] S – LC50 of standard insecticides 50 The unit is milligrams per liter (mg / L);

[0193] M – LC of the mixture 50 The unit is milligrams per liter (mg / L).

[0194] TTI = TI A *P A +TI B *PB ······(4)

[0195] In the formula:

[0196] TTI – Theoretical Toxicity Index of Mixtures;

[0197] TI A —A. Toxicity index of drug A;

[0198] P A —Percentage content of drug A in the mixture, expressed as percentage (%);

[0199] TI B —Toxicity index of drug B;

[0200] P B —Percentage content of agent B in the mixture, expressed as percentage (%).

[0201]

[0202] In the formula:

[0203] CTC – Cotoxicity Coefficient;

[0204] ATI – Actual Measured Toxicity Index of Mixtures;

[0205] TTI – Theoretical Toxicity Index of Mixtures.

[0206] 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.

[0207] The experimental results are shown in Tables 1 and 2.

[0208] Table 1. Combined toxicity of trifluralin and spinosad in the treatment of rice stem borer.

[0209]

[0210] As shown in the table above, when the mass ratio of bis(triflufenican) to spinosad is 1:30 to 25:1, the co-toxicity coefficient is greater than 120, showing a synergistic effect; when the mass ratio of bis(triflufenican) to spinosad is 1:10 to 25:1, the co-toxicity coefficient is greater than 150, showing a significant synergistic effect.

[0211] Table 2. Combined toxicity of trifluralin and spinosad on armyworms.

[0212]

[0213] As shown in the table above, when the mass ratio of bispyribac-triflufenoxam to spinosad is 1:10 to 8:1, the co-toxicity coefficient is greater than 120, indicating a synergistic effect; when the mass ratio of bispyribac-triflufenoxam to spinosad is 1:8 to 6:1, the co-toxicity coefficient is greater than 150, indicating a significant synergistic effect.

[0214] Indoor test 2: Co-toxicity of bispyribac-triflufenoxam and dinotefuran mixed on whiteflies

[0215] Experimental method: Agar moisturizing leaf immersion method.

[0216] The test target was the adult greenhouse whitefly (Trialeurodea vaporirum (Westwood)). The insect source was a population that had been continuously bred and reproduced indoors for multiple generations at the group's R&D center.

[0217] Test agents: 94.7% diflubenzuron technical grade and 98% diflubenzuron technical grade, both provided by the group's R&D center.

[0218] Experimental steps:

[0219] (1) Preparation of liquid agar:

[0220] Place agar powder in an Erlenmeyer flask, add water, and place in a microwave oven. Heat until the agar is completely dissolved. After slightly cooling, use a pipette to add 2 mL of liquid agar to the bottom of a flat-bottomed glass tube. Allow the liquid agar to cool and solidify, and for the vapor on the tube wall to evaporate completely, before use. During the cooling process, avoid agar adhering to the tube wall and prevent air bubbles from forming during solidification.

[0221] (2) Drug preparation: Prepare single-dose mother liquor separately, and design 5 sets of ratios according to the purpose of mixing and drug activity. Each single agent and each set of mixed agents are prepared into 5 series of mass concentrations according to the equal ratio method.

[0222] (3) Chemical treatment:

[0223] Fresh, flat cucumber leaves were punched into leaf discs. The leaf discs were immersed in the test solution for 10 seconds, then removed and dried. Using tweezers, the leaf discs were laid face down in a flat-bottomed glass tube containing agar, ensuring tight contact between the leaf disc, agar, and the tube wall without gaps. Each treatment was repeated four times, with a control group containing no reagent.

[0224] (3) Inoculation: Place the glass tube with the leaf discs laid out on the cucumber leaves where whiteflies are being cultured, tilt it, and gently tap the leaves to allow the whiteflies to enter the glass tube. Inoculate 20 whiteflies into each tube, turn the tube upside down and wait for the whiteflies to fly into the leaf discs at the bottom of the tube. Then, plug the tube with a cotton plug about 15mm from the bottom of the tube to force the whiteflies to stay on the leaf discs at the bottom of the tube.

[0225] (4) Feeding and observation:

[0226] The treated test insects were inverted and raised and observed under conditions of (25±1)℃, 65%±5% relative humidity, and a photoperiod of L:D=14:10h.

[0227] (5) Survey:

[0228] Forty-eight hours after treatment, the number of live worms in each tube was checked and recorded. Worms that did not move or could not move normally were considered dead. Based on the survey data, the corrected mortality rate for each treatment was calculated. The formula for calculating the experimental data is as described above.

[0229] The test results are shown in Table 3.

[0230] Table 3. Combined toxicity of bispyribac-triflufenican and dinotefuran on whiteflies.

[0231]

[0232]

[0233] As shown in the table above, when the mass ratio of bispyribac-to-diflubenzuron to fipronil is 1:15 to 10:1, the co-toxicity coefficient is greater than 120, showing a synergistic effect; when the mass ratio of bispyribac-to-diflubenzuron to fipronil is 2:9 to 10:1, the co-toxicity coefficient is greater than 150, showing a significant synergistic effect.

[0234] Indoor test of the combined toxicity of trifluralin and flonicamid against whiteflies

[0235] Experimental method: Agar moisturizing leaf immersion method.

[0236] The test target was the adult greenhouse whitefly (Trialeurodea vaporirum (Westwood)). The insect source was a population that had been continuously bred and reproduced indoors for multiple generations at the group's R&D center.

[0237] Test agents: 94.7% bis(triflufenoxam) technical grade and 96% flonicamid technical grade, both provided by the group's R&D center.

[0238] Experimental steps:

[0239] (1) Preparation of liquid agar:

[0240] Place agar powder in an Erlenmeyer flask, add water, and place in a microwave oven. Heat until the agar is completely dissolved. After slightly cooling, use a pipette to add 2 mL of liquid agar to the bottom of a flat-bottomed glass tube. Allow the liquid agar to cool and solidify, and for the vapor on the tube wall to evaporate completely, before use. During the cooling process, avoid agar adhering to the tube wall and prevent air bubbles from forming during solidification.

[0241] (2) Drug preparation: Prepare single-dose mother liquor separately, and design 5 sets of ratios according to the purpose of mixing and drug activity. Each single agent and each set of mixed agents are prepared into 5 series of mass concentrations according to the equal ratio method.

[0242] (3) Chemical treatment:

[0243] Fresh, flat cucumber leaves were punched into leaf discs. The leaf discs were immersed in the test solution for 10 seconds, then removed and dried. Using tweezers, the leaf discs were laid face down in a flat-bottomed glass tube containing agar, ensuring tight contact between the leaf disc, agar, and the tube wall without gaps. Each treatment was repeated four times, with a control group containing no reagent.

[0244] (3) Inoculation: Place the glass tube with the leaf discs laid out on the cucumber leaves where whiteflies are being cultured, tilt it, and gently tap the leaves to allow the whiteflies to enter the glass tube. Inoculate 20 whiteflies into each tube, turn the tube upside down and wait for the whiteflies to fly into the leaf discs at the bottom of the tube. Then, plug the tube with a cotton plug about 15mm from the bottom of the tube to force the whiteflies to stay on the leaf discs at the bottom of the tube.

[0245] (4) Feeding and observation:

[0246] The treated test insects were inverted and raised and observed under conditions of (25±1)℃, 65%±5% relative humidity, and a photoperiod of L:D=14:10h.

[0247] (5) Survey:

[0248] Forty-eight hours after treatment, the number of live worms in each tube was checked and recorded. Worms that did not move or could not move normally were considered dead. Based on the survey data, the corrected mortality rate for each treatment was calculated. The formula for calculating the experimental data is as described above.

[0249] The test results are shown in Table 4.

[0250] Table 4. Combined toxicity of bis(triflufenoxam) and flonicamid against whiteflies.

[0251]

[0252] As shown in the table above, when the mass ratio of bis(triflufenican) to flonicamid is 1:25 to 10:1, the co-toxicity coefficient is greater than 120, showing a synergistic effect; when the mass ratio of bis(triflufenican) to flonicamid is 2:15 to 2:3, the co-toxicity coefficient is greater than 150, showing a significant synergistic effect.

[0253] Indoor test 4: Combined toxicity of tebufenozide and acetamiprid against whiteflies

[0254] Experimental method: Agar moisturizing leaf immersion method.

[0255] The test target was the adult greenhouse whitefly (Trialeurodea vaporirum (Westwood)). The insect source was a population that had been continuously bred and reproduced indoors for multiple generations at the group's R&D center.

[0256] Test agents: 94.7% bis(triflufenoxam) technical grade and 98% acetamiprid technical grade, both provided by the group's R&D center.

[0257] Experimental steps:

[0258] (1) Preparation of liquid agar:

[0259] Place agar powder in an Erlenmeyer flask, add water, and place in a microwave oven. Heat until the agar is completely dissolved. After slightly cooling, use a pipette to add 2 mL of liquid agar to the bottom of a flat-bottomed glass tube. Allow the liquid agar to cool and solidify, and for the vapor on the tube wall to evaporate completely, before use. During the cooling process, avoid agar adhering to the tube wall and prevent air bubbles from forming during solidification.

[0260] (2) Drug preparation: Prepare single-dose mother liquor separately, and design 5 sets of ratios according to the purpose of mixing and drug activity. Each single agent and each set of mixed agents are prepared into 5 series of mass concentrations according to the equal ratio method.

[0261] (3) Chemical treatment:

[0262] Fresh, flat cucumber leaves were punched into leaf discs. The leaf discs were immersed in the test solution for 10 seconds, then removed and dried. Using tweezers, the leaf discs were laid face down in a flat-bottomed glass tube containing agar, ensuring tight contact between the leaf disc, agar, and the tube wall without gaps. Each treatment was repeated four times, with a control group containing no reagent.

[0263] (3) Inoculation: Place the glass tube with the leaf discs laid out on the cucumber leaves where whiteflies are being cultured, tilt it, and gently tap the leaves to allow the whiteflies to enter the glass tube. Inoculate 20 whiteflies into each tube, turn the tube upside down and wait for the whiteflies to fly into the leaf discs at the bottom of the tube. Then, plug the tube with a cotton plug about 15mm from the bottom of the tube to force the whiteflies to stay on the leaf discs at the bottom of the tube.

[0264] (4) Feeding and observation:

[0265] The treated test insects were inverted and raised and observed under conditions of (25±1)℃, 65%±5% relative humidity, and a photoperiod of L:D=14:10h.

[0266] (5) Survey:

[0267] Forty-eight hours after treatment, the number of live worms in each tube was checked and recorded. Worms that did not move or could not move normally were considered dead. Based on the survey data, the corrected mortality rate for each treatment was calculated. The formula for calculating the experimental data is as described above.

[0268] The test results are shown in Table 5.

[0269] Table 5. Combined toxicity of tebufenozide and acetamiprid against whiteflies.

[0270]

[0271] As shown in the table above, when the mass ratio of bispyribac-to-acetamiprid is 1:10 to 7:1, the co-toxicity coefficient is greater than 120, showing a synergistic effect; when the mass ratio of bispyribac-to-acetamiprid is 1:7 to 5:1, the co-toxicity coefficient is greater than 150, showing a significant synergistic effect.

[0272] Field efficacy examples

[0273] Field trial 1: Field control efficacy of a mixture of trifluralin and spinosad against armyworms.

[0274] Experimental crop: maize;

[0275] Test target: armyworm;

[0276] Experiment location: Cornfield in Pingdu, Qingdao;

[0277] Test date: June 10, 2020;

[0278] Experimental environment: The corn was damaged to a uniform degree, and the cultivation conditions in all experimental plots were uniform, with the same level of fertilizer and water management.

[0279] Test reagents: 30% bis(triflufenoxam)·spamicide water-dispersible granules (1:2), 20% bis(triflufenoxam)·spamicide water-dispersible granules (1:3), 28% bis(triflufenoxam)·spamicide suspension (2:5), 42% bis(triflufenoxam)·spamicide water-dispersible granules (4:3), 10% bis(triflufenoxam) suspension, 25 g / L spinosad suspension. All reagents were provided by the Group's R&D Center.

[0280] Experimental method: Conducted at the initial stage of pest occurrence, with one application of pesticide.

[0281] Cell size and duplication: 20 square meters per cell, 4 replicates per treatment.

[0282] Survey method: Five sampling points were taken in each community, with each point measuring 1 meter. 2 Before applying the pesticide, the initial population of armyworms was investigated. The number of surviving armyworms was investigated 3 and 7 days after application. The control efficacy of each treatment against armyworms was calculated based on the investigation results.

[0283] Calculation formulas and data analysis:

[0284]

[0285]

[0286] The calculation result is rounded to two decimal places.

[0287] The test results are shown in Table 6.

[0288] Table 6. Field control efficacy of a mixture of tebufenozide and spinosad against armyworms.

[0289]

[0290]

[0291] Table 6 shows that the combination of tebufenozide and spinosad exhibited good control effects against armyworms. Among them, 7 days after application, the 28% tebufenozide·spinosad suspension (2:5) showed the best control effect against armyworms, with a control efficacy of 90.85%.

[0292] Field trial 2: Field control efficacy of a mixture of trifluralin and spinosad against the rice stem borer.

[0293] Experimental crop: Rice;

[0294] Experimental target: Rice stem borer;

[0295] Experimental location: Rice paddies in Jimo, Qingdao;

[0296] Test date: June 10, 2020;

[0297] Experimental environment: The rice plants were uniformly damaged, and all experimental plots were cultivated under the same conditions, with the same level of fertilizer and water management.

[0298] Test reagents: 30% bis(triflufenoxam)·spamicide water-dispersible granules (1:2), 20% bis(triflufenoxam)·spamicide water-dispersible granules (1:3), 28% bis(triflufenoxam)·spamicide suspension (2:5), 10% bis(triflufenoxam) suspension, 25 g / L spinosad suspension. All reagents were provided by the Group's R&D Center.

[0299] Experimental method: Conducted at the initial stage of pest occurrence, with one application of pesticide.

[0300] Cell area and duplication: 20 square meters per cell, 4 duplications per treatment.

[0301] Survey method: When the damage in the blank control area was obvious (10 days after the pesticide was applied), parallel skip sampling was used. 45 rice clumps were investigated in each plot, and the dead heart rate and mortality rate were counted.

[0302] Calculation formulas and data analysis:

[0303]

[0304]

[0305] CK—Heart failure rate after drug administration in the blank control area;

[0306] PT—Post-treatment heart rate in the treated area.

[0307] The calculation result is rounded to two decimal places.

[0308] The test results are shown in Table 7.

[0309] Table 7. Field control efficacy of the combination of tebufenozide and spinosad against rice stem borer.

[0310]

[0311] Table 7 shows that the combination of tebufenozide and spinosad exhibited good control effects against the rice stem borer. Ten days after application, the control efficacy of 30% tebufenozide·spinosad water-dispersible granules (1:2), 20% tebufenozide·spinosad water-dispersible granules (1:3), and 28% tebufenozide·spinosad suspension concentrate (2:5) against the rice stem borer was all above 83%.

[0312] Field trial 3: Field control efficacy of a mixture of bispyribac-methyl, dinotefuran, flonicamid, and acetamiprid against greenhouse whiteflies. Crop: cucumber;

[0313] Experimental target: Greenhouse whitefly;

[0314] Experimental location: The experiment was conducted in a greenhouse at a vegetable base in Weifang City, Shandong Province; the cucumbers were planted on March 15, 2020, and the variety was Jinyou.

[0315] The experimental site had loamy soil with an organic matter content of 1.2%–1.3%. The planting density was 3500–3700 plants per mu (approximately 0.067 hectares), and the cucumbers grew uniformly and were well managed.

[0316] Experimental method: The experiment used foliar spraying, where the test agent was evenly sprayed onto both sides of the leaves. Each plot covered an area of ​​20m². 2 Each treatment was repeated 4 times.

[0317] Survey time and number of times: The experiment was conducted on May 12, 2020. The insect population was surveyed before the pesticide was applied, and the number of live insects was surveyed 3 days and 10 days after the pesticide was applied, for a total of 3 surveys.

[0318] Survey method: Five sampling points were taken in each plot. Five cucumber plants were fixed at each point and tagged with the upper two leaves. A total of 25 plants were surveyed in each plot. The initial population and remaining surviving whiteflies on the fixed points and plants were investigated.

[0319] Methods for calculating drug efficacy:

[0320]

[0321]

[0322] The calculation result is rounded to two decimal places.

[0323] The test results are shown in Table 8.

[0324] Table 8. Field control efficacy of mixtures of tebufenozide, dinotefuran, flonicamid, and acetamiprid against greenhouse whiteflies.

[0325]

[0326] As shown in Table 8, the field efficacy test results indicate that the control efficacy of bispyribac-triflufenoxam mixed with fipronil, flonicamid, and acetamiprid against greenhouse whiteflies is superior to that of the control single agent.

[0327] In summary, through indoor and field efficacy trials, the insecticidal composition containing bis(triflufenican) described in this invention exhibits good control effects against a variety of agricultural, forestry, and horticultural pests. Compared to single-agent formulations, the insecticidal composition of this invention reduces the amount of pesticide used, lowers pesticide residues on crops, and mitigates environmental pollution.

Claims

1. An insecticidal composition containing bis(triflufenoxuron), characterized in that, The insecticidal composition includes active ingredient A and active ingredient B, where active ingredient A is bis(triflufenoxuron) and active ingredient B is flonicamid, and the mass ratio of active ingredient A to active ingredient B is 2:15 to 7:

1.

2. The insecticidal composition according to claim 1, characterized in that, The content of active ingredient A and active ingredient B in the insecticidal composition is 1~80wt%.

3. The insecticidal composition according to claim 2, characterized in that, The content of active ingredient A and active ingredient B in the insecticidal composition is 2-60 wt%.

4. The insecticidal composition according to claim 1, characterized in that, In addition to the active ingredient, the insecticidal composition also includes an adjuvant, which is selected from one or more of the following: wetting agent, dispersant, emulsifier, thickener, disintegrant, antifreeze, defoamer, solvent, stabilizer, penetrant and carrier.

5. The insecticidal composition according to claim 4, characterized in that, The insecticidal composition can be prepared into any agriculturally acceptable formulation.

6. The insecticidal composition according to claim 5, characterized in that, The formulation is selected from any one of suspension concentrates, emulsifiable concentrates, water-dispersible granules, and dispersible oil suspensions.

7. The use of the insecticidal composition according to any one of claims 1-6 in the control of whiteflies.

8. The application according to claim 7, characterized in that, The insecticidal composition is applied in an effective dose to the pests that need to be controlled or their growth medium.

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