A composition containing a bisamide insecticide and its use
By combining compound I with diamide insecticides in specific ratios, various formulations can be formed, solving the problems of insecticide resistance and environmental pollution, and achieving improved insect control efficacy and reduced costs.
Patent Information
- Application Number
- CN202210247899.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-03-14
- Publication Date
- 2026-02-27
- Estimated Expiration
- 2042-03-14
AI Technical Summary
In the existing technology, the problem of pest resistance to Compound I and diamide insecticides has not been effectively solved, and the use of single compounds leads to reduced control efficacy, increased pesticide usage, and serious environmental pollution.
Compound I is compounded with various diamide insecticides (such as chlorantraniliprole and flubendiamide) in specific proportions to form a variety of formulations, including wettable powders, water-dispersible granules, and suspensions, achieving synergistic effects through different mechanisms of action.
It improves the effectiveness of pest control, broadens the spectrum of insecticides, delays the development of resistance, reduces the amount of pesticides applied and the cost of use, and reduces the number of applications.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the technical field of pesticide combination, and specifically relates to a composition containing a biologically effective amount of compound I and a biamide insecticide, and a method thereof for preventing and treating pests in agronomic and non-agronomic environments. BACKGROUND
[0002] In recent years, the occurrence of various crop pests has shown a trend of increasing year by year, and the occurrence area has increased year by year, which has brought great harm to crops, thus leading to problems such as crop yield reduction and agricultural production cost increase. In order to improve the control effect on pests, farmers increase the amount of pesticide or randomly mix pesticides, which is unscientific use of pesticides. This not only does not achieve the effect of increasing efficiency, but also leads to problems such as waste of pesticides, excessive pesticide residues, pollution of the environment, and resistance of pests to pesticides. Therefore, it is urgent to develop a synergistic composition for pests, which can achieve the effects of expanding the range of control objects, reducing the amount of pesticide, and delaying the generation of resistance.
[0003] In the actual process of agricultural production, long-term continuous and single use of the same pesticide will quickly lead to pesticide resistance of pests, resulting in reduced control effect, increased pesticide use, and aggravated damage to pesticide residues in agricultural products and the ecological environment. Through combination with insecticides of completely different action mechanisms, it is an effective way to delay the generation of pesticide resistance of pests, expand the insecticidal spectrum, prolong the service life, and reduce the amount of pesticide used. However, how to combine the drugs so as to produce synergistic rather than antagonistic effect between the drugs is a big difficulty.
[0004] Patent document CN 111909143 A discloses compound I, which has broad-spectrum insecticidal activity, especially good control effect on pests such as Lepidoptera, Hemiptera, Coleoptera, Thysanoptera, Diptera, and mites. However, how to combine it with other drugs to achieve the purpose of synergism is not disclosed.
[0005] The structural formula of compound I is as follows,
[0006] .
[0007] The diamide insecticides are the hotspot in the field of insecticide research in recent years, mainly acting on the ryanodine receptor of insects, and having the following characteristics: (1) novel mechanism of action, high efficiency, and no cross-resistance with traditional pesticides: the diamide insecticides have very outstanding effects on Lepidoptera pests in the field, and have better effects in the egg stage and low-age larval stage, long persistence period, and significant leaf retention effect; (2) safety to non-target organisms and good environmental compatibility: the diamide insecticide products are highly safe to bees, fish, natural enemy organisms, humans and animals, and birds, and have certain risk to crustaceans; (3) effects on both adults and larvae: the effects on larvae are mainly through stomach toxicity, and the effects on adults are mainly through contact toxicity. The diamide insecticides have very high activity on low-age larvae, high activity on high-age larvae, and moderate activity on adults, and have very high ovicidal activity.
[0008] However, the two compounds still have the problems of resistance and insecticidal activity to be improved. SUMMARY
[0009] In order to improve the deficiencies of the prior art, the present application provides a composition comprising compound I and a diamide insecticide selected from at least one of chlorantraniliprole, flubendiamide, cyantraniliprole, broflanilide, tetrachloraniliprole, cycloxaprid, tetraniliprole, flubendiamide, flupyradifurone, clofentezine, and hexythiazox.
[0010] The structural formula of compound I is as follows,
[0011] .
[0012] According to an embodiment of the present application, the compound I is prepared by the method of Example 1 in the patent document CN 111909143 A, which is incorporated herein by reference in its entirety.
[0013] According to an embodiment of the present application, the mass ratio of the compound I and the diamide insecticide is 80-1:1-80.
[0014] According to an embodiment of the present application, the mass ratio of the compound I and the diamide insecticide is 50-1:1-50, for example, 50:1, 40:1, 30:1, 20:1, 10:1, 5:1, 4:1, 3:1, 2:1, 1:1, 1:2, 1:3, 1:4, 1:5, 1:10, 1:20, 1:30, 1:40, or 1:50.
[0015] According to a preferred embodiment of the present application, the mass ratio of the compound I and the diamide insecticide is 10-1:1-10.
[0016] According to the embodiment of the present application, the sum of the mass of the compound I and the biamide insecticide in the composition is 1-80%, preferably 2-70%, or 5-65%; 10-60%, for example 1%, 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45% or 50%, based on the total weight of the composition.
[0017] According to the embodiment of the present application, the composition can be prepared into a liquid preparation or a solid preparation.
[0018] According to the embodiment of the present application, the content of the effective active ingredient in the preparation varies according to different preparation types, generally, the liquid preparation contains 1-60% of the effective active ingredient by weight, preferably 5-50%; the solid preparation contains 5-80% of the effective active ingredient by weight, preferably 10-70%.
[0019] According to the embodiment of the present application, the composition further comprises at least one of deionized water, organic solvent, emulsifier, dispersant, wetting agent, thickening agent, antifoaming agent, stabilizer, binder, disintegrant, anti-freezing agent, anti-caking agent, suspending agent, film-forming agent, preservative, colorant, high molecular capsule wall material, pH regulator or filler, etc.
[0020] According to the embodiment of the present application, the composition can be diluted by the user before use or used directly. The preparation thereof can be prepared by the processing method known to those skilled in the art, i.e. mixing the effective active ingredient with one or more of deionized water, organic solvent, emulsifier, dispersant, wetting agent, thickening agent, antifoaming agent, stabilizer, binder, disintegrant, anti-freezing agent, anti-caking agent, suspending agent, film-forming agent, preservative, colorant, high molecular capsule wall material, pH regulator or filler, etc. to obtain the composition.
[0021] According to the embodiment of the present application, the composition can be prepared into various dosage forms, preferably, the dosage forms include wettable powder, water dispersible granule, suspension concentrate, emulsion, suspension seed coating, microcapsule suspension concentrate, microcapsule suspension-suspension concentrate, emulsifiable concentrate, microemulsion, dispersible liquid, granule.
[0022] According to the embodiment of the present application, when the composition is prepared into wettable powder, it comprises the following components and contents: compound I 1-80%, biamide insecticide 1-80%, dispersant 0-10%, wetting agent 0-8%, and the balance is filler.
[0023] Preferably, the compound I in the composition is 2-70%, 5-65%, 10-60%, 15-50%, etc.
[0024] The diamide insecticide is 2-70%, 5-65%, 10-60%, 15-50%, etc.
[0025] The dispersing agent is 1-8%, 2-7%, 3-6%, or 4-5%;
[0026] The wetting agent is 1-8%, 2-7%, 3-6%, or 4-5%.
[0027] According to an embodiment of the present application, the composition, when made into a water dispersible granule, comprises the following components and contents: Compound I 1-80%, diamide insecticide 1-80%, dispersing agent 0-10%, wetting agent 0-16%, disintegrating agent 0-20%, and the balance is a filler.
[0028] Preferably, Compound I in the composition is 2-70%, 5-65%, 10-60%, 15-50%, etc.
[0029] The diamide insecticide is 2-70%, 5-65%, 10-60%, 15-50%, etc.
[0030] The dispersing agent is 1-8%, 2-7%, 3-6%, or 4-5%;
[0031] The wetting agent is 1-8%, 2-7%, 3-6%, or 4-5%.
[0032] The disintegrating agent is 1-18%, 2-16%, 3-15%, 4-12%, 5-10%, or 6-8%.
[0033] According to an embodiment of the present application, the composition, when made into a suspension concentrate, comprises the following components and contents: Compound I 1-50%, diamide insecticide 1-50%, dispersing agent 0-5%, wetting agent 0-8%, thickening agent 0-0.3%, anti-freezing agent 0-5%, and the balance is deionized water.
[0034] Preferably, Compound I in the composition is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.
[0035] The diamide insecticide is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.
[0036] The dispersing agent is 1-4% or 2-3%.
[0037] The wetting agent is 1-8%, 2-7%, 3-6%, or 4-5%.
[0038] The thickening agent is 0.1-0.25%.
[0039] Antifreeze 1-4% or 2-3%.
[0040] According to an embodiment of the present application, the composition when made into a water emulsion comprises the following components and contents: Compound I 1-50%, a diamide insecticide 1-50%, an organic solvent 0-95%, an emulsifier 0-10%, an antifreeze 0-5%, an antifoaming agent 0-0.2%, a thickening agent 0-0.5%, and the balance being deionized water.
[0041] Preferably, Compound I in the composition is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.
[0042] The diamide insecticide is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.
[0043] The organic solvent is 1-90%, 2-80%, 5-70%, 10-60%, 15-50%, 20-50%, 30-40%, etc.
[0044] The emulsifier is 1-8%, 2-7%, 3-6%, or 4-5%.
[0045] The antifreeze is 1-4% or 2-3%.
[0046] The antifoaming agent is 0.05-0.1%, or
[0047] The thickening agent is 0.1-0.4%, 0.2-0.3%.
[0048] According to an embodiment of the present application, the composition when made into a water emulsion comprises the following components and contents: Compound I 1-50%, a diamide insecticide 1-50%, an organic solvent 0-95%, an emulsifier 0-10%, an antifreeze 0-5%, an antifoaming agent 0-0.2%, a thickening agent 0-0.5%, and the balance being deionized water.
[0049] Preferably, Compound I in the composition is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.
[0050] The diamide insecticide is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.
[0051] The dispersing agent is 2-10%, 3-8%, 4-7%, or 5-6%;
[0052] The wetting agent is 1-8%, 2-7%, 3-6%, or 4-5%;
[0053] The anti-freezing agent is 1-8%, 2-7%, 3-6%, or 4-5%;
[0054] The anti-caking agent is 0.5-9%, 1-8%, 2-7%, 3-6%, or 4-5%;
[0055] The suspending agent is 0.2-4%, 0.5-3.5%, 1-3%, 1.5-2.5%, or 1.8-2%;
[0056] The film-forming agent is 2-9%, 3-8%, 4-7%, or 5-6%;
[0057] The preservative is 0.2-4%, 0.5-3.5%, 1-3%, 1.5-2.5%, or 1.8-2%;
[0058] The coloring agent is 2-25%, 3-20%, 5-15%, 8-12%, or 9-10%;
[0059] The pH adjusting agent is 0.1-5%, 0.2-4%, 0.5-3.5%, 1-3%, 1.5-2.5%, or 1.8-2%;
[0060] The thickening agent is 0.5-7, 1-6%, 2-5%, or 3-4%.
[0061] According to an embodiment of the present application, when the composition is made into a microcapsule suspension agent, it comprises the following components and contents: Compound I 1-50%, a bisamide insecticide 1-50%, a high molecular capsule wall material 1-30%, a dispersing agent 2-10%, an organic solvent 1-50%, an emulsifying agent 1-7%, a pH adjusting agent 0.1-5%, an antifoaming agent 0.01-2%, a thickening agent 0.1-8%, an anti-freezing agent 0.1-8%, and the balance is deionized water.
[0062] Preferably, Compound I in the composition is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.
[0063] The bisamide insecticide is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.
[0064] The high molecular capsule wall material is 2-25%, 5-20%, 6-18%, or 10-15%, etc.
[0065] Dispersant is 3% to 8%, 4% to 7%, or 5% to 6%;
[0066] Organic solvent is 2% to 45%, 5% to 40%, 10% to 35%, 15% to 30%; or 20% to 25%, etc.
[0067] Emulsifier is 2% to 6% or 4% to 5%;
[0068] pH regulator is 0.2% to 4%, 0.5% to 3.5%, 1% to 3%, 1.5% to 2.5%, or 1.8% to 2%;
[0069] Defoaming agent is 0.05% to 1.8%, 0.1% to 1.5%, 0.5% to 1.3%, 0.8% to 1.0%;
[0070] Thickening agent is 0.2% to 7, 0.5% to 6%, 1% to 5%, 1.5% to 4%, or 2% to 3%;
[0071] Anti-freezing agent is 0.5% to 7%, 1% to 6%, 2% to 5%, or 3% to 4%.
[0072] According to the embodiment of the present application, when the composition is made into a microcapsule suspension-suspension agent, it comprises the following components and contents: Compound I 1% to 50%, bisamide insecticide 1% to 50%, high molecular capsule wall material 1% to 12%, dispersant 1% to 12%, wetting agent 1% to 8%, organic solvent 1% to 50%, emulsifier 1% to 8%, defoaming agent 0.01% to 2%, thickening agent 0.1% to 8%, pH regulator 0.1% to 5%, anti-freezing agent 0.1% to 8%, and the balance is deionized water.
[0073] According to the embodiment of the present application, when the composition is made into an emulsion, it comprises the following components and contents: Compound I 1% to 50%, bisamide insecticide 1% to 50%, emulsifier 0% to 10%, anti-freezing agent 0% to 5%, stabilizer 0% to 0.5%, and the balance is organic solvent.
[0074] Alternatively, Compound I 1% to 50%, bisamide insecticide 1% to 50%, emulsifier 0% to 12%, stabilizer 0% to 0.5%, and the balance is organic solvent.
[0075] According to the embodiment of the present application, when the composition is made into a microemulsion, it comprises the following components and contents: Compound I 1% to 50%, bisamide insecticide 1% to 50%, organic solvent 1% to 50%, emulsifier 1% to 30%, anti-freezing agent 1% to 10%, stabilizer 0.1% to 5%, and the balance is deionized water.
[0076] According to the embodiment of the present application, the composition, when made into a dispersible liquid, comprises the following components and contents: Compound I 1% to 50%, a bisamide insecticide 1% to 50%, an emulsifier 1 to 30%, an anti-freezing agent 1% to 10%, a stabilizer 0.1% to 5%, and the balance being an organic solvent.
[0077] According to the embodiment of the present application, the composition, when made into a granule, comprises the following components and contents: Compound I 0.1% to 10%, a bisamide insecticide 0.1% to 10%, a dispersant 0% to 5%, a wetting agent 0% to 5%, a binder 0% to 3%, and the balance being a filler.
[0078] According to the embodiment of the present application, the emulsifier can be at least one selected from the group consisting of sodium lignosulfonate, Farmol, phenyl phenol polyoxyethylene ether phosphate, tristyryl phenol polyoxyethylene ether phosphate triethanolamine salt, benzyl dimethyl phenol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether, sorbitan oleate (Span-80), fatty alcohol polyoxyethylene ether, sodium alkyl naphthalene sulfonate, isooctanol succinate sodium sulfonate, nonyl phenol polyoxyethylene ether phosphate, and castor oil polyoxyethylene ether phosphate.
[0079] According to the embodiment of the present application, the dispersant can be at least one selected from the group consisting of glycerol fatty acid polyoxyethylene ether, polyoxyethylene alkyl aryl ether, sodium lignosulfonate, naphthalene sulfonate formaldehyde condensate, fatty alcohol polyoxyethylene ether sulfate, naphthalene sulfonate formaldehyde condensate, naphthalene sulfonate formaldehyde condensate sodium salt, nonyl phenol polyoxyethylene ether, polyoxyethylene lanolin alcohol, alkyl phenol polyoxyethylene ether formaldehyde condensate, fatty alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene ether phosphate, polyoxyethylene sorbitan fatty acid ester, and phosphate ester.
[0080] According to the embodiment of the present application, the wetting agent can be at least one selected from the group consisting of trisiloxane polyoxyethylene ether, sodium N-lauroyl glutamate, sodium dodecyl sulfate, sodium lauroyl sarcosinate, sodium methyl naphthalene sulfonate formaldehyde condensate, castor oil polyoxyethylene ether, tristyryl phenol polyoxyethylene ether, sodium dodecylbenzenesulfonate, sodium alkyl naphthalene sulfonate, isooctanol succinate sodium sulfonate, polyoxyethylene alkyl aryl ether, fatty alcohol polyether glycerol fatty acid polyoxyethylene ether, and fatty alcohol polyoxyethylene ether.
[0081] According to the embodiment of the present application, the binder can be at least one selected from the group consisting of xanthan gum, starch, urea-formaldehyde resin, gelatin, gum arabic, carboxymethyl cellulose, carboxyethyl cellulose, and polyvinyl alcohol.
[0082] According to the embodiment of the present application, the disintegrant can be at least one selected from the group consisting of sodium bicarbonate, ammonium sulfate, sodium sulfate, calcium sulfate, and magnesium chloride.
[0083] According to an embodiment of the present application, the thickening agent can be selected from at least one of magnesium aluminum silicate, polyvinyl acetate, xanthan gum, gelatin, gum arabic, and polyvinyl alcohol.
[0084] According to an embodiment of the present application, the antifoaming agent can be selected from at least one of silicone oil, n-octanol, silicone, butyl phosphate, isobutyl phosphate, and the like.
[0085] According to an embodiment of the present application, the antifreezing agent can be selected from at least one of propylene glycol, ethylene glycol, glycerol, and the like.
[0086] According to an embodiment of the present application, the stabilizer can be selected from at least one of triethanolamine, epichlorohydrin, butyl glycidyl ether, triphenyl phosphite, N-soybean oil-based triethylene diamine, and dialkyl succinate acid sulfonate.
[0087] According to an embodiment of the present application, the filler includes a solid filler and a liquid filler, wherein the solid filler can be selected from at least one of kaolin, attapulgite, diatomite, white carbon, bentonite, montmorillonite, calcium carbonate, and talc powder. The liquid filler can be selected from at least one of soybean oil, castor oil, and mineral oil.
[0088] According to an embodiment of the present application, the organic solvent can be selected from at least one of ethyl acetate, acetone, isopropyl alcohol, 2,2,2-trifluoroethanol, propylene carbonate, benzene, toluene, xylene, dimethylformamide, dimethyl sulfoxide, dichloromethane, cyclohexane, cyclohexanone, N-methyl pyrrolidone, and solvent oil (e.g., 150# solvent oil).
[0089] The present application also provides a use of the above composition for controlling pests in agriculture and non-agriculture.
[0090] According to an embodiment of the present application, the pests are selected from Lepidoptera, Hemiptera, Coleoptera, Thysanoptera, Diptera, mites, and the like.
[0091] As an embodiment, the pests are selected from the group consisting of corn earworm, cabbage looper, and diamondback moth.
[0092] The present application also provides a method for controlling pests in agriculture or non-agriculture, which includes applying the above composition to plants where the pests exist.
[0093] The composition of the present application can be provided in the form of finished preparation, or in the form of single agent, which is mixed directly before use, then mixed with water to the required concentration, and can be applied to the crop in any way, such as spraying, irrigation at the root of the plant, smearing, etc. In specific application, it can also be mixed with other agents, such as growth regulator, soil conditioner, herbicide, nematicide, etc.
[0094] The present application also provides a composition for controlling invertebrate pests, which comprises a biologically effective amount of compound I, a diamide insecticide and at least one other component selected from the group consisting of a surfactant, a solid diluent and a liquid diluent, said composition optionally further containing an effective amount of at least one other biologically active compound or active agent, said diamide insecticide being selected from at least one of chlorantraniliprole, flubendiamide, cyantraniliprole, broflanilide, tetraniliprole, cyenopyrafen, tetrahydropyran-4-ylmethyl N-[(6-chloro-3-fluoropyridin-2-yl)methyl]-N-cyanocarbamate, flupylthannilide, sulfoxaflor, chlorfenapyr.
[0095] The present application also provides a method for controlling invertebrate pests, which comprises contacting said invertebrate pests or their environment with a biologically effective amount of the composition of the present application as described above.
[0096] The present application also provides a spray composition, which comprises the composition of the present application as described above and a propellant.
[0097] The present application also provides a bait composition, which comprises the composition of the present application as described above; one or more food materials; optionally an attractant; and optionally a wetting agent.
[0098] Advantages of the present application:
[0099] The synergistic composition of the present application has the following advantages:
[0100] 1) synergistic effect, which can improve the control effect of pests; 2) expand the insecticidal spectrum, mixed occurrence of field pests, stronger effect on pests; 3) different action mechanisms of the two effective components, mixed use can delay the development of pest resistance; 4) reduce the amount of application, reduce the use frequency, and reduce the use cost. DETAILED DESCRIPTION
[0101] The present application will be further described in detail below with reference to specific examples. It should be understood that the following examples are only illustrative and explanatory of the present application, and should not be interpreted as limiting the scope of protection of the present application. Any technology realized based on the above description of the present application is covered within the scope intended to be protected by the present application.
[0102] The experimental methods used in the following examples are conventional methods unless otherwise specified; the reagents, materials, etc. used in the following examples are commercially available unless otherwise specified.
[0103] The insecticidal effect of the composition is tested by indoor bioassay and field test. It should be noted that any modification, equivalent replacement and improvement within the spirit and principles of the present application shall be included in the protection scope of the present application.
[0104] The compound I used in the following examples is prepared by the method of Example 1 in the patent document CN 111909143 A.
[0105] The % of each component in the preparation of the following preparation examples and examples refers to the mass percentage if not specifically stated.
[0106] I. Preparation Example of Preparation:
[0107] Preparation Example 1: Wettable powder
[0108]
[0109]
[0110] The above materials are coarsely pulverized in proportion and then mixed uniformly in a mixer, and then the finished product is obtained after air flow pulverization.
[0111] Preparation Example 2: Water dispersible granule
[0112]
[0113] The effective active ingredient and various adjuvants are mixed uniformly in proportion to the formula, and then powder is obtained after air flow pulverization, and then a certain amount of water is mixed and extruded to granulate, and then the finished product is obtained after drying and screening.
[0114] Preparation Example 3: Suspension concentrate
[0115]
[0116] The effective active ingredient and various adjuvants are mixed uniformly in proportion to the formula, and then the finished product is obtained after high-speed shearing and sand milling.
[0117] Preparation Example 4: Emulsifiable concentrate
[0118]
[0119] The above raw materials are mixed in proportion to dissolve into a uniform oil phase; after passing the inspection, metering and packaging are carried out to obtain the finished product.
[0120] Preparation Example 5: Emulsion in water
[0121]
[0122] The above raw materials are added into a batching kettle according to the formulation requirements, mixed uniformly by a high-speed shearing machine to prepare a water emulsion, and after inspection, the product is obtained by metering and packaging.
[0123] Preparation Example 6: emulsifiable concentrate
[0124]
[0125] The above raw materials are mixed in proportion to dissolve into a uniform oil phase; after inspection, the product is obtained by metering and packaging.
[0126] Preparation Example 7: granules
[0127]
[0128] The components are mixed in the formulation proportion, crushed, wetted with water, and then fully stirred, granulated by a screw extrusion granulator, dried, and sieved to obtain the finished product.
[0129] The bisamide insecticide in the above preparation example is selected from at least one of the following: chlorantraniliprole, flubendiamide, cyantraniliprole, halofenozide, tebufenozide, chromafenozide, tetraniliprole, tolfenpyrad, sulfoxaflor, flupyradifurone, sulfoxaflor.
[0130] II. Indoor toxicity determination example
[0131] (1) Test insect: Plutella xylostella, Mythimna separata Walker, Spodoptera exigua.
[0132] (2) Determination method:
[0133] Pest toxicity determination method
[0134] The pest toxicity determination uses Plutella xylostella, Mythimna separata Walker, and Spodoptera exigua as test materials, and uses a leaf dipping method to determine the toxicity of compound I, bisamide insecticides, and their mixed formulations.
[0135] Reference to the People's Republic of China, NY / T 1154.14-2008 "agricultural industry standards indoor biological test guidelines" insecticides Part 14: leaf dip method, first test agent (including compound I, diamide insecticides) with the appropriate solvent (solvent types such as acetone, methanol, N, N dimethylformamide and dimethyl sulfoxide, and according to its solubility of the sample to choose) prepared into 5 concentration gradient (according to the compound on different pests LC 50 values, set concentration gradient according to geometric or arithmetic progression), compound I, diamide insecticides mixed respectively according to its LC 50 value according to the mass proportion of a series of proportion, according to the different proportion of the final mass concentration (refers to the total mass of compound I, diamide insecticides).
[0136] The leaf disc or leaf segment is immersed in the test agent solution, 10 s (can be appropriately extended or shortened according to the characteristics of the agent) after taking out and drying in the culture dish containing 1% water agar or moisture filter paper, access to test insects, each repeat not less than 10 head. Each treatment not less than 4 times repeated, and set up without drug (containing all organic solvents and emulsifiers) as blank control.
[0137] According to Sun Yunpei method to calculate the two different proportion of the drug CTC (CTC value), the CTC of the mixture (CTC) ≥ 120 for synergistic effect, CTC ≤ 80 for antagonism; 80 < CTC < 120 for additive effect. The CTC of the mixture (CTC) is calculated according to formula (1), formula (2), formula (3):
[0138]
[0139] In the formula:
[0140] ATI - the measured toxicity index of the mixture;
[0141] S - the LC 50 of the standard insecticide, unit: milligrams per liter (mg / L);
[0142] M - the LC 50 of the mixture, unit: milligrams per liter (mg / L)
[0143] TTI = TI A × P A + TI B × P B (2)
[0144] In the formula:
[0145] TTI - the theoretical CTC of the mixture;
[0146] TI AToxicity index of A agent;
[0147] P A Percentage content of A agent in the mixture, in percentage (%);
[0148] TI B Toxicity index of B agent;
[0149] P B Percentage content of B agent in the mixture, in percentage (%).
[0150]
[0151] In the formula:
[0152] CTC - Co-toxicity coefficient;
[0153] ATI - Actual toxicity index of the mixture;
[0154] TTI - Theoretical toxicity index of the mixture.
[0155] After mixing of different varieties of pesticides, three types of action, namely additive action, synergistic action and antagonistic action, are usually exhibited, but the specific action cannot be predicted. The composition described in the present application takes compound I and a biamide insecticide as the effective active ingredients, and is illustrated by means of biological determination examples.
[0156] Laboratory activity determination test of cabbage moth with insecticides
[0157] In this test, leaf dipping method was used to conduct laboratory activity determination test of compound on cabbage moth, so as to determine the activity of the insecticidal composition of examples 1-4 on cabbage moth.
[0158] Example 1: In order to verify the effect of different proportions of compound I and chlorantraniliprole on cabbage moth, indoor toxicity determination of different proportions of compound I and chlorantraniliprole on cabbage moth was carried out, and the corresponding concentration was prepared according to the mass ratio in the table, and indoor insecticidal test was carried out, and the test results are as follows:
[0159] Table 1 Toxicity determination results of compound I and chlorantraniliprole single agent and their mixture on cabbage moth
[0160] Active ingredient Ratio Regression equation <![CDATA[LC 50 ]]> Co-toxicity factor Evaluation Compound I - y = 6.8787 + 2.1062x 0.1282 - - chlorantraniliprole - y = 6.1385 + 1.0609x 0.1386 - - Compound I: chlorantraniliprole 50:1 y = 5.9033 + 0.8952x 0.0863 148.77 Synergism Compound I: chlorantraniliprole 10:1 y = 6.2752 + 1.0639x 0.0469 275.22 Synergism Compound I: chlorantraniliprole 5:1 y = 6.6903 + 1.1801x 0.0608 213.53 Synergism Compound I: chlorantraniliprole 3:1 y = 6.7710 + 1.2620x 0.0540 241.95 Synergism Compound I: chlorantraniliprole 1:1 y = 6.4432 + 1.2430x 0.0407 327.27 Synergism Active ingredient 1:3 Ratio 0.0489 277.80 Regression equation Co-toxicity factor 1:5 Evaluation 0.0596 229.45 Compound I y = 6.8787 + 2.1062x 1:10 cyantraniliprole 0.0614 224.08 y = 6.1022 + 0.9468x Compound I: cyantraniliprole 1:50 y = 6.2445 + 1.1474x 0.0972 142.37 Synergism
[0161] From the results in table 1, it can be seen that the activity of different proportions of compound I and chlorantraniliprole mixed for cabbage moth has obvious synergistic effect.
[0162] Example 2: To verify the effect of different proportions of Compound I and chlorfenapyr on Plutella xylostella, indoor toxicity determination of different proportions of Compound I and chlorfenapyr on Plutella xylostella was carried out, and the corresponding concentration was prepared according to the mass ratio in the table, and indoor insecticidal test was carried out. The test results are as follows:
[0163] Table 2 Toxicity determination results of Compound I and chlorfenapyr single agent and its mixture on Plutella xylostella
[0164] Compound I: cyantraniliprole y = 6.3647 + 1.0284x Synergism LC 50 ]] Compound I: cyantraniliprole y = 6.5000 + 1.1012x Synergism - Compound I: cyantraniliprole 0.1282 - - y = 6.4909 + 0.9961x - Synergism 0.0845 - - Compound I: cyantraniliprole 50:1 y = 6.4229 + 1.1279x 0.0979 129.64 Synergism Active ingredient 10:1 Ratio 0.0633 193.43 Regression equation Co-toxicity factor 1:1 Evaluation 0.0369 276.05 Compound I y = 5.7178 + 2.0073x 1:10 tetraniliprole 0.0395 220.77 y = 5.3619 + 0.8025x Compound I: tetraniliprole 1:50 y = 5.5053 + 0.9662x 0.0690 123.29 Synergism
[0165] From the results in Table 2, it can be seen that the activity of different proportions of Compound I and chlorfenapyr mixed with different proportions of Compound I and chlorfenapyr on Plutella xylostella has obvious synergistic effect.
[0166] Example 3: To verify the effect of different proportions of Compound I and cyantraniliprole on Plutella xylostella, indoor toxicity determination of different proportions of Compound I and cyantraniliprole on Plutella xylostella was carried out, and the corresponding concentration was prepared according to the mass ratio in the table, and indoor insecticidal test was carried out. The test results are as follows:
[0167] Table 3 Toxicity determination results of Compound I and cyantraniliprole single agent and its mixture on Plutella xylostella
[0168] Compound I: tetraniliprole y = 5.6563 + 0.9572x Synergism LC 50 ]]> Compound I: tetraniliprole y = 5.6737 + 1.0292x Synergism - Compound I: tetraniliprole 0.1282 - - y = 5.6864 + 1.0018x - Synergism 0.0685 - - Compound I: tetraniliprole 50:1 y = 5.8027 + 0.9132x 0.0823 153.15 Synergism Compound I: tetraniliprole 10:1 y = 5.7124 + 0.9182x 0.0471 252.20 Synergism Compound I: tetraniliprole 1:1 y = 5.7802 + 0.9570x 0.0434 205.74 Synergism Compound I: tetraniliprole 1:10 y = 6.0566 + 1.2068x 0.0319 224.23 Synergism 1:50 0.0548 126.15
[0169] From the results in Table 3, it can be seen that the activity of different proportions of Compound I and cyantraniliprole mixed with different proportions of Compound I and cyantraniliprole on Plutella xylostella has obvious synergistic effect.
[0170] Example 4: To verify the effect of different proportions of Compound I and flubendiamide on Plutella xylostella, indoor toxicity determination of different proportions of Compound I and flubendiamide on Plutella xylostella was carried out, and the corresponding concentration was prepared according to the mass ratio in the table, and indoor insecticidal test was carried out. The test results are as follows:
[0171] Table 4 Toxicity determination results of Compound I and flubendiamide single agent and its mixture on Plutella xylostella
[0172]
[0173]
[0174] From the results in Table 4, it can be seen that the activity of different proportions of Compound I and flubendiamide mixed with different proportions of Compound I and flubendiamide on Plutella xylostella has obvious synergistic effect.
[0175] Insecticide activity determination test of corn borer in laboratory
[0176] In this test, leaf dipping method was used to determine the activity of the insecticidal composition of Examples 5-7 on corn borer in laboratory.
[0177] Example 5: To verify the effect of different proportions of compound I and chlorantraniliprole on corn armyworm, indoor toxicity determination of different proportions of compound I and chlorantraniliprole on corn armyworm was carried out, and the corresponding concentration was prepared according to the mass ratio in the table, and indoor insecticidal test was carried out. The test results are as follows:
[0178] Table 5 Toxicity determination results of compound I and chlorantraniliprole single agent and their mixtures on corn armyworm
[0179] LC 50 ]]> - 0.4389 - - - 0.3540 - - 50:1 0.2999 145.66 10:1 0.2063 208.21 5:1 0.2215 190.53 3:1 0.2065 200.52 1:1 0.1321 296.67 1:3 0.1675 222.08 1:5 0.1530 239.08 1:10 0.1332 270.52 Compound I: tetraniliprole 1:50 y = 5.7362 + 1.0454x 0.1976 179.83 synergism
[0180] From the results in Table 5, the activity of different proportions of compound I and chlorantraniliprole mixed for corn armyworm has obvious synergistic effect.
[0181] Example 6: To verify the effect of different proportions of compound I and cyproflumetofen on corn armyworm, indoor toxicity determination of different proportions of compound I and cyproflumetofen on corn armyworm was carried out, and the corresponding concentration was prepared according to the mass ratio in the table, and indoor insecticidal test was carried out. The test results are as follows:
[0182] Table 6 Toxicity determination results of compound I and cyproflumetofen single agent and their mixtures on corn armyworm
[0183]
[0184]
[0185] From the results in Table 6, the activity of different proportions of compound I and cyproflumetofen mixed for corn armyworm has obvious synergistic effect.
[0186] Example 7: To verify the effect of different proportions of compound I and tetraniliprole on corn armyworm, indoor toxicity determination of different proportions of compound I and tetraniliprole on corn armyworm was carried out, and the corresponding concentration was prepared according to the mass ratio in the table, and indoor insecticidal test was carried out. The test results are as follows:
[0187] Table 7 Toxicity determination results of compound I and tetraniliprole single agent and their mixtures on corn armyworm
[0188] active ingredient ratio regression equation LC 50 ]] co-toxicity factor evaluation Compound I - y = 5.7178 + 2.0073x 0.4389 - - tetraniliprole - y = 5.3573 + 1.0980x 0.4727 - - Compound I: tetraniliprole 50:1 y = 5.6068 + 1.2195x 0.3180 138.21 synergism Compound I: tetraniliprole 10:1 y = 5.9459 + 1.3735x 0.2048 215.71 synergism Compound I: tetraniliprole 1:1 y = 5.9190 + 1.2893x 0.1937 234.99 synergism Compound I: tetraniliprole 1:10 y = 5.8547 + 1.3559x 0.2342 200.43 synergism Compound I: tetraniliprole 1:50 y = 5.6206 + 1.3757x 0.3539 133.37 synergism
[0189] From the results in Table 7, the activity of different proportions of compound I and tetraniliprole mixed for corn armyworm has obvious synergistic effect.
[0190] Laboratory activity determination test of beet armyworm
[0191] The indoor activity determination test of the compounds on the cabbage beet armyworm was carried out by the leaf dipping method to determine the activity of the insecticidal compositions of Examples 8-11 on the cabbage beet armyworm.
[0192] Example 8: To verify the effect of different proportions of compound I and flubendiamide on the cabbage beet armyworm, indoor toxicity determination of different proportions of compound I and flubendiamide on the cabbage beet armyworm was carried out, and the corresponding concentrations were prepared according to the mass ratio in the table, and indoor insecticidal test was carried out, and the test results were as follows:
[0193] Table 8 Toxicity determination results of compound I and flubendiamide single agent and their mixtures on the cabbage beet armyworm
[0194]
[0195]
[0196] It can be known from the results in Table 8 that the activity of different proportions of compound I and flubendiamide mixed for the cabbage beet armyworm has obvious synergistic effect.
[0197] Example 9: To verify the effect of different proportions of compound I and flubendiamide on the cabbage beet armyworm, indoor toxicity determination of different proportions of compound I and flubendiamide on the cabbage beet armyworm was carried out, and the corresponding concentrations were prepared according to the mass ratio in the table, and indoor insecticidal test was carried out, and the test results were as follows:
[0198] Table 9 Toxicity determination results of compound I and flubendiamide single agent and their mixtures on the cabbage beet armyworm
[0199] active ingredient ratio regression equation LC 50 ]] co-toxicity factor evaluation Compound I - y = 6.9486 + 1.7989x 0.0826 - - flubendiamide - y = 5.9346 + 0.9260x 0.0979 - - Compound I: flubendiamide 50:1 y = 6.0448 + 0.8462x 0.0583 142.12 synergism Compound I: flubendiamide 10:1 y = 6.5482 + 1.0692x 0.0356 235.37 synergism Compound I: flubendiamide 1:1 y = 6.2703 + 0.9357x 0.0439 204.10 synergism Compound I: flubendiamide 1:10 y = 6.7927 + 1.2407x 0.0359 268.19 synergism Compound I: flubendiamide 1:50 y = 6.0614 + 0.9285x 0.0719 135.67 synergism
[0200] It can be known from the results in Table 9 that the activity of different proportions of compound I and flubendiamide mixed for the cabbage beet armyworm has obvious synergistic effect.
[0201] Example 10: To verify the effect of different proportions of compound I and flubendiamide on the cabbage beet armyworm, indoor toxicity determination of different proportions of compound I and flubendiamide on the cabbage beet armyworm was carried out, and the corresponding concentrations were prepared according to the mass ratio in the table, and indoor insecticidal test was carried out, and the test results were as follows:
[0202] Table 10 Toxicity determination results of compound I and flubendiamide single agent and their mixtures on the cabbage beet armyworm
[0203] active ingredient ratio regression equation LC 50 ]]> co-toxicity factor evaluation Compound I - y = 6.9486 + 1.7989x 0.0826 - - clothianidin - y = 4.5611 + 0.9048x 3.0551 - - Compound I: clothianidin 50:1 y = 6.3127 + 1.0484x 0.0560 150.37 synergism Compound I: clothianidin 10:1 y = 6.5371 + 1.1064x 0.0408 222.10 synergism Compound I: clothianidin 1:1 y = 6.2863 + 1.1327x 0.0732 219.74 synergism Compound I: clothianidin 1:10 y = 5.5475 + 0.9906x 0.2801 255.35 synergism Compound I: clothianidin 1:50 y = 4.9553 + 0.6608x 1.1684 153.30 synergism
[0204] It can be known from the results in Table 10 that the activity of different proportions of compound I and flubendiamide mixed for the cabbage beet armyworm has obvious synergistic effect.
[0205] Example 11: To verify the effect of different proportions of compound I and chlorantraniliprole on the cabbage beet armyworm, indoor toxicity determination of different proportions of compound I and chlorantraniliprole on the cabbage beet armyworm was carried out, and the corresponding concentration was prepared according to the mass ratio in the table, and indoor insecticidal test was carried out, and the test results were as follows:
[0206] Table 11 Toxicity determination results of compound I and chlorantraniliprole single agent and its mixture on cabbage beet armyworm
[0207] active ingredient ratio regression equation LC 50 ]] co-toxicity factor evaluation Compound I - y = 6.9486 + 1.7989x 0.0826 - - sulfoxaflor - y = 5.3701 + 1.4741x 0.5610 - - Compound I: sulfoxaflor 50:1 y = 6.4396 + 1.1239x 0.0524 160.31 synergism Compound I: sulfoxaflor 10:1 y = 6.3942 + 1.0424x 0.0460 194.66 synergism Compound I: sulfoxaflor 1:1 y = 6.3697 + 1.0919x 0.0557 258.52 synergism Compound I: sulfoxaflor 1:10 y = 5.7476 + 0.9513x 0.1637 224.50 synergism Compound I: sulfoxaflor 1:50 y = 5.3794 + 0.7610x 0.3173 158.77 synergism
[0208] From the results in Table 11, the activity of different proportions of compound I and chlorantraniliprole mixed for cabbage beet armyworm has obvious synergistic effect.
[0209] Three, field efficacy examples
[0210] In order to clarify the prevention and control effect of compound I and biamide insecticide single agent and mixture on cabbage moth, corn stalk borer and cabbage beet armyworm, multiple efficacy tests were carried out in different regions of China. The used preparations were processed according to preparation examples 1-7, and the preparation in table 12 was taken as an example (other test preparations refer to the same preparation example), and the specific preparation method was as follows:
[0211] Table 12 Preparation of compound I·bromofenprox double amide suspension concentrate with different proportions
[0212]
[0213] Cabbage moth, cabbage beet armyworm field efficacy test
[0214] Test method: According to the application method specified in “People's Republic of China national standard GB / T 17980.13-2000”. The first application was carried out when there were enough number of larvae (1-3 heads of three instar larvae per plant).
[0215] Investigation method: According to the investigation method specified in “People's Republic of China national standard GB / T 17980.13-2000”, count the number of live larvae of different instars on not less than 10 plants per plot, and investigate the whole plant. Investigate the number of live insects before application, and investigate the number of live insects 1-3 days, 7-14 days after treatment respectively. The control effect (control effect) calculation formula is:
[0216]
[0217]
[0218] Corn stalk borer field efficacy test
[0219] Test method: The application method was according to the "People's Republic of China National Standard GB / T 17980.80-2004". The application was carried out when the larvae were at the 2nd and 3rd instar.
[0220] Investigation method: According to the investigation method of "People's Republic of China National Standard GB / T 17980.80-2004", 5 points were sampled in each plot, and 1 m 2 was taken in each point to investigate the number of live insects on the crop. The insect population base was investigated before application, and each was investigated once at 1, 3, and 7 days after application. The control effect (control effect) calculation formula is:
[0221]
[0222]
[0223] Table 13 Field efficacy test of compound I and chlorantraniliprole against cabbage moth in cabbage
[0224]
[0225] Note: The same column data with different letters means that the difference is significant at the P <0.05 level by Duncan's new range difference test, and the same below.
[0226] In the above table, the 10% compound I · chlorantraniliprole suspension concentrate (1:4) of example 12 is prepared according to the preparation example 3, wherein 10% refers to the total mass percentage of active substances (compound I and chlorantraniliprole), and 1:4 refers to the mass ratio of the two active ingredients compound I and chlorantraniliprole.
[0227] The 10% compound I · chlorantraniliprole suspension concentrate (1:3) in example 13 is prepared according to the preparation example 3, wherein 10% refers to the total mass percentage of active substances (compound I and chlorantraniliprole), and 1:3 refers to the mass ratio of the two active ingredients compound I and chlorantraniliprole.
[0228] The 10% compound I suspension concentrate in comparative example 1 is also prepared according to the preparation example 3, wherein 10% refers to the mass percentage of active substance compound I.
[0229] The following other examples and comparative examples are also prepared in this way, which will not be described in detail here.
[0230] As can be seen from the test results in the table, when controlling cabbage moth, the 1-day, 3-day, and 7-day control effects of compound I and chlorantraniliprole complex are significantly higher than those of single agent at the same effective ingredient dosage (comparative examples 1 and 2 corresponding to examples 12-18). The 7-day control effect can still reach more than 94.36%, and the effective period is longer.
[0231] Table 14 Field efficacy test of compound I and chlorantraniliprole on beet armyworm
[0232]
[0233] From the results in the table, in the prevention of beet armyworm, compound I and chlorantraniliprole complex are significantly higher than single agent in 1 day, 3 days and 7 days control effect on beet armyworm under the same amount of active ingredient (comparative examples 3 and 4 corresponding to examples 19-25). Among them, the 7-day control effect can still reach more than 94.23%, and the effective period is longer.
[0234] Table 15 Field efficacy test of compound I and tetraniliprole on corn armyworm
[0235]
[0236]
[0237] From the results, in the prevention of corn armyworm, compound I and tetraniliprole complex are significantly higher than single agent in 1 day, 3 days and 7 days control effect on corn armyworm under the same amount of active ingredient (comparative examples 5 and 6 corresponding to examples 26-32). Among them, the 7-day control effect can still reach more than 93.60%, and the effective period is longer.
[0238] Table 16 Field efficacy test of compound I and tetraniliprole on cabbage moth
[0239]
[0240] From the results, in the prevention of cabbage moth, compound I and tetraniliprole complex are significantly higher than single agent in 1 day, 3 days and 7 days control effect on cabbage moth under the same amount of active ingredient (comparative examples 7 and 8 corresponding to examples 33-39). Among them, the 7-day control effect can still reach more than 93.26%, and the effective period is longer.
[0241] Table 17 Field efficacy test of compound I and flubendiamide on cabbage moth
[0242]
[0243] From the results of the determination in the table, in the prevention and treatment of diamondback moth, the 1-day, 3-day and 7-day control effects of the compound I and flubendiamide complex on diamondback moth are obviously higher than those of the single agent at the same active ingredient dosage (comparative examples 9 and 10 correspond to examples 40-46).
[0244] Table 18 Field efficacy test of compound I and flubendiamide complex on corn earworm
[0245]
[0246] From the results of the determination in the table, in the prevention and treatment of diamondback moth, the 1-day, 3-day and 7-day control effects of the compound I and flubendiamide complex on diamondback moth are obviously higher than those of the single agent at the same active ingredient dosage (comparative examples 9 and 10 correspond to examples 40-46).
[0247] The above describes the embodiments of the present application. However, the present application is not limited to the above-described embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims
1. A composition comprising compound I and a diamide insecticide, characterized in that, The diamide insecticide is selected from one of the following: chlorantraniliprole, broflanilide, tetrachlorantraniliprole, cyclopropamide, tetrazolium acetamiprid, thiofenoxam, and fluchlorfenapyr. The structure of compound I is shown below. I The mass ratio of compound I to the diamide insecticide is 50~1:1~50.
2. The composition according to claim 1, characterized in that, The mass ratio of compound I to the diamide insecticide is 50:1, 40:1, 30:1, 20:1, 10:1, 5:1, 4:1, 3:1, 2:1, 1:1, 1:2, 1:3, 1:4, 1:5, 1:10, 1:20, 1:30, 1:40 or 1:
50.
3. The composition according to claim 1 or 2, characterized in that, The composition further includes at least one of the following: deionized water, organic solvent, emulsifier, dispersant, wetting agent, thickener, defoamer, stabilizer, binder, disintegrant, antifreeze, anticaking agent, suspending agent, film-forming agent, preservative, colorant, polymeric capsule wall material, pH adjuster, or filler.
4. The composition according to claim 1, characterized in that, The composition is prepared into a pesticide formulation, which includes wettable powder, water-dispersible granules, suspension concentrate, water-in-oil emulsion, suspension seed coating agent, microcapsule suspension, microcapsule suspension-suspension agent, emulsifiable concentrate, microemulsion, dispersible liquid, or granules.
5. Use of the composition according to any one of claims 1-4 for the prevention and control of pests in agriculture or non-agriculture.
6. The use according to claim 5, characterized in that, The pests mentioned are selected from Lepidoptera, Hemiptera, Coleoptera, Thysanoptera, Diptera, and Mite pests.
7. A method for controlling pests in agricultural or non-agricultural fields, characterized in that, This includes applying the composition of any one of claims 1-4 to plants infested with pests.
8. A composition for controlling invertebrate pests, characterized in that, It contains a biologically effective amount of compound I, a diamide insecticide, and at least one other component selected from surfactants, solid diluents, and liquid diluents, wherein the diamide insecticide is selected from one of the following: chlorantraniliprole, broflanipromide, tetrachlorantraniliprole, cyclopropamide, tetrazolium acetamiprid, thiophanate-methyl, and fluchlorfenapyr. The mass ratio of compound I to the diamide insecticide is 50~1:1~50; The structure of compound I is shown below. I。 9. A method for controlling invertebrate pests, characterized in that, This includes contacting invertebrate pests or their environment with a biologically effective amount of the composition according to any one of claims 1-4.
10. A spray composition comprising the composition according to any one of claims 1-4 and a propellant.
11. A bait composition comprising the composition according to any one of claims 1-4 and one or more food materials.
Citation Information
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