A composition containing a nicotine-based insecticide and its use

Abstract

The present application relates to a composition containing a biologically effective amount of compound I and a nicotinic insecticide, and a method for controlling pests in agricultural and non-agricultural environments. The compound I has a synergistic effect with the nicotinic insecticide, which can improve the pest control effect, reduce the amount of application, reduce the use frequency, and reduce the use cost.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of pesticide combination, and specifically relates to a composition comprising a biologically effective amount of compound I and a neonicotinoid insecticide, and a method thereof for controlling 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, resulting in 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. This unscientific use of pesticides not only fails to achieve the effect of increasing efficiency, but also leads to problems such as waste of pesticides, excessive pesticide residues, pollution of the environment, and development of pesticide resistance by pests. 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 development of resistance.

[0003] In the actual process of agricultural production, long-term continuous use of the same pesticide will quickly lead to pesticide resistance of pests, resulting in reduced control effect and increased use of pesticides, which aggravates the damage to the ecological environment and the residues of agricultural products. By combining with insecticides of completely different mechanisms, the development of pesticide resistance by pests can be delayed, the insecticidal spectrum can be expanded, the service life can be prolonged, and the use of pesticides can be reduced. However, how to combine the drugs to produce synergistic rather than antagonistic effects is a major 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] Neonicotinoid insecticides can be divided into competitive modulators, allosteric modulators, and channel blockers of nicotinic acetylcholine receptors (nAChR). This type of insecticide has a unique mechanism of action and no cross-resistance with conventional insecticides. It not only has high efficiency, broad spectrum, and good root systemicity, contact toxicity, and stomach toxicity, but also has low toxicity to mammals, can effectively control pests such as Homoptera, Coleoptera, Diptera, and Lepidoptera, and has good activity against pests that have developed resistance to traditional insecticides. Neonicotinoid insecticides can be used for stem and leaf treatment, soil treatment, and seed treatment.

[0008] However, the above two compounds still have the problem of 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 neonicotinoid insecticide selected from at least one of acetamiprid, nitenpyram, clothianidin, dinotefuran, imidacloprid, flupyradifurone, thiacloprid, thiamethoxam, sulfoxaflor, triflumezopyrim, dichlorophenylpyridazin (CAS: 2413390-32-4), spinetoram, spinosad, avermectin;

[0010] The structure of compound I is shown below,

[0011]

[0012] The structure of fenmezoditiaz is shown below:

[0013]

[0014] 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, the whole of which is incorporated herein by reference.

[0015] According to an embodiment of the present application, the mass ratio of the compound I and the neonicotinoid insecticide is 80-1:1-80.

[0016] According to an embodiment of the present application, the mass ratio of the compound I and the neonicotinoid 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.

[0017] According to a preferred embodiment of the present application, the mass ratio of the compound I and the neonicotinoid insecticide is 10-1:1-10.

[0018] According to an embodiment of the present application, the sum of the mass of the compound I and the neonicotinoid 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 being 100%.

[0019] According to an embodiment of the present application, the composition can be prepared into a liquid preparation or a solid preparation.

[0020] According to the embodiments of the present application, the content of the effective active ingredient in the formulation varies according to different formulation types. Generally, the content of the effective active ingredient in the liquid formulation is 1% to 60% by weight, preferably 5% to 50%; the content of the effective active ingredient in the solid formulation is 5% to 80% by weight, preferably 10% to 70%.

[0021] According to the embodiments 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 adjustor, or filler, etc.

[0022] According to the embodiments of the present application, the composition can be diluted by the user before use or used directly. The preparation thereof can be prepared by 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 adjustor, or filler, etc., to obtain the composition.

[0023] According to the embodiments 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, microcapsule suspension-suspension, emulsifiable concentrate, microemulsion, dispersible liquid, granule.

[0024] According to the embodiments of the present application, when the composition is prepared into wettable powder, the composition comprises the following components and contents: compound I 1% to 80%, nicotinic insecticide 1% to 80%, dispersant 0% to 10%, wetting agent 0% to 8%, and the balance is filler.

[0025] Preferably, the content of compound I in the composition is 2% to 70%, 5% to 65%, 10% to 60%, 15% to 50%, etc.

[0026] The content of nicotinic insecticide is 2% to 70%, 5% to 65%, 10% to 60%, 15% to 50%, etc.

[0027] The content of dispersant is 1% to 8%, 2% to 7%, 3-6%, or 4% to 5%.

[0028] The content of wetting agent is 1% to 8%, 2% to 7%, 3-6%, or 4% to 5%.

[0029] According to embodiments of the present application, the composition, when formulated as a water dispersible granule, comprises the following components and amounts: Compound I 1% to 80%, a neonicotinoid insecticide 1% to 80%, a dispersing agent 0% to 10%, a wetting agent 0% to 16%, a disintegrant 0% to 20%, and the balance being a filler.

[0030] Preferably, Compound I in the composition is 2% to 70%, 5% to 65%, 10% to 60%, 15% to 50%, etc.

[0031] The neonicotinoid insecticide is 2% to 70%, 5% to 65%, 10% to 60%, 15% to 50%, etc.

[0032] The dispersing agent is 1% to 8%, 2% to 7%, 3-6%, or 4% to 5%.

[0033] The wetting agent is 1% to 8%, 2% to 7%, 3-6%, or 4% to 5%.

[0034] The disintegrant is 1% to 18%, 2% to 16%, 3-15%, 4% to 12%, 5% to 10%, or 6-8%.

[0035] According to embodiments of the present application, the composition, when formulated as a suspension concentrate, comprises the following components and amounts: Compound I 1% to 50%, a neonicotinoid insecticide 1% to 50%, a dispersing agent 0% to 5%, a wetting agent 0% to 8%, a thickening agent 0% to 0.3%, an anti-freeze agent 0% to 5%, and the balance being deionized water.

[0036] Preferably, Compound I in the composition is 2% to 45%, 5% to 40%, 10% to 35%, 15% to 30%, 20% to 25%, etc.

[0037] The neonicotinoid insecticide is 2% to 45%, 5% to 40%, 10% to 35%, 15% to 30%, 20% to 25%, etc.

[0038] The dispersing agent is 1% to 4% or 2% to 3%.

[0039] The wetting agent is 1% to 8%, 2% to 7%, 3-6%, or 4% to 5%.

[0040] The thickening agent is 0.1% to 0.25%.

[0041] The anti-freeze agent is 1% to 4% or 2% to 3%.

[0042] 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 nicotinic insecticide 1-50%, an organic solvent 0-95%, an emulsifier 0-10%, an anti-freezing agent 0-5%, an antifoaming agent 0-0.2%, a thickening agent 0-0.5%, and the balance being deionized water.

[0043] Preferably, Compound I in the composition is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.

[0044] The nicotinic insecticide is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.

[0045] The organic solvent is 1-90%, 2-80%, 5-70%, 10-60%, 15-50%, 20-50%, 30-40%, etc.

[0046] The emulsifier is 1-8%, 2-7%, 3-6%, or 4-5%.

[0047] The anti-freezing agent is 1-4% or 2-3%.

[0048] The antifoaming agent is 0.05-0.1%, or

[0049] The thickening agent is 0.1-0.4%, 0.2-0.3%.

[0050] 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 nicotinic insecticide 1-50%, an organic solvent 0-95%, an emulsifier 0-10%, an anti-freezing agent 0-5%, an antifoaming agent 0-0.2%, a thickening agent 0-0.5%, and the balance being deionized water.

[0051] Preferably, Compound I in the composition is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.

[0052] The nicotinic insecticide is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.

[0053] The dispersing agent is 2-10%, 3-8%, 4-7%, or 5-6%.

[0054] The wetting agent is 1-8%, 2-7%, 3-6%, or 4-5%.

[0055] Anti-freezing agent is 1-8%, 2-7%, 3-6%, or 4-5%;

[0056] Anti-caking agent is 0.5-9%, 1-8%, 2-7%, 3-6%, or 4-5%;

[0057] Suspending agent is 0.2-4%, 0.5-3.5%, 1-3%, 1.5-2.5%, or 1.8-2%;

[0058] Film forming agent is 2-9%, 3-8%, 4-7%, or 5-6%;

[0059] Preservative is 0.2-4%, 0.5-3.5%, 1-3%, 1.5-2.5%, or 1.8-2%;

[0060] Coloring agent is 2-25%, 3-20%, 5-15%, 8-12%, or 9-10%;

[0061] pH adjusting agent is 0.1-5%, 0.2-4%, 0.5-3.5%, 1-3%, 1.5-2.5%, or 1.8-2%;

[0062] Thickening agent is 0.5-7, 1-6%, 2-5%, or 3-4%.

[0063] According to the embodiments of the present application, the composition, when made into a microcapsule suspension agent, comprises the following components and contents: Compound I 1-50%, a nicotinic 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.

[0064] Preferably, Compound I in the composition is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.

[0065] The nicotinic insecticide is 2-45%, 5-40%, 10-35%, 15-30%, 20-25%, etc.

[0066] The high molecular capsule wall material is 2-25%, 5-20%, 6-18%, or 10-15%, etc.

[0067] The dispersing agent is 3-8%, 4-7%, or 5-6%;

[0068] The organic solvent is 2% to 45%, 5% to 40%, 10% to 35%, 15% to 30%, or 20% to 25%, etc.

[0069] The emulsifier is 2% to 6% or 4% to 5%.

[0070] The 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%.

[0071] The antifoaming agent is 0.05% to 1.8%, 0.1% to 1.5%, 0.5% to 1.3%, or 0.8% to 1.0%.

[0072] The thickening agent is 0.2% to 7%, 0.5% to 6%, 1% to 5%, 1.5% to 4%, or 2% to 3%.

[0073] The antifreeze agent is 0.5% to 7%, 1% to 6%, 2% to 5%, or 3% to 4%.

[0074] According to an 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%, a nicotinic insecticide 1% to 50%, a high molecular capsule wall material 1% to 12%, a dispersing agent 1% to 12%, a wetting agent 1% to 8%, an organic solvent 1% to 50%, an emulsifier 1% to 8%, an antifoaming agent 0.01% to 2%, a thickening agent 0.1% to 8%, a pH regulator 0.1% to 5%, an antifreeze agent 0.1% to 8%, and the balance is deionized water.

[0075] According to an embodiment of the present application, when the composition is made into an emulsifiable concentrate, it comprises the following components and contents: Compound I 1% to 50%, a nicotinic insecticide 1% to 50%, an emulsifier 0 to 10%, an antifreeze agent 0% to 5%, a stabilizer 0% to 0.5%, and the balance is an organic solvent.

[0076] Alternatively, Compound I 1% to 50%, a nicotinic insecticide 1% to 50%, an emulsifier 0 to 12%, a stabilizer 0% to 0.5%, and the balance is an organic solvent.

[0077] According to an 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%, a nicotinic insecticide 1% to 50%, an organic solvent 1% to 50%, an emulsifier 1% to 30%, an antifreeze agent 1% to 10%, a stabilizer 0.1% to 5%, and the balance is deionized water.

[0078] According to an embodiment of the present application, when the composition is made into a dispersible liquid, it comprises the following components and contents: Compound I 1% to 50%, a nicotinic insecticide 1% to 50%, an emulsifier 1% to 30%, an antifreeze agent 1% to 10%, a stabilizer 0.1% to 5%, and the balance is an organic solvent.

[0079] According to the embodiment of the present application, when the composition is made into granules, the composition comprises the following components and contents: Compound I 0.1% to 10%, a nicotine insecticide 0.1% to 10%, a dispersing agent 0% to 5%, a wetting agent 0% to 5%, a binder 0% to 3%, and the rest is a filler.

[0080] According to the embodiment of the present application, the emulsifier can be selected from at least one of the following: sodium lignosulfonate, Farmol, phenol polyoxyethyl ether phosphate, triphenyl ethyl styryl 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, castor oil polyoxyethylene ether phosphate.

[0081] According to the embodiment of the present application, the dispersing agent can be selected from at least one of the following: 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, phosphate ester.

[0082] According to the embodiment of the present application, the wetting agent can be selected from at least one of the following: trisiloxane polyoxyethylene ether, sodium N-lauroyl glutamate, sodium dodecyl sulfate, sodium lauroyl sarcosinate, sodium methyl naphthalene sulfonate formaldehyde condensate, castor oil polyoxyethylene ether, triphenyl ethyl phenol polyoxyethylene ether, sodium dodecyl benzene sulfonate, sodium alkyl naphthalene sulfonate, isooctanol succinate sodium sulfonate, polyoxyethylene alkyl aryl ether, fatty alcohol polyether glycerol fatty acid polyoxyethylene ether, fatty alcohol polyoxyethylene ether.

[0083] According to the embodiment of the present application, the binder can be selected from at least one of the following: xanthan gum, starch, urea-formaldehyde resin, gelatin, gum arabic, carboxymethyl cellulose, carboxyethyl cellulose, polyvinyl alcohol.

[0084] According to the embodiment of the present application, the disintegrant can be selected from at least one of the following: sodium bicarbonate, ammonium sulfate, sodium sulfate, calcium sulfate, magnesium chloride.

[0085] According to the embodiment of the present application, the thickening agent can be selected from at least one of the following: magnesium aluminum silicate, polyvinyl acetate, xanthan gum, gelatin, gum arabic, polyvinyl alcohol.

[0086] According to an embodiment of the present application, the defoaming agent can be selected from at least one of silicone oil, n-octanol, silicone, butyl phosphate, isobutyl phosphate, and the like.

[0087] According to an embodiment of the present application, the anti-freezing agent can be selected from at least one of propylene glycol, ethylene glycol, glycerol, and the like.

[0088] 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, dialkyl succinate acid sulfonate, and the like.

[0089] 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, talc powder. The liquid filler can be selected from at least one of soybean oil, castor oil, mineral oil.

[0090] 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, solvent oil (e.g., 150# solvent oil).

[0091] The present application also provides a use of the above composition for controlling pests in agriculture and non-agriculture.

[0092] According to an embodiment of the present application, the pests are Lepidoptera, Hemiptera, Coleoptera, Thysanoptera, Diptera, mites, and the like.

[0093] As an embodiment, the pests are selected from the group consisting of cotton aphid, whitefly, tea green leafhopper, and pear woodlouse.

[0094] The present application also provides a method for controlling pests in agriculture or non-agriculture, comprising applying the above composition to plants where pests exist.

[0095] The composition of the present application can be provided in the form of a finished preparation, or in the form of a single agent, which is directly mixed before use, and then diluted with water to the desired concentration, and can be applied to crops in any manner, such as spraying, plant root irrigation, smearing, and the like. In specific applications, it can also be mixed with other agents, such as growth regulators, soil conditioners, herbicides, nematicides, and the like.

[0096] The present application also provides a composition for controlling invertebrate pests comprising a biologically effective amount of Compound I, a neonicotinoid insecticide and at least one additional 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 additional biologically active compound or agent, said neonicotinoid insecticide being selected from at least one of acetamiprid, nitenpyram, clothianidin, dinotefuran, imidacloprid, flupyradifurone, thiacloprid, thiamethoxam, sulfoxaflor, triflumuron, clorsulfron, fenmezoditiaz (CAS: 2413390-32-4), spinetoram, spinosad, avermectin.

[0097] The present application also provides a method for controlling invertebrate pests comprising contacting said invertebrate pests or their environment with a biologically effective amount of a composition of the present application as described above.

[0098] The present application also provides a spray composition comprising a composition of the present application as described above and a propellant.

[0099] The present application also provides a bait composition comprising a composition of the present application as described above; one or more food materials; optionally an attractant; and optionally a humectant.

[0100] Advantages of the present application:

[0101] The synergistic composition of the present application has the following advantages:

[0102] 1) has synergistic effect, can improve the effect of pest control; 2) expand the insecticidal spectrum, mixed occurrence of field insect pests, stronger effect on pests; 3) the mechanism of action of two effective components is different, mixed use can delay the development of pest resistance; 4) reduce the amount of application, reduce the use of times, reduce the use cost. DETAILED DESCRIPTION

[0103] The present application will be further described in conjunction with 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 encompassed within the scope of the present application intended to be protected.

[0104] The experimental methods used in the following examples are conventional methods unless otherwise specified; the reagents, materials, etc. used in the following examples can be obtained from commercial channels unless otherwise specified.

[0105] The insecticidal effect of the composition is tested by combining indoor biological testing and field testing. 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.

[0106] The compound I used in the following examples was prepared according to the method of Example 1 in the patent document CN 111909143 A.

[0107] The % of each component in the preparation of the following Preparation Examples and Examples refers to the mass percentage content if not specifically stated.

[0108] Preparation Example 1: Wettable powder

[0109]

[0110]

[0111] The above materials are roughly crushed in proportion and then mixed uniformly in a mixer. After air flow crushing, the finished product is obtained.

[0112] Preparation Example 2: Water dispersible granule

[0113]

[0114] The effective active ingredient and various adjuvants are mixed uniformly in proportion to the formula. After air flow crushing, the powder is obtained. A certain amount of water is added to mix and extrude granulation. After drying and screening, the finished product is obtained.

[0115] Preparation Example 3: Suspension concentrate

[0116]

[0117] The effective active ingredient and various adjuvants are mixed uniformly in proportion to the formula. After high-speed shearing and sand milling, the finished product is obtained.

[0118] Preparation Example 4: Emulsifiable concentrate

[0119]

[0120]

[0121] 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.

[0122] Preparation Example 5: Emulsion in water

[0123]

[0124] The above raw materials are added into a batching kettle according to the requirements of the formula, uniformly mixed by a high-speed shearing machine to prepare a water emulsion, and after inspection, the product is obtained by metering and packaging.

[0125] Preparation Example 6: emulsifiable concentrate

[0126]

[0127] 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.

[0128] Preparation Example 7: granules

[0129]

[0130]

[0131] The components are mixed in the formula proportion, crushed, wetted with water, and then fully stirred, granulated by a screw extrusion granulator, dried, and sieved to obtain the finished product.

[0132] The nicotinic insecticide is selected from at least one of the following: acetamiprid, nitenpyram, clothianidin, dinotefuran, imidacloprid, flupyradifurone, thiacloprid, thiamethoxam, sulfoxaflor, triflumezopyrim, dichlorophenylpyridazin, fenmezoditiaz (CAS: 2413390-32-4), spinetoram, spinosad, and chlorfenapyr.

[0133] II. Indoor toxicity determination example

[0134] (1) Test insect: cotton aphid (Aphis gossypii Glover), whitefly (Bemisia tabaci), tea green leafhopper (Empoasca pirisuga Matumura), pear psylla (Psylla chinensis Yang et Li).

[0135] (2) Determination method:

[0136] Pest toxicity determination method

[0137] The cotton aphid, tea green leafhopper, and other pests are used as test materials for the toxicity determination of compound I, nicotinic insecticides, and their mixed formulations by the immersion method.

[0138] Reference to the People's Republic of China agricultural industry standard NY / T 1154.6-2006 "Pesticide indoor biological determination test guidelines" insecticide part 6: insecticide activity test insect immersion method, first test agent (including compound I, nicotinic insecticide) with the appropriate solvent (solvent types such as acetone, methanol, N, N dimethylformamide and dimethyl sulfoxide, and according to its solubility of the sample is selected) is prepared into 5 concentration gradient (according to the LC 50 value of compound for different pests, set concentration gradient according to equal ratio or equal difference), compound I, nicotinic insecticide for mixing is set according to the LC 50 value of mass proportion of a series of proportion, according to different proportion of the final mass concentration (referring to the total mass of compound I, nicotinic insecticide).

[0139] The target insects enter the liquid medicine for 5s-10s, and the excess liquid medicine is absorbed with filter paper, and the test insects are transferred to normal conditions for feeding. Each treatment has 4 repeats, each repeat has 10-20 insects, and the treatment without the agent is set as the control.

[0140] The pest toxicity determination uses whitefly, pear wood lice and other pests as test materials, and adopts leaf immersion method to determine the toxicity of compound I, nicotinic insecticide and its mixed preparation.

[0141] Reference to the People's Republic of China agricultural industry standard NY / T 1154.14-2008 "Pesticide indoor biological determination test guidelines" insecticide part 14: leaf immersion method, first test agent (including compound I, nicotinic insecticide) with the appropriate solvent (solvent types such as acetone, methanol, N, N dimethylformamide and dimethyl sulfoxide, and according to its solubility of the sample is selected) is prepared into 5 concentration gradient (according to the LC 50 value of compound for different pests, set concentration gradient according to equal ratio or equal difference), compound I, nicotinic insecticide for mixing is set according to the LC 50 value of mass proportion of a series of proportion, according to different proportion of the final mass concentration (referring to the total mass of compound I, nicotinic insecticide).

[0142] The leaf disc or leaf segment is immersed in the test agent solution, and after 10s (the immersion time can be appropriately prolonged or shortened according to the characteristics of the agent), it is taken out and dried, placed in a culture dish containing 1% water agar or moisture filter paper, and the test insects are introduced, with not less than 10 heads per repeat. Each treatment has not less than 4 repeats, and the treatment without the agent (containing all organic solvents and emulsifiers) is set as the blank control.

[0143] According to Sun Yunpei method, the different proportion of two drugs CTC (CTC value) is calculated, the CTC (CTC) of the mixed agent is greater than or equal to 120, which shows synergistic effect, CTC is less than or equal to 80, which shows antagonistic effect; 80 < CTC < 120 shows additive effect. The CTC (CTC) of the mixed agent is calculated according to formula (1), formula (2) and formula (3):

[0144]

[0145] In the formula:

[0146] ATI - the measured toxicity index of the mixed agent;

[0147] S - the LC of the standard insecticide, unit: milligrams per liter (mg / L); 50

[0148] M - the LC of the mixed agent, unit: milligrams per liter (mg / L) 50

[0149] TTI = TI A × P A + TI B × P B (2)

[0150] In the formula:

[0151] TTI - the theoretical CTC of the mixed agent;

[0152] TI A - the toxicity index of A agent;

[0153] P A - the percentage content of A agent in the mixed agent, unit: percentage (%);

[0154] TI B - the toxicity index of B agent;

[0155] P B - the percentage content of B agent in the mixed agent, unit: percentage (%).

[0156]

[0157] In the formula:

[0158] CTC - CTC;

[0159] ATI - the actual toxicity index of the mixed agent;

[0160] TTI - the theoretical toxicity index of the mixed agent.

[0161] ​​When different pesticides are mixed, they typically exhibit three types of effects: additive, synergistic, and antagonistic. However, the specific type of effect cannot be predicted. The composition described in this invention uses compound I and a neonicotinoid insecticide as the active ingredients, and bioassay examples are used to illustrate this.

[0162] Indoor pesticide activity assay for aphids

[0163] This experiment used the immersion method to conduct an indoor activity test of the compounds against cotton aphids, in order to determine the activity of the insecticidal compositions of Examples 1-6 against cotton aphids.

[0164] Example 1: To verify the effects of different ratios of Compound I and Thiamethoxam on cotton aphids, indoor toxicity tests were conducted on different ratios of Compound I and Thiamethoxam against cotton aphids. The corresponding concentrations were prepared according to the weight ratios in the table, and indoor insecticidal experiments were performed. The results are as follows:

[0165] Table 1. Results of toxicity assays of Compound I and thiamethoxam, alone and in mixtures, against cotton aphids.

[0166] Active ingredient Ratio Regression equation LC 50 ]]> Co-toxicity coefficient Evaluation Compound I — y = 3.1194 + 1.5769x 15.5816 — — thiamethoxam — y = 4.6117 + 1.1192x 2.2229 — — Compound I: thiamethoxam 50：1 y = 3.3723 + 1.8449x 7.6255 182.8034 Synergism Compound I: thiamethoxam 10：1 y = 3.7690 + 1.7758x 4.9341 204.2295 Synergism Compound I: thiamethoxam 1：1 y = 4.8918 + 0.8734x 1.3299 292.5588 Synergism Compound I: thiamethoxam 1：10 y = 4.9552 + 1.0785x 1.1004 219.0819 Synergism Compound I: thiamethoxam 1：50 y = 4.8495 + 1.0941x 1.3726 164.7160 Synergism

[0167] As shown in Table 1, different ratios of compound I and thiamethoxam in combination significantly enhanced the activity of compound I against cotton aphids.

[0168] Example 2: To verify the effects of different ratios of Compound I and imidacloprid on cotton aphids, indoor toxicity tests were conducted on different ratios of Compound I and imidacloprid against cotton aphids. The corresponding concentrations were prepared according to the weight ratios in the table, and indoor insecticidal experiments were performed. The results are as follows:

[0169] Table 2. Results of toxicity assays of Compound I and imidacloprid, alone and in mixtures, against cotton aphids.

[0170] Active ingredient Ratio Regression equation LC 50 ]]> Co-toxicity coefficient Evaluation Compound I — y = 3.1194 + 1.5769x 15.5816 — — pirimicarb — y = 4.1931 + 1.6073x 3.1769 — — Compound I: pirimicarb 50：1 y = 3.3403 + 1.7419x 8.9708 161.3445 Synergism Compound I: pirimicarb 10：1 y = 4.1489 + 1.3234x 4.3962 261.5873 Synergism Compound I: pirimicarb 1：1 y = 4.5718 + 1.2658x 2.1792 242.1868 Synergism Compound I: pirimicarb 1：10 y = 4.8312 + 1.1903x 1.3862 247.0593 Synergism Compound I: pirimicarb 1：50 y = 4.5479 + 1.2718x 2.2670 142.3581 Synergism

[0171] As shown in Table 2, different ratios of compound I and imidacloprid significantly enhanced the activity of the cotton aphid.

[0172] Example 3: To verify the effects of different ratios of Compound I and acetamiprid on cotton aphids, indoor toxicity tests were conducted on different ratios of Compound I and acetamiprid against cotton aphids. The corresponding concentrations were prepared according to the weight ratios in the table, and indoor insecticidal experiments were performed. The results are as follows:

[0173] Table 3. Results of toxicity assays of Compound I and acetamiprid (single agents and mixtures) against cotton aphids.

[0174]

[0175]

[0176] From the results of Table 4, it can be seen that the activity of compound I and flonicamid in different proportions and amounts of mixture against cotton aphids has obvious synergistic effect.

[0177] Example 4: In order to verify the effect of compound I and flonicamid in different proportions and amounts on cotton aphids, indoor toxicity determination of compound I and flonicamid in different proportions on cotton aphids was carried out, and the corresponding concentration was prepared according to the weight ratio in the table, and indoor insecticidal test was carried out, and the test results were as follows:

[0178] Table 4 Toxicity determination results of compound I and flonicamid single agent and their mixture on cotton aphids

[0179] Active ingredient Ratio Regression equation LC 50 ]]> Co-toxicity coefficient Evaluation Compound I — y = 3.1194 + 1.5769x 15.5816 — — sulfoxaflor — y = 5.0245 + 1.2389x 0.9554 — — Compound I: sulfoxaflor 50：1 y = 4.0219 + 1.1989x 6.5435 183.1639 Synergism Compound I: sulfoxaflor 10：1 y = 4.3338 + 1.3783x 3.0434 214.0755 Synergism Compound I: sulfoxaflor 1：1 y = 5.2904 + 1.5020x 0.6407 281.0062 Synergism Compound I: sulfoxaflor 1：10 y = 5.4184 + 1.3049x 0.4780 218.5200 Synergism Compound I: sulfoxaflor 1：50 y = 5.4093 + 1.6895x 0.5725 170.0100 Synergism

[0180] From the results of Table 4, it can be seen that the activity of compound I and flonicamid in different proportions and amounts of mixture against cotton aphids has obvious synergistic effect.

[0181] Example 5: In order to verify the effect of compound I and thiacloprid in different proportions and amounts on cotton aphids, indoor toxicity determination of compound I and thiacloprid in different proportions on cotton aphids was carried out, and the corresponding concentration was prepared according to the weight ratio in the table, and indoor insecticidal test was carried out, and the test results were as follows:

[0182] Table 5 Toxicity determination results of compound I and thiacloprid single agent and their mixture on cotton aphids

[0183] Active ingredient Ratio Regression equation LC 50 ]] Co-toxicity coefficient Evaluation Compound I — y = 3.1194 + 1.5769x 15.5816 — — acetamiprid — y = 4.9593 + 1.2634x 1.0769 — — Compound I: acetamiprid 50：1 y = 3.4432 + 1.7761x 7.5260 163.7962 Synergism Compound I: acetamiprid 10：1 y = 4.3951 + 1.3921x 2.7195 257.5873 Synergism Compound I: acetamiprid 1：1 y = 5.0609 + 1.2832x 0.8965 224.7146 Synergism Compound I: acetamiprid 1：10 y = 5.3312 + 1.4492x 0.5909 199.0943 Synergism Compound I: acetamiprid 1：50 y = 5.1956 + 1.2626x 0.7000 156.7019 Synergism

[0184] From the results of Table 5, it can be seen that the activity of compound I and thiacloprid in different proportions and amounts of mixture against cotton aphids has obvious synergistic effect.

[0185] Example 6: In order to verify the effect of compound I and fenmezoditiaz in different proportions and amounts on cotton aphids, indoor toxicity determination of compound I and fenmezoditiaz in different proportions on cotton aphids was carried out, and the corresponding concentration was prepared according to the weight ratio in the table, and indoor insecticidal test was carried out, and the test results were as follows:

[0186] Table 6 Toxicity determination results of compound I and fenmezoditiaz single agent and their mixture on cotton aphids

[0187] Active ingredient Ratio Regression equation LC 50 ]]> Co-toxicity coefficient Evaluation Compound I — y = 3.1194 + 1.5769x 15.5816 — — fenmezoditiaz — y = 5.5432 + 1.3858x 0.4055 — — Compound I: fenmezoditiaz 50：1 y = 3.7775 + 1.7132x 5.1708 173.8280 Synergism Compound I: fenmezoditiaz 10：1 y = 4.7198 + 1.3425x 1.6169 218.9171 Synergism Compound I: fenmezoditiaz 1：1 y = 5.7001 + 1.5455x 0.3524 224.2990 Synergism Compound I: fenmezoditiaz 1：10 y = 6.0901 + 1.6150x 0.2113 210.5480 Synergism Compound I: fenmezoditiaz 1：50 y = 5.8555 + 1.3897x 0.2423 170.6115 Synergism

[0188] From the results of Table 6, it can be seen that the activity of compound I and fenmezoditiaz in different proportions and amounts of mixture against cotton aphids has obvious synergistic effect.

[0189] Example 7: To verify the effect of different proportions of compound I and fenmezoditiaz on cotton aphids, indoor toxicity tests of different proportions of compound I and DPX-RAB55 on cotton aphids were carried out, and the corresponding concentrations were prepared according to the weight ratio in the table, and indoor insecticidal tests were carried out. The test results are as follows:

[0190] Table 7 Toxicity test results of compound I and fenmezoditiaz single agent and its mixture on cotton aphids

[0191] Active ingredient Ratio Regression equation LC 50 ]]> Co-toxicity factor Evaluation Compound I — y = 3.1194 + 1.5769x 15.5816 — — fenmezoditiaz y = 5.8285 + 0.9138x 0.1240 — — Compound I: fenmezoditiaz 50：1 y = 4.5730 + 0.9890x 2.7026 167.3911 Synergism Compound I: fenmezoditiaz 10：1 y = 5.2492 + 0.6964x 0.4387 287.9993 Synergism Compound I: fenmezoditiaz 1：1 y = 5.9228 + 0.9603x 0.1094 224.9013 Synergism Compound I: fenmezoditiaz 1：10 y = 6.1880 + 0.9342x 0.0535 254.7505 Synergism Compound I: fenmezoditiaz 1：50 y = 5.9193 + 0.8568x 0.0845 149.6567 Synergism

[0192] As can be seen from the results in Table 7, the activity of different proportions of compound I and fenmezoditiaz mixed with different proportions of compound I and fenmezoditiaz on cotton aphids has obvious synergistic effect.

[0193] Indoor insecticide activity determination test of Bemisia tabaci

[0194] In this test, leaf immersion method was used to determine the activity of the insecticidal composition of Examples 8-10 on Bemisia tabaci.

[0195] Example 8: To verify the effect of different proportions of compound I and nitenpyram on Bemisia tabaci, indoor toxicity tests of different proportions of compound I and nitenpyram on Bemisia tabaci were carried out, and the corresponding concentrations were prepared according to the weight ratio in the table, and indoor insecticidal tests were carried out. The test results are as follows:

[0196] Table 8 Toxicity test results of compound I and nitenpyram single agent and its mixture on Bemisia tabaci

[0197] Active ingredient Ratio Regression equation LC 50 ]]> Co-toxicity factor Evaluation Compound I — y = 4.0593 + 1.7553x 3.4351 — — nitenpyram — y = 2.9469 + 2.0690x 9.8243 — — Compound I: nitenpyram 50：1 y = 4.6240 + 1.2388x 2.0115 172.9780 Synergism Compound I: nitenpyram 10：1 y = 4.8616 + 0.9661x 1.3900 262.6569 Synergism Compound I: nitenpyram 1：1 y = 4.5666 + 1.2619x 2.2050 230.8546 Synergism Compound I: nitenpyram 1：10 y = 4.4458 + 1.3020x 2.6647 315.3640 Synergism Compound I: nitenpyram 1：50 y = 3.9962 + 1.4074x 5.1668 183.4549 Synergism

[0198] As can be seen from the results in Table 8, the activity of different proportions of compound I and nitenpyram mixed with different proportions of compound I and nitenpyram on Bemisia tabaci has obvious synergistic effect.

[0199] Example 9: To verify the effect of different proportions of compound I and nitenpyram on Bemisia tabaci, indoor toxicity tests of different proportions of compound I and nitenpyram on Bemisia tabaci were carried out, and the corresponding concentrations were prepared according to the weight ratio in the table, and indoor insecticidal tests were carried out. The test results are as follows:

[0200] Table 9 Toxicity test results of compound I and nitenpyram single agent and its mixture on Bemisia tabaci

[0201] Active ingredient Ratio Regression equation LC 50 ]]> Co-toxicity factor Evaluation Compound I — y = 4.0593 + 1.7553x 3.4351 — — dinotefuran — y = 4.9003 + 1.1912x 1.2126 — — Compound I: dinotefuran 50：1 y = 4.5658 + 1.3387x 2.1105 157.1181 Synergism Compound I: dinotefuran 10：1 y = 4.9030 + 1.0395x 1.2396 237.5385 Synergism Compound I: dinotefuran 5：1 y = 4.9551 + 1.1707x 1.0923 240.8847 Synergism Compound I: dinotefuran 3：1 y = 4.9630 + 1.2512x 1.0705 220.0558 Synergism Compound I: dinotefuran 1：1 y = 5.1768 + 1.3772x 0.7441 240.8893 Synergism Compound I: dinotefuran 1：3 y = 5.2212 + 1.3852x 0.6924 208.9232 Synergism Compound I: dinotefuran 1：5 y = 5.2831 + 1.4101x 0.6299 215.7795 Synergism Compound I: dinotefuran 1：10 y = 5.3026 + 1.6936x 0.6628 194.3832 Synergism Compound I: dinotefuran 1：50 y = 5.2200 + 1.5442x 0.7203 170.5088 Synergism

[0202] As can be seen from the results in Table 9, the activity of different proportions of compound I and nitenpyram mixed with different proportions of compound I and nitenpyram on Bemisia tabaci has obvious synergistic effect.

[0203] Example 10: To verify the effect of different proportions of compound I and fluorofurane ketone on the whitefly, indoor toxicity determination of different proportions of compound I and fluorofurane ketone on the whitefly was carried out, and the corresponding concentration was prepared according to the weight ratio in the table, and indoor insecticidal test was carried out, and the test results were as follows:

[0204] Table 10 Toxicity determination results of compound I and fluorofurane ketone single agent and its mixture on the whitefly

[0205]

[0206]

[0207] From the results in Table 10, the activity of different proportions of compound I and fluorofurane ketone mixed with different proportions of compound I and fluorofurane ketone on the whitefly has obvious synergistic effect.

[0208] Indoor insecticide activity determination test of tea green leafhopper

[0209] In this test, the indoor activity determination test of compound on tea green leafhopper was carried out by dipping insect method, in order to determine the activity of insecticidal composition of examples 11-13 on tea green leafhopper.

[0210] Example 11: To verify the effect of different proportions of compound I and clothianidin on tea green leafhopper, indoor toxicity determination of different proportions of compound I and clothianidin on tea green leafhopper was carried out, and the corresponding concentration was prepared according to the weight ratio in the table, and indoor insecticidal test was carried out, and the test results were as follows:

[0211] Table 11 Toxicity determination results of compound I and clothianidin single agent and its mixture on tea green leafhopper

[0212] Active ingredient Ratio Regression equation LC 50 ]]> Co-toxicity factor Evaluation Compound I — y = 6.0469 + 1.9612x 0.2926 — — clothianidin — y = 4.4911 + 1.3926x 2.3196 — — Compound I: clothianidin 50：1 y = 6.0722 + 1.5801x 0.2096 142.0319 Synergism Compound I: clothianidin 10：1 y = 6.4431 + 1.7747x 0.1538 206.6631 Synergism Compound I: clothianidin 5：1 y = 6.3309 + 1.6020x 0.1477 231.8832 Synergism Compound I: clothianidin 3：1 y = 6.3631 + 1.6056x 0.1416 264.4005 Synergism Compound I: clothianidin 1：1 y = 5.8969 + 1.3772x 0.2232 232.8181 Synergism Compound I: clothianidin 1：3 y = 5.4637 + 1.3252x 0.4468 190.0366 Synergism Compound I: clothianidin 1：5 y = 5.3593 + 1.2740x 0.5224 206.0623 Synergism Compound I: clothianidin 1：10 y = 5.2850 + 1.5698x 0.6583 216.2110 Synergism Compound I: clothianidin 1：50 y = 4.8383 + 1.3919x 1.3067 156.2943 synergism

[0213] From the results in Table 11, the activity of different proportions of compound I and clothianidin mixed with different proportions of compound I and clothianidin on tea green leafhopper has obvious synergistic effect.

[0214] Example 12: To verify the effect of different proportions of compound I and triflumezopyrim on tea green leafhopper, indoor toxicity determination of different proportions of compound I and triflumezopyrim on tea green leafhopper was carried out, and the corresponding concentration was prepared according to the weight ratio in the table, and indoor insecticidal test was carried out, and the test results were as follows:

[0215] Table 12 Toxicity determination results of compound I and triflumezopyrim single agent and its mixture on tea green leafhopper

[0216]

[0217]

[0218] From the results of Table 12, it can be seen that the activity of compound I and trifluminuron mixed in different proportions and amounts has obvious synergistic effect on Empoasca on the tea.

[0219] Example 13: To verify the effect of compound I and insecticidal ring mixed in different proportions and amounts on Empoasca on the tea, indoor toxicity determination of compound I and insecticidal ring mixed in different proportions on Empoasca on the tea was carried out, and indoor insecticidal test was carried out according to the weight ratio of the corresponding concentration in the table, and the test results are as follows:

[0220] Table 13 Toxicity determination results of compound I and insecticidal ring single agent and their mixture on Empoasca on the tea

[0221] active ingredient ratio regression equation LC 50 ]]> co-toxicity factor evaluation compound I — y = 6.0469 + 1.9612x 0.2926 — — thiodicarb — y = 2.2723 + 1.5261x 61.2920 — — compound I: thiodicarb 50：1 y = 6.0929 + 1.6308x 0.2137 139.6449 synergism compound I: thiodicarb 10：1 y = 6.3601 + 1.5244x 0.1282 250.9386 synergism compound I: thiodicarb 1：1 y = 6.0800 + 1.5195x 0.1946 299.2907 synergism compound I: thiodicarb 1：10 y = 4.7833 + 1.7551x 1.3288 231.2042 synergism compound I: thiodicarb 1：50 y = 3.7068 + 1.4924x 7.3546 163.8556 synergism

[0222] From the results of Table 13, it can be seen that the activity of compound I and insecticidal ring mixed in different proportions and amounts has obvious synergistic effect on Empoasca on the tea.

[0223] Laboratory activity determination test of Cacopsylla pyri

[0224] In this test, leaf immersion method was used to carry out indoor activity determination test of compound on Cacopsylla pyri, in order to determine the activity of insecticidal composition of examples 14 and 15 on Cacopsylla pyri.

[0225] Example 14: To verify the effect of compound I and spinosad mixed in different proportions and amounts on Cacopsylla pyri, indoor toxicity determination of compound I and spinosad mixed in different proportions on Cacopsylla pyri was carried out, and indoor insecticidal test was carried out according to the weight ratio of the corresponding concentration in the table, and the test results are as follows:

[0226] Table 14 Toxicity determination results of compound I and spinosad single agent and their mixture on Cacopsylla pyri

[0227]

[0228]

[0229] From the results of Table 14, it can be seen that the activity of compound I and spinosad mixed in different proportions and amounts has obvious synergistic effect on Cacopsylla pyri.

[0230] Example 15: To verify the effect of compound I and ethyl spinosad mixed in different proportions and amounts on Cacopsylla pyri, indoor toxicity determination of compound I and ethyl spinosad mixed in different proportions on Cacopsylla pyri was carried out, and indoor insecticidal test was carried out according to the weight ratio of the corresponding concentration in the table, and the test results are as follows:

[0231] Table 15 Toxicity determination results of compound I and ethyl spinosad single agent and their mixture on Cacopsylla pyri

[0232] active ingredient ratio regression equation LC 50 ]]> co-toxicity factor evaluation compound I — y = 3.5233 + 1.7442x 7.0250 — — spinosad — y = 3.9025 + 1.5143x 5.3058 — — compound I: spinosad 50：1 y = 4.0759 + 1.5154x 4.0718 171.4393 synergism compound I: spinosad 10：1 y = 4.3112 + 1.4799x 2.9203 233.6749 synergism compound I: spinosad 5：1 y = 4.2379 + 1.5051x 3.2086 207.7228 synergism compound I: spinosad 3：1 y = 4.2940 + 1.5232x 2.9075 223.5109 synergism compound I: spinosad 1：1 y = 4.4048 + 1.5466x 2.4258 249.2189 synergism compound I: spinosad 1：3 y = 4.4003 + 1.4508x 2.5903 218.1821 synergism compound I: spinosad 1：5 y = 4.4285 + 1.4406x 2.4928 221.8975 synergism compound I: spinosad 1：10 y = 4.5882 + 1.2722x 2.1072 257.5226 synergism compound I: spinosad 1：50 y = 4.3447 + 1.3028x 3.1843 167.4268 synergism

[0233] From the results of Table 15, it can be seen that the different proportions of compound I and spinetoram have obvious synergistic effects on the activity of pear psylla.

[0234] Three, field efficacy examples

[0235] In order to clarify the effect of compound I and nicotine insecticide on cotton aphids, tomato whitefly, tea green leafhopper and pear psylla, a number of efficacy tests were carried out in different areas of the country. The preparation was processed according to preparation examples 1-7, for example, the preparation in table 16 (other test preparations refer to the same preparation example), the specific preparation method is as follows:

[0236] Table 16 I·spinetoram suspension of different proportions

[0237]

[0238]

[0239] Cotton aphid field efficacy test

[0240] According to the method of "the People's Republic of China national standard GB / T 17980.75-2004", when the cotton plant has more than 20% of aphids, the pesticide is applied.

[0241] Investigation method: according to the investigation method of "the People's Republic of China national standard GB / T 17980.75-2004", after 4 leaf stage (true leaf) of cotton, 5 points were sampled in each plot, 2 plants were fixed in each point, 1-2 leaves with aphids were fixed in the middle of each plant, and the number of aphid heads on the fixed leaves was investigated. The number of live insects was investigated 1, 3 and 7 days after the drug. The formula for calculating the control effect (control effect) is:

[0242]

[0243]

[0244] Tomato whitefly field efficacy test

[0245] According to the method of "pesticide field efficacy test criteria (GB / T17980.16-2000)", the stems and leaves of tomato were sprayed.

[0246] Investigation method: according to the investigation method of "pesticide field efficacy test criteria (GB / T17980.16-2000)", 10 plants were calibrated in each plot, and the number of live insects was recorded under the condition of not disturbing the insects. The number of live insects was investigated 1-3 days and 7 days after the drug. The formula for calculating the control effect (control effect) is:

[0247]

[0248]

[0249] Field efficacy test of Empoasca flavescens

[0250] According to the method of GB / T 17980.56-2004, the tea plants were sprayed with the test compound.

[0251] Investigation method: According to the method of GB / T 17980.56-2004, 100 tender leaves (usually the second tender leaf under the bud) in each plot were randomly investigated for the number of nymphs. The initial population was investigated before treatment, and the investigation was conducted 1, 3 and 7 days after treatment. The control effect was calculated according to the following formula:

[0252]

[0253]

[0254] Field efficacy test of Cacopsylla pyricola

[0255] According to the method of GB / T 17980.10-2000, the pear trees were sprayed with the test compound.

[0256] Investigation method: According to the method of GB / T 17980.10-2000, 2-3 trees in each plot were investigated, 5 short branches in 5 directions were fixed in each group, and the number of live insects on 10 leaves in each branch was randomly investigated. The number of nymphs in each treatment was not less than 200. The initial population was investigated before treatment, and the investigation was conducted 5, 10 and 15 days after each treatment. The control effect was calculated according to the following formula:

[0257]

[0258]

[0259] Table 17 Field efficacy test of compound I and acetamiprid on cotton aphids

[0260]

[0261] Note: The same column data with different letters represent significant difference at the level of P<0.05 by Duncan's new multiple range test, and the same below.

[0262] Example 16 20% compound I·acetamiprid suspension concentrate (1:4) was prepared according to the preparation example 3, wherein 20% refers to the total mass percentage of active substances (compound I and acetamiprid), and 1:4 refers to the mass ratio of the two active ingredients compound I and acetamiprid.

[0263] Example 17 20% compound I·acetamiprid suspension concentrate (1:3) was prepared according to the preparation example 3, wherein 20% refers to the total mass percentage of active substances (compound I and acetamiprid), and 1:3 refers to the mass ratio of the two active ingredients compound I and acetamiprid.

[0264] Example 18 20% compound I·acetamiprid suspension concentrate (1:2) was prepared according to the preparation example 3, wherein 20% refers to the total mass percentage of active substances (compound I and acetamiprid), and 1:2 refers to the mass ratio of the two active ingredients compound I and acetamiprid.

[0265] The following examples and comparative examples are also prepared in this way, which will not be described in detail here.

[0266] From the results in the table, it can be seen that when controlling cotton aphids, the 1-day, 3-day and 7-day control effects of compound I and acetamiprid complex on cotton aphids are significantly higher than those of single agent at the same active ingredient dosage (comparative examples 1 and 2 correspond to examples 16-22). The 7-day control effect can still reach more than 93.05%, and the duration is longer.

[0267] Table 18 Field efficacy test of compound I and acetamiprid complex on tea green leafhopper

[0268]

[0269] From the results in the table, it can be seen that when controlling tea green leafhopper, the 1-day, 3-day and 7-day control effects of compound I and acetamiprid complex on tea green leafhopper are significantly higher than those of single agent at the same active ingredient dosage (comparative examples 3 and 4 correspond to examples 23-29). The 7-day control effect can still reach more than 89.40%, and the duration is longer.

[0270] Table 19 Field efficacy test of compound I and dinotefuran on cotton aphids

[0271]

[0272] From the results in the table, it can be seen that when controlling cotton aphids, the 1-day, 3-day and 7-day control effects of compound I and dinotefuran complex on cotton aphids are significantly higher than those of single agent at the same active ingredient dosage (comparative examples 5 and 6 correspond to examples 30-36). The 7-day control effect can still reach more than 92.92%, and the duration is longer.

[0273] Table 20 Field efficacy test of compound I and dinotefuran mixture against Bemisia tabaci

[0274]

[0275] From the determination results, in the prevention and treatment of Bemisia tabaci, compound I and dinotefuran mixture and single agent are compared, under the same amount of active ingredient (comparative examples 7 and 8 correspond to examples 37-43), the 1-3, 7 day control effect of compound I and dinotefuran mixture on Bemisia tabaci is significantly higher than that of single agent. Among them, the 7 day control effect can still reach more than 92.88%, and the effective period is longer.

[0276] Table 21 Field efficacy test of compound I and flufenerim mixture against Bemisia tabaci

[0277]

[0278] From the determination results, in the prevention and treatment of Bemisia tabaci, compound I and flufenerim mixture and single agent are compared, under the same amount of active ingredient (comparative examples 9 and 10 correspond to examples 44-50), the 1-3, 7 day control effect of compound I and flufenerim mixture on Bemisia tabaci is significantly higher than that of single agent. Among them, the 7 day control effect can still reach more than 93.28%, and the effective period is longer.

[0279] Table 22 Field efficacy test of compound I and flufenerim mixture against Empoasca flavescens

[0280]

[0281] From the determination results in the table, in the prevention and treatment of Empoasca flavescens, compound I and flufenerim mixture and single agent are compared, under the same amount of active ingredient (comparative examples 11 and 12 correspond to examples 51-57), the 1 day, 3 day control effect and 7 day control effect of compound I and flufenerim mixture on Empoasca flavescens is significantly higher than that of single agent. Among them, the 7 day control effect can still reach more than 90.64%, and the effective period is longer.

[0282] Table 23 Field efficacy test of compound I and spinetoram mixture against Cacopsylla pyri

[0283]

[0284]

[0285] From the determination results in the table, in the prevention and treatment of Cacopsylla pyri, compound I and spinetoram mixture and single agent are compared, under the same amount of active ingredient (comparative examples 13 and 14 correspond to examples 58-63), the 5 day, 10 day control effect and 15 day control effect of compound I and spinetoram mixture on Cacopsylla pyri is significantly higher than that of single agent. Among them, the 15 day control effect can still reach more than 94.67%, and the effective period is longer. From the determination results, in the prevention and treatment of Bemisia tabaci, compound I and dinotefuran mixture and single agent are compared, under the same amount of active ingredient (comparative examples 7 and 8 correspond to examples 37-43), the 1-3, 7 day control effect of compound I and dinotefuran mixture on Bemisia tabaci is significantly higher than that of single agent. Among them, the 7 day control effect can still reach more than 92.88%, and the effective period is longer.

[0286] Table 24 Field efficacy test of compound I and spinetoram combination against Bemisia tabaci

[0287]

[0288] From the determination results, in the prevention and treatment of Bemisia tabaci, the 1-3, 7-day control effects of compound I and spinetoram combination on Bemisia tabaci were obviously higher than those of single agent at the same active ingredient dosage (comparative examples 15 and 16 correspond to examples 65-71). The 7-day control effect still reached more than 94.33%, and the effective period was longer.

[0289] 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 neonicotinoid insecticide, characterized in that, The neonicotinic insecticide is selected from one of the following: acetamiprid, nitenpyram, thiamethoxam, dinotefuran, imidacloprid, thiamethoxam, and flonicamid. The structural formula of compound I is shown below. I The mass ratio of compound I to the nicotine-based insecticide is 50~1:1~50.

2. The composition according to claim 1, characterized in that, The mass ratio of compound I to the nicotine-based insecticide is 10~1:1~10.

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 neonicotinoid insecticide, and at least one other component selected from surfactants, solid diluents, and liquid diluents, wherein the neonicotinoid insecticide is selected from one of the following: acetamiprid, nitenpyram, thiamethoxam, dinotefuran, imidacloprid, thiamethoxam, flonicamid; The structural formula of compound I is shown below. I The mass ratio of compound I to the nicotine-based insecticide is 50~1:1~50.

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.

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