Acaricidal composition and application thereof

Through the composition of nicofluprole and pyflubumide, flupentiiofenox or isocycloseram, the problem of existing acaricides being poor in the control of spider mites and gall mites is solved, achieving efficient and safe acaricidal effects, and being environmentally friendly.

CN120240455APending Publication Date: 2025-07-04YINGTAN SHUANGSHOU PESTICIDE CO LTD
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Patent Information

Application Number
CN202510386539.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-07-24
Publication Date
2025-07-04

AI Technical Summary

Technical Problem

The existing acaricides have poor control of spider mites and gall mites, and are harmful to natural enemies and beneficial mites, which may lead to drug damage and environmental pollution.

Method used

The composition of nicofluprole and pyflubumide, flupentiiofenox or isocycloseram is used to form acaric composition through the combination of agents of different mechanisms of action, with a mass ratio of 50:1 to 1:45. It is used to prepare various agricultural preparations, including emulsion oil, suspension agent and wettable powder, etc., and is applied to the growth medium of mites.

Benefits of technology

It has achieved excellent prevention and control effects on spider mites and gall mites, with good rapidity and long validity period, safe for natural enemies and beneficial mites, no medicine to crops, and environmentally friendly.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention belongs to the technical field of pesticide mite killing, and discloses a mite killing composition and application thereof.The mite killing composition comprises an active ingredient A and an active ingredient B. The active ingredient A is nicofluprole, the active ingredient B is any one of pyflubumide, flupentifenox or isocycloseram, and the mass ratio of the active ingredient A to the active ingredient B is 50: 1-1: 45. The acaricidal composition disclosed by the invention has an excellent control effect on spider mites and gall mites, is harmless to natural enemies and beneficial mites, and is safe to target crops.
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Description

[0001] This divisional application is a divisional application of the application with the application number 202310904130.7, the application date of July 24, 2023, and the invention title of "A miticidal composition and its uses". Technical Field

[0002] The present invention belongs to the technical field of pesticidal miticides, and discloses a miticidal composition and its uses. Background Art

[0003] Nicofluprole is a novel fluorine-containing insecticidal and miticidal agent, with the CAS registration number: 1771741-86-6, and the chemical name is N-methyl-N-cyclopropyl-2-chloro-5-[1-(2,6-dichloro-4-heptafluoroisopropylphenyl)-pyrazol-4-yl]nicotinamide. Nicofluprole shows good insecticidal activities against the Lepidoptera pests Plutella xylostella and Mythimna separata, the Hemiptera pest Myzus persicae, and the Acarina pests. Its structural formula is shown as follows:

[0004]

[0005] Pyflubumide is a formanilide miticidal agent, with the CAS registration number: 926914-55-8, and the chemical name is: 3'-isobutyl-N-isobutyryl-1,3,5-trimethyl-4'-[2,2,2-trifluoro-1-methoxy-1-(trifluoromethyl)ethyl]pyrazole-4-carboxanilide. Its mechanism of action is to inhibit the action of mitochondrial complex II in the respiratory chain of harmful mites. Pyflubumide has good control effects on Tetranychus urticae, Panonychus citri, Panonychus ulmi, etc. at all growth stages, but has poor activities against Tarsonemus spp. and Eriophyidae. Its structural formula is shown as follows:

[0006]

[0007] Flupentiofenox, Chinese name: (trifluoromethyl)5-[2-fluoro-4-chloro-5-((2,2,2-trifluoroethyl)sulfinyl)phenoxy]pentyl sulfide, is a novel sulfur ether type fluorine-containing insecticidal and miticidal agent developed by the Japanese company Kumi Chemical Co., Ltd., and is applicable to the control of pests or mites on fruits, vegetables, rice, etc. Its structural formula is as follows:

[0008]

[0009] Isocycloseram is an isoxazoline insecticide and acaricide, which is a non-competitive inhibitor of the γ-aminobutyric acid (GABA) receptor. Its chemical name is 4-[5-(3,5-dichloro-4-fluorophenyl)-4,5-dihydro-5-(trifluoromethyl)-3-isoxazolyl]-N-(2-ethyl-3-oxo-4-isoxazolidinyl)-2-methylbenzamide, and it has good insecticidal activity against pests such as Lepidoptera, Hemiptera, Coleoptera, etc. Its structural formula is as follows:

[0010]

[0011] Spider mites, also known as red spider mites, mainly damage crops such as melons, beans, eggplants, peppers, fruit trees, etc. Adult mites or nymphs suck the leaves of host plants on the back of the leaves. Grayish-white small dots appear on the damaged leaves. When the damage is severe, adult mites and nymphs can damage all parts above the ground of the plant, spin silk to form webs, gather in groups, causing the entire leaf to turn grayish-white until the whole plant dies.

[0012] Eriophyid mites mainly damage many economic crops such as wolfberries and citrus fruits. Adult and nymph mites suck the tissue sap of plant leaves, flower spikes and fruits. On the back of the damaged young leaves, yellowish-green patches first appear. The damaged spots are sunken, and the damaged parts are distorted to form hair galls. The host tissue in the hair galls is stimulated to produce grayish-white fluff, which gradually turns yellowish-brown, reddish-brown to dark brown, resembling a felt-like shape, with an uneven surface, losing luster, and even swelling and twisting; the damaged parts of the leaves show hyperplasia and thickening phenomena. Summary of the Invention

[0013] Based on the above situation, the purpose of the present invention is to provide a miticidal composition and its use. The miticidal composition has excellent control effects on spider mites and eriophyid mites, has good quick-acting property, long-lasting efficacy, is harmless to natural enemies and beneficial mites, is safe for crops, and does not cause phytotoxicity.

[0014] In order to achieve the above purpose, the present invention adopts the following technical scheme: A miticidal composition, the miticidal composition contains active ingredient A and active ingredient B, the active ingredient A is nicofluprole, and the active ingredient B is any one of pyflubumide, flupentiofenox or isocycloseram. The mass ratio of the active ingredient A to the active ingredient B is 50:1 to 1:45;

[0015] Further, the active ingredient B is pyflubumide, and the mass ratio of the active ingredient A to the active ingredient B is 50:1 to 1:35;

[0016] The active ingredient B is flupentiofenox, and the mass ratio of the active ingredient A to the active ingredient B is 35:1 to 1:35;

[0017] The active ingredient B is isocycloseram, and the mass ratio of the active ingredient A to the active ingredient B is 45:1 to 1:35;

[0018] Furthermore, the active ingredient B is pyflubumide, and the mass ratio of the active ingredient A to the active ingredient B is 25:1 to 1:30;

[0019] The active ingredient B is flupentiofenox, and the mass ratio of the active ingredient A to the active ingredient B is 35:1 to 1:30;

[0020] The active ingredient B is isocycloseram, and the mass ratio of the active ingredient A to the active ingredient B is 35:1 to 1:30;

[0021] Further, based on 100 wt% of the total weight of the acaricidal composition, the total weight of the active ingredient A and the active ingredient B accounts for 1 wt% to 80 wt% of the total weight of the acaricidal composition;

[0022] Further, based on 100 wt% of the total weight of the acaricidal composition, the total weight of the active ingredient A and the active ingredient B accounts for 1 wt% to 70 wt% of the total weight of the acaricidal composition;

[0023] Further, in addition to the active ingredients, the acaricidal composition further includes agriculturally acceptable auxiliary ingredients, and the auxiliary ingredients are selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreezing agents, defoaming agents, solvents, preservatives, stabilizers, synergists or carriers;

[0024] Further, the wetting agent is selected from one or more of alkylbenzene sulfonates, alkylnaphthalene sulfonates, lignin sulfonates, sodium dodecyl sulfate, sodium dioctyl sulfosuccinate, α-olefin sulfonates, alkylphenol polyoxyethylene ethers, castor oil polyoxyethylene ethers, alkylphenol ethoxylates, fatty alcohol ethoxylates, sodium fatty alcohol polyoxyethylene ether sulfate, silkworm excrement, Chinese honey locust powder, sapindus powder, SOPA, detergent, emulsifier 2000 series and wetting penetrant F; and / or

[0025] The dispersant is selected from one or more of lignin sulfonates, alkylnaphthalene sulfonate formaldehyde condensates, naphthalene sulfonates, triphenylvinylphenol ethoxylate phosphates, fatty alcohol ethoxylates, alkylphenol polyoxyethylene ethers, alkylphenol polyoxyethylene ether methyl ether condensate sulfates, fatty amine polyoxyethylene ethers, glycerol fatty acid ester polyoxyethylene ethers, polycarboxylates, polyacrylates, phosphates, EO-PO block copolymers and EO-PO graft copolymers; and / or

[0026] The thickener(s) is / are selected from one or more of xanthan gum, polyvinyl alcohol, organobentonite, magnesium aluminum silicate, carboxymethyl cellulose; and / or

[0027] The disintegrant(s) is / are selected from one or more of sodium sulfate, ammonium sulfate, aluminum chloride, sodium chloride, ammonium chloride, bentonite, glucose, sucrose, starch, cellulose, urea, sodium carbonate, sodium bicarbonate, citric acid and tartaric acid; and / or

[0028] The emulsifier(s) is / are selected from one or more of fatty alcohol polyoxyethylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, phenethylphenol polyoxyethylene polyoxypropylene ether, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, alkylbenzene sulfonate, styrylphenol polyoxyethylene ether, fatty acid polyoxyethylene ester; and / or

[0029] The defoamer(s) is / are selected from one or more of silicone oil, C 10 ~C 20 saturated fatty acid compounds, C8-C 10 fatty alcohol compounds or silicone compounds; and / or

[0030] The preservative(s) is / are selected from one or more of sorbic acid, sodium sorbate, potassium sorbate, benzoic acid, sodium benzoate, sodium p-hydroxybenzoate, methyl p-hydroxybenzoate; and / or

[0031] The stabilizer(s) is / are selected from one or more of disodium hydrogen phosphate, oxalic acid, succinic acid, adipic acid, borax, 2,6-di-tert-butyl-p-cresol, epoxidized vegetable oil; and / or

[0032] The synergist(s) is / are selected from synergistic phosphorus, synergistic ether; and / or

[0033] The carrier(s) is / are selected from one or more of kaolin, bentonite, attapulgite, light calcium carbonate, diatomite, silica white; and / or

[0034] The solvent(s) is / are selected from one or more of benzene, toluene, xylene, methanol, ethanol, isopropanol, n-butanol, diesel, N,N-dimethylformamide, cyclohexanone, ethyl acetate, N-methylpyrrolidone, propanol, butanol, ethylene glycol, diethylene glycol, ethylene glycol methyl ether, butyl ether, solvent oil, vegetable oil, vegetable oil derivatives and deionized water; and / or

[0035] Further, the acaricidal composition can be prepared into a preparation dosage form permitted in agriculture, and the preparation dosage form is any one of powder, granule, sphere, tablet, strip, wettable powder, oil-dispersed powder, milk powder, water-dispersible granule, milk granule, water-dispersible tablet, soluble powder, soluble tablet, soluble granule, soluble solution, soluble sol, oil agent, film-forming oil agent, emulsifiable concentrate, latex, dispersible liquid agent, paste, water emulsion, oil emulsion, microemulsion, lipid suspension agent, microcapsule suspension agent, oil suspension agent, dispersible oil suspension agent, suspension emulsion, microcapsule suspension-suspension agent, microcapsule suspension-water emulsion or microcapsule suspension-suspension emulsion;

[0036] Furthermore, the preparation dosage form is emulsifiable concentrate, suspension agent or wettable powder.

[0037] The present invention also discloses the use of the acaricidal composition as described above for controlling plant pest mites;

[0038] The plant pest mites are pest mites of Tetranychidae and Eriophyidae.

[0039] Further, the plant pest mites are pest mites of Tetranychidae and / or Eriophyidae, the pest mites of Tetranychidae are Tetranychus cinnabarinus, Tetranychus urticae, Tetranychus truncatus, Panonychus citri or cotton red spider, and the pest mites of Eriophyidae are Phyllocoptruta oleivora and / or Aceria pallida;

[0040] Furthermore, the pest mites of Tetranychidae are Tetranychus cinnabarinus, Tetranychus urticae, Tetranychus truncatus, and the pest mites of Eriophyidae are Aceria pallida;

[0041] Further, the plant is an economic crop and / or a food crop.

[0042] Further, the acaricidal composition as described above or its preparation is applied to pest mites and their growth medium in an effective dose.

[0043] Advantages of the present invention:

[0044] 1) The acaricidal composition of the present invention rationally combines agents with different action mechanisms, has excellent control effects on plant pest mites such as Tetranychidae and Eriophyidae, has good quick-acting property and long-lasting effect, and can effectively control the generation and development of pest mite resistance;

[0045] 2) The acaricidal composition of the present invention is safe for natural enemies and beneficial mites, has no phytotoxicity to target crops, and is safe for the environment. Specific embodiments

[0046] In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below with reference to embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0047] Formulation Preparation Examples:

[0048] Preparation Example 1: 24% nicofluprole·pyflubumide EC (5:1)

[0049] Formulation: By weight percentage, 20% nicofluprole, 4% pyflubumide, 20% N-methylpyrrolidone, 10% triphenylvinylphenol polyoxyethylene ether, 1% calcium dodecylbenzenesulfonate, 7% DMF, and trimethylbenzene to make up the balance.

[0050] Preparation method: According to the formulation ratio, add the active ingredient, solvent, and co-solvent to a blending kettle and stir to dissolve. Then add the emulsifier and make up the balance with the remaining solvent. Stir evenly in the stirring kettle, and filter to obtain the required EC.

[0051] Preparation Example 2: 21% nicofluprole·flupentiofenox EC (2:1)

[0052] Formulation: By weight percentage, 14% nicofluprole, 7% flupentiofenox, 15% block polyether, 12% acetophenone, 10% ethylene carbonate, 2% calcium dodecylbenzenesulfonate, and xylene to make up the balance.

[0053] Preparation method: The same as Preparation Example 1.

[0054] Preparation Example 3: 24% nicofluprole·pyflubumide SC (1:1)

[0055] Formulation: By weight percentage, 12% pyflubumide, 12% nicofluprole, 2% sodium dodecyl sulfate, 2% alkylaryl polyoxyethylene polyoxypropylene ether, 3% triphenylvinylphenol ethoxylate phosphate, 1% sodium polycarboxylate, 0.2% xanthan gum, 1% magnesium aluminum silicate, 4% propylene glycol, 0.01% potassium benzisothiazolinone, 0.5% silicone oil, and deionized water to make up the balance.

[0056] Preparation method: According to the formulation ratio, place pyflubumide, nicofluprole, surfactant, and other functional additives in a reaction kettle in sequence, add water and mix evenly. After high-speed shearing and wet grinding, finally homogenize and filter to obtain the SC product.

[0057] Preparation Example 4: 20% nicofluprole·flupentiofenox SC (1:1)

[0058] Formulation: By weight percentage, 10% flupentiofenox, 10% nicofluprole, 1% naphthalene sulfonate formaldehyde condensate, 1% sodium dodecylbenzenesulfonate, 1% isomeric tridecyl alcohol polyoxyethylene ether, 2% alkylaryl polyoxyethylene ether polyoxypropylene ether, 3% alkylphenol polyoxyethylene ether methyl ether condensate sulfate, 0.2% xanthan gum, 1% magnesium aluminum silicate, 4% propylene glycol, 0.01% potassium benzisothiazolinone, 0.5% silicone oil, deionized water to make up the balance;

[0059] Preparation method: The same as Preparation Example 3.

[0060] Preparation Example 5: 30% nicofluprole·pyflubumide wettable powder (1:3)

[0061] Formulation: By weight percentage, 7.5% pyflubumide, 22.5% nicofluprole, 5% sodium lignosulfonate, 5% naphthalene sulfonate formaldehyde condensate, 1% Nekal BX, kaolin to make up the balance.

[0062] Preparation method: According to the formulation ratio, mix the active ingredients, dispersant, wetting agent and filler, stir evenly in a stirring kettle, and pulverize and mix evenly for multiple times by an air flow pulverizer to obtain the wettable powder of the composition of the present invention.

[0063] Preparation Example 6: 40% nicofluprole·flupentiofenox wettable powder (1:3)

[0064] Formulation: By weight percentage, 10% nicofluprole, 30% flupentiofenox, 8% naphthalene sulfonate formaldehyde condensate, 2% polycarboxylate sodium salt, 3% sodium dodecyl sulfate, 4% sodium sulfate, kaolin to make up the balance.

[0065] Preparation method: The same as Preparation Example 5.

[0066] Preparation Example 7: 33% nicofluprole·flupentiofenox wettable powder (1:2)

[0067] Formulation: By weight percentage, 11% nicofluprole, 22% flupentiofenox, 10% sodium lignosulfonate, 2% polycarboxylate sodium salt, 2% Nekal BX, kaolin to make up the balance.

[0068] Preparation method: The same as Preparation Example 5.

[0069] Preparation Example 8: 18% nicofluprole·isocycloseram dispersible oil suspension (1:5)

[0070] Formulation: By weight percentage, 3% nicofluprole, 15% isocycloseram, 12% castor oil polyoxyethylene ether, 2% fatty alcohol polyoxyethylene ether, 2% calcium dodecylbenzenesulfonate, 2% sulfosuccinate, 1% organic bentonite, and the balance is corn oil.

[0071] Preparation method: According to the formulation ratio, the active ingredients, surfactants, and other functional auxiliaries are sequentially placed in a reaction kettle, mixed evenly with oil, subjected to high-speed shearing, wet grinding, and finally homogenized and filtered to obtain a dispersible oil suspension agent product.

[0072] Preparation Example 9: 24% nicofluprole·isocycloseram suspension (1:1)

[0073] Formulation: By weight percentage, 12% nicofluprole, 12% isocycloseram, 3% fatty alcohol polyoxyethylene ether phosphate salt, 2% naphthalene sulfonate formaldehyde condensate, 4% alkylaryl polyoxyethylene ether polypropylene ether, 0.2% xanthan gum, 1% magnesium aluminum silicate, 5% propylene glycol, 0.01% potassium benzisothiazolinone, 0.5% silicone oil, and the balance is made up with deionized water.

[0074] Preparation method: The same as Preparation Example 3.

[0075] Preparation Example 10: 30% nicofluprole·isocycloseram wettable powder (5:1)

[0076] Formulation: By weight percentage, 25% nicofluprole, 5% isocycloseram, 10% sodium polycarboxylate, 4% naphthalene sulfonate formaldehyde condensate, 2% sodium dodecyl sulfate, 3% white carbon black, 15% starch, and the balance is made up with kaolin.

[0077] Preparation method: The same as Preparation Example 5.

[0078] Indoor bioassay

[0079] Example 1: Indoor activity test of the combination of nicofluprole and pyflubumide, flupentiofenox against Tetranychus urticae

[0080] Test basis: The test refers to NY / T 1154.13-2008 "Guidelines for Pesticide Indoor Bioassay - Insecticides - Part 13: Leaf Disc Spray Method".

[0081] Test target: Tetranychus urticae Koch, select adult mites with consistent physiological states.

[0082] Test agents: The original drugs of nicofluprole, pyflubumide, and flupentiofenox were all provided by the company's R & D center.

[0083] Preparation of test materials: Choose broad bean leaves with consistent growth and no previous application of pesticides. Use a hole punch to make appropriate leaf discs. Place a wet sponge in a petri dish, put filter paper on the wet sponge, and place the punched leaf discs on the filter paper. Put 2 leaf discs in each petri dish. Transfer the target mites reared indoors onto the leaf discs, with 15 mites on each leaf disc.

[0084] Preparation of agents: Dissolve the above - mentioned original drugs with appropriate solvents. Design 5 groups of ratios according to the purpose of mixing and the activity of the agents. Prepare 5 series of mass concentration gradients for each single agent and each mixture ratio.

[0085] Test method: Adjust the pressure of the Potter spray tower to a stable state of 1.47×10 5 Pa. First, wash the spray head with acetone 2 times, and then wash it with distilled water 2 times.

[0086] Place the petri dish on the bottom plate of the Potter spray tower for spraying. The liquid spraying amount is 1 mL. After the liquid medicine has settled for 1 min, take it out. Each treatment has 4 replicates, and a treatment without the agent is set as a blank control.

[0087] Rearing and observation: Place the treated test insects under the conditions of a temperature of (25±1)°C and a photoperiod of L:D=(16:8)h for rearing and observation. Check the mortality of the test insects after 48 h, and record the total number of insects and the number of dead insects respectively.

[0088] Calculation method:

[0089] Calculate the mortality of each treatment according to the survey data. Calculate according to the following formula:

[0090]

[0091] In the formula:

[0092] P - Mortality rate, in percentage (%);

[0093] K - Represents the number of dead insects, in number;

[0094] N - Represents the total number of insects in the treatment, in number.

[0095]

[0096] In the formula:

[0097] P1 - Corrected mortality rate, in percentage (%);

[0098] P t —— Mortality rate for treatment, in percentage (%).

[0099] P0 —— Mortality rate of blank control, in percentage (%).

[0100] If the control mortality rate < 5%, no correction is required; if the control mortality rate is between 5% and 20%, correction should be made according to the corrected mortality rate formula; if the control mortality rate > 20%, the test needs to be redone.

[0101] Use the DPS statistical analysis system for analysis to obtain the virulence regression equation, correlation coefficient, and LC 50 value, and evaluate the activity of the test agent against the biological test material.

[0102] The co-toxicity coefficient (CTC value) of the mixture is calculated as follows:[[]]

[0103]

[0104] In the formula:

[0105] ATI —— Observed toxicity index of the mixture;

[0106] S —— LC 50 of the standard acaricide, in milligrams per liter (mg / L);

[0107] M —— LC 50 of the mixture, in milligrams per liter (mg / L).

[0108] TTI = TI A × P A + TI B × P B .

[0109] In the formula:

[0110] TTI —— Theoretical toxicity index of the mixture;

[0111] TI A —— Toxicity index of agent A;

[0112] P A —— Percentage content of agent A in the mixture, in percentage (%).

[0113] TI B —— Toxicity index of agent B;

[0114] P B —— Percentage content of agent B in the mixture, in percentage (%).

[0115]

[0116] In the formula:

[0117] CTC——Coefficient of co-toxicity;

[0118] ATI——Actual toxicity index of the mixture;

[0119] TTI——Theoretical toxicity index of the mixture.

[0120] When the co-toxicity coefficient CTC of the compounding is ≥120, it shows a synergistic effect; when CTC ≤ 80, it shows an antagonistic effect; when 80 < CTC < 120, it shows an additive effect. The results of the indoor test are shown in the following table:

[0121] Table 1 Results of indoor activity test on Tetranychus urticae Koch by the mixture of nicofluprole and pyflubumide

[0122]

[0123] Table 2 Results of indoor activity test on Tetranychus urticae Koch by the mixture of nicofluprole and flupentiofenox

[0124]

[0125]

[0126] The results of the indoor activity determination test show (as shown in Table 1 and Table 2) that reasonable compounding of nicofluprole with pyflubumide and flupentiofenox has a good control effect on Tetranychus urticae Koch. When the mass ratio of nicofluprole to pyflubumide is 50:1 to 1:35, the co-toxicity coefficient is greater than 120, and the combined effect shows synergism; when the mass ratio of nicofluprole to flupentiofenox is 35:1 to 1:35, the co-toxicity coefficient is greater than 120, and the combined effect shows synergism.

[0127] Example 2: Indoor activity test on Tetranychus cinnabarinus Boisduval by the mixture of nicofluprole and isocycloseram

[0128] Test basis: The test refers to NY / T 1154.13-2008 "Pesticide - Guidelines for laboratory bioassays - Part 13: Leaf disc spraying method for insecticides" and NY / T 1154.7-2008 "Pesticide - Guidelines for laboratory bioassays - Part 7: Determination of combined effects of mixtures".

[0129] Test target: Tetranychus cinnabarinus Boisduval, select adult mites with consistent physiological states.

[0130] Test agents: nicofluprole technical and isocycloseram technical, which are provided by the company's R & D center.

[0131] Test materials: Select kidney bean leaves that have not been treated with any agents. Place a sponge block in a petri dish for moisturizing, place a filter paper on the sponge block, and place the kidney bean leaves punched with a puncher on the filter paper. Inoculate the test insects onto the leaves, with 30 insects per treatment.

[0132] Agent preparation: After dissolving the technical agent with a solvent, dilute it with distilled water containing 0.1% Tween 80 to prepare single-agent mother liquors respectively, and design a reasonable ratio according to the purpose of mixing and the activity of the agent. Each treatment is prepared with a series of mass concentrations required by the equal ratio method.

[0133] Agent treatment: Set the spray pressure of the Potter spray tower to a stable state of 1.47×10 5 Pa. Wash the spray head twice with acetone first, and then twice with distilled water. Place the petri dish on the Potter spray tower chassis for spraying, with a spray volume of 1 mL. Take it out after the liquid has settled for 1 min and transfer it to the feeding conditions for feeding. Each treatment has 4 replicates, and a treatment without the agent is set as a blank control.

[0134] Feeding and observation: Place the test insects of each treatment under suitable conditions for feeding and observation.

[0135] Data statistics and analysis: Check the death situation of the test insects 48 h after treatment, and record the total number of insects and the number of dead insects respectively.

[0136] According to the survey data, calculate the corrected mortality rate of each treatment. Calculate according to formulas (1) and (2), and keep the calculation results to two decimal places:

[0137]

[0138] In the formula:

[0139] P——Mortality rate, in percentage (%);

[0140] K——Represents the number of dead insects, in number;

[0141] N——Represents the total number of insects in the treatment, in number.

[0142]

[0143] In the formula:

[0144] P1——Corrected mortality rate, in percentage (%);

[0145] P t——Treatment mortality rate, expressed as percentage (%);

[0146] P0——blank control mortality rate, in percentage (%).

[0147] If the control mortality rate is less than 5%, no correction is required; if the control mortality rate is between 5% and 20%, correction should be made according to formula (2); if the control mortality rate is greater than 20%, the test needs to be repeated.

[0148] The data were processed by probability value analysis. The DPS statistical analysis system was used to obtain the toxicity regression equation, LC 50 Value, to evaluate the activity of the test agent on the biological test material.

[0149] The co-toxicity coefficient (CTC value) of the mixture is calculated according to formula (3), formula (4) and formula (5):

[0150]

[0151] Where:

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

[0153] S——LC of standard acaricide 50 , the unit is milligrams per liter (mg / L);

[0154] M——LC of the mixture 50 , the unit is milligrams per liter (mg / L).

[0155] TTI=TI A *P A +TI B *P B ·······(4)

[0156] Where:

[0157] TTI – Theoretical Toxicity Index of Mixtures;

[0158] TI A ——A: toxicity index of the agent;

[0159] P A ——The percentage of agent A in the mixture, in percentage (%);

[0160] TI B ——Toxicity index of agent B;

[0161] P B ——The percentage of agent B in the mixture, in percentage (%).

[0162]

[0163] In the formula:

[0164] CTC——coefficient of co-toxicity;

[0165] ATI——actual toxicity index of the mixture;

[0166] TTI——theoretical toxicity index of the mixture.

[0167] When the coefficient of co-toxicity CTC of the compounding is ≥ 120, it shows a synergistic effect; when CTC ≤ 80, it shows an antagonistic effect; when 80 < CTC < 120, it shows an additive effect.

[0168] The results of the indoor bioactivity test are shown in the following table:

[0169] Table 3 Results of the indoor activity test of the compound of nicofluprole and isocycloseram against Tetranychus cinnabarinus

[0170]

[0171] As shown by the results of the indoor activity determination test (Table 3), when nicofluprole and isocycloseram are rationally compounded at a mass ratio of 50:1 to 1:45, the coefficient of co-toxicity is greater than 120, and the combined effect shows a synergistic effect.

[0172] Example 3: Results of the indoor activity test of the compound of nicofluprole and flupentiofenox, pyflubumide or isocycloseram against Aceria pallida

[0173] Test basis: The test refers to NY / T 1154.13-2008 "Pesticide indoor bioassay test guidelines Insecticides Part 13: Leaf disc spray method" and NY / T 1154.7-2008 "Pesticide indoor bioassay test guidelines Insecticides Part 7: Determination of combined effects of mixtures".

[0174] Test target: Aceria pallida Keifer, select adult mites with consistent physiological states.

[0175] Test agents: nicofluprole technical, pyflubumide technical, flupentiofenox technical, isocycloseram technical, all provided by the company's R & D center.

[0176] Instrument and equipment: microscope, puncher, sponge block, culture dish, Potter spray tower, constant temperature incubator.

[0177] Preparation of test materials: Select wolfberry leaves that have grown uniformly and have not been treated with any pesticides. Place a sponge block in a petri dish for moisture retention, place a filter paper on it, and place wolfberry leaves on the filter paper. Inoculate adult mites raised indoors onto the leaves, with 30 mites per dish.

[0178] Preparation of pesticides: After dissolving the original pesticides with solvents respectively, dilute them with 0.1% Tween 80 aqueous solution. Prepare single-agent mother liquors respectively, and design reasonable ratios according to the purpose of mixing and the activity of pesticides. Prepare the required series of mass concentrations for each single agent and the mixed agents of each group ratio according to the method of geometric progression.

[0179] Pesticide treatment: The spray pressure of the Potter spray tower is in a stable state of 1.47×10 5 Pa. First, wash the spray head twice with acetone, and then wash it twice with distilled water.

[0180] Place the petri dish on the chassis of the Potter spray tower for spraying. The liquid spraying amount is 1 mL. After the liquid medicine has settled for 1 minute, take it out and transfer it to normal feeding conditions for feeding.

[0181] Each treatment has 4 replicates, and a treatment without pesticides is set as a blank control.

[0182] Data statistics and analysis: Check the death situation of test insects 48 hours after treatment, and record the total number of insects and the number of dead insects respectively.

[0183] According to the survey data, calculate the corrected mortality of each treatment. Calculate according to formulas (1) and (2), and keep the calculation results to two decimal places:

[0184]

[0185] In the formula:

[0186] P——Mortality rate, unit: percentage (%)

[0187] K——Represents the number of dead insects, unit: head

[0188] N——Represents the total number of insects in the treatment, unit: head

[0189]

[0190] In the formula:

[0191] P1——Corrected mortality rate, unit: percentage (%)

[0192] P t ——Treatment mortality rate, unit: percentage (%)

[0193] P0——Mortality rate of blank control, unit: percentage (%)

[0194] If the control mortality rate < 5%, no correction is required; if the control mortality rate is between 5% and 20%, correction should be made according to formula (2); if the control mortality rate > 20%, the test needs to be redone.

[0195] The data was processed using the probit analysis method. Analyzed with the DPS statistical analysis system to obtain the virulence regression equation and LC 50 value to evaluate the activity of the test agent against the biological test material.

[0196] The co-toxicity coefficient (CTC value) of the mixture is calculated according to formulas (3), (4), and (5):

[0197]

[0198] Where:

[0199] ATI - Measured virulence index of the mixture;

[0200] S - LC of the standard acaricide 50 , in milligrams per liter (mg / L);

[0201] M - LC of the mixture 50 , in milligrams per liter (mg / L).

[0202] TTI = TI A *P A +TI B *P B ·······(4)

[0203] Where:

[0204] TTI - Theoretical virulence index of the mixture;

[0205] TI A - Virulence index of agent A;

[0206] P A - Percentage content of agent A in the mixture, in percentage (%);

[0207] TI B - Virulence index of agent B;

[0208] P B - Percentage content of agent B in the mixture, in percentage (%).

[0209]

[0210] Where:

[0211] CTC - Co-toxicity coefficient;

[0212] ATI - Measured virulence index of the mixture;

[0213] TTI - Theoretical toxicity index of the mixture.

[0214] When the co - toxicity coefficient CTC of the mixture is ≥ 120, it shows a synergistic effect; when CTC ≤ 80, it shows an antagonistic effect; when 80 < CTC < 120, it shows an additive effect. The results of indoor bioactivity tests are shown in the following table:

[0215] Table 4 Results of indoor activity tests of the mixture of pyflubumide and nicofluprole against Aceria pallida

[0216]

[0217] Table 5 Results of indoor activity tests of the mixture of nicofluprole and flupentiofenox against Aceria pallida

[0218]

[0219] Table 6 Results of indoor activity tests of the mixture of nicofluprole and isocycloseram against Aceria pallida

[0220]

[0221] The results of indoor activity determination tests (as shown in Table 4 and Table 5) show that reasonable mixtures of nicofluprole with pyflubumide, flupentiofenox, and isocycloseram have good control effects against Tetranychus urticae. The mass ratio of nicofluprole to pyflubumide is 25:1 - 1:30, the co - toxicity coefficient is greater than 120, and the combined effect shows synergism; the mass ratio of nicofluprole to flupentiofenox is 35:1 - 1:30, the co - toxicity coefficient is greater than 120, and the combined effect shows synergism; the mass ratio of nicofluprole to isocycloseram is 45:1 - 1:30, the co - toxicity coefficient is greater than 120, and the combined effect shows synergism.

[0222] Field efficacy control test

[0223] Example 3: Field efficacy control test of the mixture of nicofluprole with pyflubumide and flupentiofenox against Tetranychus

[0224] Test basis: The test refers to GB / T 17980.17 - 2000 "Pesticide field efficacy test guidelines (I) Acaricides for controlling Tetranychus on legumes and vegetables".

[0225] Test target: Tetranychus

[0226] Test crop: Cowpea (Lvfengjin 99).

[0227] Test site: The test was carried out in the cowpea planting area of Xuejiacun, Liuzhen, Shouguang District, Weifang City. The test field was sandy loam with medium to high fertility and relatively uniform management level.

[0228] Test design: The test was arranged in a randomized block design, with each treatment replicated 4 times and each plot being 30m 2 . Pesticide application was carried out at the initial stage of spider mite occurrence. The spider mites were a mixed population of Tetranychus cinnabarinus Boisduval, Tetranychus urticae Koch, and Tetranychus truncates Ehara, with Tetranychus urticae Koch being the dominant species. During pesticide application, it was ensured to be even and thorough so that both the front and back sides of the cowpea plant leaves and the stems were evenly covered with the pesticide. The test was carried out with a total of 1 pesticide application.

[0229] Investigation method: The initial mite population was investigated before pesticide application, and investigations were carried out 3 days and 14 days after pesticide application. When investigating, 20 leaves were fixed and taken from each plot to count the number of live mites.

[0230] Calculation method of control efficacy:

[0231]

[0232] The results of the field efficacy test are shown in the following table:

[0233] Table 7 Field efficacy control test results of the combination of nicofluprole with pyflubumide, flupentiofenox, and isocycloseram against spider mites

[0234]

[0235] It can be seen from the results of field efficacy tests that the compounding of nicofluprole with pyflubumide and flupentiofenox showed good acaricidal effects. 3 days after application, the overall control efficacy of each compound preparation was above 80%, showing good quick-acting properties. 14 days after application, the control efficacies of 20% nicofluprole·flupentiofenox suspension concentrate (1:1), 24% nicofluprole·pyflubumide emulsifiable concentrate (5:1), and 18% nicofluprole·isocycloseram dispersible oil suspension concentrate (1:5) against spider mites reached 94.41%, 90.84%, and 92.64% respectively. Thus, it can be seen that the acaricidal composition of the present invention can comprehensively control various spider mites such as Tetranychus cinnabarinus, Tetranychus urticae, and Tetranychus truncatus, is safe for target crops, has good quick-acting properties and long-lasting efficacy, and can be widely applied to the control of phytophagous spider mites in the field.

[0236] Example 4: Field efficacy control test of Aceria pallida Keifer

[0237] Test crop: Lycium barbarum (Ningqi No. 1).

[0238] Test object: Aceria pallida Keifer.

[0239] Test site: The test was carried out in a Lycium barbarum planting base in Xixia District, Yinchuan City, Ningxia in July 2020. The test field was irrigated and silty soil with medium soil fertility, flat terrain, uniform fertility, and good irrigation conditions. The management level of the test field was relatively high, and the management conditions of each test plot were uniform. The Lycium barbarum in the test field was 5-year-old, and the planting density was 3000 plants / hm 2 。

[0240] Test design: A total of 8 treatments were designed in the test, with each treatment replicated 4 times. The test plots were arranged in a randomized block design, and the area of each plot was 30m 2 。The test was applied with pesticides once on July 5, 2020. First, the control was sprayed, and then the pesticides were sprayed in sequence from low concentration to high concentration, with uniform and even spraying. When changing different pesticides, the sprayer was cleaned three times first.

[0241] Test investigation: The test was investigated 3 days, 7 days, and 15 days after application. During the investigation, 5-point sampling was adopted. At each point, 1 plant was randomly investigated. On each plant, 1 new branch was randomly selected and marked at 5 positions: east, south, west, north, and middle. During the investigation, 3 leaves were taken from the front, middle, and rear sections of each branch to investigate the number of surviving gall mites on the fixed sample branches, and the control efficacy was calculated.

[0242] Calculation method of control efficacy:

[0243]

[0244] Investigation method for safety evaluation:

[0245] The experiment investigated the presence of phytotoxicity and phytotoxicity symptoms in the leaves, flowers, and fruits of Lycium barbarum plants 30 days after application of the drug. For each plant, one branch with a length of no less than 50 cm was selected from the east, south, west, north, and middle to investigate all the leaves, flowers, and fruits.

[0246] Phytotoxicity grading standard:

[0247] - No phytotoxicity;

[0248] + Slight phytotoxicity, which does not affect the normal growth of leaves, flowers, and fruits;

[0249] ++ Obvious phytotoxicity, which can be restored;

[0250] +++ High phytotoxicity, which affects the normal growth of leaves, flowers, and fruits;

[0251] ++++ Severe phytotoxicity, which inhibits the growth of leaves, flowers, and fruits.

[0252] Table 8 Field efficacy control test of the combination of nicofluprole and isocycloseram, pyflubumide, or flupentiofenox against Aceria pallida Keifer on Lycium barbarum

[0253]

[0254] Table 9 Safety test of the combination of pyflubumide and nicofluprole on Lycium barbarum

[0255]

[0256] During the above-mentioned field trials, irregular observations were carried out. At the tested concentrations, the acaricidal composition of the present invention did not have any adverse effects on Lycium barbarum plants and was safe for predatory mites.

[0257] In summary, through indoor bioactivity tests and field trials, the acaricidal composition of the present invention has significant efficacy against spider mites and gall mites, good quick-acting property, long-lasting effect, and is safe for natural enemies and beneficial mites, has no phytotoxicity to target crops, and is safe for crops.

[0258] Although the present invention has been described in detail with general descriptions and specific embodiments above, based on the present invention, some modifications or improvements can be made, which are obvious to those skilled in the art. Therefore, these modifications or improvements made without departing from the spirit of the present invention all fall within the scope of protection required by the present invention.

Claims

1. A miticidal composition, characterized in that, The described acaricidal composition comprises active ingredient A and active ingredient B. The active ingredient A is nicofluprole, and the active ingredient B is isocycloseram. The mass ratio of active ingredient A to active ingredient B is 50:1 to 1:

45.

2. The acaricidal composition according to claim 1, characterized in that, The mass ratio of active ingredient A to active ingredient B is 45:1 to 1:

35.

3. The acaricidal composition according to claim 2, characterized in that, The mass ratio of active ingredient A to active ingredient B is 35:1 to 1:

30.

4. The acaricidal composition according to claim 1, characterized in that, Taking the total weight of the described acaricidal composition as 100 wt%, the total weight of active ingredient A and active ingredient B accounts for 1 wt% - 80 wt% of the total weight of the acaricidal composition, preferably 1 wt% - 70 wt%.

5. The acaricidal composition according to claim 1, characterized in that, In addition to the active ingredients, the described acaricidal composition also includes agriculturally acceptable auxiliary ingredients, which are selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreezing agents, defoaming agents, solvents, preservatives, stabilizers, synergists or carriers.

6. The acaricidal composition according to claim 1, characterized in that, The described acaricidal composition can be prepared into agriculturally acceptable formulation forms, and the formulation forms are any one of powders, granules, balls, tablets, strips, wettable powders, oil-dispersed powders, milk powders, water-dispersible granules, milk granules, water-dispersible tablets, soluble powders, soluble tablets, soluble granules, soluble solutions, soluble sols, oils, film-forming oils, emulsifiable concentrates, latexes, dispersible liquid formulations, ointments, water-in-oil emulsions, oil-in-water emulsions, microemulsions, lipid suspensions, microcapsule suspensions, oil suspensions, dispersible oil suspensions, suspension emulsions, microcapsule suspension-suspensions, microcapsule suspension-water-in-oil emulsions or microcapsule suspension-suspension emulsions.

7. The acaricidal composition according to claim 6, characterized in that, The formulation form is an emulsifiable concentrate, a suspension or a wettable powder.

8. Use of the acaricidal composition according to any one of claims 1 - 7 for controlling phytophagous mites.

9. The use according to claim 8, wherein The phytophagous mites are mites of the family Tetranychidae and / or eriophyid mites. The mites of the family Tetranychidae are Tetranychus cinnabarinus, Tetranychus urticae, Tetranychus truncatus, Panonychus citri or Tetranychus cinnabarinus Boisduval; the eriophyid mites are Phyllocoptruta oleivora and / or Aceria pallida. Preferably, the mites of the family Tetranychidae are Tetranychus cinnabarinus, Tetranychus urticae, Tetranychus truncatus, and the eriophyid mite is Aceria pallida.

10. The use according to claim 8, characterized in that, The described acaricidal composition is applied to mites and their growth media at an effective dose.