Acaricidal composition and application thereof

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.

Description

[0001] This divisional application of the present invention has the application number 202310904130.7, the filing 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 Lepidoptera pests such as Plutella xylostella and Mythimna separata, Hemiptera pest Myzus persicae, and Acarina pests. Its structural formula is shown as follows:

[0004]

[0005] Pyflubumide is a formanilide miticide 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 pest 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 Kumi Chemical Co., Ltd. of Japan, and is applicable to controlling 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. The damaged leaves show small grayish-white dots. When the damage is severe, adult mites and nymphs can damage all parts of the plant above the ground, 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 various 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 then 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. 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 properties, a long-lasting effect, is harmless to natural enemies and beneficial mites, is safe for crops, and does not cause phytotoxicity.

[0014] To achieve the above purpose, the present invention adopts the following technical solution: A miticidal composition, the miticidal composition contains active ingredient A and active ingredient B, the active ingredient A is nicofluprole, the active ingredient B is any one of pyflubumide, flupentiofenox or isocycloseram, and 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 alkyl benzene sulfonates, alkyl naphthalene 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, sophora powder, sapindus powder, SOPA, detergents, emulsifier 2000 series and wetting penetrant F; and / or

[0025] The dispersant is selected from one or more of lignin sulfonates, alkyl naphthalene 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) selected from one or more of xanthan gum, polyvinyl alcohol, organobentonite, magnesium aluminum silicate, carboxymethyl cellulose; and / or

[0027] The disintegrant(s) 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) selected from one or more of fatty alcohol polyoxyethylene ether, fatty alcohol ethylene oxide - propylene oxide copolymer, phenethylphenol polyoxyethylene polypropylene ether, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, alkylbenzene sulfonate, styrylphenol polyoxyethylene ether, fatty acid polyoxyethylene ester; and / or

[0029] The defoamer(s) selected from one or more of silicone oil, C 10 ~C 20 saturated fatty acid compounds, C 8 ~C 10 fatty alcohol compounds or silicone compounds; and / or

[0030] The preservative(s) 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) 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) selected from synergistic phosphorus, synergistic ether; and / or

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

[0034] The solvent(s) 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 naphtha, vegetable oil, vegetable oil derivatives and deionized water; and / or

[0035] Furthermore, 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, ball, 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, microcapsule suspension, oil suspension, dispersible oil suspension, 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] Furthermore, 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 Tetranychus cinnabarinus Boisduval, 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] Furthermore, the plant is an economic crop and / or a food crop.

[0042] Furthermore, 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 reasonably combines agents with different action mechanisms, has excellent control effects on plant pest mites such as Tetranychus 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% triphenylethylene phenol 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 cosolvent to a blending kettle and stir to dissolve them. 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% triphenylethylene phenol 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 auxiliaries 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 dodecyl benzene sulfonate, 1% isomeric tridecyl alcohol polyoxyethylene ether, 2% alkyl aryl polyoxyethylene ether polyoxypropylene ether, 3% sulfate of alkyl phenol polyoxyethylene ether methyl ether condensate, 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 many times by an air stream pulverizer to prepare 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% sodium polycarboxylate, 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% sodium polycarboxylate, 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% succinate sulfonate, 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 the 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 oxide 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 Tests 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 pest mites reared indoors onto the leaf discs, with 15 mites on each leaf disc.

[0084] Preparation of agents: Dissolve the above 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, clean the spray head with acetone 2 times, and then clean it with distilled water 2 times.

[0086] 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 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] P 1 - Corrected mortality rate, in percentage (%);

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

[0099] P 0 —— Mortality rate of blank control, in percentage (%).

[0100] If the control mortality rate < 5%, no correction is needed; 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 to evaluate the activity of the test agent against the biological test materials.

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

[0103]

[0104] Where:

[0105] ATI - Measured virulence 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] Where:

[0110] TTI - Theoretical virulence index of the mixture;

[0111] TI A - Virulence index of agent A;

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

[0113] TI B - Virulence 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 combined toxicity;

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

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

[0120] When the coefficient of combined toxicity 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 the indoor test are shown in the following table:

[0121] Table 1 Results of indoor bioassay of the mixture of nicofluprole and pyflubumide against Tetranychus urticae

[0122]

[0123] Table 2 Results of indoor bioassay of the mixture of nicofluprole and flupentiofenox against Tetranychus urticae

[0124]

[0125]

[0126] The results of the indoor bioassay (as shown in Table 1 and Table 2) show that reasonable mixtures of nicofluprole with pyflubumide and flupentiofenox have good control effects against Tetranychus urticae. When the mass ratio of nicofluprole to pyflubumide is 50:1 to 1:35, the coefficient of combined toxicity is greater than 120, and the combined effect shows a synergistic effect; when the mass ratio of nicofluprole to flupentiofenox is 35:1 to 1:35, the coefficient of combined toxicity is greater than 120, and the combined effect shows a synergistic effect.

[0127] Example 2: Indoor bioassay of the mixture of nicofluprole and isocycloseram against Tetranychus cinnabarinus

[0128] Test basis: The test was carried out with reference to NY / T 1154.13-2008 "Pesticide bioassay in the laboratory - Part 13: Leaf disc spraying method for insecticides" and NY / T 1154.7-2008 "Pesticide bioassay in the laboratory - Part 7: Determination of combined effects of mixtures".

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

[0130] Test agents: the original nicofluprole drug and the original isocycloseram drug. The above original drugs 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 original drug 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 agents. Each treatment is prepared with the required series of mass concentrations by the method of geometric progression.

[0133] Agent treatment: Set the spray pressure of the Potter spray tower to a stable state of 1.47×10 5 Pa. First, wash the spray head with acetone twice, and then wash it with distilled water twice. 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 and transfer it to be raised under the feeding conditions. Each treatment has 4 replicates, and a treatment without the agent is set as a blank control.

[0134] Feeding and observation: Raise and observe the test insects of each treatment under suitable conditions.

[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 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 treated insects, in number.

[0142]

[0143] In the formula:

[0144] P 1 ——Corrected mortality rate, in percentage (%);

[0145] P t —— Mortality rate, in percentage (%);

[0146] P 0 —— Mortality rate of the blank control, in percentage (%).

[0147] 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.

[0148] Use the probit analysis method to process the data. Analyze with the DPS statistical analysis system to obtain the toxicity regression equation and LC 50 value, and 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 formulas (3), (4), and (5):

[0150]

[0151] In the formulas:

[0152] ATI——Actual toxicity index of the mixture;

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

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

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

[0156] In the formulas:

[0157] TTI——Theoretical toxicity index of the mixture;

[0158] TI A ——Toxicity index of agent A;

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

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

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

[0162]

[0163] In the formula:

[0164] CTC - Co - toxicity coefficient;

[0165] ATI - Measured toxicity index of the mixture;

[0166] TTI - Theoretical toxicity index of the mixture.

[0167] 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.

[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 mixture of nicofluprole and isocycloseram against Tetranychus cinnabarinus

[0170]

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

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

[0173] Test basis: The test refers to NY / T 1154.13 - 2008 "Pesticide - Bioassay in the Laboratory - Part 13: Leaf - disc Spray Method for Insecticides" and NY / T 1154.7 - 2008 "Pesticide - Bioassay in the Laboratory - Part 7: Determination of the Combined Action of Mixed Pesticides".

[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 moisturizing, 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. Configure the required series of mass concentrations for each single agent and each group of mixed agents according to the equal-ratio method.

[0179] Pesticide treatment: The spray pressure of the Potter spray tower is in a stable state of 1.47×10 5 Pa. Wash the spray head twice with acetone first, and then 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 min, 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 h 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, unit: percentage (%);

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

[0188] N——Represents the total number of treated insects, unit: head.

[0189]

[0190] In the formula:

[0191] P 1 ——Corrected mortality, unit: percentage (%);

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

[0193] P 0——Blank control mortality rate, in 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 is processed by the probit analysis method. Analyzed using 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——Actual toxicity 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 toxicity index of the mixture;

[0205] TI A ——Toxicity index of agent A;

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

[0207] TI B ——Toxicity 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 - Actual toxicity index of the mixture;

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

[0214] When the co - toxicity coefficient CTC of the compounding ≥ 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 bioactivity test are shown in the following table:

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

[0216]

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

[0218]

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

[0220]

[0221] The results of the indoor activity determination test show (as shown in Table 4 and Table 5) that reasonable compounding of nicofluprole with pyflubumide, flupentiofenox, and isocycloseram has a good control effect on Tetranychus urticae. The mass ratio of nicofluprole to pyflubumide is 25:1 - 1:30, and 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, and 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, and 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 compound of nicofluprole with pyflubumide and flupentiofenox against Tetranychus

[0224] Basis for the test: The test was carried out with reference to GB / T 17980.17-2000 "Pesticide Field Efficacy Test Guidelines (I) Acaricides for Controlling Spider Mites on Beans and Vegetables".

[0225] Test target: Spider mites.

[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 30 m 2 . The pesticide was applied 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 that the application was 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 the investigation was carried out 3 days and 14 days after pesticide application. When investigating, 20 leaves were fixed in each plot to count the number of live mites.

[0230] Calculation method for control efficacy:

[0231]

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

[0233] Table 6 Field Efficacy Test Results of the Compound 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 combination of nicofluprole with pyflubumide and flupentiofenox showed good acaricidal effects. Three days after treatment, the overall control efficacy of each compound preparation was above 80%, showing good quick-acting properties. Fourteen days after treatment, 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 residual 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 macrodonis Keifer

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

[0238] Test object: Aceria macrodonis 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 from low concentration to high concentration in sequence, with uniform and constant-speed spraying. When changing different pesticides, the sprayer was cleaned three times.

[0241] Test investigation: The test was investigated 3 days, 7 days, and 15 days after treatment. 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 test 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 not 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 7 Field efficacy control test of the combination of nicofluprole and isocycloseram, pyflubumide, or flupentiofenox against Aceria pallida Keifer on Lycium barbarum

[0253]

[0254] Table 8 Safety test of the combination of pyflubumide and nicofluprole on Lycium barbarum

[0255]

[0256] During the above-mentioned field trials, irregular observations were made. 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 fast-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 above with general descriptions and specific embodiments, 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 of the present invention.

Claims

1. A acaricidal composition, characterized in that, the acaricidal composition comprises active ingredient A and active ingredient B, the active ingredient A is nicofluprole, the active ingredient B is flupentiofenox, and 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 35:1 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 acaricidal composition as 100 wt%, the total weight of active ingredient A and active ingredient B accounts for 1 wt% to 80 wt% of the total weight of the acaricidal composition, preferably 1 wt% to 70 wt%.

5. The acaricidal composition according to claim 1, characterized in that, in addition to the active ingredients, the acaricidal composition further comprises 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.

6. The acaricidal composition according to claim 1, characterized in that, the acaricidal composition can be prepared into agriculturally acceptable formulation dosage forms, and the formulation dosage forms are powder, granule, ball, tablet, strip, wettable powder, oil-dispersible powder, milk powder, water-dispersible granule, milk granule, water-dispersible tablet, soluble powder, soluble tablet, soluble granule, soluble solution, soluble sol, oil, film-forming oil, emulsifiable concentrate, latex, dispersible liquid, paste, water emulsion, oil emulsion, microemulsion, lipid suspension, microcapsule suspension, oil suspension, dispersible oil suspension, suspension emulsion, microcapsule suspension-suspension, microcapsule suspension-water emulsion or microcapsule suspension-suspension emulsion.

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

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

9. The use according to claim 8, characterized in that, the plant pest mites are Tetranychidae mites and / or Eriophyidae mites, the Tetranychidae mites are Tetranychus cinnabarinus, Tetranychus urticae, Tetranychus truncatus, Panonychus citri or Tetranychus cinnabarinus Boisduval, and the Eriophyidae mites are Phyllocoptruta oleivora and / or Aceria palida; preferably, the Tetranychidae mites are Tetranychus cinnabarinus, Tetranychus urticae, Tetranychus truncatus, and the Eriophyidae mites are Aceria palida.

10. The use according to claim 8, characterized in that, applying the acaricidal composition to pest mites and their growth medium at an effective dose.

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