CN116941623A - Mite-killing composition and application thereof - Google Patents

Abstract

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

Description

A kind of acaricide composition and its use

Technical field

The invention belongs to the technical field of pesticide acaricide and discloses an acaricide composition and its use.

Background technique

Nicofluprole is a new type of fluorine-containing insecticide and acaricide. The CAS registration number is: 1771741-86-6. The chemical name is N-methyl-N-cyclopropyl-2-chloro-5-[1-(2 ,6-dichloro-4-heptafluoroisopropylphenyl)-pyrazol-4-yl]nicotinamide, nicofluprole is effective against lepidopteran pests diamondback moth and armyworm, hemipteran pest myzus aphid and acarid pests It shows good insecticidal activity, and its structural formula is as follows:

Pyflubumide is a formanilide acaricide, CAS registration number: 926914-55-8, chemical name: 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 mitochondrial complex of pest mite respiratory chain The effect of substance II. Pyflubumide has a good control effect against two-spotted spider mites, citrus spider mites, apple spider mites, etc. in all growth stages, but has poor activity against tarsal line mites and gall mites. Its structural formula is as follows:

flupentiofenox, Chinese name: (trifluoromethyl)5-[2-fluoro-4-chloro-5-((2,2,2-trifluoroethyl)sulfinyl)phenoxy]pentyl sulfide, It is a new thioether-based fluorine-containing insecticide and acaricide developed by Japan Combination Chemical Company. It is suitable for controlling pests or mites in fruits, vegetables, rice, etc. Its structural formula is as follows:

Isocycloseram is an isoxazoline insecticide, acaricide, and a non-competitive inhibitor of gamma-aminobutyric acid (GABA) receptors. Its chemical name is 4-[5-(3,5-dichloro-4-fluorophenyl)-4,5-monohydro-5-(trifluoromethyl)-3-isoxazolyl]-N- (2-Ethyl-3-oxo-4-isoxazolidinyl)-2-methylbenzamide has good insecticidal activity against Lepidoptera, Hemiptera, Coleoptera and other pests . Its structural formula is as follows:

Spider mites, also known as red spiders, mainly harm crops such as melons, beans, eggplants, peppers, and fruit trees. They pierce and suck the leaves of host plants as adults or nymphs on the back of the leaves. Small gray-white spots appear on the affected leaves. When the occurrence is severe, adult mites and nymphal mites can harm various parts of the plant above ground, spin silk webs, and gather into clumps, causing the entire leaf to turn gray until the entire plant dies.

Gall mites mainly harm various economic crops such as wolfberry and citrus. Adult and nymph mites suck the juice from plant leaves, flower spikes and fruit tissues. The injured parts of young leaves first appear yellow-green patches on the back of the leaf, and the infected patches are sunken, and the injured parts are deformed to form hair galls. The host tissue in the hair galls is stimulated to produce gray-white hairs, and then the hairs gradually turn into yellow-brown and red. Brown to dark brown, with a felt-like shape, uneven surface, loss of luster, and even swelling and distortion; hyperplasia and thickening appear on the damaged parts of the leaves.

Contents of the invention

Based on the above situation, the object of the present invention is to provide an acaricidal composition and its use. The acaricidal composition has excellent control effect on spider mites and gall mites, has good quick-acting properties, has a long duration of effect, and is effective against natural enemies and Beneficial mites are harmless, safe for crops, and cause no phytotoxicity.

In order to achieve the above object, the present invention adopts the following technical solution: an acaricidal composition, the acaricidal 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, and the mass ratio of the active ingredient A to active ingredient B is 50:1 to 1:45;

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

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

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

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

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

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

Further, the total weight of the acaricidal composition is calculated as 100wt%, and the total weight of the active ingredient A and active ingredient B accounts for 1 to 80wt% of the total weight of the acaricidal composition;

Further, the total weight of the acaricidal composition is calculated as 100wt%, and the total weight of the active ingredient A and active ingredient B accounts for 1 to 70wt% of the total weight of the acaricidal composition;

Further, in addition to the active ingredients, the acaricidal composition also includes agriculturally acceptable auxiliary ingredients, and the auxiliary ingredients are selected from the group consisting of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, One or more of antifreeze, defoamers, solvents, preservatives, stabilizers, synergists or carriers;

Further, the wetting agent is selected from alkyl benzene sulfonate, alkyl naphthalene sulfonate, lignosulfonate, sodium lauryl sulfate, sodium dioctyl sulfonate succinate, α-olefin Sulfonate, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol ethoxylate, fatty alcohol ethoxylate, fatty alcohol polyoxyethylene ether sodium sulfate, silkworm excrement, saponin powder, One or more of soapberry powder, SOPA, detergent, emulsifier 2000 series and wetting penetrant F; and/or

The dispersant is selected from lignin sulfonate, alkyl naphthalene sulfonate formaldehyde condensate, naphthalene sulfonate, tristyrylphenol ethoxylate phosphate, fatty alcohol ethoxylate, alkylphenol Polyoxyethylene ether, alkylphenol polyoxyethylene ether methyl ether condensate sulfate, fatty amine polyoxyethylene ether, glycerin fatty acid ester polyoxyethylene ether, polycarboxylates, polyacrylic acid, phosphates, EO - one or more of PO block copolymer and EO-PO graft copolymer; and/or

The thickener is selected from one or more types of xanthan gum, polyvinyl alcohol, organic bentonite, magnesium aluminum silicate, and carboxymethyl cellulose; and/or

The disintegrant is selected from 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 one or more of; and/or

The emulsifier is selected from fatty alcohol polyoxyethylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, phenethylphenol polyoxyethylene polyoxypropylene ether, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene. One or more of oxyethylene ether, alkyl benzene sulfonate, styrylphenol polyoxyethylene ether, fatty acid polyoxyethylene ester; and/or

The defoaming agent is selected from one or more of silicone oil, C ₁₀ to C ₂₀ saturated fatty acid compounds, C ₈ to C ₁₀ fatty alcohol compounds or silicone compounds; and/or

The preservative is selected from one or more of sorbic acid, sorbic acid sodium salt, sorbic acid potassium salt, benzoic acid, benzoic acid sodium salt, parahydroxybenzoic acid sodium salt, and methyl parahydroxybenzoate; and/or

The stabilizer is 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

The synergist is selected from synergist phosphorus and synergist ether; and/or

The carrier is selected from one or more types of kaolin, bentonite, attapulgite, light calcium carbonate, diatomite, and white carbon black; and/or

The solvent is selected from benzene, toluene, xylene, methanol, ethanol, isopropanol, n-butanol, diesel, N,N-dimethylformamide, cyclohexanone, ethyl acetate, N-methylpyrrolidone, One or more of propanol, butanol, ethylene glycol, diethylene glycol, ethylene glycol methyl ether, butyl ether, mineral spirits, vegetable oil, vegetable oil derivatives and deionized water; and/or

Further, the acaricidal composition can be prepared into agriculturally acceptable preparations, and the preparations are powders, granules, pellets, tablets, strips, wettable powders, oil-dispersible powders, and milk powders. , water-dispersible granules, emulsions, water-dispersible tablets, soluble powders, soluble tablets, soluble granules, soluble agents, soluble gels, oils, film-spreading oils, emulsifiable concentrates, latex, dispersible liquids agent, ointment, aqueous emulsion, oil emulsion, microemulsion, lipid suspension, microencapsulated suspension, oil suspension, dispersible oil suspension, suspoemulsion, microencapsulated suspension-suspension, microencapsulated suspension-aqueous emulsion or Any of microencapsulated suspensions and suspoemulsions;

Furthermore, the preparation dosage form is emulsifiable concentrate, suspension or wettable powder.

The present invention also discloses the use of the acaricidal composition as described above for preventing and controlling plant pest mites;

The plant pest mites are pest mites of the family Tetranychus and gall mites.

Further, the plant pest mites are spider mites and/or gall mites, and the spider mites are cinnabar spider mites, two-spotted spider mites, truncated spider mites, citrus panonychus or cotton red mites. Spiders, the gall mite pests are citrus rust ticks and/or wolfberry gall mites;

Furthermore, the pest mites belonging to the family Tetranychus are Tetranychus cinnabar, Tetranychus two-spotted, and Tetranychus truncatula, and the pest mites from the family Gallidae are Lycium barbarum gall mites;

Further, the plants are cash crops and/or food crops.

Further, the acaricidal composition or preparation thereof as described above is applied to the harmful mites and their growth medium at an effective dose.

Beneficial effects of the present invention:

1) The acaricidal composition of the present invention rationally combines agents with different mechanisms of action, and has excellent control effects on plant harmful mites such as spider mites and gall mites. It has good quick-acting properties and a long duration of effect, and can effectively control harmful mites. The emergence and development of drug resistance;

2) The acaricidal composition of the present invention is safe to natural enemies and beneficial mites, causes no phytotoxicity to target crops, and is safe to the environment.

Detailed ways

In order to make the purpose, technical solutions and advantages of the present invention more clear, the present invention will be further described in detail below in conjunction with the embodiments. It should be understood that the specific embodiments described here are only used to explain the present invention and are not intended to limit the present invention.

Preparation example:

Preparation Example 1: 24% nicofluprole·pyflubumide emulsifiable concentrate (5:1)

Formula: by weight, 20% nicofluprole, 4% pyflubumide, 20% N-methylpyrrolidone, 10% tristyrylphenol polyoxyethylene ether, 1% calcium dodecylbenzene sulfonate, 7% DMF, Trimethylbenzene makes up the balance.

Preparation method: According to the formula proportion, add the active ingredients, solvents and co-solvents to the mixing kettle and stir to dissolve, then add the emulsifier, use the remaining solvent to make up the balance, stir evenly in the mixing kettle, and filter to obtain the desired product. Cream.

Preparation Example 2: 21% nicofluprole·flupentiofenox emulsifiable concentrate (2:1)

Formula: By weight, 14% nicofluprole, 7% flupentiofenox, 15% block polyether, 12% acetophenone, 10% ethylene carbonate, 2% calcium dodecylbenzene sulfonate, and xylene make up the balance .

Preparation method: Same as Preparation Example 1.

Preparation Example 3: 24%·nicofluprole·pyflubumide suspension (1:1)

Formula: By weight, 12% pyflubumide, 12% nicofluprole, 2% sodium lauryl sulfate, 2% alkylaryl polyoxyethylene ether polyoxypropylene ether, 3% tristyrylphenol ethoxylate Phosphate ester, 1% polycarboxylate sodium salt, 0.2% xanthan gum, 1% magnesium aluminum silicate, 4% propylene glycol, 0.01% potassium benzisothiazolinone, 0.5% silicone oil, and deionized water make up the balance.

Preparation method: According to the formula proportion, place pyflubumide, nicofluprole, surfactant and other functional additives in the reaction kettle in sequence, add water and mix evenly, undergo high-speed shearing, wet sanding, and finally homogeneous filtration to obtain the suspension. product.

Preparation Example 4: 20% nicofluprole·flupentiofenox suspension (1:1)

Formula: by weight, 10% flupentiofenox, 10% nicofluprole, 1% naphthalene sulfonate formaldehyde condensate, 1% sodium dodecyl benzene sulfonate, 1% isotridecyl polyoxyethylene ether, 2% Alkyl aryl 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% benzo Potassium isothiazolinone, 0.5% silicone oil, and deionized water make up the remaining amount;

Preparation method: Same as Preparation Example 3.

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

Formula: By weight, 7.5% pyflubumide, 22.5% nicofluprole, 5% sodium lignosulfonate, 5% naphthalene sulfonate formaldehyde condensate, 1% open powder BX, and kaolin make up the balance.

Preparation method: Mix the active ingredients, dispersant, wetting agent and filler according to the proportion of the formula, stir evenly in a stirring tank, crush and mix multiple times with an airflow mill, and then the wettability composition of the present invention can be prepared powder.

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

Formula: By weight, 10% nicofluprole, 30% flupentiofenox, 8% naphthalene sulfonate formaldehyde condensate, 2% polycarboxylic acid sodium salt, 3% sodium lauryl sulfate, 4% Yuanming powder, kaolin supplement margin.

Preparation method: Same as Preparation Example 5.

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

Formula: By weight, 11% nicofluprole, 22% flupentiofenox, 10% sodium lignosulfonate, 2% polycarboxylate sodium salt, 2% open powder BX, and kaolin make up the balance.

Preparation method: Same as Preparation Example 5.

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

Formula: By weight, 3% nicofluprole, 15% isocycloseram, 12% castor oil polyoxyethylene ether, 2% fatty alcohol polyoxyethylene ether, 2% calcium dodecyl benzene sulfonate, 2% succinate sulfonate acid salt, 1% organic bentonite, and the remainder of corn oil.

Preparation method: According to the formula proportion, place the active ingredients, surfactants and other functional additives in the reaction kettle in sequence, add oil and mix evenly, undergo high-speed shearing, wet sanding, and finally homogeneous filtration to obtain the dispersible oil. Suspension products.

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

Formula: By weight, 12% nicofluprole, 12% isocycloseram, 3% fatty alcohol polyoxyethylene ether phosphate ester salt, 2% naphthalene sulfonate formaldehyde condensate, 4% alkylaryl polyoxyethylene ether polyoxypropylene Ether, 0.2% xanthan gum, 1% magnesium aluminum silicate, 5% propylene glycol, 0.01% potassium benzisothiazolinone, 0.5% silicone oil, and deionized water to make up the balance.

Preparation method: Same as Preparation Example 3.

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

Formula: by weight, 25% nicofluprole, 5% isocycloseram, 10% polycarboxylate sodium salt, 4% naphthalene sulfonate formaldehyde condensate, 2% sodium lauryl sulfate, 3% silica, 15% Starch and kaolin make up the balance.

Preparation method: Same as Preparation Example 5.

Indoor biometric testing

Example 1: Indoor activity test of nicofluprole, pyflubumide, and flupentiofenox against two-spotted spider mites

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

Test target: Two-spotted spider mite (Tetranychus urticae Koch), select adult mites with consistent physiological status.

Test drugs: nicofluprole original drug, pyflubumide original drug, flupentiofenox original drug, all provided by the company's R&D center.

Test material preparation: Select broad bean leaves that have consistent growth and have not been treated with pesticides, use a hole punch to make a suitable leaf disc, place a wet sponge in the petri dish, put filter paper on the wet sponge, and place the prepared leaf disc Place on the filter paper, 2 leaf discs per petri dish, move the target pest mites raised indoors to the leaf discs, 15 mites per leaf disc.

Pharmaceutical preparation: Dissolve the above original medicines in appropriate solvents, design 5 groups of proportions according to the mixing purpose and pharmaceutical activity, and configure 5 series of mass concentration gradients for each single dose and each group of mixtures.

Test method: Adjust the pressure of the Potter spray tower to a stable state of 1.47×10 ⁵ Pa. Clean the cleaned spray head first with acetone twice and then with distilled water twice.

Place the petri dish on the bottom of the Potter spray tower for spraying. The spray volume is 1 mL. After the liquid settles for 1 minute, take it out. Each treatment is repeated 4 times, and the treatment without the drug is used as a blank control.

Raising and observation: The treated test insects were raised and observed under the conditions of a temperature of (25±1)℃ and a photoperiod of L:D=(16:8)h. After 48 hours, check the death of test insects, and record the total number of insects and the number of dead insects respectively.

Calculation method:

Based on the survey data, the mortality rate of each treatment was calculated. Calculate according to the following formula:

In the formula:

P——mortality rate, unit is percentage (%);

K——Indicates the number of dead insects, the unit is head;

N——Indicates the total number of insects treated, the unit is head.

In the formula:

P ₁ ——Corrected mortality rate, unit is percentage (%);

_Pt ——treatment mortality rate, unit is percentage (%);

P ₀ ——Blank control mortality rate, unit is percentage (%).

If the control mortality rate is <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 is >20%, the test needs to be redone.

Use the DPS statistical analysis system to analyze, obtain the toxicity regression equation, correlation coefficient and LC ₅₀ value, and evaluate the activity of the test agent on biological test materials.

The co-toxicity coefficient (CTC value) of the mixture is calculated according to the following formula:

In the formula:

ATI - measured toxicity index of mixture;

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

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

TTI＝TI _A ×P _A +TI _B ×P _B

In the formula:

TTI - theoretical toxicity index of mixture;

TI _A - toxicity index of agent A;

P _A - the percentage content of agent A in the mixture, the unit is percentage (%);

TI _B - toxicity index of agent B;

P _B - the percentage content of agent B in the mixture, the unit is percentage (%).

In the formula:

CTC - co-toxicity coefficient;

ATI - measured toxicity index of mixture;

TTI - Theoretical toxicity index of a mixture.

The compound co-toxicity coefficient CTC ≥ 120 shows synergistic effect; CTC ≤ 80 shows antagonism; 80 < CTC < 120 shows additive effect. The indoor test results are shown in the table below:

Table 1 Indoor activity test results of nicofluprole and pyflubumide against two-spotted spider mites

Table 2 Indoor activity test results of nicofluprole and flupentiofenox compound against two-spotted spider mites

The indoor activity measurement test results show that a reasonable combination of nicofluprole with pyflubumide and flupentiofenox has a good control effect on two-spotted spider mites. 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 is synergistic; 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 is synergistic. To increase efficiency.

Example 2: Indoor activity test of nicofluprole and isocycloseram compound against cinnabar spider mites

Test basis: The test refers to NY/T 1154.13-2008 "Pesticide Indoor Bioassay Test Guidelines for Pesticides Part 13: Leaf Disk Spray Method", NY/T 1154.7-2008 "Pesticide Indoor Bioassay Test Guidelines for Pesticides Part 7 : Determination of combined effects of blends.

Test target: Tetranychus cinnabarinus Boisduval. Adult mites with consistent physiological status were selected.

Test drugs: nicofluprole original drug, isocycloseram original drug, the above technical drugs are provided by the company's R&D center.

Test materials: Select kidney bean leaves that have not been treated with any chemicals, place a sponge block in a petri dish to moisturize, place filter paper on the sponge block, place the kidney bean leaves punched with a hole punch on the filter paper, and inoculate the test insects into the leaves on, 30 heads per treatment.

Pharmaceutical preparation: After dissolving the original medicinal solvent, dilute it with distilled water containing 0.1% Tween 80, prepare single-dose mother liquor respectively, and design a reasonable proportion according to the purpose of mixing and pharmaceutical activity. Ratio method to prepare the required series of mass concentrations.

Chemical treatment: Set the spray pressure of the Potter spray tower to a stable state of 1.47×10 ⁵ Pa. Clean the cleaned spray head first with acetone twice and then with distilled water twice. Place the petri dish on the bottom of the Potter spray tower for spraying. The spray volume is 1 mL. After the liquid settles for 1 minute, take it out and transfer it to the feeding conditions. Each treatment was repeated 4 times, and the treatment without chemicals was set as a blank control.

Raising and observation: The test insects of each treatment were raised and observed under appropriate conditions.

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

Based on the survey data, the corrected mortality rate for each treatment was calculated. Calculate according to formulas (1) and (2), and the calculation results are kept to two decimal places:

In the formula:

P——mortality rate, unit is percentage (%);

K——Indicates the number of dead insects, the unit is head;

N——Indicates the total number of insects treated, the unit is head.

In the formula:

P ₁ ——Corrected mortality rate, unit is percentage (%);

_Pt ——treatment mortality rate, unit is percentage (%);

P ₀ ——Blank control mortality rate, unit is percentage (%).

If the control mortality rate is <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 >20%, the test needs to be repeated.

The data were processed using probability value analysis. Use DPS statistical analysis system analysis to calculate the toxicity regression equation and LC ₅₀ value to evaluate the activity of the test agent on biological test materials.

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

In the formula:

ATI - measured toxicity index of mixture;

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

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

TTI＝TI _A *P _A +TI _B *P _B ········(4)

In the formula:

TTI - theoretical toxicity index of mixture;

TI _A - toxicity index of agent A;

P _A - the percentage content of agent A in the mixture, the unit is percentage (%);

TI _B - toxicity index of agent B;

P _B - the percentage content of agent B in the mixture, the unit is percentage (%).

In the formula:

CTC - co-toxicity coefficient;

ATI - measured toxicity index of mixture;

TTI - Theoretical toxicity index of a mixture.

The compound co-toxicity coefficient CTC ≥ 120 shows synergistic effect; CTC ≤ 80 shows antagonism; 80 < CTC < 120 shows additive effect.

The results of the indoor biological activity test are shown in the table below:

Table 3 Results of the indoor activity test of nicofluprole and isocycloseram against spider mites

The indoor activity measurement test results show (as shown in Table 3) that when nicofluprole and isocycloseram are reasonably compounded, the mass ratio is 50:1 to 1:45, the co-toxicity coefficient is greater than 120, and the combined effect is synergistic.

Example 3: Indoor activity test results of nicofluprole and flupentiofenox, pyflubumide or isocycloseram against wolfberry gall mites

Test basis: The test refers to NY/T 1154.13-2008 "Pesticide Indoor Bioassay Test Guidelines for Pesticides Part 13: Leaf Disk Spray Method", NY/T 1154.7-2008 "Pesticide Indoor Bioassay Test Guidelines for Pesticides Part 7 : Determination of combined effects of blends.

Test target: wolfberry gall mite (Aceria pallida Keifer), select adult mites with consistent physiological status.

Test drugs: nicofluprole original drug, pyflubumide original drug, flupentiofenox original drug, and isocycloseram original drug, all provided by the company's R&D center.

Instruments and equipment: microscope, hole punch, sponge block, petri dish, Potter spray tower, constant temperature incubator.

Test material preparation: Select wolfberry leaves that have grown consistently and have not been treated with any chemicals, place a sponge block in a petri dish to moisturize, put filter paper on it, put wolfberry leaves on the filter paper, and inoculate the adult mites raised indoors onto the leaves. 30 heads per dish.

Pharmaceutical preparation: Dissolve the original medicinal solvents respectively, and then dilute with 0.1% Tween 80 aqueous solution. Prepare the single-dose mother liquor separately, and design a reasonable proportion according to the mixing purpose and pharmaceutical activity. Each single dose and each group of proportioned mixtures are configured with the required series of mass concentrations according to the equal ratio method.

Chemical treatment: The spray pressure of the Potter spray tower is in a stable state of 1.47×105Pa. Clean the cleaned spray head first with acetone twice and then with distilled water twice.

Place the petri dish on the bottom of the Potter spray tower and spray with a spray volume of 1 mL. After the liquid settles for 1 minute, take it out and transfer it to normal feeding conditions for breeding.

Each treatment was repeated 4 times, and the treatment without chemicals was set as a blank control.

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

Based on the survey data, the corrected mortality rate for each treatment was calculated. Calculate according to formulas (1) and (2), and the calculation results are kept to two decimal places:

In the formula:

P——mortality rate, unit is percentage (%);

K——Indicates the number of dead insects, the unit is head;

N——Indicates the total number of insects treated, the unit is head.

In the formula:

P ₁ ——Corrected mortality rate, unit is percentage (%);

_Pt ——treatment mortality rate, unit is percentage (%);

P ₀ ——Blank control mortality rate, unit is percentage (%).

If the control mortality rate is <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 >20%, the test needs to be repeated.

The data were processed using probability value analysis. Use DPS statistical analysis system analysis to calculate the toxicity regression equation and LC ₅₀ value to evaluate the activity of the test agent on biological test materials.

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

In the formula:

ATI - measured toxicity index of mixture;

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

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

TTI＝TI _A *P _A +TI _B *P _B ········(4)

In the formula:

TTI - theoretical toxicity index of mixture;

TI _A - toxicity index of agent A;

P _A - the percentage content of agent A in the mixture, the unit is percentage (%);

TI _B - toxicity index of agent B;

P _B - the percentage content of agent B in the mixture, the unit is percentage (%).

In the formula:

CTC - co-toxicity coefficient;

ATI - measured toxicity index of mixture;

TTI - Theoretical toxicity index of a mixture.

The compound co-toxicity coefficient CTC ≥ 120 shows synergistic effect; CTC ≤ 80 shows antagonism; 80 < CTC < 120 shows additive effect. The results of the indoor biological activity test are shown in the table below:

Table 4 Results of the indoor activity test of pyflubumide and nicofluprole on wolfberry gall mites

Table 5 Indoor activity test results of nicofluprole and flupentiofenox compound against wolfberry gall mites

Table 6 Indoor activity test results of nicofluprole and isocycloseram compound against wolfberry gall mites

The indoor activity measurement test results show that a reasonable combination of nicofluprole with pyflubumide, flupentiofenox, and isocycloseram has a good control effect on two-spotted spider mites. The mass ratio of nicofluprole to pyflubumide is 25:1~1:30, the co-toxicity coefficient is greater than 120, and the combined effect is synergistic; the mass ratio of nicofluprole to flupentiofenox is 35:1~1:30, the co-toxicity coefficient is greater than 120, and the combined effect is synergistic. It is synergistic; the mass ratio of nicofluprole and isocycloseram is 45:1 to 1:30, and the co-toxicity coefficient is greater than 120, so the combined effect is synergistic.

Field efficacy control test

Example 3: Field efficacy control test of nicofluprole, pyflubumide, and flupentiofenox on spider mites

Test basis: The test is based on GB/T 17980.17-2000 "Pesticide Field Efficacy Test Guidelines (1) Acaricides for Control of Spider Mites on Beans and Vegetables".

Test target: spider mites.

Experimental crop: Cowpea (Lvfengjin 99).

Test site: The test was carried out in the cowpea planting land in Xuejia Village, Liu Town, Shouguang District, Weifang City. The test land is sandy loam soil with medium-to-high fertility and a relatively uniform management level.

Experimental design: The experiment adopts random block arrangement, with each treatment repeated 4 times, and each plot is 30m ² . Apply pesticides at the early stage of the occurrence of spider mites. The spider mites are a mixed population of Tetranychus cinnabarinus Boisduval, Tetranychus urticae Koch and Tetranychus truncates Ehara. The dominant species is Tetranychus urticae Koch. For spider mites, the pesticide should be applied evenly and thoughtfully, so that the front and back sides of the leaves and stems of the cowpea plants are evenly sprayed. The test was conducted with a total of 1 pesticide application.

Investigation method: The test was carried out to investigate the base number of mites before the treatment, and the investigation was carried out 3 days and 14 days after the treatment. During the investigation, 20 leaves were taken from each plot to count the number of live mites.

Prevention effectiveness calculation method:

The results of the field efficacy test are shown in the table below:

Table 6 Field efficacy test results of nicofluprole combined with pyflubumide, flupentiofenox, and isocycloseram on spider mites

It can be seen from the field efficacy test results that the combination of nicofluprole, pyflubumide and flupentiofenox shows better miticidal effect. Three days after treatment, the overall preventive effect of each compound preparation was over 80%, showing good quick-acting properties. The control effect of 20% nicofluprole·flupentiofenox suspension (1:1), 24% nicofluprole·pyflubumide emulsifiable concentrate (5:1), and 18% nicofluprole·isocycloseram dispersible oil suspension (1:5) on spider mites 14 days after treatment. Reaching 94.41%, 90.84%, 92.64%. It can be seen that the acaricidal composition of the present invention can comprehensively control multiple spider mites such as spider mites, spider mites, and spider mites. It is safe for target crops, has good quick-acting properties, has a long duration of effect, and can be widely used. Used for the control of herbivorous spider mites in the field.

Example 4: Field efficacy control test of wolfberry gall mites

Experimental crop: Lycium barbarum (Ningqi No. 1).

Test subject: wolfberry gall mite.

Test site: The test was conducted in the wolfberry planting base in Xixia District, Yinchuan City, Ningxia in July 2020. The test site was irrigation silt soil. The soil fertility of the test site was medium, the terrain was flat, the fertility was uniform, and the irrigation conditions were good. The management level of the experimental site is high, and the management conditions of each experimental plot are uniform. The wolfberries in the experimental site are 5-year-old wolfberries, and the planting density is 3000 plants/hm ² .

Experimental design: The experiment was designed with 8 treatments in total, and each treatment was repeated 4 times. The experimental plots were arranged in random blocks, and the area of each plot was 30m ² . The test was carried out once on July 5, 2020. The control was sprayed first, and was carried out in sequence from low concentration to high concentration, spraying evenly and evenly. When changing different chemicals, clean the sprayer three times.

Experimental investigation: The experiment was conducted on 3d, 7d, and 15d after treatment. During the investigation, 5 sampling points were used. One plant was randomly surveyed at each point. One new plant was randomly selected from each plant in 5 directions: east, south, west, north, and middle. The branches were marked, and during the investigation, 3 leaves were taken from the front, middle and back sections of each branch to investigate the number of surviving gall mites on the fixed branches, and the control effect was calculated.

Prevention effectiveness calculation method:

Safety evaluation survey methods:

In the test, 30 days after treatment, the leaves, flowers, and fruits of the wolfberry trees were investigated for phytotoxicity and symptoms of phytotoxicity. For each plant, a branch of no less than 50cm was selected from the east, south, west, and north to investigate all leaves, Flowers, fruits.

Pesticide hazard classification standards:

-No harmful effects;

+ Mild phytotoxicity, does not affect the normal growth of leaves, flowers and fruits;

++Obvious drug damage can be recovered;

+++ Highly phytotoxic, affecting the normal growth of leaves, flowers and fruits;

++++Severe phytotoxicity, inhibiting the growth of leaves, flowers and fruits.

Table 7 Field efficacy control test of nicofluprole and isocycloseram, pyflubumide or flupentiofenox on wolfberry gall mites

Table 8 Safety test of pyflubumide and nicofluprole on wolfberry

Irregular observations were made during each of the above field tests. At the tested concentrations, the acaricidal composition of the present invention did not have any adverse effects on wolfberry plants and was safe against predatory mites.

In summary, through indoor activity tests and field tests, the acaricidal composition of the present invention has a significant control effect on spider mites and gall mites, has good quick-acting properties, and has a long duration of effect, and the acaricidal composition of the present invention is effective against natural enemies and It is safe for beneficial mites, has no phytotoxicity on target crops, and is safe for crops.

Although the present invention has been described in detail with general descriptions and specific embodiments above, some modifications or improvements can be made on the basis of the present invention, which is obvious to those skilled in the art. Therefore, These modifications or improvements made without departing from the spirit of the present invention all belong to the scope of protection claimed by the present invention.

Claims (10)

1. An acaricidal composition, characterized in that the acaricidal composition comprises active ingredient A and active ingredient B, the active ingredient A is nicofluprole, and the active ingredient B is pyflubumide, flupentiofenox or isocycloseram In any one of them, 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, wherein the active ingredient B is pyflubumide, and the mass ratio of the active ingredient A to active ingredient B is 50:1 to 1:35; The active ingredient B is flupentiofenox, and the mass ratio of the active ingredient A to active ingredient B is 35:1 to 1:35; The active ingredient B is isocycloseram, and the mass ratio of the active ingredient A to active ingredient B is 45:1 to 1:35. 3. The acaricidal composition according to claim 2, wherein the active ingredient B is pyflubumide, and the mass ratio of the active ingredient A to active ingredient B is 25:1 to 1:30; The active ingredient B is flupentiofenox, and the mass ratio of the active ingredient A to active ingredient B is 35:1 to 1:30; The active ingredient B is isocycloseram, and the mass ratio of the active ingredient A to active ingredient B is 35:1 to 1:30. 4. The acaricidal composition according to claim 1, characterized in that, the total weight of the acaricidal composition is calculated as 100wt%, and the total weight of the active ingredient A and active ingredient B accounts for the total weight of the acaricidal composition. The total weight of the acaricidal composition is 1 wt% to 80 wt%, 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 also includes agriculturally acceptable auxiliary ingredients, and the auxiliary ingredients are selected from wetting agents. , one or more of dispersants, emulsifiers, thickeners, disintegrants, antifreezes, 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 an agriculturally acceptable preparation form, and the preparation form is powder, granule, pellet, or tablet. agent, strip, wettable powder, oil-dispersible powder, milk powder, water-dispersible granule, emulsion granule, water-dispersible tablet, soluble powder, soluble tablet, soluble granule, soluble agent, soluble gel, Oil, film spreading oil, emulsifiable concentrate, latex, dispersible liquid, ointment, water emulsion, oil emulsion, microemulsion, fat suspension, microcapsule suspension, oil suspension, dispersible oil suspension, suspoemulsion , any one of microcapsule suspension-suspension agent, microcapsule suspension-aqueous emulsion or microcapsule suspension-suspended emulsion. 7. The acaricidal composition according to claim 6, characterized in that the preparation form is emulsifiable concentrate, suspension concentrate or wettable powder. 8. Use of the acaricidal composition according to any one of claims 1 to 7 for controlling plant pest mites. 9. The use according to claim 8, characterized in that the plant pest mites are Tetranychus tetranychidae and/or Gall mites, and the Tetranychus mites are Tetranychus cinnabar, Tetranychus two-spotted, Tetranychus truncata, Panonychus citrus or cotton spider mite, and the gall mites are citrus rust ticks and/or wolfberry gall mites; Preferably, the pest mites of the family Tetranychidae are Tetranychus cinnabar, Tetranychus two-spotted, and Tetranychus truncatula, and the pest mites of the family Gallidae are wolfberry gall mites. 10. The use according to claim 8, characterized in that the acaricidal composition is applied to harmful mites and their growth medium at an effective dose.