CN112889836B

CN112889836B - Acaricidal composition containing Acynonapyr

Info

Publication number: CN112889836B
Application number: CN202110091917.7A
Authority: CN
Inventors: 张永芳; 孙翠; 王均竹; 王伟香
Original assignee: QINGDAO KAIYUANXIANG CHEMICAL CO Ltd
Current assignee: Qingdao Kaiyuanxiang Chemical Co.,Ltd.
Priority date: 2020-01-11
Filing date: 2020-01-11
Publication date: 2021-12-14
Anticipated expiration: 2040-01-11
Also published as: CN112889836A; CN111184007A; CN112715565B; CN112715565A

Abstract

The invention belongs to the technical field of pesticides, and relates to an acaricidal composition containing Acynonapyr; the active ingredients of the acaricidal composition comprise an active ingredient A and an active ingredient B; the active ingredient A is Acynonapyr, and the active ingredient B is selected from azocyclotin, clofentezine and spirotetramat. The acaricidal composition or the preparation thereof can enhance the pesticide effect, expand the acaricidal spectrum, reduce the use cost, reduce the dosage, prolong the lasting period and delay the development of pesticide resistance.

Description

Acaricidal composition containing Acynonapyr

Technical Field

The invention relates to the technical field of pesticide compounding, in particular to an acaricidal composition containing Acynonapyr, azocyclotin, clofentezine and spirotetramat.

Background

Glutamate, a key neurotransmitter, conducts primarily excitatory in vertebrate organisms, but in invertebrates it is not only an excitatory neurotransmitter, but also an inhibitory neurotransmitter. When glutamate mediates nerve impulses as an inhibitory neurotransmitter, glutamate contacts postsynaptic receptors, which turn on its gated corresponding chloride channel, known as glutamate-gated chloride channel (GluCl), also known as inhibitory glutamate receptors (IGluRs) channel.

Known ligand molecules that act on GluCl are fipronil, Nodulisporic acid, Spinosad, Moxidectin, abamectin and derivatives thereof.

Acynonapyr is a novel acaricide with cyclic amine skeleton developed by Nippon Caoda corporation, which acts on inhibitory glutamate receptors (IGlurs), interferes with neurotransmission of harmful mites, makes muscle cells lose original motor ability, shows a paralytic state, further affects feeding or exercise, and finally kills the harmful mites. Has good control effect on fruit trees, vegetables and tea tree mites. The CAS of Acynonapyr is chemically (3-endo) -3- [ 2-propoxy-4- (trifluoromethyl) phenoxy ] -9- [ [5- (trifluoromethyl) -2-pyridinyl ] oxy ] -9-azabicyclo [3.3.1] nonanyl (CAS: No.1332838-17-1), having the chemical structure:

azocyclotin is an organotin broad-spectrum acaricide, interferes ATP formation by inhibiting oxidative phosphorylation, has good control effect on nymph mites, adult mites and summer eggs, and is ineffective on winter eggs. The structural formula is as follows:

the clofentezine belongs to a clofentezine acaricide, and is an embryo development inhibitor which mainly kills mite eggs, but also has certain effect on young mites, has long lasting period which is as long as 50-60 days, can achieve the highest mite killing effect 2-3 weeks after application, has good effect on winter eggs, but is ineffective on adult mites. The product is harmless to predatory mites and natural enemies, and is very suitable for comprehensive control of pests. The structural formula is as follows:

spirotetramat is tetronic acid compound, lipid biosynthesis inhibitor, and has effects of inhibiting acetyl coenzyme A carboxylase, resisting stomach toxicity, killing by contact, and defatting spirotetramat after permeating into leaves, and can conduct bidirectionally at xylem and phloem.

The chemical structural formula is as follows:

the agricultural pest mites are small in size, rapid in propagation, multiple in generation number and strong in applicability, are typical r-countermeasure explosive pests, and are one of the most difficult pest communities to control. In recent years, with the large-area popularization of facility agriculture, mite damage is in a situation of increasing year by year. The phytophagous harmful mites include tetranyhidae (tetranyhidae), goiter (Eriophyoidea), rhizomorpha (rhizomorph), and the like, wherein the Tetranychus and goiter are the most harmful, and Tetranychus cinnabarinus (Tetranychus cinnabarinus boisdruval) is the main harmful mite. The number of harmful plants can be as much as 113, so that if mites suck juice on the back of leaves, the leaves become grey white, and if the mites are serious, the leaves are dried and shed, and the growth of the plants is influenced. In the agricultural production process, chemical agents are the most effective means for controlling pests and diseases. The long-term continuous high-dose use of a single chemical agent easily causes a series of problems of drug resistance of pest mites, environmental pollution and the like. The reasonable compounding or mixing of the chemical agents has the positive characteristics of expanding the insecticidal spectrum, improving the control effect, prolonging the application period, reducing the dosage, reducing the phytotoxicity, reducing the residue, delaying the occurrence of the drug resistance and the drug resistance of pests and the like. The applicant surprisingly discovers that the compounded combination of Acynonapyr, azocyclotin, clofentezine and spirotetramat has an obvious synergistic effect through an indoor toxicity test and a field efficacy test, and the acaricide composition compounded by the Acynonapyr, azocyclotin, clofentezine and spirotetramat and the application thereof are not reported at present.

Disclosure of Invention

Based on the situation, the invention aims to provide a pesticide acaricidal composition containing Acynonapyr and a preparation thereof, which are mainly used for controlling phytophagous mites.

In order to achieve the above object, the present invention provides an acaricidal composition containing acytonapyr, characterized in that: comprises an active component A of Acynonapyr and an active component B of any one of azocyclotin, clofentezine or spirotetramat.

Wherein the mass ratio of the active component A to the active component B is 50: 1-1: 50, preferably 10: 1-1: 10, and more preferably 5: 1-1: 5.

Preferably, the mass ratio of Acynonapyr to azocyclotin is 50: 1-1: 50, and preferably 5: 1-1: 5.

Preferably, the mass ratio of the Acynonapyr to the clofentezine is 50: 1-1: 50, and preferably 5: 1-1: 5.

Preferably, the mass ratio of Acynonapyr to spirotetramat is 50: 1-1: 50, preferably 5: 1-1: 5.

Preferably, the acaricidal composition containing Acynonapyr and azocyclotin, clofentezine or spirotetramat accounts for 100 wt% of the total weight of the acaricidal composition, and the sum of the contents of the active ingredient A and the active ingredient B in the acaricidal composition is 1-95 wt%, preferably 5-80 wt%, and more preferably 10-50 wt%;

preferably, the sum of the content of the Acynonapyr and the azocyclotin in the acaricidal composition is 10-25 wt% based on 100 wt% of the total mass of the acaricidal composition;

preferably, the sum of the content of the Acynonapyr and the clofentezine in the acaricidal composition is 10-40 wt% based on 100 wt% of the total weight of the acaricidal composition;

preferably, the sum of the content of the Acynonapyr and the spirotetramat in the acaricidal composition is 10-45 wt% based on 100 wt% of the total weight of the acaricidal composition.

Preferably, the acaricidal composition further comprises adjuvants selected from one or more of wetting agents, dispersing agents, emulsifiers, thickeners, disintegrants, antifreeze agents, antifoaming agents, solvents, preservatives, stabilizers, synergists and carriers;

the invention provides an acaricidal composition containing Acynonapyr, azocyclotin, clofentezine or spirotetramat, wherein the preparation is selected from missible oil, aqueous emulsion, microemulsion, suspending agent, wettable powder and water dispersible granules; preferably, the formulation is selected from suspending agents, wettable powder and water dispersible granules.

The invention provides an acaricidal composition containing Acynonapyr, azocyclotin, clofentezine or spirotetramat, and application of any acaricidal composition or preparation in controlling phytophagous mites.

The invention provides an acaricidal composition containing Acynonapyr and azocyclotin, clofentezine or spirotetramat.

Detailed description of the invention

In some examples of the invention, the active ingredients of the acaricidal composition comprise active ingredient a and active ingredient B; the active ingredient A is Acynonapyr, and the active ingredient B is selected from azocyclotin, clofentezine and spirotetramat.

Wherein the mass ratio of the active component A to the active component B is 50: 1-1: 50, preferably 10: 1-1: 10, and more preferably 5: 1-1: 5;

preferably, the mass ratio of the Acynonapyr to the azocyclotin is 50: 1-1: 50, preferably 5: 1-1: 5; specifically, the mass ratio of the acyclonapyr to the azocyclotin in the acaricidal composition is 50:1, 20:1, 10:1, 5:1, 3:1, 1:3, 1:5, 1:10, 1:20 or 1: 50.

Preferably, the mass ratio of the Acynonapyr to the clofentezine is 50: 1-1: 50, preferably 5: 1-1: 5; specifically, the mass ratio of the acyclonapyr to the clofentezine in the acaricidal composition is 50:1, 20:1, 10:1, 5:1, 3:1, 1:3, 1:5, 1:10, 1:20 or 1: 50.

Preferably, the mass ratio of the Acynonapyr to the spirotetramat is 50: 1-1: 50, preferably 5: 1-1: 5; specifically, the mass ratio of the acyclonapyr to the clofentezine in the acaricidal composition is 50:1, 20:1, 10:1, 5:1, 3:1, 1:3, 1:5, 1:10, 1:20 or 1: 50.

An acaricidal composition containing Acynonapyr, azocyclotin, clofentezine and spirotetramat is preferably used, wherein the sum of the contents of the active ingredient A and the active ingredient B in the acaricidal composition is 1-95 wt%, preferably 5-80 wt%, and more preferably 10-50 wt%, based on 100 wt% of the total weight of the acaricidal composition.

In a preferred embodiment, the sum of the content of Acynonapyr and azocyclotin in the acaricidal composition is 10-25 wt%, for example, the sum of the content of Acynonapyr and azocyclotin is 25%, 20% or 18%.

In a preferred embodiment, the sum of the content of the acyclonapryr and the clofentezine in the acaricidal composition is 10 to 40 wt%, for example, the sum of the content of the acyclonapryr and the clofentezine is 40%, 24%, 20% and 18%.

In a preferred embodiment, the sum of the content of Acynonapyr and spirotetramat in the acaricidal composition is 10-45 wt%, for example, the sum of the content of Acynonapyr and spirotetramat is 45%, 24%, 20% and 12%.

The invention optimizes the content of the active ingredients in the acaricidal composition, so that the toxicity and the residue of the acaricidal composition are well balanced, the pesticide effect can be enhanced, the dosage can be reduced, and the cost can be reduced.

According to the acaricidal composition containing Acynonapyr, azocyclotin, clofentezine and spirotetramat, the acaricidal composition preferably further comprises an auxiliary agent, wherein the auxiliary agent is selected from one or more of a wetting agent, a dispersing agent, an emulsifying agent, a thickening agent, a disintegrating agent, an antifreezing agent, an antifoaming agent, a solvent, a preservative, a stabilizing agent, a synergist and a carrier.

The wetting agent is selected from one or more of alkyl benzene sulfonate, alkyl naphthalene sulfonate, lignosulfonate, sodium dodecyl sulfate, dioctyl sodium sulfosuccinate, alpha olefin sulfonate, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol ethoxylate, fatty alcohol polyoxyethylene ether sodium sulfate, silkworm excrement, Chinese honeylocust fruit powder, soapberry powder, SOPA, detergent, emulsifier 2000 series and wetting penetrant F; and/or

The dispersing agent is selected from one or more of lignosulfonate, alkyl naphthalene sulfonate formaldehyde condensate, naphthalene sulfonate, tristyrylphenol ethoxylate phosphate, fatty alcohol ethoxylate, alkylphenol polyoxyethylene ether methyl ether condensate sulfate, fatty amine polyoxyethylene ether, glycerol fatty acid ester polyoxyethylene ether, polycarboxylate, polyacrylic acid, phosphate, EO-PO block copolymer and EO-PO graft copolymer; and/or

The emulsifier is selected from one or more of calcium dodecylbenzene sulfonate, alkylphenol formaldehyde resin polyoxyethylene ether, phenethyl phenol polyoxyethylene polyoxypropylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, styryl phenol polyoxyethylene ether, castor oil polyoxyethylene ether and alkylphenol ether phosphate; and/or

The thickener is one or more selected from xanthan gum, organic bentonite, gum arabic, sodium alginate, magnesium aluminum silicate, carboxymethyl cellulose and white carbon black; and/or

Disintegrant the disintegrant is 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

The antifreezing agent is selected from one or more of alcohols, alcohol ethers, chlorohydrocarbons and inorganic salts; and/or

The defoaming agent is selected from C₁₀-C₂₀Saturated fatty acid compound, silicone oil, silicone compound, C₈-C₁₀One or more of fatty alcohols; and/or

The solvent is selected from one or more of benzene, toluene, xylene, durene, methanol, ethanol, isopropanol, n-butanol, dimethyl sulfoxide, dimethylformamide, cyclohexanone, alkylene carbonate, diesel oil, solvent oil, vegetable oil derivative and water; and/or

The preservative is selected from one or more of propionic acid, sodium propionate, sorbic acid, sodium sorbate, potassium sorbate, benzoic acid, sodium benzoate, sodium parahydroxybenzoate, methyl parahydroxybenzoate, carbazone and 1, 2-benzisothiazoline 3-one; 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, triethanolamine oleate, epoxidized vegetable oil, kaolin, bentonite, attapulgite, white carbon black, talcum powder, montmorillonite and starch; and/or

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

The carrier is selected from one or more of ammonium salt, ground natural mineral, ground artificial mineral, silicate, resin, wax, solid fertilizer, water, organic solvent, mineral oil, vegetable oil and vegetable oil derivative.

The preparation formulation comprises but is not limited to missible oil, aqueous emulsion, microemulsion, suspending agent, wettable powder and water dispersible granule; preferably, the preparation is in the form of a suspending agent, wettable powder or water dispersible granules.

Wettable powders are mixtures of the compositions in a certain proportion with suitable surfactants and inert substances. Wettable powders are formulations which are uniformly dispersible in water and which contain, in addition to the active substance and inert substance, a certain amount of an anionic or nonionic surfactant. The wettable powder does not use solvent and emulsifier, is safe to plants, is not easy to generate phytotoxicity and is safe to the environment.

The suspending agent is prepared by mixing the composition with proper surfactant, water or organic solvent in a certain proportion, grinding by a colloid mill, and grinding for 1-2 times by a sand mill to a certain fineness. The suspending agent is divided into an aqueous suspending agent and an oil suspending agent, and has small particle size, high biological activity, no dust flying problem, and no flammability and explosion. The suspending agent consists of active ingredients, a dispersing agent, a thickening agent, an anti-settling agent, a defoaming agent, an antifreezing agent, water and the like.

The water dispersible granule is obtained by re-granulating wettable powder or suspending agent into water dispersible granule, mixing the composition with appropriate surfactant and inert substance (kaolin, diatomite and pottery clay) powder according to a certain proportion to form a mixture, and then granulating by a fluidized bed granulation method, a spray granulation method or a disc granulation method. The raw materials are pulverized by airflow in the mixing process to ensure that the fineness of the powder particles meets the requirement, and the product is uniformly mixed by using a double-helix mixer and a coulter type mixer for multiple times. The preparation has good fluidity, convenient use, no dust flying, safety and reliability.

The technical scheme of the invention is realized by the following measures:

an acaricidal composition containing Acynonapyr, azocyclotin, clofentezine and spirotetramat has a mass ratio of active ingredients of Acynonapyr to azocyclotin, clofentezine and spirotetramat of 50: 1-1: 50, and toxicity measurement experiments prove that the acaricidal composition has a better synergistic effect when the mass ratio of Acynonapyr to spirotetramat is 5: 1-1: 5.

The insecticidal composition can be prepared into missible oil, aqueous emulsion, microemulsion, suspending agent, wettable powder and water dispersible granules; the preferable preparation formulation is suspending agent, wettable powder and water dispersible granule. The total mass of the Acynonapyr, azocyclotin, clofentezine and spirotetramat in the preparation accounts for 1-95% of the total mass of the preparation, wherein when the total mass accounts for 10-50%, the toxicity and the residue are well balanced, and the cost is low.

The specific implementation scheme of the pesticide formulation prepared by the insecticidal composition is as follows:

when the insecticidal composition is an emulsifiable concentrate preparation, the insecticidal composition comprises the following components in parts by weight: 1-40 parts of Acynonapyr; 1-40 parts of azocyclotin or clofentezine or spirotetramat; 10-30 parts of a conventional emulsifier; 20-50 parts of a conventional solvent; 1-5 parts of a conventional synergist. The specific production steps of the missible oil preparation are that the effective components Acynonapyr and azocyclotin or clofentezine or spirotetramat are added into a solvent to be completely dissolved, then an emulsifier and a synergist are added to be uniformly stirred to form uniform and transparent oily liquid, and the uniform and transparent oily liquid is filled to prepare the missible oil preparation of the composition.

When the insecticidal composition is an aqueous emulsion, the components in parts by weight are as follows: 1-40 parts of Acynonapyr; 1-40 parts of azocyclotin or clofentezine or spirotetramat; 3-30 parts of an emulsifier; 5-15 parts of a solvent; 2-15 parts of a stabilizer; 1-5 parts of an antifreezing agent; 0.1-8 parts of a defoaming agent; 0.2-2 parts of a thickening agent; deionized water and the balance. The specific production steps of the aqueous emulsion are as follows: firstly, adding Acynonapyr, azocyclotin or clofentezine or spirotetramat, a solvent, an emulsifier and a cosolvent together to dissolve the mixture into a uniform oil phase; mixing part of deionized water, antifreeze agent, antimicrobial agent and other pesticide auxiliary agents together to form a uniform water phase; adding the oil phase into the water phase while stirring at a high speed in a reaction kettle, slowly adding water until a phase inversion point is reached, starting a shearing machine to carry out high-speed shearing, adding the rest water, and shearing for about half an hour to form an oil-in-water emulsion, thus preparing the composition in the form of the emulsion in water.

When the insecticidal composition is a microemulsion, the components in parts by weight are as follows: 1-40 parts of Acynonapyr, 1-40 parts of azocyclotin or clofentezine or spirotetramat, 10-30 parts of emulsifier, 1-8 parts of antifreezing agent, 0.5-10 parts of stabilizer and 20-50 parts of conventional solvent cosolvent. The preparation method comprises the steps of completely dissolving Acynonapyr and azocyclotin or clofentezine or spirotetramat with a cosolvent, adding other components such as an emulsifier, an antifreeze stabilizer and the like, uniformly mixing, finally adding water, and fully stirring to prepare the microemulsion.

When the insecticidal composition is a suspending agent, the insecticidal composition comprises the following components in parts by weight: 1-40 parts of Acynonapyr; 1-40 parts of azocyclotin or clofentezine or spirotetramat; 1-10 parts of a dispersing agent; 1-5 parts of an antifreezing agent; 0.1-2 parts of a thickening agent; 0.1-0.8 part of defoaming agent; 0-10 parts of a solvent; 1-5 parts of a stabilizer; and deionized water is used for complementing the balance. The suspension formulation of the composition of the present invention can be prepared by wet-pulverizing D90 (particle size of 90% of particles) < 10 μm using glass beads with a sand mill.

When the insecticidal composition is wettable powder, the components in parts by weight are as follows: 1-40 parts of Acynonapyr; 1-40 parts of azocyclotin or clofentezine or spirotetramat; 3-10 parts of a dispersing agent; 1-5 parts of a wetting agent; filling and deionized water to make up the balance. The wettable powder has the specific production steps as follows: according to the formula, the effective component Acynonapyr is mixed with azocyclotin or clofentezine or spirotetramat, the dispersant, the wetting agent and the filler, the mixture is uniformly stirred in a stirring kettle, and the mixture is uniformly mixed after airflow crushing, so that the wettable powder of the composition can be prepared.

When the insecticidal composition is a water dispersible granule, the insecticidal composition comprises the following components in parts by weight: 1-40 parts of Acynonapyr; 1-40 parts of azocyclotin or clofentezine or spirotetramat; 3-10 parts of a dispersing agent; 1-10 parts of a wetting agent; 1-5 parts of a disintegrating agent; and the balance of the filler. The water dispersible granule comprises the following specific production steps: according to the formula, the active ingredients Acynonapyr, azocyclotin or clofentezine or spirotetramat, a dispersing agent, a wetting agent, a disintegrating agent and a filler are uniformly mixed, crushed by a superfine jet mill, kneaded, added into a fluidized bed granulation dryer for granulation, drying and screening, and then sampled and analyzed to prepare the water dispersible granule of the composition.

The emulsifier is selected from the mixture consisting of calcium dodecyl benzene sulfonate and any one or more than one of fatty acid polyoxyethylene ether, alkylphenol polyoxyethylene ether sulfosuccinate, styrylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, fatty acid polyoxyethylene ester and polyoxyethylene fatty alcohol ether in any ratio.

The solvent is any one or a mixture of more than one of xylene or biodiesel, toluene, diesel oil, methanol, ethanol, n-butanol, isopropanol, turpentine, solvent oil, dimethylformamide, dimethyl sulfoxide, water and the like in any ratio.

The dispersing agent is selected from one or a mixture of more than one of polycarboxylate, lignosulfonate, EO-PO block copolymer, alkylphenol polyoxyethylene ether methyl ether condensate sulfate, alkyl sulfonate calcium salt, naphthalene sulfonic acid formaldehyde condensate sodium salt, alkylphenol polyoxyethylene, fatty acid polyoxyethylene ester, fatty amine polyoxyethylene ether and glycerin fatty acid ester polyoxyethylene ether in any ratio.

The wetting agent is selected from one or more of sodium dodecyl sulfate, alpha-olefin sulfonate, calcium dodecyl benzene sulfonate, nekal BX, wetting penetrant F, alkylbenzene sulfonate polyoxyethylene triphenyl ethyl phosphate, saponin powder, silkworm excrement and soapberry powder.

The disintegrating agent is selected from one or more of bentonite, urea, ammonium carbonate, aluminum chloride, citric acid, succinic acid and sodium bicarbonate.

The thickener is selected from one or more than one of xanthan gum, carboxymethyl cellulose, carboxyethyl cellulose, methyl cellulose, magnesium aluminum silicate and polyvinyl alcohol.

The stabilizer is one or two of sodium citrate and resorcinol.

The antifreezing agent is one or two or three of ethylene glycol, propylene glycol and glycerol.

The defoaming agent is selected from silicone oil, silicone compounds and C_10-20Saturated fatty acid compound, C_8-10One or more than one of fatty alcohol in any ratio.

The filler is selected from one or a mixture of more than one of kaolin, diatomite, bentonite, attapulgite, white carbon black, starch and light calcium carbonate in any ratio.

The insecticidal composition obtained by compounding the active ingredient Acynonapy with any one of azocyclotin, clofentezine and spirotetramat has obvious synergistic effect, can delay the generation of harmful drug resistance, can reduce the production cost and the use cost, and can effectively prevent and control phytophagous harmful mites.

Compared with the prior art, the technical scheme of the invention has the following beneficial effects:

(1) by compounding Acynonapy with any one of azocyclotin, clofentezine and spirotetramat, the composition obtains excellent mite control effect, enlarges the mite killing spectrum and has synergistic effect;

(2) the using amount of pesticides is reduced, and the agricultural cost is reduced;

(3) the pesticide is friendly to crops, non-target organisms and environment, increases the quick-acting property of the pesticide to pests, delays the generation of pesticide resistance of the pests and prolongs the pesticide persistence.

Detailed Description

To make the technical solutions, objects, and advantages of the present invention more apparent, the present invention is described with the following specific examples, but the present invention may be implemented in various forms and should not be limited by the embodiments set forth herein.

Examples reference indoor bioassay test guidelines for pesticides part 13: leaf disc spraying method NT/T1154.13-2008; section 7: combined Effect determination of blending NT/T1154.7-2008

1.1 test Material preparation

Acynonapyr is provided by Helier pharmaceutical group, Inc.;

the azacyclotin raw drug is provided by the Helier pharmaceutical industry group, Inc.;

the clofentezine active compound is provided by Qingdao Kaiyuan Xiang chemical Co Ltd;

the spirotetramat raw medicine is provided by Shandong Hailier chemical Co., Ltd;

test targets: tetranychus cinnabarinus (Tetranychus cinnabarinum Boisdival)

Selecting indoor feeding nymphs with consistent physiological state. The temperature is 25 +/-1 ℃ C. Relative humidity 65% +/-5%, illumination period 16/8h (L/D)

Selecting host plant leaves (broad beans) with consistent growth, making into leaf discs with the diameter of 2cm by using a puncher, placing agar in a culture dish for moisturizing, placing filter paper on the agar, placing leaf discs on the filter paper, wherein each leaf disc contains 4 leaf discs, and inoculating 10 mites which are bred indoors on the leaf discs.

1.2 Experimental procedures

1.2.1 preparation of the medicament

The water soluble medicine is directly dissolved in water, and other medicines are dissolved in proper organic solvent (acetone, chloroform, ethanol, etc.), and then diluted with 0.1% Tween-80 water solution. Preparing single-dose mother liquor respectively, designing 5 groups of proportioning according to the mixing purpose and the medicament activity, and preparing 5 series of mass concentrations of each single dose and each group of proportioning mixing agent according to an equal ratio method.

1.2.2 treatment with pharmaceutical Agents

Placing the culture dish on a bottom plate of a Potter spray tower for spraying, wherein the spraying liquid amount is 1ml, taking out after the liquid medicine is settled for 1min, and transferring to a breeding condition for breeding. The treatment is repeated for not less than 4 times, the number of the tested insects is not less than 120 per dose, and the treatment without medicament (containing all organic solvent and emulsifier) is used as a blank control. 1.2.3 data statistics and analysis

And (5) checking the death condition of the test insects 48 hours after treatment, and respectively recording the total number of the insects and the number of the dead insects. From the survey data, corrected mortality for each treatment was calculated. Calculating according to the formulas (1) and (2), and reserving the calculation results to the last two decimal points:

in the formula:

p-mortality in percent (%);

k-represents the number of dead insects, in head;

n-represents the total number of insects treated, in heads.

In the formula:

P₁corrected mortality in percent (%);

P_t-treatment mortality in percent (%);

P₀blank mortality in percent (%).

If the control mortality rate is less than 5%, no correction is needed; the control mortality rate is between 5% and 20%, and the correction is carried out according to the formula (2); control mortality was > 20%, and the test was redone.

And processing the data by adopting a method of analyzing a few rate value. Can be analyzed by an IBM SPSS Statistics2.0 statistical analysis system to obtain LC of a virulence regression line₅₀The values and their 95% confidence limits, the b values and their standard errors (SD), the activity of the test agents on the biological test material was evaluated.

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

in the formula:

ATI-actually measured toxicity index of mixed agent;

S-Standard mite killingLC of agent₅₀In milligrams per liter (mg/L);

LC of M-mixtures₅₀In milligrams per liter (mg/L).

TTI＝TI_A*P_A+TI_B*P_B·······(4)

In the formula:

TTI-mixture theory virulence index;

TI_A-agent virulence index a;

P_A-the percentage of agent a in the mixture in percent (%);

TI_B-agent B virulence index;

P_B-the percentage of the agent B in the mixture in percent (%).

In the formula:

CTC-co-toxicity coefficient;

ATI-actually measured toxicity index of mixed agent;

TTI-mixture theory virulence index.

The compounded co-toxicity coefficient CTC is more than or equal to 120, and the synergistic effect is shown; CTC is less than or equal to 80 and shows antagonism; 80 < CTC < 120 showed additive effects.

Example 1

Determining the joint toxicity of the Acynonapyr and azocyclotin in different ratios to tetranychus cinnabarinus:

as can be seen from table 1: the toxicity of different acaricides to tetranychus cinnabarinus is greatly different. Acynonapy has good acaricidal activity on tetranychus cinnabarinus, LC₅₀The value is 5.188mg/L, the killing effect of azocyclotin on tetranychus cinnabarinus is poor, and LC₅₀The Acynonapyr/azocyclotin has a value of 190.029mg/L, and has the best effect on Tetranychus cinnabarinus (20: 1), LC₅₀The value is 4.280mg/L, the cotoxicity coefficient is 122.51, the synergy is shown, the co-toxicity coefficient of Acynonapyr and azocyclotin is 204.53, LC₅₀Has a value of13.391 mg/L. The blending of the mixture according to the ratio tested in the test shows a synergistic effect on tetranychus cinnabarinus and nymph.

Table 1 Joint toxicity determination of Acynonapyr and azocyclotin in different ratios on tetranychus cinnabarinus

Example 2

Determining the joint toxicity of the Acynonapyr and the clofentezine to the tetranychus cinnabarinus in different proportions:

as can be seen from table 2: tetramethylpyrazine has good acaricidal activity on tetranychus cinnabarinus, LC₅₀Value of 5.538mg/L, Acynonapyr: clofentezine ═ 5:1 has the best effect on Tetranychus cinnabarinus, and LC₅₀The value is 2.528mg/L, the cotoxicity coefficient is 207.406, Acynonapyr and clofentezine are mixed according to the proportion of 1:50, 1:20, 1:10, 1:5, 1:3, 1:1, 3:1, 5:1, 10:1, 20:1 and 50:1, the synergistic effect is shown on Tetranychus cinnabarinus and Tetranychus cinnabarinus, and the minimum cotoxicity coefficient is 135.802.

Table 2 Joint toxicity assay for Tetranychus cinnabarinus by different proportions of Acynonapyr and clofentezine

Example 3

Determining the joint toxicity of the Acynonapyr and the spirotetramat in different proportions to tetranychus cinnabarinus:

an indoor combined toxicity determination test of the combination of Acynonapyr and spirotetramat on tetranychus cinnabarinus is carried out by a leaf disc spraying method, and the results shown in the table 3 show that: the mixture of the Acynonapyr and the spirotetramat with different proportions has synergistic effect on tetranychus cinnabarinus, wherein the synergistic effect range of the mixture of the Acynonapyr and the spirotetramat is 150.294, LC₅₀The value was 4.650 mg/L.

Table 3 Joint toxicity assay for Tetranychus cinnabarinus by different ratios of Acynonapyr to spirotetramat

The different acaricides have larger difference in the control effect on spider mites in different development stages, and the Acynonapyr is mixed with medicaments with different acaricidal characteristics such as azocyclotin, clofentezine, spirotetramat and the like for use, so that the pesticide effect can be increased, the pesticide cost can be reduced, the resistance development rate can be delayed, the service life of the medicaments can be prolonged, and the pesticide residue can be reduced, but the ideal control effect can not necessarily be achieved by mixing different acaricides. The experiment shows that Acynonapyr is mixed with azocyclotin, clofentezine and spirotetramat to determine the toxicity of tetranychus cinnabarinus and screen an optimal formula, and the result shows that the Acynonapyr: azacyclotin ═ 1:5, acyclonapyr: clofentezine ═ 5:1, Acynonapyr: the spirotetramat 1:5 is the optimal formula, and provides theoretical support for reasonable blending and using of acaricide.

Preparation example 1: 25% Acynonapyr azocyclotin suspension

3g of an alkylnaphthalenesulfonate formaldehyde condensate, 1g of an EO-PO block copolymer, 2g of sodium lauryl sulfate and 0.5g of an organosilicon antifoaming agent were dispersed in 50g of water, 5g of an Acynonapyr base drug and 20g of a azocyclotin base drug were dispersed therein, and wet-pulverization was carried out using glass beads by a sand mill to D90 (particle diameter of 90% of particles) < 10 μm, to obtain a pulverized slurry. Adding 0.2g of xanthan gum, 1g of magnesium aluminum silicate, 5g of ethylene glycol and 0.5g of sodium benzoate into the crushed slurry, uniformly mixing, complementing deionized water to 100g, and uniformly shearing at high speed to obtain the suspending agent with the mass content of the effective component of 25 wt%.

Preparation example 2: 20% Acynonapyr azocyclotin suspension

3g of an alkylnaphthalenesulfonate formaldehyde condensate, 1g of an EO-PO block copolymer, 2g of sodium lauryl sulfate and 0.5g of an organosilicon antifoaming agent were dispersed in 50g of water, 4g of a raw Acynonapyr and 16g of a raw azocyclotin were dispersed therein, and wet-pulverization was carried out using glass beads by a sand mill to D90 (particle diameter of 90% of particles) < 10 μm, to obtain a pulverized slurry. Adding 0.2g of xanthan gum, 1.0g of magnesium aluminum silicate, 5g of ethylene glycol and 0.5g of sodium benzoate into the crushed slurry, uniformly mixing, complementing deionized water to 100g, and uniformly shearing at high speed to obtain the suspending agent with the mass content of the effective component of 20 wt%.

Preparation example 3: 20% Acynonapyr azocyclotin wettable powder

2g of Acynonapyr technical, 18g of azocyclotin technical, 10g of sodium lignosulfonate, 3g of sodium dodecyl sulfate and 100g of kaolin are added, pre-crushed and mixed uniformly, and then crushed by an airflow crusher until the fineness meets the requirement that at least 98 wt% passes through a 45 mu m test sieve, so as to prepare the wettable powder with the mass content of the effective components of 20 wt%.

Preparation example 4: 18% Acynonapyr azocyclotin wettable powder

Adding 3g of Acynonapyr raw drug, 15g of azocyclotin raw drug, 10g of sodium lignosulfonate, 3g of sodium dodecyl sulfate and 100g of kaolin to obtain a mixture, pre-crushing and uniformly mixing the mixture, and crushing the mixture by using an airflow crusher until the fineness of the mixture meets the requirement that at least 98 wt% of the mixture passes through a 45-micron test sieve to obtain wettable powder with the mass content of active ingredients of 18 wt%.

Preparation example 5: 40% Acynonapyr clofentezine wettable powder

Adding 35g of Acynonapyr raw drug, 5g of clofentezine raw drug, 10g of sodium lignosulfonate, 3g of sodium dodecyl sulfate and 100g of kaolin to obtain a mixture, pre-crushing and uniformly mixing the mixture, and crushing the mixture by using an airflow crusher until the fineness of the mixture meets the requirement that at least 98 wt% of the mixture passes through a 45-micron test sieve to obtain the wettable powder with the mass content of the effective components of 40 wt%.

Preparation example 6: 24% Acynonapyr clofentezine wettable powder

Adding 20g of Acynonapyr technical, 4g of clofentezine technical, 10g of sodium lignosulphonate, 3g of sodium dodecyl sulfate and 100g of kaolin to 100g, pre-crushing and mixing uniformly, and crushing by using an airflow crusher until the fineness meets the requirement that at least 98 wt% passes through a 45-micron test sieve to prepare the wettable powder with the mass content of the effective component of 24 wt%.

Preparation example 7: 20% Acynonapyr clofentezine suspension

3g of an alkylnaphthalenesulfonate formaldehyde condensate, 1g of an EO-PO block copolymer, 2g of sodium lauryl sulfate and 0.4g of an organosilicon antifoaming agent were dispersed in 50g of water, 16g of a raw drug Acynonapyr and 4g of a raw drug clofentezine were dispersed therein, and wet-pulverization was carried out using glass beads by a sand mill to D90 (particle diameter of 90% of particles) < 10 μm, to obtain a pulverized slurry. Adding 0.2g of xanthan gum, 1g of magnesium aluminum silicate, 5g of ethylene glycol and 0.5g of sodium benzoate into the crushed slurry, uniformly mixing, complementing deionized water to 100g, and uniformly shearing at high speed to obtain the suspending agent with the mass content of the effective component of 20 wt%.

Preparation example 8: 18% Acynonapyr clofentezine suspension

3g of an alkylnaphthalenesulfonate formaldehyde condensate, 1g of an EO-PO block copolymer, 2g of sodium lauryl sulfate, and 0.4g of an organosilicon antifoaming agent were dispersed in 50g of water, 15g of a raw drug Acynonapyr and 3g of a raw drug clofentezine were dispersed therein, and wet-pulverization was carried out using glass beads by a sand mill to D90 (particle diameter of 90% of particles) < 10 μm, to obtain a pulverized slurry. Adding 0.2g of xanthan gum, 1.0g of magnesium aluminum silicate, 5g of ethylene glycol and 0.5g of sodium benzoate into the crushed slurry, uniformly mixing, complementing deionized water to 100g, and uniformly shearing at high speed to obtain the suspending agent with the mass content of the effective component of 20 wt%.

Preparation example 9: 45% Acynonapyr spirotetramat water dispersible granule

Adding 5g of Acynonapyr raw drug, 40g of spirotetramat raw drug, 6g of lignosulfonate, 2g of alpha-olefin sulfonate, 2g of ammonium carbonate and bentonite to 100g, uniformly mixing, crushing by an airflow crusher to be less than 15 mu m, uniformly mixing with 15g of water, granulating by a rotary granulator, drying at 60 ℃ until the water content is less than or equal to 1%, screening by using a 20-mesh and 60-mesh test sieve, and discarding upper large particles and dust filtered at the bottom to obtain the water dispersible granule with the effective component mass content of 45 wt%.

Preparation example 10: 24% Acynonapyr spirotetramat suspending agent

3g of an alkylnaphthalenesulfonate formaldehyde condensate, 1g of an EO-PO block copolymer, 2g of sodium lauryl sulfate, and 0.4g of an organosilicon antifoaming agent were dispersed in 50g of water, 20g of a raw Acynonapyr and 4g of a raw spirotetramat were dispersed therein, and wet-pulverization was carried out using glass beads by a sand mill to D90 (particle diameter of 90% of particles) < 10 μm, to obtain a pulverized slurry. Adding 0.2g of xanthan gum, 1g of magnesium aluminum silicate, 5g of ethylene glycol and 0.5g of sodium benzoate into the crushed slurry, uniformly mixing, complementing deionized water to 100g, and uniformly shearing at high speed to obtain the suspending agent with the mass content of the effective component of 24 wt%.

Preparation example 11: 20% Acynonapyr spirotetramat water dispersible granule

Adding 4g of Acynonapyr raw drug, 16g of spirotetramat raw drug, 6g of lignosulfonate, 2g of alpha-olefin sulfonate, 2g of urea and bentonite to 100g, uniformly mixing, crushing by an airflow crusher to be less than 15 mu m, uniformly mixing with 15g of water, granulating by a rotary granulator, drying at 60 ℃ until the water content is less than or equal to 1%, screening by using a 20-mesh and 60-mesh test sieve, discarding upper large particles and dust filtered at the bottom, and preparing the water dispersible granule with the mass content of the effective component of 20 wt%.

Preparation example 12: 12% Acynonapyr spirotetramat suspending agent

4g of an alkylnaphthalenesulfonate formaldehyde condensate, 2g of an EO-PO block copolymer, 3g of sodium lauryl sulfate, and 0.5g of an organosilicon antifoaming agent were dispersed in 50g of water, 2g of an Acynonapyr crude drug and 10g of a spirotetramat crude drug were dispersed therein, and wet-pulverization was carried out using glass beads by a sand mill to D90 (particle diameter of 90% of particles) < 10 μm, to obtain a pulverized slurry. Adding 0.2g of xanthan gum, 1g of magnesium aluminum silicate, 5g of ethylene glycol and 0.5g of sodium benzoate into the crushed slurry, uniformly mixing, complementing deionized water to 100g, and uniformly shearing at high speed to obtain the suspending agent with the mass content of the active ingredient of 12 wt%.

Comparative example 1:20 wt% Acynonapy suspending agent

3g of a phosphate dispersant, 1g of calcium dodecylbenzenesulfonate and 0.2g of an organosilicon antifoaming agent were dispersed in 50g of water, 20g of Acynonapyr was dispersed therein, and wet-grinding was performed using glass beads to D90 (particle size of 90% particles) < 10 μm using a sand mill to obtain 80g of a ground slurry. 0.3g of xanthan gum, 4g of ethylene glycol and 0.5g of sodium benzoate are added into 80g of the crushed slurry, mixed, supplemented with water to 100g, and uniformly sheared at high speed to prepare suspension with the mass content of the active ingredients of 20 wt%.

Comparative example 2: 20 wt% azocyclotin suspension

2g of polycarboxylate, 2g of calcium dodecylbenzenesulfonate and 0.2g of silicone antifoaming agent were dispersed in 50g of water, and 20g of raw azocyclotin was dispersed therein, and wet-pulverized using glass beads by a sand mill to D90 (particle diameter of 90% particles) < 10 μm, to obtain a pulverized slurry. Adding 0.3g of xanthan gum, 0.4g of organic bentonite, 4g of ethylene glycol and 0.5g of sodium benzoate into the crushed slurry, mixing, supplementing water to 100g, and uniformly shearing at high speed to obtain suspension with the mass content of the active ingredients of 20 wt%.

Comparative example 3: 30 wt% clofentezine suspension

3g of an alkylnaphthalenesulfonate formaldehyde condensate, 1g of an EO-PO block copolymer, 1g of a Morwet EFW and 0.2g of a silicone antifoaming agent were dispersed in 50g of water, 30g of a clofentezine base drug was further dispersed therein, and wet-pulverization was carried out using glass beads by a sand mill to D90 (particle diameter of 90% of particles) < 10 μm, to obtain a pulverization slurry. Adding 0.2g of xanthan gum, 0.5g of white carbon black, 4g of ethylene glycol and 0.5g of sodium benzoate into the crushed slurry, mixing, supplementing water to 100g, and uniformly shearing at high speed to obtain the suspending agent with the mass content of the active ingredient of 30 wt%.

Comparative example 4: 22.4% spirotetramat suspension

3g of an alkylnaphthalenesulfonate formaldehyde condensate, 1g of an EO-PO block copolymer, 1g of a Morwet EFW and 0.2g of a silicone antifoaming agent were dispersed in 50g of water, 22.4g of a crude spirotetramat was further dispersed therein, and wet-pulverization was carried out using glass beads by a sand mill to D90 (particle diameter of 90% of particles) < 10 μm, to obtain a pulverized slurry. Adding 0.2g of xanthan gum, 0.5g of white carbon black, 4g of ethylene glycol and 0.5g of sodium benzoate into the crushed slurry, mixing, supplementing water to 100g, and uniformly shearing at high speed to obtain the suspending agent with the mass content of the active ingredient of 30 wt%.

Example 5 field test for controlling Tetranychus cinnabarinus

Test protocol

Test work: cotton Gossypium spp

Test subjects: tetranychus cinnabarinus

The cotton seed with higher damage degree (more than 20% of cotton plant with mite) of Tetranychus cinnabarinus in Jining city of Shandong province in 7 th LaueAnd (4) carrying out plantation. The soil fertility of the test field is medium, the terrain is smooth, the fertility is uniform, and the irrigation condition is good. All test plot cultivation conditions (soil type, fertilization, cultivation, row spacing, etc.) were uniform and consistent with local agricultural cultivation practices (GAP). The preparation treatment, control treatment and blank control are arranged in random blocks, and the cell area is 20m²Repeating the steps for 4 times, wherein the pesticide application instrument is a WS-16D guard electric sprayer, the spray head is a single fan-shaped fog spray head, the working pressure is 0.15-0.4Mpa, and the dosage is accurately measured according to the dosage requirement of the pesticide and the area of a cell. When dispensing, firstly adding clean water with one third of actual water consumption into the sprayer, adding a little water into the small measuring cup to uniformly stir the medicament, pouring the medicament into the sprayer, and finally adding the rest water and uniformly mixing. When the pesticide is applied, the control is sprayed firstly, and the spraying is carried out from low concentration to high concentration in sequence, and the constant spraying method is adopted, and the uniform spraying is carried out at a constant speed according to the calculated step speed. When different medicaments are replaced, the sprayer is cleaned for three times, and water in the spray rod is completely sprayed out.

The weather during the test period is good, and on the reagent day, the daily average temperature is 20 ℃, the highest temperature is 27 ℃, the lowest temperature is 19 ℃ and the relative humidity is 72%.

The investigation method comprises the following steps: investigating population base number before reagent, investigating 40 leaves of each district strain setting hang tag, and the population number of mites before treatment is not less than 500; live mite numbers were investigated 1d, 7d, 14d after application.

The drug effect calculation method comprises the following steps: the drug effect is calculated by the following formula (6) and formula (7):

during the test period, the cotton growth in each treatment cell is observed to be good, and no phytotoxicity is found in each treatment.

The test results of the treatment medicaments for preventing and treating cotton tetranychus cinnabarinus are as follows:

TABLE 4 field test results of different test agents on Tetranychus cinnabarinus

Note: the control (%) in the table above is the average of each repetition. Lower case letters represent 5% level difference and upper case letters represent 1% level difference.

As can be seen from the results of field tests of different test agents on tetranychus cinnabarinus in Table 4, the acaricide composition obtained by compounding Acynonapyr with azocyclotin, Acynonapyr with clofentezine, and Acynonapyr with spirotetramat has good quick-acting property on tetranychus cinnabarinus. 1d after the application, the control effect of each compound medicament is more than 77.93 percent, the IBM SPSS data processing software is used for processing test data by a Duncan new double-pole error (Duncan) method, and the analysis result of variance shows that the compound treatments are at the level of 0.01, so that the compound treatments have no difference, but have difference with single agents of azocyclotin, clofentezine and spirotetramat in the control example; after application, the control effect of 25 percent of Acynonapyr azocyclotin suspending agent reaches 97.30 percent at 7d, the control effect of 12 percent of Acynonapyr spirotetramat suspending agent in each compound group is lower and is 86.49 percent, and compared with a control example, the control effect is obviously different at the levels of 0.01 and 0.05 and is higher than that of a single agent.

TABLE 5 field test results of different test agents on tetranychus cinnabarinus

As can be seen from the results of field tests of different test agents on tetranychus cinnabarinus in Table 5, the acaricide composition prepared by compounding Acynonapyr with azocyclotin, Acynonapyr with clofentezine, and Acynonapyr with spirotetramat has good persistent effect on tetranychus cinnabarinus. 14d after the suspension is applied, the control effect of the 20% Acynonapyr clofentezine suspension is 96.86%, each compound medicament is above 83.20%, and test data are processed by using IBM SPSS data processing software through a Duncan method, wherein the analysis of variance shows that under the level of 0.01, no significant difference exists between the 12% Acynonapyr spirotetramat suspension and the 45% Acynonapyr spirotetramat water dispersible granule, and the control effect of the 22.4% spirotetramat suspension is the highest after the 14d after the suspension is applied; 61.96 percent, the control effect of the single-dose control medicament of the 20 percent azocyclotin suspending agent and the 30 percent clofentezine suspending agent is increased along with the increase of the application time, and the control effect is the highest at 21d after the application, namely 71.92 percent and 78.39 percent respectively; the control effect of 12% Acynonapyr spirotetramat after application for 21d is 76.58, and other compound medicines are more than 92.43%. The quick-acting performance and the lasting effect of the compounded acaricidal composition on tetranychus cinnabarinus of cotton are superior to the control effect of a single agent, which shows that the acaricidal composition or the preparation thereof obtained by compounding has obvious control effect.

Example 6 field test for control of Panonychus citri

Test protocol

Test work: citrus fruit

Test subjects: panonychus citri (Panocychs citri Wcgregov)

The test was conducted in a citrus plantation with high damage degree (average live mites per leaf is greater than 2) for the red mites of the south Fengju in the west of the middle ten days of 4 months. The soil fertility of the test field is medium, the terrain is smooth, the fertility is uniform, and the irrigation condition is good. All test plot cultivation conditions (soil type, fertilization, cultivation, row spacing, etc.) were uniform and consistent with local agricultural cultivation practices (GAP). The preparation treatment, the comparison treatment and the blank comparison are arranged in a random block group, the area of a cell is 2-3 fruit trees and is repeated for 4 times, the pesticide application apparatus is a WS-16D guard electric sprayer, a spray head is a single fan-shaped fog spray head, the working pressure is 0.15-0.4Mpa, and the dosage is accurately measured according to the area of the cell according to the dosage requirement of the pesticide. When dispensing, firstly adding clean water with one third of actual water consumption into the sprayer, adding a little water into the small measuring cup to uniformly stir the medicament, pouring the medicament into the sprayer, and finally adding the rest water and uniformly mixing. When the pesticide is applied, the control is sprayed firstly, and the spraying is carried out from low concentration to high concentration in sequence, and the constant spraying method is adopted, and the uniform spraying is carried out at a constant speed according to the calculated step speed. When different medicaments are replaced, the sprayer is cleaned for three times, and water in the spray rod is completely sprayed out.

The weather during the test period is good, and on the test medicine day, the daily average temperature is 17 ℃, the highest temperature is 20 ℃, the lowest temperature is 15 ℃ and the relative humidity is 68%.

The investigation method comprises the following steps: the tender tips are marked in five directions of east, west, south, north and middle of the tree in each district, 25 leaves of a plant-fixing hang tag in each district are investigated, and the number of the mites is not less than 250 before treatment; live mite numbers were investigated 1d, 7d, 14d after application.

during the test period, the growth of the citrus in each treatment cell is observed to be good, and no phytotoxicity is generated in each treatment.

The test results of the treatment medicaments for preventing and treating panonychus citri are as follows:

TABLE 6 field test results of different test agents on Panonychus citri Paniculatus

The results of field tests show (table 6) that different test agents have good control effects on panonychus citri, 1d after the application of the acaricide composition, the control effects of the acaricide composition obtained by compounding Acynonapyr with azocyclotin, Acynonapyr with clofentezine, Acynonapyr with spirotetramat on panonychus citri are above 89.22%, each combination shows good quick-acting performance, test data are processed by using an IBM SPSS data processing software through a Duncan method, and the results of variance analysis show that at the levels of 0.01 and 0.05, each compound group and a control group have differences. The 20 wt% of Acynonapyr suspending agent and the 20 wt% of azocyclotin suspending agent have no obvious difference in control effect after being applied for 1 day, the 30% of clofentezine suspending agent and the 22.4% of spirotetramat suspending agent have poor control effect and quick action after being applied for 1 day, and the control effect increases to 62.59% and 63.03% after being applied for 3 days along with the increase of time, so that the difference between the two does not exist. The 12% Acynonapyr spirotetramat suspending agent has better quick-acting performance on panonychus citri, and the control effect is 93.51% after 1 day of application. According to test results, when the panonychus citri is initially developed, the damage of the panonychus citri can be effectively controlled in a short time by using each compound acaricide, the economic loss of the insect pest to the citrus is reduced, uniform spraying is recommended when the acaricide is applied, and the leaf back is sprayed intensively.

TABLE 7 field test results of different test agents on Panonychus citri Paniculatus

The results of field tests show (table 7) that different test agents have good control effects on panonychus citri, after application of the acaricide composition, after 21d, the control effects of the acaricide composition obtained by compounding Acynonapyr with azocyclotin, Acynonapyr with clofentezine, Acynonapyr with spirotetramat on panonychus citri are above 89.03%, each combination shows good persistence, test data are processed by IBM SPSS data processing software through a Duncan method, and the results of variance analysis show that no difference exists between each compounded group and the control group at the levels of 0.01 and 0.05, and the differences exist between the compounded groups and the control group. There was no significant difference in 21d control between the 20 wt% acyclononapyr suspension and the 20% azocyclotin suspension after application, and there was a difference in the control between the 30% clofentezine suspension and the 22.4% spirotetramat suspension at levels lower than the 20 wt% acyclononapyr suspension and the 20% azotin suspension at both the 0.01 and 0.05 levels. 25% of Acynonapyr/azocyclotin suspension, 20% of Acynonapyr/azocyclotin wettable powder, 40% of Acynonapyr/clofentezine wettable powder, 24% of Acynonapyr/clofentezine wettable powder, 20% of Acynonapyr/clofentezine suspension, 18% of Acynonapyr/clofentezine suspension, 24% of Acynonapyr/spirotetramat suspension, 20% of Acynonapyr/spirotetramat water dispersible granules and 12% of Acynonapyr/spirotetramat suspension have the highest 14d control effect after the pesticide. The test results show that the Acynonapyr, azocyclotin, clofentezine and spirotetramat have better control effect on panonychus citri, and have low toxicity and low residue, and the phenomena of phytotoxicity generated by oranges in various application treatment areas and natural enemy insect killing are not seen.

Through indoor toxicity measurement and tests on field cotton and citrus, the acaricidal composition compounded by any one of Acynonapyr, azocyclotin, clofentezine and spirotetramat has a good control effect on phytophagous harmful mites. The acaricidal composition or the preparation thereof obtained by compounding the acaricidal composition has obvious control effect, and is superior to a single preparation in the aspects of delaying the generation of drug resistance and prolonging the drug-holding property. And the compound pesticide is not found to cause phytotoxicity to crops in the test, which shows that the production cost and the use cost can be reduced and the pesticide is safe to crops under the condition that the acaricidal synergy of the obtained acaricidal composition or the preparation is improved.

Claims

1. The acaricidal composition containing Acynonapyr is characterized by comprising an active ingredient A, Acynonapyr and an active ingredient B, namely azocyclotin, wherein the mass ratio of the active ingredient A to the active ingredient B is 50: 1-1: 50.

2. The acaricidal composition according to claim 1, wherein the mass ratio of Acynonapyr to azocyclotin is 10: 1-1: 10.

3. The acaricidal composition according to claim 1, wherein the mass ratio of Acynonapyr to azocyclotin is 5: 1-1: 5.

4. An acaricidal composition according to claim 1, wherein the sum of the contents of active ingredient a and active ingredient B in the acaricidal composition is 1 to 95 wt%, based on 100 wt% of the total weight of the acaricidal composition.

5. An acaricidal composition according to claim 4, characterized in that the sum of the contents of active ingredient A and active ingredient B in the acaricidal composition is 5 to 80 wt%, based on 100 wt% of the total weight of the acaricidal composition.

6. The acaricidal composition according to claim 5, wherein the sum of the content of Acynonapyr and azocyclotin in the acaricidal composition is 10-25 wt% based on 100 wt% of the total weight of the acaricidal composition.

7. An acaricidal composition according to claim 1, characterized in that it further comprises adjuvants selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, antifoaming agents, solvents, preservatives, stabilizers, synergists and carriers.

8. A miticidal composition according to claim 7, in the form of an emulsion selected from the group consisting of emulsifiable concentrates, aqueous emulsions, microemulsions, suspensions, wettable powders, water dispersible granules.

9. An acaricidal composition according to claim 8, characterized in that it is in the form of a suspension, wettable powder, water dispersible granules.

10. Use of an acaricidal composition according to any one of claims 1 to 9 for controlling phytophagous mites.

11. The use of claim 10, wherein the phytophagous pest mites are tetranychus cinnabarinus, panonychus ulmi.