CN111789123A

CN111789123A - Insecticidal composition containing fluorine-containing chlorantraniliprole

Info

Publication number: CN111789123A
Application number: CN201910279015.9A
Authority: CN
Inventors: 葛家成; ***; 司国栋
Original assignee: Hailir Pesticides and Chemicals Group Co Ltd
Current assignee: Hailir Pesticides and Chemicals Group Co Ltd
Priority date: 2019-04-09
Filing date: 2019-04-09
Publication date: 2020-10-20

Abstract

The invention discloses a fluorine-containing chlorantraniliprole insecticidal composition, which comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is chlorantraniliprole, the active ingredient B is one selected from ethiprole, buprofezin, fipronil, butynitrile, chlorfenapyr, pyrimethanil and cyromazine, and the weight ratio of the active ingredient A to the active ingredient B is 1: 80-80: 1. The composition has a synergistic effect on prevention and control of various pests which are harmful to agricultural production, reduces the pesticide dosage, reduces the residual quantity of pesticides on crops, lightens environmental pollution, is safe to human and livestock, has good environmental compatibility, and is not easy to cause drug resistance of pests.

Description

Insecticidal composition containing fluorine-containing chlorantraniliprole

Technical Field

The invention relates to the field of biological pesticide preparation and research and development, and particularly relates to a fluorine-containing chlorantraniliprole insecticidal composition.

Background

Crop diseases and insect pests are one of the main agricultural disasters in China, and the crop diseases and insect pests have the characteristics of multiple varieties, great influence and frequent outbreak of disasters, and the occurrence range and the severity of the crop diseases and insect pests cause great loss to national economy, particularly agricultural production in China. The following types of plant diseases and insect pests are common in crops in China: the pesticide composition is characterized by comprising the following components of rice leaf rollers, striped rice borers, asparagus caterpillars, diamond back moths, rice planthoppers, powdery mildew, corn borers, cotton bollworms, wheat rust diseases, cotton aphids, rice sheath blight diseases, rice blast, wheat aphids, wheat red spiders, locusts, wheat scabs and the like, and has become important plant diseases and insect pests which seriously affect the agricultural production in China.

The flubendiamide is a new compound independently innovated and developed by our company, belongs to benzamide insecticides, and can efficiently activate insect ryanodine (muscle) receptors to excessively release calcium ions in intracellular calcium stores, so that insects die by paralysis. High activity to lepidoptera pest larva, broad spectrum and high durability. The active ingredient shows very significant selectivity difference to mammalian and pest ryanodine receptors, greatly improving safety to mammals and other vertebrates.

Ethiprole is a phenylpyrazole insecticide and is a chlorine channel blocker regulated and controlled by GABA. Is used for preventing and controlling chewing and sucking pests (such as thrips, plant louse, stinkbug, weevil, leaf miner, aphid, stink bug, rice planthopper and grasshopper), and is used for seed treatment or foliage spraying in rice, fruit trees and vegetable planting.

Buprofezin is a chitin synthesis inhibitor that has an effect after deposition of the outer skin and also has an effect on the hormone levels of the larvae. The buprofezin is a residual-effect type insecticide and acaricide, has contact poisoning and stomach poisoning activities, has no systemic property, can inhibit death of larvae caused by skin change, also can inhibit ovulation of adults, and can cause inactive eggs produced by insects.

Fipronil is a pyrazole insecticide, the mechanism of action is to destroy central transmission in the central nervous system by hindering chloride transmission regulated by GABA, and pests with drug resistance and drug resistance to pyrethroid, organophosphorus and carbamate insecticides are sensitive to fipronil. Fipronil is a broad-spectrum pesticide with contact and stomach poisoning activities, can prevent and treat thrips harming most crops by foliar spraying, soil treatment or seed treatment, can prevent and treat corn rootworm, wireworm and termite by foliar spraying, can prevent and treat cotton weevil and lygus, and can also prevent and treat cruciferous plutella xylostella, potato beetle and rice stem borer, plant hopper, thrips and rice beetle.

The chlorfenapyr belongs to aryl pyrrole insecticidal and acaricidal agents, the action mechanism of the chlorfenapyr is that N-ethoxy methyl groups in a living body are oxidized and removed to generate an active substance, namely a mitochondrion decoupling agent, the poisoning effect of the chlorfenapyr is mainly stomach poisoning effect, and the chlorfenapyr has partial contact activity and can be used for preventing and controlling various pests and mites of cotton, vegetables, oranges and tangerines and soybeans.

Cyromazine is a 1,3, 5-triazine insect growth regulator, has special activity on dipteran larvae, can induce dipteran larvae and pupae to be morphologically distorted, and enable adult eclosion to be incomplete or inhibited, and can be used for controlling flies in animal barns and controlling agricultural pests such as Liriomyza sativae on cucumbers, eggplants, kidney beans, leafy vegetables and flowers.

In the actual production process of agricultural production, the most easily generated problem for controlling pests is the generation of drug resistance of pests. The composition with different action mechanisms is a very effective method for controlling resistant pests, namely different compositions are compounded, and whether certain compounding is synergistic, additive or antagonistic is judged according to the actual application effect. Through the research of the inventor, the excellent synergistic effect can be generated after the flubendiamide is compounded with any one of ethiprole, buprofezin, fipronil, buthionil, chlorfenapyr, pyrimethanil and cyromazine, and no related report about the compounding of the flubendiamide and any one of the ethiprole, the buprofezin, the fipronil, the chlorfenapyr and the cyromazine is available.

Disclosure of Invention

The invention aims to provide the insecticidal composition containing the fluorine-containing cloxacarb-diamide, which has the advantages of synergistic interaction, low use cost and good control effect;

another object of the present invention is to provide a formulation of a pesticidal composition comprising a flubendiamide;

still another object of the present invention is to provide the use of the above composition for controlling crop pests.

The composition containing the fluorine-containing cloxachlor diamide comprises an active ingredient A and an active ingredient B, wherein the weight ratio of the active ingredient A to the active ingredient B is 1: 80-80: 1, the active ingredient A is the fluorine-containing clofenamide, and the active ingredient B is selected from one of ethiprole, buprofezin, fipronil, butronitrile, chlorfenapyr, pyrimethanil and cyromazine;

further, the active ingredient B is preferably one of ethiprole, buprofezin, fipronil, chlorfenapyr and cyromazine;

further, the weight ratio of the active ingredient A to the active ingredient B is 1: 50-50: 1;

further, the weight ratio of the fipronil bisamide to the ethiprole is 1: 30-30: 1, the weight ratio of the fipronil bisamide to the buprofezin is 1: 20-20: 1, and the weight ratio of the fipronil bisamide to the fipronil is 1: 30-20: 1, the weight ratio of the chlorofluorobisphenol to the chlorfenapyr is 1: 30-20: 1; the weight ratio of the flubendiamide to the cyromazine is 1: 30-30: 1;

further, the weight ratio of the fipronil bisamide to the ethiprole is 1: 10-10: 1, the weight ratio of the fipronil bisamide to the buprofezin is 1: 5-5: 1, and the weight ratio of the fipronil bisamide to the fipronil is 1: 5-5: 1, the weight ratio of the chlorofluorobisphenol to the chlorfenapyr is 1: 5-5: 1, and the weight ratio of the chlorofluorobisphenol to the cyromazine is 1: 10-10: 1.

Generally, the weight of active ingredient in the composition is from 0.5% to 90%, preferably from 5% to 80% by weight of the total weight. The range of the content of the active ingredient varies depending on the dosage form. Generally, the weight of the active ingredients of the liquid preparation accounts for 1 to 70 percent of the total weight, and preferably 5 to 50 percent; the active ingredients of the solid preparation account for 5-80 percent of the total weight, preferably 10-80 percent.

The composition of the present invention may be diluted or directly used by a user before use, and its formulation may be prepared by a general processing method known to those skilled in the art.

The insecticidal composition preparation is prepared into any one of formulations allowed in the field of pesticides by active ingredients and pesticide auxiliary ingredients;

further, the auxiliary components of the pesticide preparation comprise a carrier and an auxiliary agent;

further, the carrier is any one, two or three of water, a solvent or a filler, and the water is preferably deionized water;

further, the solvent is selected from one or a mixture of more of N, N-dimethylformamide, cyclohexanone, toluene, xylene, dimethyl sulfoxide, methanol, ethanol, trimethylcyclohexanone, N-octylpyrrolidone, ethanolamine, triethanolamine, isopropylamine, N-methylpyrrolidone, propanol, butanol, ethylene glycol, diethylene glycol, ethylene glycol methyl ether, butyl ether, ethanolamine, isopropylamine, ethyl acetate or acetonitrile;

further, the filler is selected from one or a mixture of more of kaolin, diatomite, bentonite, attapulgite, white carbon black, starch or light calcium carbonate;

furthermore, the auxiliary agent at least comprises a surfactant, and other functional auxiliary agents such as an antifreezing agent, a thickening agent, a stabilizing agent, a disintegrating agent, a defoaming agent and the like can be added according to different use occasions and requirements;

further, the surfactant is selected from one or more of an emulsifier, a dispersant, a wetting agent or a penetrant;

further, the other functional auxiliary agents are selected from one or more of an antifreezing agent, a thickening agent, a stabilizing agent, a disintegrating agent or a defoaming agent;

further, the emulsifier is selected from one or more of agricultural milk 500# (calcium alkyl benzene sulfonate), OP series phosphate ester (nonylphenol polyoxyethylene ether phosphate ester), 600# phosphate ester (phenylphenol polyoxyethylene ether phosphate ester), styrene polyoxyethylene ether ammonium sulfate salt, magnesium salt of alkyl diphenyl ether disulfonate, triethanolamine salt, agricultural milk 400# (benzyldimethylphenol polyoxyethylene ether), agricultural milk 700# (alkylphenol formaldehyde resin polyoxyethylene ether), Ningru 36# (phenethylphenol formaldehyde resin polyoxyethylene ether), agricultural milk 1600# (phenethylphenol polyoxyethylene polyoxypropylene ether), ethylene oxide-propylene oxide block copolymer, OP series (nonylphenol polyoxyethylene ether), BY series (castor oil polyoxyethylene ether), agricultural dehydrated milk 33# (alkylaryl polyoxyethylene polyoxypropylene ether), span series (sorbitan monostearate), Tween series (sorbitan fatty acid ester polyoxyethylene ether) or AEO series (fatty alcohol polyoxyethylene ether) A mixture of seed constituents;

further, the dispersing agent is selected from one or a mixture of a plurality of polycarboxylate, lignosulfonate, alkylphenol polyoxyethylene formaldehyde condensate sulfate, calcium alkylbenzene sulfonate, naphthalene sulfonic acid formaldehyde condensate sodium salt, alkylphenol polyoxyethylene, fatty amine polyoxyethylene, fatty acid polyoxyethylene or glycerol fatty acid ester polyoxyethylene;

further, the wetting agent is selected from one or a mixture of more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, nekal BX, wetting penetrant F, Chinese honeylocust fruit powder, silkworm excrement or soapberry powder;

further, the penetrating agent is selected from a mixture consisting of one or more of penetrating agent JFC (fatty alcohol-polyoxyethylene ether), penetrating agent T (diisooctyl maleate sulfonate), azone or organic silicon;

further, the antifreezing agent is a mixture consisting of one or more of ethylene glycol, propylene glycol, glycerol or urea;

further, the thickening agent is selected from one or more of xanthan gum, polyvinyl alcohol, bentonite, carboxymethyl cellulose or magnesium aluminum silicate;

further, the stabilizer is selected from one or more of epoxidized soybean oil, epichlorohydrin, BHT, ethyl acetate and triphenyl phosphate;

further, the disintegrating agent is selected from one or more of bentonite, urea, ammonium sulfate, aluminum chloride, low-substituted hydroxypropyl cellulose, lactose, citric acid, succinic acid or sodium bicarbonate;

further, the defoaming agent is selected from one or a mixture of more of silicone oil, silicone compounds, C10-C20 saturated fatty acid compounds or C8-C10 fatty alcohol compounds;

all of the above are commercially available.

The composition can be processed into agriculturally acceptable dosage forms, wherein the preferred dosage forms are wettable powder, suspending agent, water dispersible granule and suspension seed coating agent;

further, the composition is prepared into wettable powder, and the components and the content of the wettable powder are preferably as follows: 0.1-80% of active ingredient A, 0.1-80% of active ingredient B, 2-10% of dispersing agent, 2-10% of wetting agent and the balance of filler;

further, the composition is prepared into a suspending agent, and the components and the content of the suspending agent are preferably as follows: 0.1-80% of active ingredient A, 0.1-80% of active ingredient B, 2-10% of dispersing agent, 2-10% of wetting agent, 0.01-2% of defoaming agent, 0-2% of thickening agent, 0-8% of antifreeze agent and the balance of deionized water;

further, the composition is prepared into water dispersible granules, and the components and the content of the water dispersible granules are preferably as follows: 0.1-80% of active ingredient A, 0.1-80% of active ingredient B, 3-12% of dispersing agent, 1-8% of wetting agent, 1-10% of disintegrating agent and the balance of filler;

further, the composition is prepared into a suspension seed coating agent, and the components and contents of the suspension seed coating agent are preferably as follows: 0.1-80% of active ingredient A, 0.1-80% of active ingredient B, and water-retaining agent: 1% -3%, film-forming agent: 0.5-3%, wetting dispersant: 1% -3%, thickening agent: 1% -2% of an antifreezing agent: 1% -2%, warning color: 0.5 to 3 percent and deionized water for complementing the balance.

The composition can be used as a control agent for crop pests.

The invention has the advantages that:

1. the composition shows obvious synergistic effect in a certain proportioning range, and the control effect on pests is improved;

2. the composition can reduce the dosage of the compound in application, thereby reducing the use cost and reducing the environmental pollution;

3. the active ingredients in the composition have different action mechanisms, so that the problem of cross resistance does not exist, the occurrence of drug resistance of pests can be delayed, and the control effect can be effectively improved.

Detailed Description

The present invention will be described in more detail with reference to examples. The practice of the invention is not limited to the following examples, and any variations or modifications in practice of the invention are intended to fall within the scope of the invention. The methods in the following examples are conventional in the art unless otherwise specified.

Preparation of the preparation

Example 1: 18% wettable powder of biformamide and ethiprole (10:8)

The formula is as follows: 10% of chlorofluorobisphenol, 8% of ethiprole, 5% of octylphenol polyoxyethylene ether, 6% of sodium dodecyl benzene sulfonate and the balance of white carbon black.

The preparation method comprises the following steps: according to the formula proportion of the embodiment, the active ingredients of the fipronil bisamide and the ethiprole are added into the carrier, the surfactant and other functional additives are added into the carrier, the mixture is mixed, and the wettable powder is prepared by mixing the components after airflow pulverization.

Example 2: 22% wettable powder of biformamide and ethiprole (2:20)

The formula is as follows: 2% of chlorofluorobisphenol, 20% of ethiprole, 3% of lignosulfonate, BX 7% of nekal and the balance of kaolin.

The preparation method comprises the following steps: the same as in example 1.

Example 3: 25% wettable powder of flubendiamide buprofezin (5:20)

The formula is as follows: 5% of flubendiamide, 20% of buprofezin, 7% of benzyl dimethyl phenol polyoxyethylene ether, 6% of sodium dodecyl benzene sulfonate and the balance of white carbon black.

The preparation method comprises the following steps: the same as in example 1.

Example 4: 30% biflorfon-fipronil wettable powder (10:20)

The formula is as follows: 10% of chlorofluorobisphenol, 20% of fipronil, 7% of alkylphenol polyoxyethylene, 6% of nekal BX, and the balance of kaolin.

The preparation method comprises the following steps: the same as in example 1.

Example 5: 20% wettable powder of bifloram and chlorfenapyr (5:15)

The formula is as follows: 5% of flubendiamide, 15% of chlorfenapyr, 5% of lignosulfonate, 6% of sodium lauryl sulfate and the balance of white carbon black.

The preparation method comprises the following steps: the same as in example 1.

Example 6: 25% wettable powder of bifloramide and cyromazine (20:5)

The formula is as follows: 20% of flubendiamide, 5% of cyromazine, 5% of polycarboxylate, 7% of sodium dodecyl benzene sulfonate and the balance of kaolin.

The preparation method comprises the following steps: the same as in example 1.

Example 7: 40% Flucloxacarbdiamide ethiprole suspending agent (20:20)

The formula is as follows: 20% of chlorofluorobisphenol, 20% of ethiprole, 6% of naphthalene sulfonic acid formaldehyde condensate, 7% of sodium lauryl sulfate, 1% of silicone oil, 1% of sodium acrylate, 7% of glycerol and the balance of deionized water.

The preparation method comprises the following steps: according to the formula proportion, the active ingredient, namely the biformamide, the ethiprole, the surfactant and other functional auxiliaries are sequentially placed in a reaction kettle, water is added for uniform mixing, and the product is obtained through high-speed shearing, wet sanding and finally homogeneous filtration.

Example 8: 25% of fipronil bisamide ethiprole suspending agent (10:15)

The formula is as follows: 10% of fipronil bisamide, 15% of ethiprole, 7% of polycarboxylate, 7% of saponin powder, 1% of silicone, 1% of sodium tripolyphosphate and the balance of deionized water.

The preparation method comprises the following steps: the same as in example 7.

Example 9: 10% of Flucloxacarbdiamide buprofezin suspending agent (1:9)

The formula is as follows: 1% of flubendiamide, 9% of buprofezin, 7% of alkylphenol polyoxyethylene, 8% of sodium dodecyl sulfate, 1.5% of N, N-dimethylformamide, 1.5% of polyvinylpyrrolidone and the balance of deionized water.

The preparation method comprises the following steps: the same as in example 7.

Example 10: 30% of fipronil bisamide fipronil suspending agent (5:25)

The formula is as follows: 5% of flubendiamide, 25% of fipronil, 6% of benzyl dimethyl phenol polyoxyethylene ether, 7% of tea seed cake, 1.5% of silicone oil, 1% of fatty acid polyoxyethylene ether and the balance of deionized water.

The preparation method comprises the following steps: the same as in example 7.

Example 11: 15% of fipronil bisamide fipronil suspending agent (5:10)

The formula is as follows: 5% of chlorofluorobisphenol, 10% of fipronil, 7% of naphthalene sulfonic acid formaldehyde condensate, 6% of sodium dodecyl benzene sulfonate, 1% of silicone, 1% of phenolic resin, 5% of triethylene glycol and the balance of deionized water.

The preparation method comprises the following steps: the same as in example 7.

Example 12: 30% of fipronil bisamide and chlorfenapyr suspending agent (10:20)

The formula is as follows: 10% of flubendiamide, 20% of chlorfenapyr, 6% of fatty acid polyoxyethylene ether, 7% of nekal BX, 1% of amide, 1% of methyl cellulose, 6% of glycerol and the balance of deionized water.

The preparation method comprises the following steps: the same as in example 7.

Example 13: 8% of biformamide-ethiprole water dispersible granule (6:2)

The formula is as follows: 6% of chlorofluorobisphenol, 2% of ethiprole, 4% of lignosulfonate, 3% of sodium dodecyl benzene sulfonate, 5% of aluminum chloride and the balance of white carbon black.

The preparation method comprises the following steps: according to the formula proportion of the embodiment, adding active ingredients of the fipronil bisamide and the ethiprole into a carrier, adding a surfactant and other functional auxiliaries, mixing, performing jet milling, adding 10-25% of water, kneading, granulating, drying and screening to obtain a water dispersible granule product; or spraying water to the pulverized powder in a boiling granulator, granulating, drying, and sieving to obtain the final product.

Example 14: 12% of Flucloxacarbdiamide buprofezin water dispersible granule (6:6)

The formula is as follows: 6% of chlorofluorobisphenol, 6% of buprofezin, 5% of naphthalene sulfonic acid formaldehyde condensate sodium salt, 5% of nekal BX, 3% of bentonite and the balance of kaolin.

The preparation method comprises the following steps: the same as in example 13.

Example 15: 30% of flumiclorac diamide buprofezin water dispersible granule (1:29)

The formula is as follows: 1% of flubendiamide, 29% of buprofezin, lignosulfonate, nekal BX, aluminum chloride and kaolin for the balance.

Example 16: 30% of biformamide fipronil water dispersible granule (10:20)

The formula is as follows: 10% of chlorofluorobisphenol, 20% of fipronil, 4% of naphthalene sulfonic acid formaldehyde condensate sodium salt, 6% of sodium dodecyl benzene sulfonate, 6% of bentonite and the balance of white carbon black.

Example 17: 10% of biflorfon-diamides-chlorfenapyr water dispersible granule (6:4)

The formula is as follows: 6% of chlorofluorobisphenol, 4% of chlorfenapyr, 8% of lignosulfonate, 5% of nekal BX, 4% of aluminum chloride and the balance of white carbon black.

Example 18: 25% of biflorfon-diamides-chlorfenapyr water dispersible granule (24:1)

The formula is as follows: 24% of chlorofluorobisphenol, 1% of chlorfenapyr, 4% of sodium naphthalenesulfonic acid-formaldehyde condensate, 6% of sodium dodecyl benzene sulfonate, 7% of bentonite and the balance of white carbon black.

Example 19: 30% of biformamide-cyromazine water dispersible granule (1:29)

The formula is as follows: 1% of fluorochlordiamide, 29% of cyromazine, 3% of lignosulfonate, 7% of nekal BX, 5% of aluminum chloride and the balance of kaolin.

Example 20: 15% of biformamide-cyromazine water dispersible granule (5:10)

The formula is as follows: 5% of chlorofluorodiamide, 10% of cyromazine, 5% of lignosulfonate, 4% of sodium dodecyl benzene sulfonate, 3% of bentonite and the balance of white carbon black.

Example 21: 11% of fipronil bisamide fipronil suspension seed coating agent (10:1)

The formula is as follows: 10% of chlorofluorobisphenol, 1% of fipronil, 1% of polyacrylamide, 0.5% of sodium carboxymethylcellulose, 1% of nonylphenol polyoxyethylene ether, 1% of xanthan gum, 1% of ethylene glycol, 1.5% of acid scarlet G and the balance of deionized water.

The preparation method comprises the following steps: weighing the components respectively, crushing solid components by using air flow, and then uniformly mixing the solid components with the components; adding the mixture into a sand mill with the rotation speed of 1100rpm by adopting a wet grinding process, and grinding for 4 hours; grinding, filtering the mixture, and shearing with high-shear emulsifier at 8000 rpm for 30 min; and finally, detecting the particle size of the sample by using a laser particle size analyzer, wherein the average particle size of more than 95 percent is 1-5 mu m, and the sample is qualified.

Example 22: 15% of fipronil bisamide fipronil suspension seed coating agent (13:2)

The formula is as follows: 13% of fipronil bisamide, 2% of fipronil, 1.2% of polyacrylamide, 0.6% of arabic gum, 1.5% of octyl phenol polyoxyethylene ether, 1% of xanthan gum, 1% of ethylene glycol, 0.6% of fuchsin and the balance of deionized water.

The preparation method comprises the following steps: the same as in example 21.

Example 23: 20% of fipronil bisamide fipronil suspension seed coating agent (17:3)

The formula is as follows: 17% of chlorofluorobisphenol, 3% of fipronil, 1.2% of polyacrylamide, 0.6% of sodium alginate, 1.5% of phenethyl phenol polyoxyethylene ether, 1% of xanthan gum, 1% of glycerol, 0.6% of acid bright red G and the balance of deionized water.

Indoor case of activity

The embodiment of the invention adopts an indoor toxicity determination method. Through indoor toxicity measurement, co-toxicity coefficients (CTC) of two medicaments compounded according to a certain proportion are determined, wherein the CTC is less than 80 and is antagonistic, the CTC is more than 120 and is synergistic, and the addition effect is between 80 and 120.

The test method comprises the following steps: calculating the mortality of pests, correcting the mortality, solving a toxicity regression equation and calculating LC₅₀The value is obtained.

If the control mortality was > 10%, it was considered as a null test.

The calculation formula is as follows:

by LC₅₀The relatively small-value agent is a standard agent, and the virulence index TI thereof is 100.

Of active ingredient B

Theoretical virulence index of the mixture

Toxicity index TTI ═ TI of the mixture_A×P_A+TI_B×P_B

Co-toxicity coefficient

In the formula: p_A、P_BRespectively is an active ingredient AAnd B is the proportion of the composition.

A is the biformamide of the fluorine chlorine. B is selected from one of ethiprole, buprofezin, fipronil, chlorfenapyr and cyromazine.

Example 24: combined toxicity of mixing of fipronil bisamide and ethiprole on rice planthopper

The tested pests: rice planthopper

Test agents: the technical grade of the flubendiamide and the technical grade of the ethiprole are provided by the Hilier pharmaceutical industry group, Inc.

And (3) experimental design: tests prove that the half Lethal Concentration (LC) of the mixture of the technical product of the fipronil and the technical product of the ethiprole in different proportions₅₀) And co-toxicity coefficient to determine the combined action type of the mixture of the fipronil bisamide and the ethiprole on the rice planthopper.

The test basis is as follows: NY/T1154.11-2008 "indoor bioassay of pesticides test quasi-lateral insecticides part 11: dipping method of rice stem.

Preparing a medicament: dissolving the raw medicine with acetone to prepare a mother solution, and then preparing the mother solution into 5 series of mass concentrations by using Tween water according to an equal ratio method.

Medicament treatment: soaking the prepared rice stem in the prepared medicinal liquid for 30s, taking out, air drying, wrapping the root with absorbent cotton for moisturizing, wrapping with preservative film, and placing in test tubes with 3 plants per test tube. Each treatment was repeated 4 times with a blank control.

And (3) test insect treatment: transferring 15 test insects into each treatment, covering the pipe orifice with gauze, placing the test tube in an environment with the temperature of 25 +/-1 ℃ and the relative humidity of 75% for feeding and observing, observing the death condition of the test insects after 48 hours of treatment, and respectively recording the number of dead insects.

Data statistics and analysis: calculating mortality, correcting mortality, and performing statistical analysis by using DPS statistical analysis system to obtain virulence regression equation and LC₅₀And its 95% confidence limit, evaluating the activity of the test agent on the target.

And (3) test results: see table 1.

TABLE 1 Combined virulence determination of rice planthopper by blending of fipronil bisamide and ethiprole

The indoor test data in table 1 show that the co-toxicity coefficient of the flubendiamide to the indoor activity of the rice planthopper is more than 80 when the mixing ratio of the flubendiamide to the ethiprole is 1: 50-50: 1, which indicates that the combined action of the flubendiamide and the ethiprole to the rice planthopper is additive or synergistic action when the flubendiamide and the ethiprole are mixed in the ratio range; when the mixing ratio of the fipronil bisamide to the ethiprole is 1: 30-30: 1, the indoor co-toxicity coefficient to the rice planthopper is more than 120, which shows that the combined action of the two in the range of the ratio is synergistic action to the rice planthopper; when the mixing ratio of the fipronil bisamide to the ethiprole is 1: 10-10: 1, the indoor co-toxicity coefficient to the rice planthoppers is larger than 150, and the fact that the two are mixed in the ratio range shows that the combined action type of the two on the rice planthoppers is a synergistic action and the synergistic effect is obvious.

Example 25: combined toxicity of mixed pair of flubendiamide and buprofezin on tea lesser leafhoppers

The tested pests: tea lesser leafhopper

Test agents: the technical grade of the flubendiamide and the buprofezin is provided by the Heliel pharmaceutical industry group, Inc.

And (3) experimental design: tests prove that the half Lethal Concentration (LC) of the mixture of the technical grade of the flubendiamide and the technical grade of the buprofezin₅₀) And co-toxicity coefficient to determine the combined action type of the mixture of the flubendiamide and the buprofezin on the tea lesser leafhoppers.

The test basis is as follows: NY/T1154.6-2006 "indoor bioassay of pesticides test criteria part 6: insect immersion method for insecticidal activity test.

Preparing a medicament: dissolving the raw medicine with acetone, adding a proper amount of Tween water for dilution, and setting 5 series of mass concentrations according to an equal ratio method, wherein the liquid medicine amount of each mass concentration is not less than 50 ml.

Treating the medicament and the test insects: soaking target tea lesser leafhopper into the liquid medicine for 10s, sucking redundant liquid medicine by using filter paper, and transferring the test insects to normal conditions for feeding. Each treatment was repeated 4 times, each time 20-head soaking, and a blank control was set.

Data statistical analysis: the death condition of the treated test insects is investigated for 24 hours, the number of the dead insects is recorded, and the mortality is calculated and corrected. And using DPS statistical analysis system to make statistical analysis to obtain virulence regression equation and LC₅₀And a 95% confidence limit, evaluating the activity of the test agent on the target tea lesser leafhopper.

And (3) test results: see table 2.

TABLE 2 Combined virulence determination of the Flucloxacarb bisamide and buprofezin in combination with tea lesser leafhoppers

The indoor test data in table 2 show that the co-toxicity coefficient of the flubendiamide to the indoor activity of the tea lesser leafhoppers is more than 80 when the mixing ratio of the flubendiamide to the buprofezin is 1: 50-50: 1, which indicates that the combined action of the flubendiamide and the buprofezin to the tea lesser leafhoppers in the ratio range is additive or synergistic; when the mixing ratio of the flubendiamide to the buprofezin is 1: 20-20: 1, the indoor co-toxicity coefficient to the tea lesser leafhoppers is more than 120, and the synergistic effect of the two in the mixing ratio range on the combined action of the tea lesser leafhoppers is shown; when the mixing ratio of the flubendiamide to the buprofezin is 1: 5-5: 1, the indoor co-toxicity coefficient to the tea lesser leafhoppers is more than 150, and the fact that the flubendiamide and the buprofezin are mixed in the ratio range shows that the combined action type of the flubendiamide and the buprofezin to the tea lesser leafhoppers is synergistic effect and obvious in synergistic effect.

Example 26: combined toxicity of mixture of fipronil bisamide and fipronil to cabbage diamondback moth

The tested pests: cabbage diamondback moth

Test agents: the technical grade of the flubendiamide compound and the technical grade of the fipronil compound are provided by the Heliel pharmaceutical industry group, Inc.

And (3) experimental design: tests prove that the technical grade of the flubendiamide and the technical grade of the fipronil and the different preparation of the twohalf-Lethal Concentration (LC) of a specific mixture₅₀) And the co-toxicity coefficient to determine the combined action type of the mixture of the flubendiamide and the fipronil on the cabbage diamondback moth.

Treating the medicament and the test insects: and (3) soaking the target plutella xylostella in the liquid medicine for 10s, sucking the redundant liquid medicine by using filter paper, and transferring the test insects to normal conditions for feeding. Each treatment was repeated 4 times, each time 20-head soaking, and a blank control was set.

Data statistical analysis: the death condition of the treated test insects is investigated for 24 hours, the number of the dead insects is recorded, and the mortality is calculated and corrected. And using DPS statistical analysis system to make statistical analysis to obtain virulence regression equation and LC₅₀And a 95% confidence limit, evaluating the activity of the test agent on the target plutella xylostella.

And (3) test results: see table 3.

TABLE 3 measurement of the combined toxicity of the mixture of biformamide and fipronil against cabbage diamondback moth

The indoor test data in table 3 show that the co-toxicity coefficient of the flubendiamide to the indoor activity of the cabbage diamondback moth is greater than 80 when the mixing ratio of the flubendiamide to the fipronil is 1: 50-50: 1, which indicates that the combined action of the two in the ratio range is additive or synergistic action to the cabbage diamondback moth; when the mixing ratio of the chlorofluorobisphenol to the fipronil is 1: 30-20: 1, the indoor co-toxicity coefficient to the cabbage diamondback moth is greater than 120, which shows that the combination effect of the two in the ratio range is a synergistic effect to the cabbage diamondback moth; when the mixing ratio of the chlorofluorobisphenol to the fipronil is 1: 5-5: 1, the indoor co-toxicity coefficient to the cabbage diamondback moth is more than 150, which shows that the combination type of the two in the ratio range is synergistic effect to the cabbage diamondback moth, and the synergistic effect is obvious.

Example 27: combined toxicity of mixing of fipronil bisamide and chlorfenapyr on cotton red spider

The tested pests: spider of cotton flower

Test agents: the technical grade of the flubendiamide compound and the chlorfenapyr compound are provided by the Heliel pharmaceutical industry group, Inc.

And (3) experimental design: tests prove that the half Lethal Concentration (LC) of the mixture of the technical grade of the fipronil bisamide and the technical grade of the chlorfenapyr and the mixture of the two technical grade with different proportions₅₀) And co-toxicity coefficient to determine the combined action type of the mixture of the fipronil and the chlorfenapyr on the cotton red spider.

The test basis is as follows: NY/T1154.13-2008 "indoor bioassay of pesticides test criteria insecticides part 13: leaf disc spray method.

Preparing a test material: selecting cotton red spiders which are bred indoors and have consistent physiological states. Selecting cotton leaves with consistent growth, making leaf disks by using a puncher, placing a piece of wet sponge in a culture dish, placing filter paper on the wet sponge, placing the leaf disks on the filter paper, placing 2 leaf disks on each dish, inoculating red spiders to the leaf disks, and inoculating 20 heads of the red spiders to each leaf disk.

Preparing a medicament: the raw medicine is prepared into mother liquor by acetone, and is prepared into 5 series of mass concentrations by adding water for spitting in equal proportion.

Treating the medicament and the test insects: placing the culture dish on a spraying tower chassis for spraying, wherein the spraying liquid amount is 1ml, taking out after the liquid medicine is settled for 1min, and transferring to a common feeding condition (the temperature is 25 +/-1 ℃) for feeding. Each treatment was repeated 4 times and a blank control was run.

Data statistical analysis: and (4) checking the death condition of the test insects 48 hours after treatment, recording the number of the dead insects, calculating the death rate and correcting the death rate. And using DPS statistical analysis system to make statistical analysis to obtain virulence regression equation and LC₅₀And 95% confidence limit, evaluating the test agent to the target cottonActivity of spider mites of the species Calonychus.

And (3) test results: see table 4.

TABLE 4 Joint virulence determination for cotton red spider by compounding of Flucloxacarbdiamide with Chlorfenapyr

Table 4 shows that the indoor active co-toxicity coefficients of the fipronil bisamide and the chlorfenapyr are both greater than 80 when the mixing ratio of the fipronil bisamide to the chlorfenapyr is 1: 50-50: 1, which indicates that the combined action of the two in the ratio range on the cotton red spiders is additive or synergistic; when the mixing ratio of the chlorofluorobisphenol to the chlorfenapyr is 1: 30-20: 1, the indoor co-toxicity coefficient of the chlorantraniliprole to the cotton red spiders is more than 120, which shows that the combined action of the two in the range of the ratio is a synergistic action; when the mixing ratio of the chlorofluorobisphenol to the chlorfenapyr is 1: 5-5: 1, the indoor co-toxicity coefficient of the chlorantraniliprole to the cotton red spiders is more than 150, which shows that the combination effect of the two in the ratio range is a synergistic effect on the cotton red spiders, and the synergistic effect is obvious.

Example 28: combined toxicity of mixing of flubendiamide and cyromazine on cucumber leaf miners

The tested pests: cucumber leaf miner

Test agents: the technical grade of the flubendiamide and the technical grade of the cyromazine are provided by the Hilier pharmaceutical industry group, Inc.

And (3) experimental design: tests prove that the half Lethal Concentration (LC) of the mixture of the technical grade of the flubendiamide and the technical grade of the cyromazine and the mixture of the technical grade of the flubendiamide and the cyromazine in different proportions₅₀) And co-toxicity coefficient to determine the combined action type of the mixed compound of the flubendiamide and the cyromazine on the cucumber leaf miner.

Treating the medicament and the test insects: collecting leaves of liriomyza sativae larvae from the upper part and the middle part of the cucumber, and marking the positions of the larvae. Soaking marked leaves in the pesticide diluent for 5s, taking out, wrapping petioles with wet cotton balls to keep wet, placing in an insect-culturing box, keeping the humidity at 25 + -1 deg.C, feeding and observing, repeating for 4 times, and ensuring that the number of test insects is more than 15 each time.

Data statistical analysis: and (5) checking the death condition of the test insects 48 hours after treatment, recording the total number of the filled insects and the number of the dead insects, and calculating the death rate and correcting the death rate. And using DPS statistical analysis system to make statistical analysis to obtain virulence regression equation and LC₅₀And 95% confidence limits thereof, evaluating the activity of the test agent on the target cotton spider mites.

TABLE 5 Combined virulence of Flucloxacarbdiamide and cyromazine on Cucumis sativus

The indoor test data in table 5 show that the co-toxicity coefficient of the flubendiamide to the indoor activity of the cucumber leaf miner is more than 80 when the mixing ratio of the flubendiamide to the cyromazine is 1: 50-50: 1, which indicates that the combined action of the flubendiamide and the cyromazine to the cucumber leaf miner is additive or synergistic action when the flubendiamide and the cyromazine are mixed in the ratio range; when the mixing ratio of the flubendiamide to the cyromazine is 1: 30-30: 1, the indoor co-toxicity coefficient to the cucumber leaf miner is more than 120, which shows that the combined action of the flubendiamide and the cyromazine to the cucumber leaf miner in the ratio range is synergistic action; when the mixing ratio of the flubendiamide to the cyromazine is 1: 10-10: 1, the indoor co-toxicity coefficient to the cucumber leaf miner is more than 150, which shows that the type of combined action of the flubendiamide and the cyromazine to the cucumber leaf miner in the ratio range is synergistic, and the synergy is obvious.

Claims

1. The insecticidal composition is characterized by comprising an active ingredient A and an active ingredient B, wherein the active ingredient A is the fipronil bisamide, and the active ingredient B is one of ethiprole, buprofezin, fipronil, butfipronil, chlorfenapyr, pyrimethanil and cyromazine.

2. The insecticidal composition according to claim 1, comprising an active ingredient A and an active ingredient B, wherein the active ingredient B is one selected from ethiprole, buprofezin, fipronil, chlorfenapyr and cyromazine.

3. The insecticidal composition according to claim 1, wherein the weight ratio of the active ingredient A to the active ingredient B is 1: 80-80: 1.

4. The insecticidal composition according to claim 1, wherein the weight ratio of the active ingredient A to the active ingredient B is 1:50 to 50: 1.

5. The insecticidal composition according to claim 1, wherein the weight ratio of the fipronil bisamide to the ethiprole is 1: 30-30: 1; the weight ratio of the flumicloramide to the buprofezin is 1: 20-20: 1; the weight ratio of the fipronil bisamide to the fipronil is 1: 30-20: 1; the weight ratio of the chlorofluorobisphenol to the chlorfenapyr is 1: 30-20: 1; the weight ratio of the flubendiamide to the cyromazine is 1: 30-30: 1.

6. The insecticidal composition according to claim 1, wherein the weight ratio of the fipronil bisamide to the ethiprole is 1: 10-10: 1; the weight ratio of the flumicloramide to the buprofezin is 1: 5-5: 1; the weight ratio of the fipronil bisamide to the fipronil is 1: 5-5: 1. the weight ratio of the chlorofluorobisphenol to the chlorfenapyr is 1: 5-5: 1; the weight ratio of the flubendiamide to the cyromazine is 1: 10-10: 1.

7. An insecticidal composition according to any one of claims 1 to 6, wherein the composition can be prepared into wettable powder, suspending agent, water dispersible granule and suspension seed coating agent.

8. Use of the pesticidal composition according to claim 7 for controlling crop pests.