Insecticidal composition and application thereof

Abstract

The invention belongs to the technical field of pesticide disinfestation, and discloses an insecticidal composition and application thereof.The insecticidal composition comprises an active component A and an active component B. The active component A is oxazole sulfonyl pyridine, and the active component B is any one of flubendiamide, isoxaflutole or fluxaflutole amide, and the active component B is one of flubendiamide, isoxaflutole and fluxaflutole. The mass ratio of the active component A to the active component B is (1: 55)-(50: 1). According to the composition disclosed by the invention, the compounds with different action mechanisms are reasonably combined, so that the obtained composition has an enhanced control effect, the insecticidal spectrum is expanded, the quick-acting property is good, and the lasting period is long.

Description

Technical Field

[0001] The invention belongs to the technical field of pesticide insecticides and discloses an insecticide composition and application thereof. Background Art

[0002] Oxazosulfin, international common name: oxazosulfyl; chemical name: 2-(3-ethylsulfonylpyridin-2-yl)-5-(trifluoromethylsulfonyl)-1,3-benzoxazole, CAS registration number: 1616678-32-0, is a new type of benzoxazole insecticide with a unique mechanism of action and high biological activity. It has good preventive effect on a variety of pests such as Hemiptera, Lepidoptera, Coleoptera, etc.

[0003] Fluchlordiniliprole, international common name: fluchlordiniliprole; chemical name: 23-bromo-1-(3-chloropyridin-2-yl)-N-(4,6-dichloro-3-fluoro-2-(methylcarbamoyl)phenyl)-1H-pyrazole-5-carboxamide, CAS registration number: 2129147-03-9, is a new type of diamide insecticide with an o-formylaminobenzamide structure. It can efficiently activate the insect nicotinic acid receptor and cause it to excessively release calcium ions in the cell calcium store, causing the insect to paralyze and die, and has high activity against target pests.

[0004] Isocycloseramide, internationally known as isocycloseram, has a novel mechanism of action and is an allosteric modulator of γ-aminobutyric acid (GABA)-gated chloride channels, which disrupts the normal conduction of insect nerve impulses, causing insects to become overexcited and twitch. This compound has a broad insecticide spectrum and can effectively control lepidoptera, hemiptera, coleoptera, thysanoptera, dipteran pests and mites, and can be used for crops such as cotton, vegetables, fruits, and corn, as well as cash crops such as tobacco.

[0005] Fluoxathiocarb, internationally known as fluxametamide, is a GABA-gated chloride channel allosteric modulator and a neurotoxin. It inhibits the nerve transmission of target insects through stomach poison and contact killing, causing the insects to twitch and eventually die. It is mainly used in vegetables, fruit trees, field crops, oil crops, cotton, tea trees and other crops to control pests such as thrips, whiteflies, leaf miners, beetles, red spiders, rust mites and so on.

[0006] The compounding of insecticides is an essential means to effectively alleviate pest resistance and reduce the use of pesticides. The present invention selects oxazolidinone, fluchlorfenapyr, isoxazolidinone, and fluoxazolidinone, which are widely used in the prevention and control of lepidoptera and hemiptera pests and have different mechanisms of action, as compound ingredients, and studies the synergistic effect of oxazolidinone and fluchlorfenapyr, isoxazolidinone, and fluoxazolidinone, in order to obtain the best quality ratio and provide an effective compounding scheme for the chemical control of lepidoptera and hemiptera pests. Summary of the invention

[0007] Based on the above situation, the present invention provides an insecticidal composition, which rationally compounds oxazolidinone with any one of flufenac, isoxazolidinone or flufenac, has a significant synergistic effect on pests, reduces the development of pest resistance, reduces the amount of pesticide used, and can effectively alleviate environmental pressure.

[0008] In order to achieve the above-mentioned object, the present invention adopts the following technical scheme: an insecticidal composition, the insecticidal composition comprises an active ingredient A and an active ingredient B, the active ingredient A is oxadiazine, the active ingredient B is any one of flufenac, isoxadiazine or flufenac, and the mass ratio of the active ingredient A to the active ingredient B is 1:55 to 50:1, or any value between the above values.

[0009] Furthermore, the mass ratio of oxazolidinone to flufenacet is 1:20 to 45:1, or any value between the above values;

[0010] The mass ratio of oxazolidinone to isoxazolidinone is 1:25 to 20:1, or any value between the above values;

[0011] The mass ratio of oxazolidinone to fluoxetine is 1:25 to 24:1, or any value between the above values.

[0012] Furthermore, the mass ratio of oxazolidinone to flufenicol is 1:20 to 20:1, or any value between the above values;

[0013] The mass ratio of oxazolidinone to isoxazolidinone is 1:16 to 20:1, or any value between the above values;

[0014] The mass ratio of oxazolidinone to fluoxetine is 1:25 to 15:1, or any value between the above values.

[0015] Furthermore, the mass ratio of oxazolidinone to flufenicol is 1:1 to 20:1, or any value between the above values;

[0016] The mass ratio of oxazolidinone to isoxazolidinone is 1:15 to 1:1, or any value between the above values;

[0017] The mass ratio of oxazolidinone to fluoxetine is 1:10 to 12:1, or any value between the above values.

[0018] Furthermore, the total weight of the insecticidal composition is 100 wt%, and the total weight of the active ingredient A and the active ingredient B accounts for 0.5% to 80% of the total weight of the insecticidal composition, or any value in between.

[0019] Furthermore, the composition contains, in addition to the active ingredients, auxiliary ingredients permitted in pesticides, and the auxiliary ingredients are selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoaming agents, solvents, preservatives, stabilizers, synergists or carriers.

[0020] Furthermore, the composition is prepared into a formulation form permitted by pesticides, and the formulation form is a solid preparation or a liquid preparation.

[0021] Furthermore, the solid preparation is a water-dispersible granule or a wettable powder, and the liquid preparation is a suspension, an emulsion in water, a microemulsion, an emulsifiable concentrate, a dispersible oil suspension or an emulsion in water.

[0022] The invention also discloses the use of the insecticide composition for preventing and controlling pests.

[0023] Furthermore, the pests are lepidopteran pests or hemiptera pests.

[0024] Furthermore, the lepidopteran pests are Plutella xylostella, Pieris rapae and Chilo suppressalis, and the hemiptera pests are rice planthoppers.

[0025] In order to obtain the desired insecticidal effect, the amount of the insecticidal composition used varies depending on various factors, such as the crop to be protected, the type of pest, the degree of infection, climatic conditions, application site, application method, dosage form used, etc.

[0026] Beneficial effects of the present invention:

[0027] 1) The insecticidal composition and its preparation of the present invention have obvious synergistic effect on lepidopteran pests and hemiptera pests.

[0028] 2) The insecticide composition of the present invention reduces the development of pest resistance, reduces agricultural production costs, alleviates environmental pressure, and prolongs the service life of a single agent. DETAILED DESCRIPTION

[0029] In order to make the purpose and advantages of the present invention more clearly understood, the present invention is further explained in conjunction with the following specific embodiments.

[0030] Preparation Example Preparation method:

[0031] 1. Suspension concentrate: according to the formula ratio, the active ingredients, surfactants and other functional additives are placed in the reactor in sequence, water is added to mix evenly, and the suspension concentrate product is obtained by high-speed shearing, wet sand grinding, and finally homogenization filtration.

[0032] 2. Emulsifiable concentrate: according to the formula ratio, add the active ingredient, solvent and cosolvent into a mixing kettle and stir to dissolve them, then add the emulsifier, make up the surplus with the remaining solvent, stir evenly in a stirring kettle, and filter to obtain the desired emulsifiable concentrate of the present invention.

[0033] 3. Emulsion in water: According to the formula ratio, dissolve the active ingredients in the solvent and add emulsifier to make it dissolved into a uniform oil phase. Mix deionized water, antifreeze, etc. together to form a uniform water phase. Under high-speed shearing, add the oil phase to the water phase, shear to a qualified particle size, add defoamer, thickener, preservative and stir evenly to form a well-dispersed emulsion in water product.

[0034] 4. Microemulsion: According to the formula ratio, the active ingredients, solvents, emulsifiers, etc. are mixed to obtain the oil phase, and the antifreeze agent is mixed with water to obtain the water phase. The oil phase is added to the water phase under stirring and stirred evenly. The shearing is continued for 10 minutes, and then the defoaming agent is added and stirred evenly to obtain small droplets of oil phase particles of 0.01 to 0.1 microns, that is, the microemulsion product is obtained.

[0035] 5. Wettable powder: The active ingredients, dispersants, wetting agents and fillers are mixed according to the formula ratio, stirred evenly in a stirring kettle, and pulverized and mixed evenly for multiple times by a jet mill to prepare the wettable powder of the composition of the present invention.

[0036] 6. Water-dispersible granules: according to the formula ratio, add the active ingredient into the carrier, add surfactant and other functional additives thereto, mix, add 10-25% water after air flow grinding, and then knead, granulate, dry and sieve to obtain water-dispersible granule products; or spray water on the ground powder in a boiling granulator, granulate, dry, and then sieve to obtain water-dispersible granule products.

[0037] The following are some examples of preparation:

[0038] Preparation Example 1: 22% oxazolidinone·flufenacil suspension (21:1)

[0039] Formula composition: 21% oxazolidinone, 1% flufenac, 1% sodium lauryl sulfate, 2% sodium alkyl polyoxyethylene ether sulfonate, 3% polyoxyethylene sorbitan monooleate, 0.2% xanthan gum, 1% magnesium aluminum silicate, 5% ethylene glycol, 0.01% potassium benzisothiazolinone, 0.5% silicone oil, and deionized water to make up the balance.

[0040] Preparation Example 2: 11% oxazolidinone·flufenacil EC (1:10)

[0041] Formula composition: 1% oxazolidinone, 10% flufenac, 25% propylene carbonate, 8% tristyrylphenol ethoxylate phosphate, 3% sorbitan oleate polyoxyethylene ether, 1% calcium dodecylbenzene sulfonate, and rosin-based vegetable oil makes up the balance.

[0042] Preparation Example 3: 2% oxazolidinone·flufenacil emulsion (1:1)

[0043] Formula composition: 1% oxazolidinone, 1% flufenac, 4% phenethylphenol polyoxyethylene polyoxypropylene ether, 3% aromatic phenol polyoxyethylene ether phosphate, 12% cyclohexanone, 0.1% xanthan gum, 0.1% potassium benzisothiazolinone, 5% ethylene glycol, 1% urea, 0.5% sodium sorbate, 0.2% silicone defoamer, and deionized water to make up the balance.

[0044] Preparation Example 4: 30% oxazolidinone·flufenacil water dispersible granules (1:5)

[0045] Formula composition: 5% oxazolidinone, 25% flufenac, 10% sodium lignin sulfonate, 2.5% BX powder, 2% sodium alkyl polyoxyethylene ether sulfonate, 5% ammonium sulfate, and kaolin makes up the balance.

[0046] Preparation Example 5: 27% oxazolidinone·flufenacil wettable powder (2:1)

[0047] Formula composition: 18% oxazolidinone, 9% flufenac, 3% sodium lignin sulfonate, 5% fatty alcohol ethylene oxide-propylene oxide copolymer, 3% BX powder, 5% white carbon black, and kaolin makes up the balance.

[0048] Preparation Example 6: 18% oxazolidinone·isoxacillin suspension (1:2)

[0049] Formula composition: 6% oxazolidinone, 12% isoxazolidinone, 0.5% sorbitan oleate polyoxyethylene ether, 4% castor oil polyoxyethylene ether phosphate, 1% sodium lignin sulfonate, 0.25% xanthan gum, 4% propylene glycol, 0.1% sodium benzoate, 0.5% silicone oil, and deionized water to make up the balance.

[0050] Preparation Example 7: 3% oxazolidinone·isoxacillin microemulsion (2:1)

[0051] Formula composition: 2% oxazolidinone, 1% isoxazolidinone, 18% cyclohexanone, 12% glycerol fatty acid ester polyoxyethylene ether, 3% fatty amine polyoxyethylene ether, 1% alkylphenol formaldehyde resin polyoxyethylene ether sulfate, 0.05% silicone defoamer, and deionized water to make up the balance.

[0052] Preparation Example 8: 10% oxazolidinone·isoxacillin EC (1:1)

[0053] Formula composition: 5% oxazolidinone, 5% isoxazolidinone, 12% EO / PO block copolymer, 15% acetophenone, 10% N-octyl pyrrolidone, 1% naphthalenesulfonate formaldehyde condensate, and the balance is made up of trimethylol.

[0054] Preparation Example 9: 30% oxazolidinone·isoxazobactam water dispersible granules (5:1)

[0055] Formula composition: 25% oxazolidinone, 5% isoxazolidinone, 10% lignin sulfonate, 4% sodium dodecylbenzene sulfonate, 5% white carbon black, 30% starch, and kaolin makes up the balance.

[0056] Preparation Example 10: 36% oxazolidinone·isoxacillin wettable powder (1:8)

[0057] Formula composition: 4% oxadiazine, 32% isoxadiazine, 2% sodium lauryl sulfate, 5% succinate sulfonate, 6% sodium dioctyl sulfosuccinate, 10% kaolin, 8% white carbon black, and bentonite makes up the balance.

[0058] Preparation Example 11: 13% oxazolidinone·fluoxetine suspension (12:1)

[0059] Formula composition: 12% oxazolidinone, 1% fluoxetine, 1% ethylene glycol oxyethylene polyoxypropylene ether, 2% tristyrylphenol polyoxyethylene ether polyoxypropylene ether, 2% polyoxyethylene sorbitan monooleate, 1% polycarboxylic acid sodium salt, 1.5% magnesium aluminum silicate, 0.25% carboxyethyl cellulose, 1% sodium benzoate, 5% ethylene glycol, 0.5% silicone oil, and deionized water to make up the balance.

[0060] Preparation Example 12: 14% oxazolidinone·fluoxetine emulsifiable concentrate (1:6)

[0061] Formula composition: 2% oxazolidinone, 12% fluoxathiocarb, 13% DMF, 12% isomeric tridecanol polyoxyethylene ether, 2% calcium dodecylbenzene sulfonate, 22% propylene carbonate, and xylene makes up the balance.

[0062] Preparation Example 13: 32% oxazolidinone·fluoxetine water dispersible granules (1:3)

[0063] Formula composition: 8% bistrifluanuron, 24% flonicamid, 12% lignin sulfonate, 5% sodium alkyl polyoxyethylene ether sulfonate, 2% sodium lauryl sulfate, 25% starch, and kaolin makes up the balance.

[0064] Preparation Example 14: 24% oxazolidinone·fluoxetine wettable powder (5:1)

[0065] Formula composition: 20% oxazolidinone, 4% fluoxathiocarboxylate, 5% sodium salt of polycarboxylate, 3% sodium alkylnaphthalene sulfonate, 2% BX powder, 8% white carbon black, and kaolin makes up the balance.

[0066] Example 1: Indoor joint action test on Plutella xylostella

[0067] Test basis: The test refers to NY / T1154.14-2008 "Guidelines for Indoor Bioassay Tests of Pesticides Insecticides Part 14: Leaf Dipping Method"; NY / T1154.7-2006 "Guidelines for Indoor Bioassay Tests of Pesticides Insecticides Part 7: Determination of Combined Action of Mixtures".

[0068] Test target: Diamondback moth, third instar larvae of the same physiological state. They were reared indoors for multiple generations using the vermiculite radish seedling method and were not exposed to any pesticides during the rearing process.

[0069] Experimental agents: oxazolidinone, flufenac, isoxazolidinone, and fluoxetine amide original drugs.

[0070] Drug preparation: After dissolving the above drugs with appropriate solvents, dilute them with 0.1% Tween-80 aqueous solution respectively to prepare single-dose stock solutions, and design the ratio according to the purpose of mixing and the activity of the drugs. Each single dose and each group of mixed drugs shall be prepared according to the required series of mass concentrations in equal proportions.

[0071] Use a 9 cm diameter hole puncher to take leaves of uniform size from clean cabbage leaves, immerse them in the prepared solution for 10 seconds, take them out, dry them at room temperature, and place them in a 9 cm diameter culture dish. Inoculate 20 3rd instar larvae of the same size in each dish (the culture dish is sealed with a double layer of absorbent paper to prevent the test insects from escaping). Each group of treatments was repeated 4 times. After 48 hours, the number of dead larvae in each treatment was counted. The insect body was gently touched with a small brush or tweezers. Individuals that could not coordinate movement or whose insect body was too different from the control were considered dead.

[0072] Statistics and analysis:

[0073] Based on the survey data, calculate the adjusted mortality rate of each treatment. Calculate as follows:

[0074]

[0075] Where:

[0076] P——mortality rate, in percentage (%);

[0077] K——Number of dead insects, in heads;

[0078] N——Total number of insects treated, in heads.

[0079]

[0080] Where:

[0081] P1——adjusted mortality rate, in percentage (%);

[0082] P t ——Treatment mortality rate, expressed as percentage (%);

[0083] P0——blank control mortality rate, in percentage (%).

[0084] If the control mortality rate is less than 5%, no correction is required; if the control mortality rate is between 5% and 20%, correction should be performed according to the correction formula; if the control mortality rate is greater than 20%, the test needs to be repeated.

[0085] Use DPS software to analyze and find the toxicity regression line, LC 50 The co-toxicity coefficient (CTC value) of the mixture is calculated as follows:

[0086]

[0087] Where:

[0088] ATI——Actual Toxicity Index of Mixture;

[0089] S——LC of standard pesticide 50 , the unit is milligrams per liter (mg / L);

[0090] M——LC of the mixture 50 , the unit is milligrams per liter (mg / L).

[0091] TTI=TI A ×P A +TI B ×P B

[0092] Where:

[0093] TTI – Theoretical Toxicity Index of Mixtures;

[0094] TI A ——A: toxicity index of the agent;

[0095] P A ——The percentage of agent A in the mixture, in percentage (%);

[0096] TI B ——Toxicity index of agent B;

[0097] P B ——The percentage of agent B in the mixture, in percentage (%).

[0098]

[0099] Where:

[0100] CTC – Co-toxicity coefficient;

[0101] ATI——Actual Toxicity Index of Mixture;

[0102] TTI - Theoretical Toxicity Index of Mixture.

[0103] The co-toxicity coefficient of the compound is CTC ≥ 120, which indicates a synergistic effect; CTC ≤ 80 indicates an antagonistic effect; and 80 < CTC < 120 indicates an additive effect. The test results are shown in the following table:

[0104] Table 1 Results of indoor biological activity test on Plutella xylostella with oxazolidinone and fluoxathiocarb

[0105]

[0106]

[0107] From the indoor test results in the above table, it can be seen that the combination of oxathiapiprolin and fluoxathiapiprolin in an appropriate mass ratio has good insecticidal activity against Plutella xylostella, among which the mass ratio of oxathiapiprolin to fluoxathiapiprolin is 1:50-15:1, and its co-toxicity coefficient is greater than 120, showing a synergistic effect; the mass ratio of oxathiapiprolin to fluoxathiapiprolin is 1:35-5:1, and the co-toxicity coefficient is greater than 130, showing a significant synergistic effect; the mass ratio of oxathiapiprolin to fluoxathiapiprolin is 1:12-2:1, and the co-toxicity coefficient is greater than 140, showing a significant synergistic effect.

[0108] Table 2 Results of indoor biological activity test on Plutella xylostella with oxazolidinone and flufenac

[0109]

[0110] The results of the indoor tests in the table above show that the compounding of oxazolidinone and flufenac in an appropriate mass ratio has obvious insecticidal activity against Plutella xylostella. When the mass ratio of oxazolidinone and flufenac is 1:20-20:1, the co-toxicity coefficient is greater than 120, showing a synergistic effect; when the mass ratio of oxazolidinone and flufenac is 1:10-1:1, the co-toxicity coefficient is greater than 130, and the synergistic effect is obvious; when the mass ratio of oxazolidinone and flufenac is 1:5-1:1, the co-toxicity coefficient is greater than 140, and the synergistic effect is significant.

[0111] Table 3 Results of indoor biological activity test of oxazolidinone and isoxazolidinone against Plutella xylostella

[0112]

[0113]

[0114] The results of the indoor tests in the above table show that the compounding of oxathiapyrim and isoxathiapyrim in an appropriate mass ratio exhibits excellent insecticidal activity against Plutella xylostella. The mass ratio of isoxathiapyrim to oxathiapyrim is 1:20-16:1, and the co-toxicity coefficient to Plutella xylostella is greater than 120, showing a synergistic effect; the mass ratio of isoxathiapyrim to oxathiapyrim is 1:10-2:1, and the co-toxicity coefficient is greater than 140, showing a significant synergistic effect; the mass ratio of isoxathiapyrim to oxathiapyrim is 1:10-1:2, and the co-toxicity coefficient is greater than 150, showing a significant synergistic effect.

[0115] Example 2: Indoor biological combined action test on rice stem borer

[0116] Test target: Rice stem borer. The overwintering larvae of the rice stem borer were collected from rice stumps in rice fields, raised indoors to the next generation, and the 4th instar larvae were used as test insects.

[0117] The larval rearing conditions are: photoperiod of 16h:8h (light:darkness), illuminance of 1500-2000lx, temperature of (26±1)°C, and relative humidity of 60%-70%.

[0118] Test drugs: oxazolidinone and flubendiamide original drugs.

[0119] Test method: dilute the above single agent and the agent mixed according to the set ratio with a suitable solvent into 5 series of concentration gradients, and use the drip method for determination. The drip volume for each test insect is 0.05uL. Each treatment is repeated 4 times, with 20 test insects in each repeat, and a control without agent (containing all organic solvents) is set. After 48 hours of treatment, check the death of the test insects. The test insects that shrink, turn black, and cannot move after the insect body flips are judged as dead, and the co-toxicity coefficient is calculated.

[0120] Rearing conditions: The larvae of Chilo suppressalis were reared in an artificial climate box at a temperature of (28±1)°C, a relative humidity of 80%, and a light intensity of L / D=16 / 8h.

[0121] Data statistics and analysis:

[0122] Based on the survey data, calculate the adjusted mortality rate of each treatment. Calculate as follows:

[0123]

[0124] Where:

[0125] P——mortality rate, in percentage (%);

[0126] K——Number of dead insects, in heads;

[0127] N——Total number of insects treated, in heads.

[0128]

[0129] Where:

[0130] P1——adjusted mortality rate, in percentage (%);

[0131] P t ——Treatment mortality rate, expressed as percentage (%);

[0132] P0——blank control mortality rate, in percentage (%).

[0133] If the control mortality rate is less than 5%, no correction is required; if the control mortality rate is between 5% and 20%, correction should be performed according to the correction formula; if the control mortality rate is greater than 20%, the test needs to be repeated.

[0134] Use DPS software to analyze and find the toxicity regression line, LC 50 The activity of the test agent on the biological test material was evaluated by using the value and correlation coefficient.

[0135] The co-toxicity coefficient (CTC value) of the mixture is calculated as follows:

[0136]

[0137] Where:

[0138] ATI——Actual Toxicity Index of Mixture;

[0139] S——LC of standard pesticide 50 , the unit is milligrams per liter (mg / L);

[0140] M——LC of the mixture 50 , the unit is milligrams per liter (mg / L).

[0141] TTI=TI A ×P A +TI B ×P B

[0142] Where:

[0143] TTI – Theoretical Toxicity Index of Mixtures;

[0144] TI A ——A: toxicity index of the agent;

[0145] P A ——The percentage of agent A in the mixture, in percentage (%);

[0146] TI B ——Toxicity index of agent B;

[0147] P B ——The percentage of agent B in the mixture, in percentage (%).

[0148]

[0149] Where:

[0150] CTC – Co-toxicity coefficient;

[0151] ATI——Actual Toxicity Index of Mixture;

[0152] TTI - Theoretical Toxicity Index of Mixture.

[0153] The co-toxicity coefficient of the combination CTC≥120 shows a synergistic effect; CTC≤80 shows an antagonistic effect; 80<CTC<120 shows an additive effect.

[0154] The test results are shown in the following table:

[0155] Table 4 Results of indoor biological activity test on the combination of oxazolidinone and flufenac against rice stem borer

[0156]

[0157] The results of the indoor tests in the table above show that the compounding of oxazolidinone and flufenac in an appropriate mass ratio showed good insecticidal activity against the rice stem borer. The mass ratio of flufenac to oxazolidinone was 1:45-1:1, and the co-toxicity coefficient was greater than 120, showing a synergistic effect; the mass ratio of flufenac to oxazolidinone was 1:21-1:2, and the co-toxicity coefficient was greater than 130, showing a significant synergistic effect; the mass ratio of flufenac to oxazolidinone was 1:21, and the co-toxicity coefficient was greater than 150, showing a significant synergistic effect.

[0158] Example 3: Indoor joint action test on Hemiptera pest rice planthopper

[0159] Test target: Brown planthopper. Adults were collected from the field, placed in a plastic bucket containing fresh rice plants and brought back indoors. They were isolated and raised with tillering rice. The virulence of the next generation of nymphs was measured when they hatched and reached the third instar.

[0160] Target test insect rearing conditions: temperature is (28±1)℃, relative humidity is 70%~80%, and sufficient light.

[0161] Test drugs: oxazolidinone, isoxazolidinone, and fluazifop-doxazolidinone technical drugs.

[0162] Test method: Use the rice stem immersion method, pull out the rice plants in the tillering stage with roots, wash them, cut them into about 10cm long rice stems with roots, dry them, and group them into groups of 3. Immerse the rice stems in the prepared solution for 30s, take them out and dry them slightly, wrap the roots with wet absorbent cotton and put them in a culture cup. Take the third-instar nymphs of the same standard from the potted rice and put them in the above-mentioned culture cups, 40 heads per cup, and repeat each treatment 4 times. The culture cups after inoculation are placed in a constant temperature incubator with a temperature of (28±1)℃ and a light cycle of 16(L)∶8(D) for incubation. Investigate the test results 72h after inoculation. Touch the insect body with a brush lightly. If the nymph cannot coordinate movement, it is considered dead.

[0163] Data statistics and analysis:

[0164] Based on the survey data, calculate the adjusted mortality rate of each treatment. Calculate as follows:

[0165]

[0166] Where:

[0167] P——mortality rate, in percentage (%);

[0168] K——Number of dead insects, in heads;

[0169] N——Total number of insects treated, in heads.

[0170]

[0171] Where:

[0172] P1——adjusted mortality rate, in percentage (%);

[0173] P t ——Treatment mortality rate, expressed as percentage (%);

[0174] P0——blank control mortality rate, in percentage (%).

[0175] If the control mortality rate is less than 5%, no correction is required; if the control mortality rate is between 5% and 20%, correction should be performed according to the correction formula; if the control mortality rate is greater than 20%, the test needs to be repeated.

[0176] Use DPS software to analyze and find the toxicity regression line, LC 50 The activity of the test agent on the biological test material was evaluated by using the value and correlation coefficient.

[0177] The co-toxicity coefficient (CTC value) of the mixture is calculated as follows:

[0178]

[0179] Where:

[0180] ATI——Actual Toxicity Index of Mixture;

[0181] S——LC of standard pesticide 50 , the unit is milligrams per liter (mg / L);

[0182] M——LC of the mixture 50 , the unit is milligrams per liter (mg / L).

[0183] TTI=TI A ×P A +TI B ×P B

[0184] Where:

[0185] TTI – Theoretical Toxicity Index of Mixtures;

[0186] TI A ——A: toxicity index of the agent;

[0187] P A ——The percentage of agent A in the mixture, in percentage (%);

[0188] TI B ——Toxicity index of agent B;

[0189] P B ——The percentage of agent B in the mixture, in percentage (%).

[0190]

[0191]

[0192] CTC – Co-toxicity coefficient;

[0193] ATI——Actual Toxicity Index of Mixture;

[0194] TTI - Theoretical Toxicity Index of Mixture.

[0195] The co-toxicity coefficient of the combination CTC≥120 shows a synergistic effect; CTC≤80 shows an antagonistic effect; 80<CTC<120 shows an additive effect.

[0196] The test results are shown in the following table:

[0197] Table 5 Results of the indoor combined action test of oxazolidinone and fluoxathiocarb on rice planthoppers

[0198]

[0199] The results of the indoor tests in the above table show that compounding oxazolidinone and fluoxazolidinone in an appropriate mass ratio shows good insecticidal activity against rice planthoppers. The mass ratio of oxazolidinone to fluoxazolidinone is 1:25-24:1, and the co-toxicity coefficient is greater than 120, showing a synergistic effect; the mass ratio of oxazolidinone to fluoxazolidinone is 1:25-5:1, and the co-toxicity coefficient is greater than 130, showing a significant synergistic effect; the mass ratio of oxazolidinone to fluoxazolidinone is 1:10-1:2, and the co-toxicity coefficient is greater than 140, showing a significant synergistic effect.

[0200] Table 6 Results of the indoor combined action test of oxazolidinone and isoxazolidinone on rice planthoppers

[0201]

[0202]

[0203] From the indoor test results in the above table, it can be seen that the compounding of oxazolidinone and isoxazolidinone in a suitable mass ratio shows relatively excellent insecticidal activity against rice planthoppers. The mass ratio of oxazolidinone to isoxazolidinone is 1:25-20:1, and the co-toxicity coefficient is greater than 120, showing a synergistic effect; the mass ratio of oxazolidinone to isoxazolidinone is 1:15-1:1, and the co-toxicity coefficient is greater than 130, showing a significant synergistic effect; the mass ratio of oxazolidinone to isoxazolidinone is 1:8-1:4, and the co-toxicity coefficient is greater than 150, showing a significant synergistic effect.

[0204] Example 4: Field test on efficacy of controlling rice planthoppers

[0205] Test reference: The test reference is the national standard GB / T 17980.4-2000 "Guidelines for field efficacy tests of pesticides (I) Insecticides for control of rice planthoppers".

[0206] The test site is Shuangqiao Village, Dingshu Town, Yixing City, Jiangsu Province. The soil is clay loam, and rice and wheat are rotated for many years. The water and fertilizer conditions of the test site are above average, which is in line with local scientific agricultural practices.

[0207] Test target: Rice planthopper.

[0208] Experimental crops: Rice (Nanjing 3908).

[0209] Experimental design: The experiment set up 6 treatments according to the different pesticides used, among which the blank control was the application of the same amount of liquid water. Each treatment was repeated 4 times, and the area of ​​each plot was 50m 2 The specific application schemes of each treatment are shown in the table below. During the test, no other pesticides were applied to each treatment, and other cultivation management remained the same. The test was conducted on August 2 (the peak period of young nymphs of rice planthoppers), and a JACTOPJB-16 electric sprayer was used for foliar spraying once.

[0210] Before and 3, 7, and 14 days after pesticide application, the number of live insects on rice in each plot was investigated using the pan-patting method. During the investigation, an enamel pan was placed under the rice and patted 3 times in the direction of the enamel pan to make the rice planthoppers fall into the enamel pan. Ten points were investigated in each plot, with two holes at each point, and the investigation included both nymphs and adults of rice planthoppers.

[0211] Calculation formula:

[0212]

[0213] Table 7 Field efficacy test of oxazolidinone and fluoxathiocarb for rice planthopper control

[0214]

[0215] As can be seen from Table 7, 3 days after the application, the three tested pesticides, Preparation Example 14: 24% oxazolidinone·fluoxazolidinone wettable powder (5:1), Preparation Example 12: 14% oxazolidinone·fluoxazolidinone EC (1:6), Preparation Example 13: 32% oxazolidinone·fluoxazolidinone water dispersible granules (1:3), had good control effects, all of which were above 87%, among which Preparation Example 13: 32% oxazolidinone·fluoxazolidinone water dispersible granules (1:3) had the highest control effect, which was 93.82%. Preparation Example 14: 24% oxazolidinone·fluoxazolidinone wettable powder (5:1) and Preparation Example 12: 14% oxazolidinone·fluoxazolidinone EC (1:6) had the second best control effect, which was 87.17% to 90.20%. The compound preparation of the present invention has good quick-acting property in the field efficacy test for controlling rice planthoppers.

[0216] 14 days after application, all five tested pesticides had good control effects on rice planthoppers, with field control rates exceeding 77%, except for the low control rate of 77.64% for fluoxetine. Preparation Example 13: 32% oxazolidinone·fluoxetine water dispersible granules (1:3) had the best control effect of 99.12% and a long lasting effect.

[0217] Example 5: Field test on efficacy of controlling rice planthoppers

[0218] The test site was Qingfeng Village, Xinhe Town, Hanchuan City, Hubei Province. The previous crop of the test field was rapeseed. The fertilizer and water conditions of the test field were good, and the cultivation management was consistent. When the pesticide was applied, the rice growth stage was the end of the tillering stage, and the rice planthopper was in the early nymph stage.

[0219] Test target: Rice planthopper.

[0220] Experimental crops: rice.

[0221] Experimental design: The experiment set up 6 treatments, of which the blank control was the application of the same amount of liquid medicine and water. Each treatment was repeated 4 times, and the area of ​​each plot was 50m 2 Specific medication regimens for each treatment are shown in the table below.

[0222] Each treatment was sprayed once on July 31. The blank control area was sprayed with an equal amount of water first, and the pesticide treatment areas were sprayed one by one according to the plot settings. After the test pesticide was fully mixed, a Shandong Weishi WS-16 backpack manual sprayer was used to spray evenly on the middle and lower parts of the rice plants at a uniform speed using the downwind unilateral parallel propulsion method.

[0223] The insect base number was investigated before application of pesticides, and the number of live insects on rice in each plot was investigated 3, 7, and 10 days after application. Five points were investigated in each plot using the parallel jumping method, with four clumps at each point, for a total of 20 clumps of rice. The rice planthopper population was investigated using the pot-shooting method, and the insect population reduction rate and control effect were calculated.

[0224] Calculation formula:

[0225]

[0226]

[0227] Table 8 Field control efficacy test of oxazolidinone and isoxazolidinone for rice planthoppers

[0228]

[0229] 7 days after application, the control effect of the compound preparations of Example 10: 36% oxazolidinone·isoxafenamide wettable powder (1:8) on rice planthoppers was the best, at 97.48%, followed by the preparation of Example 6: 18% oxazolidinone·isoxafenamide suspension (1:2), with a control effect of 95.20%. The control effects of the three compound preparations of oxazolidinone and isoxazolidinone were all above 90%.

[0230] 10 days after application, the control effect of Preparation Example 10: 36% oxazolidinone·isoxafenamide wettable powder (1:8) was 98.83%. The worst control effect of isoxazolidinone on rice planthoppers in this test was 80.56%, which was significantly lower than the other agents.

[0231] Example 6: Field efficacy test for controlling diamondback moth

[0232] The test site is a vegetable field in Daying Village, Dahuangzhuang Town, Huailai County, Zhangjiakou City, Hebei Province. The test field has medium to high fertility and loam soil. Cabbage was planted on August 2. The growth of cabbage in the test field is basically the same.

[0233] Test target: Diamondback moth.

[0234] Experimental crops: Cabbage.

[0235] Experimental design: The experiment has 8 treatments, each treatment is repeated 4 times, and a total of 32 plots are set up, with a plot area of ​​20m 2 , randomly arranged.

[0236] Test method: The test began with the application of pesticides during the peak period of the occurrence of 2nd to 3rd instar larvae of the diamondback moth. The average number of larvae per plant was 1 to 3. When applying pesticides, an electric sprayer was used to evenly spray the leaf surface, leaf back and heart of the plant, with a water consumption of 750kg / hm2. 2 .

[0237] Survey method: Use the diagonal 5-point sampling method, survey 2 plants per point in each plot, a total of 10 plants, and survey all leaves of each plant. Investigate the insect population base before applying the pesticide, and conduct insect population surveys 3, 7, and 12 days after applying the pesticide, and calculate the corrected control effect.

[0238] Calculation method of drug efficacy:

[0239]

[0240]

[0241] Table 9 Results of field efficacy test on Plutella xylostella

[0242]

[0243] Through the test, it can be seen from the table above that the compound preparation has a good effect on the prevention and control of cabbage diamondback moth. 3 days after the application, the control effect of cabbage diamondback moth in the compound preparation treatment area reached more than 84%, and the control effect of Preparation Example 7: 3% oxazolidinone·isoxazolidinone microemulsion (2:1) reached 88.69%, which was significantly higher than the treatment areas of each single-dose control agent. 7 days after the application, the control effect of each treatment was improved, and the compound preparation treatment area reached more than 89%.

[0244] Example 7: Field test on efficacy of controlling rice stem borer

[0245] Test basis: The test reference is GB / T 17980.1-2000 "Guidelines for field efficacy tests of pesticides (I) Insecticides for controlling rice lepidopteran borers".

[0246] The test site is a transplanted rice field in Liguan Village, Jiyang Street, Jiyang District, Jinan City, Shandong Province. The previous crop is wheat. The soil fertility of the test site is uniform, the terrain is flat, the irrigation is convenient, and the soil is loamy.

[0247] Test target: Rice stem borer.

[0248] Experimental crops: rice.

[0249] Experimental design: There are 6 treatments in total. The specific dosage of each treatment is shown in the table below. Each treatment is repeated 4 times, arranged in random blocks, and the area of ​​the plot is 30m 2 A 1.5m wide isolation zone was set between each plot. When the Chilo suppressalis reached the peak period of egg hatching, chemical control was carried out according to the experimental design, using the SX-MD15DA backpack electric sprayer produced by Shixia Holdings Co., Ltd. with a water volume of 450kg / hm 2 The rice was sprayed evenly over the whole plant at an average flow rate of 0.85 L / min. No rainfall was observed on the day of application and 3 days after application, and water was maintained for 1 week after application.

[0250] Prevention effect investigation: 10 days and 20 days after the application of the medicine, when the damage in the control area is obvious or the damage is finalized, parallel jumping sampling is carried out at 10 points, with 5 clumps at each point, and a total of 50 clumps are investigated in each plot, and the total number of plants and the number of dead cores are recorded. The dead core rate and control effect are calculated.

[0251]

[0252]

[0253] Table 10 Results of field trials on efficacy of rice stem borer

[0254]

[0255] The results of the field efficacy test showed that 10 days after the application, the control effects of the compound preparations of Example 3: 2% oxazolidinone·flufenac emulsion (1:1), Example 5: 28% oxazolidinone·flufenac wettable powder (3:1), and Example 1: 23% oxazolidinone·flufenac suspension (21:2) were the best, which were 90.30%, 95.04%, and 97.59%, respectively; the control effect of oxazolidinone alone was the lowest, which was only 76.25%;

[0256] 20 days after application, the control effects of Preparation Example 3: 2% oxathiapyrim·flufenac emulsion (1:1), Preparation Example 5: 28% oxathiapyrim·flufenac wettable powder (3:1), and Preparation Example 1: 22% oxathiapyrim·flufenac suspension (21:1) were also good, all above 84%; the control effect of the single-dose treatment group was relatively low.

[0257] In summary, the insecticide composition of the present invention has excellent control effects on Lepidoptera and Hemiptera pests, and has a significant synergistic effect. In addition, the compound preparation of the present invention has reasonable components, which can reduce the amount of pesticides used and slow down the generation and development of pest resistance, thereby reducing pesticide residues.

Claims

1. An insecticidal composition, characterized in that: The insecticide composition comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is oxazolidinone, and the active ingredient B is any one of flufenac, isoxazolidinone or flufenac, and the mass ratio of the active ingredient A to the active ingredient B is 1:55 to 50:

1.

2. The insecticidal composition according to claim 1, characterized in that The mass ratio of oxazolidinone to flubendiamide is 1:20 to 45:1; The mass ratio of oxazolidinone to isoxazolidinone is 1:25 to 20:1; The mass ratio of oxazolidinone to fluoxetine is 1:25 to 24:

1.

3. The insecticidal composition according to claim 2, characterized in that The mass ratio of oxazolidinone to flubendiamide is 1:20 to 20:1; The mass ratio of oxazolidinone to isoxazolidinone is 1:16 to 20:1; The mass ratio of oxazolidinone to fluoxetine is 1:25 to 15:

1.

4. The insecticidal composition according to claim 3, characterized in that The mass ratio of oxazolidinone to flubendiamide is 1:1 to 20:1; The mass ratio of oxazolidinone to isoxazolidinone is 1:15 to 1:1; The mass ratio of oxazolidinone to fluoxetine is 1:10 to 12:

1.

5. The insecticidal composition according to claim 1, characterized in that The total weight of the insecticide composition is 100 wt %, and the total weight of the active ingredient A and the active ingredient B accounts for 0.5% to 80% of the total weight of the insecticide composition.

6. The insecticidal composition according to claim 1, characterized in that In addition to the active ingredients, the composition also contains auxiliary ingredients allowed in pesticides, and the auxiliary ingredients are selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoaming agents, solvents, preservatives, stabilizers, synergists or carriers.

7. The insecticidal composition according to claim 1, characterized in that The composition is prepared into a formulation form permitted by pesticides, and the formulation form is a solid formulation or a liquid formulation.

8. The insecticidal composition according to claim 7, characterized in that The solid preparation is a water-dispersible granule or a wettable powder, and the liquid preparation is a suspension, an emulsifiable concentrate, a dispersible oil suspension or an aqueous emulsion.

9. Use of the insecticidal composition according to any one of claims 1 to 8 for controlling pests.

10. The use according to claim 9, characterized in that: The pests are lepidoptera pests or hemiptera pests.

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