Insecticide composition and its application

Abstract

The present invention belongs to the field of pesticide insecticide technology and discloses an insecticidal composition and its use. The insecticidal 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 flufenacet, isoxazolidinone, or flufenacet. The mass ratio of the active ingredient A to the active ingredient B is 1:55 to 50:1. The composition of the present invention rationally combines compounds with different mechanisms of action, so that the resulting composition has a beneficial effect on the control effect, expands the insecticidal spectrum, has good fast-acting properties, and has a long lasting effect.

Description

Technical Field

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

[0002] Oxazosulfonylpyridin, 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 benzoxazole insecticide with a unique mechanism of action and high biological activity. It has good control effects on a variety of pests such as Hemiptera, Lepidoptera, and Coleoptera.

[0003] Fluchlordiniliprole, internationally known as 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 from the cellular calcium store, leading to paralysis and death of the insect. It has high activity against target pests.

[0004] Isocycloseramide, commonly known internationally as isocycloseram, has a novel mechanism of action. It is an allosteric modulator of γ-aminobutyric acid (GABA)-gated chloride channels, disrupting the normal conduction of insect nerve impulses, leading to hyperexcitement and convulsions. This compound has a broad spectrum of activity, effectively controlling Lepidoptera, Hemiptera, Coleoptera, Thysanoptera, Diptera, and other pests and mites. It can be used on crops such as cotton, vegetables, fruits, and corn, as well as cash crops such as tobacco.

[0005] Fluxametamide, also known internationally as fluxametamide, is a neurotoxin and allosteric modulator of γ-aminobutyric acid (GABA)-gated chloride channels. It acts as a stomach poison and contact toxicant, inhibiting neurotransmission in target insects, causing them to convulse and eventually die. It is primarily used to control pests such as thrips, whiteflies, leafminers, beetles, spider mites, and rust mites on crops such as vegetables, fruit trees, field crops, oilseed crops, cotton, and tea.

[0006] The compounding of insecticides is an essential means to effectively alleviate pest resistance and reduce pesticide use. This study selected oxazolidinone, flufenac, isoxazolidinone, and fluoxetine as compound ingredients, which are widely used in the prevention and control of Lepidoptera and Hemiptera pests and have different mechanisms of action. The synergistic effect of oxazolidinone with flufenac, isoxazolidinone, and fluoxetine was studied in order to obtain the optimal 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 flufenacet, isoxazolidinone or flufenacet, 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 solution: an insecticidal composition, which 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 flufenacet, isoxazolidinone or flufenacet, 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 in between;

[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 flufenacet 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 flufenacet 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 ingredient, 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 in pesticides, and the formulation form is a solid formulation or a liquid formulation.

[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 present invention also discloses the use of the insecticide composition for preventing and controlling pests.

[0023] Furthermore, the pests are Lepidoptera pests or Hemiptera pests.

[0024] Furthermore, the lepidopteran pests are diamondback moth, cabbage looper, and rice stem borer, and the hemiptera pests are rice planthoppers.

[0025] In order to obtain the desired insecticidal effect, the dosage of the insecticidal composition 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 effects on lepidopteran pests and hemipteran pests.

[0028] 2) The insecticide composition of the present invention reduces the development of pest resistance, lowers 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 clear, 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 and mixed 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, the active ingredient, solvent, and cosolvent are added to a mixing kettle and stirred to dissolve them. Then, an emulsifier is added and the balance is made up with the remaining solvent. The mixture is stirred evenly in a stirred kettle and filtered 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 dissolve 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. After shearing to a qualified particle size, add defoamer, thickener, and preservative and stir evenly to form a well-dispersed emulsion in water product.

[0034] 4. Microemulsion: According to the formula ratio, mix the active ingredients, solvents, emulsifiers, etc. to obtain the oil phase, mix the antifreeze and water to obtain the water phase, add the oil phase to the water phase under stirring and mix evenly, continue shearing for 10 minutes, then add the defoaming agent and mix evenly to obtain oil phase particles with small droplets of 0.01 to 0.1 microns, thus obtaining the microemulsion product.

[0035] 5. Wettable powder: The active ingredient, dispersant, wetting agent and filler are mixed according to the formula ratio, stirred evenly in a stirring tank, and pulverized and mixed evenly multiple times in 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, the active ingredient is added to the carrier, and surfactants and other functional additives are added thereto, mixed, and after air flow grinding, 10-25% water is added, and then the mixture is kneaded, granulated, dried, and sieved to obtain water-dispersible granules. Alternatively, the pulverized powder is sprayed with water in a boiling granulator, granulated, dried, and then sieved to obtain water-dispersible granules.

[0037] The following are some examples of preparation:

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

[0039] Formula composition: 21% oxazolidinone, 1% flufenacet, 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-fluanid emulsifiable concentrate (1:10)

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

[0042] Preparation Example 3: 2% oxazolidinone-fluanid emulsion in water (1:1)

[0043] Formula composition: 1% oxazolidinone, 1% flufenacet, 4% phenylethylphenol polyoxyethylene polyoxypropylene ether, 3% aromatic phenol polyoxyethylene ether phosphate, 12% cyclohexanone, 0.1% xanthan gum, 0.1% benzisothiazolinone potassium, 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-fluanid water dispersible granules (1:5)

[0045] Formula composition: 5% oxazolidinone, 25% flufenac, 10% sodium lignin sulfonate, 2.5% lakai powder BX, 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% flufenacet, 3% sodium lignin sulfonate, 5% fatty alcohol ethylene oxide-propylene oxide copolymer, 3% opening powder BX, 5% white carbon black, and kaolin makes up the balance.

[0048] Preparation Example 6: 18% oxazolidinone-isoxazolinone 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% glycerol, 0.1% sodium benzoate, 0.5% silicone oil, and deionized water to make up the balance.

[0050] Preparation Example 7: 3% oxazolidinone-isoxazolinone 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-isoxazolinone emulsifiable concentrate (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 trimethylbenzene makes up the balance.

[0054] Preparation Example 9: 30% oxazolidinone-isoxazolinone 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-isoxazolinone wettable powder (1:8)

[0057] Formula composition: 4% oxazolidinone, 32% isoxazolidinone, 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 dehydrated 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% fluoxetine, 13% DMF, 12% isotridecyl alcohol polyoxyethylene ether, 2% calcium dodecylbenzenesulfonate, 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% bistrifluan, 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% fluoxetine, 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 diamondback moth

[0067] Test basis: The test refers to NY / T1154.14-2008 "Guidelines for Indoor Bioassay Tests of Pesticides - Insecticides Part 14: Leaf Dip Method" and 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 uniform physiological state. Multiple generations were reared indoors using the vermiculite-radish seedling method and were not exposed to any pesticides during rearing.

[0069] Test agents: oxazolidinone, flufenac, isoxazolidinone, and fluoxetine amide technical.

[0070] Preparation of drugs: After dissolving the above drugs with a suitable solvent, dilute them with 0.1% Tween-80 aqueous solution to prepare single-dose stock solutions. Design the ratio according to the purpose of mixing and the activity of the drugs. Prepare the required series of mass concentrations for each single dose and each group of mixed drugs in equal proportions.

[0071] Use a 9-cm diameter cork hole to pick uniformly sized leaves from clean cabbage leaves, immerse them in the prepared solution for 10 seconds, remove them, dry them at room temperature, and place them in a 9-cm diameter petri dish. Inoculate 20 third-instar larvae of uniform size per dish (the petri dish is sealed with a double layer of absorbent paper to prevent the test insects from escaping). Each group is treated four times. After 48 hours, the number of dead larvae in each treatment is counted. Use a small brush or tweezers to gently touch the insect body. Individuals that cannot coordinate movement or whose body differs greatly from the control are considered dead.

[0072] Data 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 in 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 made 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 - measured 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 ——Agent toxicity index;

[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 - measured toxicity index of mixture;

[0102] TTI - Theoretical Toxicity Index of Mixture.

[0103] A co-toxicity coefficient (CTC) of ≥120 indicates a synergistic effect; a CTC of ≤80 indicates an antagonistic effect; and a CTC of 80 < CTC <120 indicates an additive effect. The test results are shown in the table below:

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

[0105]

[0106]

[0107] The indoor test results in the above table show that the combination of oxazolidinone and fluoxetine in an appropriate mass ratio has good insecticidal activity against Plutella xylostella. Among them, the mass ratio of oxazolidinone to fluoxetine is 1:50-15:1, and the co-toxicity coefficient is greater than 120, showing a synergistic effect; the mass ratio of oxazolidinone to fluoxetine is 1:35-5:1, and the co-toxicity coefficient is greater than 130, showing a significant synergistic effect; the mass ratio of oxazolidinone to fluoxetine 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 flufenacet

[0109]

[0110] The laboratory test results in the table above show that the combination of oxazolidinone and flufenacet at appropriate mass ratios exhibits significant insecticidal activity against Plutella xylostella. When the mass ratio of oxazolidinone to flufenacet is 1:20 to 20:1, the cotoxicity coefficient is greater than 120, indicating a synergistic effect. When the mass ratio of oxazolidinone to flufenacet is 1:10 to 1:1, the cotoxicity coefficient is greater than 130, indicating a significant synergistic effect. When the mass ratio of oxazolidinone to flufenacet is 1:5 to 1:1, the cotoxicity coefficient is greater than 140, indicating a significant synergistic effect.

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

[0112]

[0113]

[0114] The laboratory test results in the table above show that the combination of oxathiapyrim and isoxathiapyrim in appropriate mass ratios exhibited excellent insecticidal activity against Plutella xylostella. When the mass ratio of isoxathiapyrim to oxathiapyrim was 1:20 to 16:1, the co-toxicity coefficient against Plutella xylostella was greater than 120, indicating a synergistic effect. When the mass ratio of isoxathiapyrim to oxathiapyrim was 1:10 to 2:1, the co-toxicity coefficient was greater than 140, indicating a significant synergistic effect. When the mass ratio of isoxathiapyrim to oxathiapyrim was 1:10 to 1:2, the co-toxicity coefficient was greater than 150, indicating 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 were as follows: photoperiod of 16h:8h (light:dark), illuminance of 1500-2000lx, temperature of (26±1)°C, and relative humidity of 60%-70%.

[0118] Test agents: oxazolidinone and flubendiamide technical drugs.

[0119] Test Method: Single doses of the above agents and mixtures prepared in the prescribed ratios were diluted with appropriate solvents to form five concentration gradients. The test was performed using the spot test, with a 0.05 μL droplet per test insect. Each treatment was replicated four times, with 20 test insects per replicate. A control containing no agent (containing all organic solvents) was included. 48 hours after treatment, the insects were examined for mortality. Insects that showed shrinkage, blackening, or inability to move after turning over were considered dead. The co-toxicity coefficient was calculated.

[0120] Rearing conditions: Chilo suppressalis larvae were reared in an artificial climate chamber 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 in 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 made 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 - measured 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 ——Agent toxicity index;

[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 - measured toxicity index of mixture;

[0152] TTI - Theoretical Toxicity Index of Mixture.

[0153] A co-toxicity coefficient (CTC) of 120 or higher indicates a synergistic effect; a co-toxicity coefficient (CTC) of 80 or lower indicates an antagonistic effect; and a co-toxicity coefficient (CTC) of 80 or lower indicates an additive effect.

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

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

[0156]

[0157] The laboratory test results in the table above show that combining oxazolidinone and flufenacet at appropriate mass ratios exhibited good insecticidal activity against the rice stem borer. For flufenacet to oxazolidinone mass ratios of 1:45 to 1:1, the cotoxicity coefficient was greater than 120, indicating a synergistic effect. For flufenacet to oxazolidinone mass ratios of 1:21 to 1:2, the cotoxicity coefficient was greater than 130, indicating a significant synergistic effect. For flufenacet to oxazolidinone mass ratios of 1:21, the cotoxicity coefficient was greater than 150, indicating 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 reared on tillering rice. The virulence of the next generation of nymphs was determined when they hatched and reached the third instar.

[0160] The target test insect rearing conditions were as follows: temperature of (28±1)℃, relative humidity of 70% to 80%, and sufficient light.

[0161] Test agents: oxazolidinone, isoxazolidinone, and fluoxetine technical drugs.

[0162] Test method: Use the rice stem immersion method. Pull out the rice plants in the tillering stage with the roots, wash them, cut them into about 10 cm long rice stems with roots, dry them, and group them into groups of 3. Immerse the rice stems in the prepared solution for 30 seconds, take them out and dry them slightly, wrap the roots with wet absorbent cotton and place them in a culture cup. From the potted rice, the third-instar nymphs of the same standard are taken and placed in the above-mentioned culture cups, 40 heads per cup, and each treatment is repeated 4 times. After inoculation, the culture cups are placed in a constant temperature incubator with a temperature of (28±1)℃ and a light cycle of 16 (L):8 (D) for incubation. The test results are investigated 72 hours after inoculation. The insect body is lightly touched with a brush. 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 in 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 made 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 - measured 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 ——Agent toxicity index;

[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 - measured toxicity index of mixture;

[0194] TTI - Theoretical Toxicity Index of Mixture.

[0195] A co-toxicity coefficient (CTC) of 120 or higher indicates a synergistic effect; a co-toxicity coefficient (CTC) of 80 or lower indicates an antagonistic effect; and a co-toxicity coefficient (CTC) of 80 or lower indicates an additive effect.

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

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

[0198]

[0199] The laboratory test results in the table above show that combining oxazolidinone with fluoxetine at appropriate mass ratios exhibited good insecticidal activity against rice planthoppers. When the mass ratio of oxazolidinone to fluoxetine was 1:25 to 24:1, the cotoxicity coefficient was greater than 120, indicating a synergistic effect. When the mass ratio of oxazolidinone to fluoxetine was 1:25 to 5:1, the cotoxicity coefficient was greater than 130, indicating a significant synergistic effect. When the mass ratio of oxazolidinone to fluoxetine was 1:10 to 1:2, the cotoxicity coefficient was greater than 140, indicating a significant synergistic effect.

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

[0201]

[0202]

[0203] The laboratory test results in the table above show that when combined with oxazolidinone and isoxazolidinone at appropriate mass ratios, they exhibit excellent insecticidal activity against rice planthoppers. When the mass ratio of oxazolidinone to isoxazolidinone was 1:25 to 20:1, the co-toxicity coefficient was greater than 120, indicating a synergistic effect. When the mass ratio of oxazolidinone to isoxazolidinone was 1:15 to 1:1, the co-toxicity coefficient was greater than 130, indicating a significant synergistic effect. When the mass ratio of oxazolidinone to isoxazolidinone was 1:8 to 1:4, the co-toxicity coefficient was greater than 150, indicating a significant synergistic effect.

[0204] Example 4: Field efficacy test for 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 experimental site is Shuangqiao Village, Dingshu Town, Yixing City, Jiangsu Province. The soil here is clay loam, and rice and wheat rotation has been practiced for many years. The water and fertilizer conditions in the experimental 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 was conducted with 6 treatments based on different pesticides, with the same amount of liquid pesticide used as the blank control. Each treatment was repeated 4 times, and the area of ​​each plot was 50m2. 2 The specific pesticide regimen for each treatment is shown in the table below. During the experimental period, no other pesticides were applied to any treatment, and all other cultivation and management practices remained the same. The experiment was conducted on August 2 (peak season for young nymphs of rice planthoppers), with one foliar spray application using a JACTOPJB-16 electric sprayer.

[0210] Live rice planthopper counts were surveyed on rice in each plot before and 3, 7, and 14 days after pesticide application. An enamel tray was placed under the rice and tapped three times toward the tray to force the planthoppers into the tray. Ten spots were surveyed per plot, with two holes at each spot. Both nymphs and adults were included.

[0211] Calculation formula:

[0212]

[0213] Table 7 Field efficacy test of oxazolidinone and fluoxetine amide combined with rice planthoppers

[0214]

[0215] As shown in Table 7, 3 days after application, the three tested agents, Preparation Example 14: 24% oxazolidinone·fluoxetamide WP (5:1), Preparation Example 12: 14% oxazolidinone·fluoxetamide EC (1:6), and Preparation Example 13: 32% oxazolidinone·fluoxetamide WDG (1:3), showed the best control effects, all exceeding 87%. Among them, Preparation Example 13: 32% oxazolidinone·fluoxetamide WDG (1:3) had the highest control effect, reaching 93.82%. Preparation Example 14: 24% oxazolidinone·fluoxetamide WP (5:1) and Preparation Example 12: 14% oxazolidinone·fluoxetamide EC (1:6) had the second best control effects, ranging from 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] Fourteen days after application, all five test agents demonstrated significant control efficacy against rice planthoppers, reaching over 77% in the field. Only the single-dose oxazolidinone showed a relatively low efficacy of 77.64%. Preparation Example 13: 32% oxazolidinone-oxazolidinone water-dispersible granules (1:3) demonstrated the best control efficacy, achieving 99.12%, with a long-lasting effect.

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

[0218] The test was conducted in Qingfeng Village, Xinhe Town, Hanchuan City, Hubei Province. The previous crop was rapeseed. Fertilizer and water conditions were good, and cultivation and management were consistent. At the time of application, the rice was at the end of the tillering stage, and the rice planthoppers were at their 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 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 base insect population 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. The parallel jumping method was used to investigate 5 points in each plot, with 4 clumps at each point, for a total of 20 clumps of rice. The pot-patting method was used to investigate the number of rice planthoppers, and the insect population reduction rate and control effect were calculated.

[0224] Calculation formula:

[0225]

[0226]

[0227] Table 8 Field efficacy test of oxazolidinone and isoxazolidinone compound on rice planthoppers

[0228]

[0229] Seven days after application, the combination formulation (1:8:36% oxazolidinone / isoxafenamide wettable powder, Preparation Example 10) had the best control effect against rice planthoppers, achieving 97.48%. The second best control was achieved by the 18% oxazolidinone / isoxafenamide suspension concentrate (1:2, Preparation Example 6), achieving 95.20%. All three combinations of oxazolidinone and isoxazolidinone achieved control effects exceeding 90%.

[0230] Ten days after application, the control effect of the 36% oxazolidinone-isoxazolinone wettable powder (1:8) of Preparation Example 10 was 98.83%. The worst control effect of the rice planthopper in this experiment was the single-agent isoxazolidinone, with a control effect of 80.56%, which was significantly lower than the other agents.

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

[0232] The test was conducted in a vegetable field in Daying Village, Dahuangzhuang Town, Huailai County, Zhangjiakou City, Hebei Province. The soil was loamy and had medium to high fertility. Cabbage was planted on August 2. The growth of cabbage in the test field was generally consistent.

[0233] Test target: Diamondback moth.

[0234] Experimental crops: Cabbage.

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

[0236] Test method: The test began when the 2nd to 3rd instar larvae of the diamondback moth were in full bloom, with an average of 1 to 3 larvae per plant. An electric sprayer was used to evenly spray the leaves, backs, and cores of the plants, using a water rate of 750 kg / hm2. 2 .

[0237] Survey Method: Use a 5-point diagonal sampling method, surveying 2 plants per point per plot for a total of 10 plants, and inspect all leaves of each plant. Insect population baseline was determined before application, and insect populations were surveyed 3, 7, and 12 days after application, and the corrected control efficacy was calculated.

[0238] Calculation method of drug efficacy:

[0239]

[0240]

[0241] Table 9 Field efficacy test results for controlling diamondback moth

[0242]

[0243] The test results, as shown in the table above, demonstrate that the combined formulation is highly effective against Plutella brassicae. Three days after application, control rates against Plutella brassicae in the combined formulation treatment areas exceeded 84%. The 2:1 microemulsion of 3% oxazolidinone and isoxazolidinone (preparation example 7) achieved 88.69% control, significantly higher than those in the treatment areas with the single-dose control agents. Seven days after application, control rates for all treatments improved, with the combined formulation treatment areas achieving over 89%.

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

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

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

[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 up between each plot. When the Chilo suppressalis reached the peak egg hatching period, 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 / hm2. 2 The rice plant was sprayed evenly at an average flow rate of 0.85 L / min. No rainfall was observed on the day of application and for 3 days after application. Water was maintained for 1 week after application.

[0250] Efficacy survey: 10 and 20 days after application, when damage in the control area is obvious or when the damage is confirmed, sample 10 points in parallel, with 5 clumps at each point, for a total of 50 clumps per plot. Record the total number of plants and the number of dead cores. Calculate the dead core rate and control efficacy.

[0251]

[0252]

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

[0254]

[0255] The results of the field efficacy test showed that 10 days after 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 concentrate (21:2) were the best, at 90.30%, 95.04%, and 97.59%, respectively. The control effect of oxazolidinone alone was the lowest, at only 76.25%.

[0256] 20 days after the application of the medicine, the control effects of Preparation Example 3: 2% oxazolidinone·flufenacil emulsion (1:1), Preparation Example 5: 28% oxazolidinone·flufenacil wettable powder (3:1) and Preparation Example 1: 22% oxazolidinone·flufenacil 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 insecticidal composition of the present invention has excellent control effects on Lepidoptera and Hemiptera pests, with significant synergistic effects. Furthermore, the compound formulation of the present invention has reasonable components, which can reduce the dosage of pesticides while slowing the development and development of pest resistance and reducing pesticide residues.

Claims

1. An insecticidal composition, characterized in that The insecticide composition comprises active ingredient A and active ingredient B, wherein the active ingredient A is oxazolidinone, and the active ingredient B is any one of flufenacet, isoxazolidinone or flufenacet; 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 1:25-24:

1.

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

1.

3. The insecticidal composition according to claim 2, 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 1:10-12:

1.

4. 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.

5. The insecticidal composition according to claim 1, characterized in that In addition to the active ingredients, the insecticide 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.

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

7. The insecticidal composition according to claim 6, 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.

8. Use of the insecticidal composition according to any one of claims 1 to 7 for controlling pests.

9. The use according to claim 8, characterized in that The pests are lepidoptera pests or hemiptera pests.

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