An insecticidal composition containing sulfoxaflor and cellobiose

Abstract

The present application relates to a kind of insecticidal compositions containing flonicamid and celangulin, wherein the weight percentage of effective component flonicamid and celangulin is 1-80:10-0.1, which can be further preferred as 10-60:5-0.1.The total mass of two effective components flonicamid and celangulin accounts for 1%-90% of the mass of the entire preparation, which can be further preferred as 10-60%, and the rest is the common adjuvant or filler in pesticides.The insecticidal composition of the present application can be prepared into suspension concentrate, water dispersible granules, water emulsion, microemulsion, emulsifiable concentrate and wettable powder and other dosage forms.The present application carries out binary compounding of flonicamid and celangulin, has obvious synergistic effect, and the quick-acting and long-acting properties of pesticide are good, and reduces production cost and use cost, and is especially suitable for the prevention and treatment of thrips.

Description

Technical Field

[0001] This invention relates to the field of pesticide compound technology, specifically to an insecticidal composition compounded with flonicamid and cypermethrin as active ingredients. Background Technology

[0002] Flupyradifurone is a novel sulfonamide insecticide and a nicotinic acetylcholine receptor agonist. Its mechanism of action involves activating nicotinic acetylcholine receptors in insects, thereby affecting the nervous system. Specifically, after binding to acetylcholine receptors, flonicamid activates the intrinsic activity of the receptors, leading to the opening of receptor channels and the release of extracellular sodium... + It flows into the cells, thereby controlling the transmission of electrical signals between insect nerve cells, affecting the function of the nervous system, and ultimately causing the insect to die from nerve paralysis. Flupyradifurone is particularly effective against piercing-sucking pests because it is absorbed into the plant through the leaves, stems, and roots. Due to its advantages such as high systemic activity, good insecticidal effect, low pesticide residue, low toxicity to non-target organisms, and minimal environmental pollution, flupyradifurone is currently widely used in the chemical control of pests. However, with the widespread application of flupyradifurone in my country, resistance to flupyradifurone has emerged in the field.

[0003] Cuscutellarin is an active ingredient isolated from *Celastrus orbiculatus*, a plant belonging to the Celastraceae family. This plant is widely distributed in provinces along the Yangtze and Yellow Rivers in my country. Its root bark and leaves have long been used in traditional medicine as an insecticide, and it also possesses heat-clearing and detoxifying properties. Since 1980, my country has conducted multidisciplinary systematic research on *Celastrus orbiculatus*. The isolated active ingredients show that all the toxic and anesthetic components possess a dihydroargentofuran polyester structure, with different substituents determining the varying activities of the compounds. Cuscutellarin V exhibits the highest activity among the toxic components, while cuscutellarin IV exhibits the highest activity among the anesthetic components. Preliminary studies on the mechanism of action indicate that the toxic components, represented by cuscutellarin V, primarily act on the plasma membrane and endometrial system of insect intestinal cells; the anesthetic components, represented by cuscutellarin IV, may act on the neuromuscular junctions of insects, with glutamate decarboxylase likely being their primary target. As a plant-derived pesticide insecticide, cucurbitacin mainly acts through stomach poisoning and has the characteristics of not inducing drug resistance, stable physicochemical properties, low toxicity to mammals, and safety to non-target organisms.

[0004] Applying chemical pesticides is the most effective means of controlling plant pests. However, long-term, continuous, and large-scale application of a single chemical pesticide can easily lead to pesticide residues, environmental pollution, and pesticide resistance in pests. To address these problems in agricultural production, chemical pesticides with different mechanisms of action are combined with biopesticides to obtain pesticide compositions that are highly efficient, environmentally friendly, fast-acting, and have a long-lasting effect. This can delay the development of pesticide resistance in pests, reduce pesticide costs, decrease pesticide residues, and be more environmentally friendly. Summary of the Invention

[0005] Based on the above background, in order to meet the needs of agricultural production, the combination of two active components with different mechanisms of action can produce synergistic effects, improve control efficacy, reduce agricultural costs, and delay the development of pesticide resistance in pests. This invention proposes a new insecticidal composition, which is a combination of flonicamid and cypermethrin as active ingredients, and is particularly suitable for the control of thrips.

[0006] The specific technical solution of the present invention is as follows:

[0007] This invention provides an insecticidal composition containing flonicamid and cypermethrin, wherein the weight percentage of the active ingredients flonicamid and cypermethrin is 1-80:10-0.1. Based on the results of specific ratio screening experiments, the weight percentage of the active ingredients flonicamid and cypermethrin can be further preferably (15-30):1.

[0008] The insecticidal composition of the present invention comprises 1% to 90% of the total mass of the two active ingredients, flonicamid and cypermethrin, which are preferably 10% to 60% of the total mass of the formulation, with the remainder being commonly used adjuvants or fillers in pesticides.

[0009] The insecticidal composition of the present invention can be formulated into dosage forms such as suspension concentrate, water-dispersible granules, water emulsion, microemulsion, emulsifiable concentrate and wettable powder.

[0010] This invention also specifically provides a method for preparing schizophyllum extract:

[0011] (1) First, dry the bitter vine plant material until the moisture content is less than 5%, and then pulverize it to 10-30 mesh to obtain bitter vine powder; add 30-80 mL of 50-80% ethanol per gram of bitter vine powder and soak for 2 hours, then stir at 40-70℃ for 60 minutes.

[0012] (2) Microwave extraction was performed on the solution from step (1). The microwave output power was set to 400-600w, the temperature to 40-70℃, and the extraction time to 20-40 minutes. After cooling, the solution was filtered, the filtrate was collected, and the ethanol was removed to obtain the extract.

[0013] (3) Add 100-250 mL of a mixture of ethyl acetate and water in a mass ratio of 1:2-6 to each gram of extract, stir for 60 minutes, let stand to separate the layers, collect the organic layer, concentrate and dry to obtain schizophyllum extract.

[0014] The insecticidal composition of the present invention has a significant synergistic effect, expands the control spectrum and greatly improves the control efficacy, delays the development of pesticide resistance in pests, reduces the number of repeated applications, reduces the amount of chemical active ingredients used, and effectively reduces environmental pollution.

[0015] The insecticidal composition described in this invention has excellent indoor toxicity and field control effects on thrips, and is highly safe for natural enemies and non-target insects, which is of great significance to agricultural production.

[0016] The pesticide formulations that can be prepared from the insecticidal composition of the present invention are as follows:

[0017] The insecticidal composition is a suspension concentrate, and the weight percentages of the components are as follows: flonicamid 5-35%, gentianin 0.5-5%, wetting agent 0-3%, dispersant 2-10%, antifreeze 1-10%, thickener 0.1-5%, preservative 0.1-1%, pH adjuster 0-5%, defoamer 0.1-1%, and water. The specific production steps of this suspension concentrate are as follows: first, other adjuvants are added to a shearing vessel and stirred and sheared evenly; then, the active ingredients flonicamid and gentianin are added and sheared evenly; finally, the material is drawn into a sand mill and milled for 2-3 hours until the particle size is uniformly below 5 μm, thus producing the suspension concentrate formulation of the composition of this invention.

[0018] The insecticidal composition is a water-dispersible granule, and the weight percentages of the components are as follows: flonicamid 5-50%, gentianin 0.5-5%, wetting agent 1%-5%, dispersant 5%-15%, disintegrant 1%-5%, binder 0%-5%, defoamer 0.1%-2%, and the balance being filler. The specific production steps of this water-dispersible granule are as follows: flonicamid, gentianin, dispersant, wetting agent, disintegrant, binder, defoamer, and filler are mixed according to the above formula, stirred evenly in a mixing tank, and then processed through an air jet mill to obtain a master powder with a particle size of 800 mesh or higher. The mixture is then further mixed evenly, and the master powder is added in batches to a mixing mixer, sprayed with an appropriate amount of water, stirred and kneaded, and then granulated using an extrusion granulator. After drying, the water-dispersible granule of the composition of this invention is obtained.

[0019] The insecticidal composition is an oil-in-water emulsion, with the following weight percentages of components: flonicamid 5-20%, gentianin 0.5-5%, emulsifier 5-30%, solvent 5-40%, antifreeze 1-6%, defoamer 0-2%, thickener 0.2-4%, and water. The specific production steps of this oil-in-water emulsion are as follows: First, flonicamid, gentianin, solvent, and emulsifier are added together to dissolve into a homogeneous oil phase; then, a portion of water, antifreeze, and other pesticide adjuvants are mixed together to form a homogeneous aqueous phase; while stirring at high speed in a reaction vessel, the oil phase is added to the aqueous phase, and water is slowly added until the phase inversion point is reached. A shearing machine is then started for high-speed shearing, and the remaining water is added. Shearing is continued for approximately half an hour to form an oil-in-water emulsion, thus producing the oil-in-water emulsion of the composition of this invention.

[0020] The insecticidal composition is a microemulsion, and the weight percentages of the components are: flonicamid 5-25%, gentianin 0.5-5%, emulsifier 5-30%, synergist 0-5%, cosolvent 10-50%, and the balance being water. Fluonicamid and gentianin are completely dissolved in the cosolvent, then the emulsifier, synergist, and other components are added and mixed evenly. Finally, water is added and stirred thoroughly to prepare the microemulsion.

[0021] The insecticidal composition is an emulsifiable concentrate, and the weight percentages of each component are: flonicamid 5-25%, gentianin 0.5-5%, emulsifier 5-30%, synergist 0-5%, and solvent. The specific production steps of this emulsifiable concentrate are as follows: first, the active ingredients flonicamid and gentianin are completely dissolved in the solvent; then, the emulsifier and synergist are added and stirred until a homogeneous, transparent oily liquid is obtained, thus producing the emulsifiable concentrate of the composition of this invention.

[0022] The insecticidal composition is a wettable powder, and the weight percentages of the components are as follows: flonicamid 5-50%, cypermethrin 0.5-5%, wetting agent 1%-5%, dispersant 5%-15%, defoamer 0.1%-2%, and the balance being filler. The specific production steps of this wettable powder are as follows: The components are added to a mixing tank according to the above formula and stirred evenly. The material is then processed through an air jet mill to achieve a particle size of 200-300 mesh, thus producing the wettable powder of the composition of this invention.

[0023] The wetting agent mentioned above can be one or more of alkyl naphthalene sulfonate, fatty amide N-methyl taurate, alkyl sulfonate, alkyl aryl polyoxyethylene ether sulfate, fatty alcohol polyoxyethylene ether, etc.

[0024] The dispersant may be one or more of the following: polycarboxylate, lignin sulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, alkylbenzene sulfonate calcium salt, naphthalene sulfonate formaldehyde condensate sodium salt, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, fatty acid polyoxyethylene ether, and glycerol fatty acid ester polyoxyethylene ether. The disintegrant may be one or more of the following: ammonium sulfate, sodium sulfate, sodium citrate, sodium bicarbonate, aluminum chloride, sodium chloride, polyvinylpyrrolidone, cellulose, starch and its derivatives, bentonite, urea, citric acid, and succinic acid.

[0025] The filler may be one or more of the following: kaolin, light calcium carbonate, diatomaceous earth, bentonite, talc, clay, silica, corn starch, and attapulgite.

[0026] The binder may be one or more of the following: modified sodium polyacrylate, polyethylene glycol, modified polyvinyl alcohol, lignin, and carboxymethyl cellulose.

[0027] The thickener is selected from one or more of xanthan gum, carboxymethyl cellulose, carboxyethyl cellulose, methyl cellulose, magnesium aluminum silicate, and polyvinyl alcohol.

[0028] The emulsifier is selected from one or more of the following: calcium dodecylbenzenesulfonate, fatty acid polyoxyethylene ether, alkylphenol polyoxyethylene ether sulfosuccinate, styrylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, fatty acid polyoxyethylene ester, and polyoxyethylene fatty alcohol ether.

[0029] The solvent is one or more of the following: cyclohexanone, xylene, methanol, ethanol, n-butanol, isopropanol, rosin-based vegetable oil, solvent oil, dimethylformamide, dimethyl sulfoxide, and water.

[0030] The stabilizer is one or more of BHA, BHT, sodium citrate, resorcinol, and epichlorohydrin.

[0031] The antifreeze agent is selected from one or more of ethylene glycol, propylene glycol, glycerol, and polyethylene glycol.

[0032] The synergist is selected from one or more of the following: synergistic ether, organosilicon, hyperosmotic anesthetic, wax remover, and transdermal extract.

[0033] The preservative is selected from one or more of sodium benzoate, potassium sorbate, nitrite, Kathon, and dehydroacetic acid.

[0034] The defoamer is selected from silicone oil, silicone compounds, and C. 10 -C 20 Saturated fatty acid compounds, C8-C 10 One or more fatty alcohols. Detailed Implementation

[0035] To make the objectives, technical solutions, and advantages of this invention clearer, the invention is described below with reference to specific embodiments, but the invention is not limited to these examples.

[0036] In this embodiment of the invention, cuscuta extract was prepared by the following method:

[0037] (1) First, dry the bitter vine plant material until the moisture content is less than 5%, and then pulverize it to 20 mesh to obtain bitter vine powder; add 50 mL of 65% ethanol per gram of bitter vine powder and soak for 2 hours, then stir at 60°C for 60 minutes.

[0038] (2) Microwave extraction was performed on the solution from step (1). The microwave output power was set to 500w, the temperature to 50℃, and the extraction time to 30 minutes. After cooling, the solution was filtered, the filtrate was collected, and the ethanol was removed to obtain the extract.

[0039] (3) Add 200 mL of a mixture of ethyl acetate and water in a mass ratio of 1:3 to each gram of extract, stir for 60 minutes, let stand to separate the layers, collect the organic layer, concentrate and dry to obtain schizophyllum extract.

[0040] In this embodiment of the invention, the toxicity test operation method is as follows:

[0041] The leaf tube film method was used. Several small holes were punched in the cap and bottom of the 4mL centrifuge tubes, with the hole size determined to prevent thrips from escaping. The test reagent was diluted with water to five concentration gradients: 0.1, 0.5, 2.5, 12.5, and 62.5 mg / L. Each concentration was poured into a 4 mL centrifuge tube, shaken several times, and the solution was discarded. The tubes were then left to air dry indoors. Fresh cowpea pods were cut into 2 cm pieces and immersed in the test reagent solution for 10 seconds, then air-dried. These pieces were then placed in centrifuge tubes, and 20 adult cowpea thrips (bean thrips) were sucked in using a pipette and flicked into the centrifuge tubes. The centrifuge tubes were then placed in an artificial climate chamber at (26±1)℃, (65±5)% relative humidity, and a light intensity of L:D = 14h:10h. After 48 hours, the mortality of the test insects was checked (the insects were considered dead if they did not move when lightly touched with the tip of a small brush). Each tube was a replicate, and each concentration was replicated three times. Water was used as a blank control. The toxicity equation and lethal median concentration (LC50) were calculated using the least squares method. 50 Calculate the toxicity index of the drug and the co-toxicity coefficient (CTC value) of the mixture.

[0042] The synergistic effect of drug mixtures is evaluated based on the co-toxicity coefficient (CTC). CTC ≤ 80 indicates antagonistic effect, 80 < CTC < 120 indicates additive effect, and CTC ≥ 120 indicates synergistic effect.

[0043] Actual Toxicity Index (ATI) = (LC50 of the standard reagent) 50 LC-10 of the test reagent 50 )×100.

[0044] Theoretical Toxicity Index (TTI) = Toxicity index of agent A × Percentage content of agent A in the mixture + Toxicity index of agent B × Percentage content of agent B in the mixture

[0045] Co-toxicity coefficient (CTC) = [Actual toxicity index (ATI) of mixture / Theoretical toxicity index (TTI) of mixture] × 100.

[0046] Example 1 Thrips toxicity test

[0047] The toxicity test was conducted according to the proportions in Table 1, and the results are shown in Table 1. Table 1

[0048] Table 1 shows that when the ratio of flonicamid to terpineol was (15–30):1, the CTC was greater than 120, indicating that the insecticidal composition of the present invention had a synergistic effect within this ratio range and exhibited a significant toxic effect on thrips. When the ratio of flonicamid to terpineol was 20:1, the CTC reached 148.38, demonstrating a significant synergistic effect. Further field efficacy tests were conducted on the mixed formulations of the insecticidal composition of the present invention to evaluate their actual field application effects.

[0049] Example 2: 21% Flupyradifurone·Curcumarol Suspension Concentrate Mix according to the following weight ratio:

[0050] Example 3: 60% Flupyradifurone·Curcumarol Water Dispersible Granules Mix according to the following weight ratio:

[0051] Example 4: 25% flupyradifurone·cipermine water-in-oil emulsion was prepared according to the following weight ratio:

[0052] Example 5: 16% flupyradifurone·cipermine microemulsion was formulated in the following weight ratio:

[0053] Example 6: 26% Flupyridine·Curcumarol Emulsifiable Oil Mix according to the following weight ratio:

[0054] Example 7: 10.5% Flupyradifonil·Curcumarol Wettable Powder Mix according to the following weight ratio:

[0055] Comparative Example 1: 20% Flupyradifurone Microemulsion Mix according to the following weight ratio:

[0056] Example 8: Field efficacy trial for controlling thrips

[0057] The experimental plots were designed according to the standards of the State Administration for Quality and Technical Supervision's "Guidelines for Field Efficacy Testing of Pesticides (1)", with each plot having an area of ​​20m². 2 A total of 28 zones were set up, with a 1.2m isolation zone between each zone. The pesticide was applied by spraying, with an electric sprayer spraying evenly once during application.

[0058] Cowpea (cowpea) was tested.

[0059] Test reagents: Examples 2-7, Comparative Example 1, and water control (CK). Each treatment had 4 replicates.

[0060] Dosage of active ingredient: 65g / hm 2 .

[0061] Test location: Chengmai, Hainan; Meteorological conditions: sunny or cloudy, temperature 21-30℃.

[0062] Survey Methods: Before application of pesticides, the initial insect population was assessed. Five points were sampled diagonally across each plot, with 10 cowpea plants surveyed and marked at each point. A total of 50 cowpea plants were surveyed for live insects. The same method was used to survey the insects on days 1, 3, 7, and 14 after application, and the control efficacy was calculated.

[0063]

[0064] Table 2 Results of field efficacy trials for controlling thrips: Table 2

[0065] As shown in Table 2, under the same dosage, the average control efficacy of the formulation in the example reached 80% after 3 days of application, which was higher than that of the control formulation, indicating that the formulation of the present invention has rapid effect. The average control efficacy of the formulation in the example reached over 85% after 7 days of application, which was higher than that of other control formulations, indicating that the formulation in the example had a synergistic effect. The formulation in Example 2 still maintained an efficacy of over 90% after 14 days of application, indicating that the suspension concentrate of Example 2 had significant sustained efficacy. Overall, the results show that the formulation of the present invention has a significantly higher control efficacy against thrips than the control formulation, demonstrating excellent control effects.

[0066] The above description, in conjunction with specific embodiments, provides a further detailed explanation of the present invention, but it should not be construed as limiting the specific implementation of the invention to these descriptions. For those skilled in the art, several simple deductions or substitutions can be made without departing from the concept of the present invention.

Claims

1. An insecticidal composition containing flonicamid and cypermethrin, characterized in that: The weight percentage of flonicamid and styracil was 1–80:10–0.

1.

2. The insecticidal composition of flonicamid and cypermethrin according to claim 1, characterized in that: The preferred weight percentage of flupyradifurone and styracil is (15-30):

1.

3. The insecticidal composition of flonicamid and cypermethrin according to claims 1 and 2, characterized in that: The total mass of the two active ingredients, flonicamid and cypermethrin, accounts for 1% to 90% of the total mass of the preparation.

4. The insecticidal composition of flonicamid and cypermethrin according to claim 3, characterized in that: The total mass of the two active ingredients, flonicamid and styracil, can preferably account for 10-60% of the total mass of the preparation.

5. The insecticidal composition of flonicamid and cypermethrin according to claim 1, characterized in that: Suspension concentrates, water-dispersible granules, water-emulsions, microemulsions, emulsifiable concentrates, and wettable powders.

6. The insecticidal composition of flonicamid and cypermethrin according to claims 1 to 5, characterized in that: The claimed cuscuta extract was prepared by the following method: (1) First, dry the bitter vine plant material until the moisture content is less than 5%, and then pulverize it to 20 mesh to obtain bitter vine powder; add 50 mL of 65% ethanol per gram of bitter vine powder and soak for 2 hours, then stir at 60°C for 60 minutes. (2) Microwave extraction was performed on the solution from step (1). The microwave output power was set to 500w, the temperature to 50℃, and the extraction time to 30 minutes. After cooling, the solution was filtered, the filtrate was collected, and the ethanol was removed to obtain the extract. (3) Add 200 mL of a mixture of ethyl acetate and water in a mass ratio of 1:3 to each gram of extract, stir for 60 minutes, let stand to separate the layers, collect the organic layer, concentrate and dry to obtain schizophyllum extract.

7. The insecticidal composition of flonicamid and cypermethrin according to claims 1 to 5, characterized in that: The insecticidal composition described herein is used to kill thrips.

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