High-efficiency compounded pesticide composition, preparation method and application thereof

Abstract

This invention provides a highly efficient compound pesticide composition, its preparation method, and its application, belonging to the field of pesticide technology. The composition of this invention includes tetrazolium acetamiprid, plant-derived active ingredients (composed of azadirachtin, terpinene, and pyrethrin), piperine butyl ether, sulfobutyl ether-β-cyclodextrin, modified chitosan, and auxiliary components. The combination of tetrazolium acetamiprid and the plant-derived active ingredients in this invention achieves synergistic effects across multiple targets, realizing both rapid killing and long-term control. The modified chitosan, grafted with lauric acid and chloroacetic acid, possesses both hydrophobic and hydrophilic properties, forming a slow-release microcapsule structure. Sulfobutyl ether-β-cyclodextrin encapsulates the plant-derived active ingredients, improving their stability and dispersibility. This composition of the present invention can significantly reduce insect resistance, exhibits highly efficient control effects against Lepidoptera, Coleoptera, and Hemiptera pests, and has a long-lasting effect and good environmental compatibility.

Description

Technical Field

[0001] This invention relates to the field of pesticide technology, specifically to a highly efficient compound pesticide composition, its preparation method, and its application. Background Technology

[0002] In modern agricultural production, pest control is a crucial link in ensuring crop yield and quality. However, long-term use of traditional single-agent pesticides can easily lead to pesticide resistance in target pests, significantly reducing their effectiveness. This necessitates continuously increasing the dosage to achieve the desired results, which not only raises agricultural production costs but also exacerbates problems such as pesticide residues, soil pollution, and ecological damage.

[0003] Meanwhile, while mixing different types of pesticides attempts to improve control efficacy, they generally suffer from poor compatibility and uneven dispersion, easily leading to pesticide decomposition and inactivation. Furthermore, the cumulative ecotoxicity of some pesticides poses a serious threat to non-target organisms and the ecological environment. In addition, conventional pesticide formulations have a short effective period, requiring multiple applications, which not only increases the labor intensity for farmers but also further expands the scope of pesticide environmental impact.

[0004] To address these issues, attempts have been made to develop compound pesticides and slow-release formulations. However, existing compound products often lack scientifically designed synergistic ratios, resulting in insignificant synergistic effects and limited resistance control. Slow-release formulations, on the other hand, frequently suffer from drawbacks such as non-degradable coating materials and poor slow-release performance, making it difficult to balance control efficacy with environmental friendliness. Therefore, developing a compound pesticide composition with highly efficient synergistic control, low resistance risk, long-lasting effect, and good environmental compatibility has become a pressing technical challenge in the agricultural sector, and is of great significance for promoting green agriculture and ensuring the quality and safety of agricultural products. Summary of the Invention

[0005] The purpose of this invention is to provide a highly efficient compound pesticide composition, its preparation method, and its application. The highly efficient compound pesticide composition provided by this invention has a significant control effect on crop pests.

[0006] To achieve the above-mentioned objectives, the present invention provides the following technical solution: This invention provides a highly efficient compound pesticide composition comprising the following raw materials in parts by weight: 3-8 parts tetrazolium acetamiprid, 3-8 parts plant-derived active ingredients, 2-5 parts piperonyl butyl ether, 1-3 parts sulfobutyl ether-β-cyclodextrin, 4-8 parts modified chitosan, 1-2 parts penetration enhancer, 3-6 parts dispersant, and 0.5-1.5 parts stabilizer; wherein the plant-derived active ingredients are composed of azadirachtin, terpineol, and pyrethrin.

[0007] Preferably, the weight ratio of azadirachtin, terpineol and pyrethrin is (1.7-2.3):(2-4):(0.8-1.2).

[0008] Preferably, the method for preparing the modified chitosan includes: mixing chitosan, anhydrous ethanol and sodium hydroxide, microwaving, grafting with lauric acid and chloroacetic acid in sequence, washing and drying to obtain the modified chitosan.

[0009] More preferably, the weight ratio of chitosan, anhydrous ethanol and sodium hydroxide is 10:(20-30):(2-5).

[0010] More preferably, the microwave processing power is 350-450W, the temperature is 45-50℃, and the time is 30-40min.

[0011] More preferably, the weight ratio of chitosan, lauric acid and chloroacetic acid is 10:(2-3):(4-6).

[0012] Preferably, the penetration enhancer is at least one of polyether-modified trisiloxane, methyl oleate, turpentine, and limonene; the dispersant is at least one of sodium lignosulfonate, naphthalene sulfonate formaldehyde condensate, and alkyl naphthalene sulfonate; and the stabilizer is at least one of triphenyl phosphite, ascorbate palmitate, phenyl salicylate, and EDTA-2Na.

[0013] The present invention also provides a method for preparing the above-mentioned high-efficiency compound pesticide composition, comprising: mixing sulfobutyl ether-β-cyclodextrin with water, adding plant-derived active ingredients, drying to obtain an inclusion powder; mixing the inclusion powder, tetrazolium acetamiprid, and piperine butyl ether to obtain a premix; mixing modified chitosan with water, adding a penetration enhancer and a stabilizer to obtain a coating solution; spraying the coating solution onto the surface of the premix, drying, adding a dispersant to obtain the high-efficiency compound pesticide composition.

[0014] The present invention also provides an application of the above-mentioned highly efficient compound pesticide composition in the control of crop pests.

[0015] Preferably, the pests include Lepidoptera, Coleoptera, and Hemiptera pests.

[0016] Compared with the prior art, the present invention has the following beneficial effects: This invention provides a highly efficient compound pesticide composition, comprising: tetrazolium acetamiprid, plant-derived active ingredients, piperine butyl ether, sulfobutyl ether-β-cyclodextrin, modified chitosan, penetration enhancer, dispersant, and stabilizer; the plant-derived active ingredients are composed of azadirachtin, terpineol, and pyrethrin. Tetrazolium acetamiprid, in combination with the plant-derived active ingredients, achieves synergistic effects across multiple targets, enabling rapid killing and long-term control; the modified chitosan, grafted with lauric acid and chloroacetic acid, possesses both hydrophobic and hydrophilic properties, forming a slow-release microcapsule structure; sulfobutyl ether-β-cyclodextrin encapsulates the plant-derived active ingredients, enhancing their stability and dispersibility.

[0017] The experimental results show that the composition of the present invention has excellent indoor insecticidal activity and field control effect on a variety of crop pests such as Lepidoptera, Coleoptera, and Hemiptera. It also has good stability, long-lasting effect, and low risk of resistance, and has good application prospects. Detailed Implementation

[0018] This invention provides a highly efficient compound pesticide composition comprising the following raw materials in parts by weight: 3-8 parts tetrazolium acetamiprid, 3-8 parts plant-derived active ingredients, 2-5 parts piperonyl butyl ether, 1-3 parts sulfobutyl ether-β-cyclodextrin, 4-8 parts modified chitosan, 1-2 parts penetration enhancer, 3-6 parts dispersant, and 0.5-1.5 parts stabilizer; wherein the plant-derived active ingredients are composed of azadirachtin, terpineol, and pyrethrin.

[0019] The tetrazolium amide described in this invention, as the main insecticidal ingredient, works by specifically activating ryanodine receptors in the muscles of pests, causing a continuous release of intracellular calcium ions, leading to muscle spasms, paralysis, and ultimately death. This ingredient possesses contact, stomach, and systemic activity, exhibiting extremely high activity against target pests such as Lepidoptera, Coleoptera, and Hemiptera, and maintaining highly effective control, especially against pest populations resistant to traditional diamide pesticides. Its target is specific, with extremely low toxicity to vertebrates, and it is rapidly metabolized in crops, leaving residues far below national standard limits. This effectively reduces agricultural product safety risks, provides the core insecticidal efficacy of the composition, and lays the foundation for ensuring effective control.

[0020] The preferred weight ratio of azadirachtin, styraxin and pyrethrin in this invention is (1.7-2.3):(2-4):(0.8-1.2), and more preferably 2:3:1.

[0021] The azadirachtin in this invention, a plant-derived active ingredient, inhibits growth and development and blocks oviposition by interfering with the synthesis and metabolism of molting hormones in pests, and also has a feeding deterrent effect, enabling long-term control of pest population density. Cuscuta chinensis acts on the midgut cell membrane of pests, destroying cell structure and causing stomach poison death, and its strong feeding deterrent activity can rapidly reduce crop damage. Pyrethrum exerts its contact killing effect by paralyzing the nervous system of pests, exhibiting rapid efficacy. The combination of these three ingredients in a specific ratio broadens the control spectrum, avoids the shortcomings of insufficient activity of single plant-derived ingredients, and, relying on the characteristics of natural sources, reduces the amount of chemical pesticides used, improves the environmental compatibility of the composition, and, when combined with tetrazolium acetamiprid, provides rapid killing and long-lasting pest suppression.

[0022] This invention combines tetrazolium acetamiprid with plant-derived active ingredients, exhibiting a significant synergistic effect in pest control. Tetrazolium acetamiprid rapidly kills adult insects and older larvae by activating ryanodine receptors, demonstrating immediate effectiveness; azadirachtin interferes with pest growth, development, and reproduction, inhibiting the population density of the next generation for long-term control; cypermethrin's strong antifeedant and stomach poison effects rapidly reduce pest feeding damage; and pyrethroids' neuroparalytic effect enhances the immediate killing effect. The four components have no overlapping targets, avoiding the accumulation of resistance and significantly reducing the risk of resistance development in the target pests.

[0023] The piperonyl butyl ether described in this invention acts as a specific synergist. Its core function is to inhibit the activity of multifunctional oxidases in pests, blocking the metabolic detoxification pathways of target pests to tetrazolium amide and plant-derived active ingredients, thus significantly increasing the accumulation and duration of action of the active ingredients in pests. This ingredient itself has no insecticidal activity and does not increase ecotoxicity. Through synergistic action with insecticidal ingredients, it can enhance the control effect of the composition on target pests, while reducing the dosage of the main active ingredient and decreasing the probability of resistance development. It is a key auxiliary ingredient ensuring the high efficiency and economy of the composition.

[0024] The sulfobutyl ether-β-cyclodextrin described in this invention serves as an inclusion carrier with hydrophobic cavities, enabling it to encapsulate lipid-soluble plant-derived active ingredients. This significantly enhances the water solubility and stability of the plant-derived components, preventing loss of active ingredients due to oxidation and volatilization. Simultaneously, the inclusion structure slows the release rate of the plant-derived components, prolonging their duration of action, and improves the dispersibility of the composition in water, ensuring uniform distribution on the crop surface after application, thus increasing pesticide utilization and solving the problems of easy decomposition and poor dispersibility of plant-derived components.

[0025] The preferred method for preparing the modified chitosan of the present invention includes: mixing chitosan, anhydrous ethanol, and sodium hydroxide, microwave treatment, sequentially grafting with lauric acid and chloroacetic acid, washing, and drying to obtain modified chitosan; the weight ratio of chitosan, anhydrous ethanol, and sodium hydroxide is preferably 10:(20-30):(2-5), more preferably 10:25:3; the microwave treatment power is preferably 350-450W, more preferably 400W, the temperature is preferably 45-50℃, more preferably 48℃, and the time is preferably 30-40min, more preferably 38min; the weight ratio of chitosan, lauric acid, and chloroacetic acid is preferably... The ratio is preferably 10:(2-3):(4-6), more preferably 10:2.5:5; the microwave power for lauric acid grafting is preferably 450-550W, more preferably 500W, the temperature is preferably 55-65℃, more preferably 60℃, and the time is preferably 28-32min, more preferably 30min; the microwave power for chloroacetic acid grafting is preferably 450-550W, more preferably 500W, the temperature is preferably 55-65℃, more preferably 60℃, and the time is preferably 35-45min, more preferably 40min; after chloroacetic acid grafting, it is also preferable to adjust the pH value to 6.5-7 to terminate the reaction.

[0026] This invention utilizes modified chitosan as a biodegradable coating material. After grafting modification with lauric acid and chloroacetic acid, it exhibits both hydrophobic and hydrophilic properties. By coating premixed materials, it forms a slow-release microcapsule structure, achieving slow and continuous release of the active ingredient and reducing the frequency of pesticide application. It possesses strong biocompatibility, readily degrades in soil, and carries a low risk of residue. Simultaneously, it enhances the adhesion of pesticides to crop surfaces, resists rainwater erosion, and improves field application efficacy, balancing long-lasting effects with environmental friendliness.

[0027] The penetration enhancer described in this invention is preferably at least one of polyether-modified trisiloxane, methyl oleate, turpentine, and limonene. The penetration enhancer improves the wetting and spreading ability of the pesticide solution on crop leaves and the surface of pests, while simultaneously penetrating the waxy layer of the pest's epidermis and the cuticle of the crop, promoting the rapid entry of tetrazolium acetamiprid and plant-derived active ingredients into the pest's body and crop tissues, thereby enhancing systemic translocation efficiency.

[0028] The dispersant described in this invention is preferably at least one of sodium lignosulfonate, naphthalenesulfonate formaldehyde condensate, and alkylnaphthalenesulfonate. The dispersant prevents the aggregation and clumping of particles such as tetrazolium acetamiprid and plant-derived active ingredients in the formulation, ensuring the dispersibility and suspension stability of the composition in water and guaranteeing uniform application. It also avoids phytotoxicity caused by excessively high local concentrations or efficacy impairment due to excessively low concentrations.

[0029] The stabilizer described in this invention is preferably at least one of triphenyl phosphite, ascorbate palmitate, phenyl salicylate, and EDTA-2Na. The stabilizer can inhibit the oxidation and hydrolysis reactions of tetrazolium acetamiprid and plant-derived active ingredients, preventing the decomposition and inactivation of the active ingredients. In particular, it can protect plant-derived ingredients from the effects of light and high temperatures, maintaining the physicochemical stability of the composition.

[0030] The present invention also provides a method for preparing the above-mentioned high-efficiency compound pesticide composition, comprising: mixing sulfobutyl ether-β-cyclodextrin with water, adding plant-derived active ingredients, drying to obtain an inclusion powder; mixing the inclusion powder, tetrazolium acetamiprid, and piperine butyl ether to obtain a premix; mixing modified chitosan with water, adding a penetration enhancer and a stabilizer to obtain a coating solution; spraying the coating solution onto the surface of the premix, drying, adding a dispersant to obtain the high-efficiency compound pesticide composition.

[0031] The present invention also provides an application of the above-mentioned highly efficient compound pesticide composition in the control of crop pests; the pests preferably include Lepidoptera, Coleoptera, and Hemiptera pests.

[0032] This composition is suitable for the control of various food crops, cash crops and horticultural crops such as rice, wheat, corn, vegetables, and fruit trees, targeting pests such as Lepidoptera (diamond moth, rice leaf roller, cotton bollworm), Coleoptera (flea beetles, weevils), and Hemiptera (aphids, whiteflies, leafhoppers) (spotted leafminer, melon fly).

[0033] The method of using the high-efficiency compound pesticide composition of the present invention is as follows: Formulation dilution: Adjust the concentration according to the target pest and crop growth stage. For routine control, take 15-30g / mu of this composition and add 15-30kg of water (i.e., dilute 500-1000 times), and stir until completely dispersed without sediment. For high insect population density or resistant pests, the dosage can be adjusted to 25-40g / mu, and the amount of water should be maintained at 15-30kg (dilute 375-600 times).

[0034] Application equipment: Use backpack sprayers, electric sprayers or drone spraying equipment to ensure that there are no other pesticide residues on the spraying equipment, that the nozzles have good atomization effect, and to avoid dripping or excessively large droplets.

[0035] Environmental conditions: Apply pesticides on sunny or cloudy days with temperatures between 15-28℃ and wind force ≤3. Avoid applying pesticides during the midday heat (10:00-16:00), 4 hours before rain, and during windy weather to prevent the pesticide solution from evaporating too quickly or being washed away by rainwater.

[0036] Application method: Foliar spraying: Evenly spray the diluted pesticide solution onto both sides of crop leaves, stems, and fruit surfaces, ensuring the target pest habitats are fully moistened. A uniform film of pesticide should form on the leaf surface without dripping. Targeted adjustments: When controlling chewing pests (such as diamondback moth and corn borer), focus on spraying the heart leaves, tender tissues, and feeding sites of the crop; when controlling piercing-sucking pests (such as aphids and whiteflies), focus on spraying the undersides of leaves and tender shoots; when controlling fruit trees, ensure comprehensive coverage by covering the canopy, fruit surfaces, and branches. Application frequency: Based on the pest occurrence pattern, re-spray 7-10 days after the initial application, for 1-2 consecutive applications; if it rains, re-spray within 24 hours after the rain, using half the dosage.

[0037] Soil treatment: Take 20-35g / mu of this composition and mix thoroughly with 20-30kg of fine soil or well-rotted organic fertilizer to make toxic soil / fertilizer. Apply it in furrows, holes, or as base fertilizer before sowing or transplanting; or dilute it 1000-1500 times and drench the roots, using 50-200ml per plant (adjust according to plant size). Applicable scenarios: Control of underground pests (such as cutworms and grubs), boring pests (such as longhorn beetle larvae), and scenarios requiring systemic protection of the entire plant. Covering the soil after application can enhance the residual efficacy of the pesticide.

[0038] Seed treatment method: Take 0.3%-0.5% of this composition by seed weight, add an appropriate amount of water to make a paste, mix evenly with the seeds, and then dry (do not expose to direct sunlight). Sow the seeds when there is no obvious pesticide residue on the seed surface. Alternatively, use a seed coating machine to mix the composition with the coating agent and then coat the seeds. Advantages: It can prevent aphids, thrips, and underground pests during the seedling stage, reduce the number of pesticide applications during the seedling stage, ensure healthy seedling growth, and has a lasting effect of 20-30 days.

[0039] Precautions Dosage control: Strictly follow the recommended dosage and do not arbitrarily increase the dosage to prevent phytotoxicity or increase the risk of residues; different crops have different sensitivities, and pesticide application is prohibited 7-10 days before harvesting vegetables, fruit trees and other crops.

[0040] Contraindications for mixing: Do not mix with alkaline pesticides (such as Bordeaux mixture and lime sulfur) and copper preparations. If it is necessary to mix with other pesticides, a small-scale compatibility test should be conducted first to confirm that there is no precipitation or stratification before it can be widely used.

[0041] Safety precautions: Wear protective clothing, masks, gloves and goggles when applying pesticides to avoid skin contact and inhalation of the pesticide solution; do not eat or smoke during the application period, and wash your body and equipment promptly after application.

[0042] Non-target organism protection: Avoid applying pesticides during bee honey collection season, mulberry orchards, and aquaculture areas; if water sources are accidentally contaminated, timely isolation measures should be taken to prevent harm to aquatic organisms.

[0043] In this invention, unless otherwise specified, all raw material components are commercially available products well known to those skilled in the art.

[0044] The technical solutions of this invention will be clearly and completely described below with reference to the embodiments thereof. Obviously, the described embodiments are only a part of the embodiments of this invention, and not all of them. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0045] Unless otherwise specified, the following embodiments are all conventional methods.

[0046] Unless otherwise specified, all materials and reagents used in the following examples are commercially available.

[0047] Chitosan is sourced from Henan Lichi Fine Chemical Co., Ltd., with a deacetylation degree of 92.56% and a viscosity of 32 cps; naphthalene sulfonate formaldehyde condensate is sourced from Wuhan Lanabai Pharmaceutical Chemical Co., Ltd., CAS: 9084-06-4; polyether-modified trisiloxane is sourced from Wuhan Huaxiang Kejie Biotechnology Co., Ltd., CAS: 67674-67-3; azadirachtin is sourced from Xi'an Tianhe Pharmaceutical Co., Ltd., with an active ingredient content of 40%; citronella extract is sourced from Lanzhou Waterles Biotechnology Co., Ltd., with an active ingredient content of 25%; pyrethroid is sourced from Lanzhou Waterles Biotechnology Co., Ltd., with an active ingredient content of 40%; the pesticide registration certificate number for the commercially available 10% acetamiprid suspension is PD20212433, and the brand is Liumutian.

[0048] The weight parts of the plant-derived active ingredients in the examples are based on the original drug.

[0049] Example 1 S1. Preparation of modified chitosan Chitosan was mixed with anhydrous ethanol and ultrasonically dispersed at 200W and 25KHz for 10 min. Sodium hydroxide was added, and the mixture was microwaved at 400W and 48℃ for 35 min to obtain a chitosan dispersion. Lauric acid was added to the chitosan dispersion, and the mixture was treated at 500W and 60℃ for 30 min. Chloroacetic acid was added, and the mixture was treated at 500W and 60℃ for 40 min. The pH was adjusted to 6.8, the reaction was terminated, and the mixture was filtered. The precipitate was washed three times with deionized water and freeze-dried under vacuum to a water content of 2wt% to obtain modified chitosan. The weight ratio of chitosan, anhydrous ethanol, sodium hydroxide, lauric acid, and chloroacetic acid is 10:25:3:2.5:5.

[0050] S2. Weighing Accurately weigh the following components by weight: 5 parts tetrazolium amide, 5 parts plant-derived active ingredients, 3 parts piperine butyl ether, 2 parts sulfobutyl ether-β-cyclodextrin, 6 parts modified chitosan, 1.5 parts penetration enhancer, 4.5 parts dispersant, 1 part stabilizer, and 84 parts deionized water. The plant-derived active ingredients consist of azadirachtin, cuscutatin, and pyrethrin in a weight ratio of 2:3:1. The penetration enhancer is composed of polyether-modified trisiloxane and methyl oleate in a weight ratio of 1:1; The dispersant is composed of sodium lignosulfonate and naphthalenesulfonate formaldehyde condensate in a weight ratio of 2:1; The stabilizer is composed of triphenyl phosphite, EDTA-2Na and phenyl salicylate in a weight ratio of 2:2:1.

[0051] S3. Preparation of high-efficiency compound pesticide compositions Sulfobutyl ether-β-cyclodextrin was mixed with 12 parts by weight of deionized water and stirred at 45°C and 350 rpm for 15 min to obtain an aqueous cyclodextrin solution. The plant-derived active ingredient was mixed with 20 parts by weight of anhydrous ethanol solution and stirred at 30°C and 230 rpm for 25 min to obtain a plant-derived active ingredient solution. A plant-derived active ingredient solution was added to a cyclodextrin aqueous solution, stirred at 40℃ and 350 rpm for 70 min, concentrated, and vacuum dried to a water content of 2 wt% to obtain an inclusion powder. The inclusion powder, tetrazolium amide, and piperine butyl ether were mixed to obtain a premix; The modified chitosan was mixed with the remaining deionized water and ultrasonically treated at 300W and 25KHz for 25min to obtain a chitosan aqueous solution. A penetration enhancer and a stabilizer were added to the chitosan aqueous solution and stirred at 32℃ and 200rpm for 30min to obtain a coating solution. The premixed material was fed into a fluidized bed granulator, and the inlet air temperature was adjusted to 52°C. The coating liquid was sprayed onto the surface of the premixed material using a top spray method at an atomization pressure of 0.22 MPa and a spraying rate of 6 mL / min. The mixture was dried to a moisture content of 2 wt%, and a dispersant was added. The mixture was then mixed at 20 rpm for 10 min and passed through a 30-mesh sieve to obtain a high-efficiency compound pesticide composition.

[0052] Example 2 S1. Preparation of modified chitosan Chitosan was mixed with anhydrous ethanol and ultrasonically dispersed at 180W and 23KHz for 15 min. Sodium hydroxide was added, and the mixture was microwaved at 350W and 45℃ for 40 min to obtain a chitosan dispersion. Lauric acid was added to the chitosan dispersion and treated at 450W and 55℃ for 32 min. Chloroacetic acid was added and treated at 450W and 55℃ for 45 min. The pH was adjusted to 6.5, the reaction was terminated, and the mixture was filtered. The precipitate was washed three times with deionized water and freeze-dried under vacuum to a water content of 3wt% to obtain modified chitosan. The weight ratio of chitosan, anhydrous ethanol, sodium hydroxide, lauric acid, and chloroacetic acid is 10:20:2:2:4.

[0053] S2. Weighing Accurately weigh the following components by weight: 3 parts tetrazolium amide, 3 parts plant-derived active ingredients, 2 parts piperine butyl ether, 1 part sulfobutyl ether-β-cyclodextrin, 4 parts modified chitosan, 1 part penetration enhancer, 3 parts dispersant, 0.5 parts stabilizer, and 68 parts deionized water. The plant-derived active ingredients consist of azadirachtin, linalool, and pyrethrin in a weight ratio of 1.7:2:0.8; The penetration enhancer is composed of polyether-modified trisiloxane and turpentine oil in a weight ratio of 3:2; The dispersant is composed of naphthalene sulfonate formaldehyde condensate and sodium alkyl naphthalene sulfonate in a weight ratio of 1:1; The stabilizer is composed of ascorbate palmitate and phenyl salicylate in a weight ratio of 2:1.

[0054] S3. Preparation of high-efficiency compound pesticide compositions Sulfobutyl ether-β-cyclodextrin was mixed with 8 parts by weight of deionized water and stirred at 40°C and 300 rpm for 18 min to obtain an aqueous cyclodextrin solution. The plant-derived active ingredient was mixed with 15 parts by weight of anhydrous ethanol solution and stirred at 28°C and 200 rpm for 30 min to obtain a plant-derived active ingredient solution. A plant-derived active ingredient solution was added to a cyclodextrin aqueous solution, stirred at 38°C and 300 rpm for 80 min, concentrated, and vacuum dried to a water content of 3 wt% to obtain an inclusion powder. The inclusion powder, tetrazolium amide, and piperine butyl ether were mixed to obtain a premix; The modified chitosan was mixed with the remaining deionized water and ultrasonically treated at 250W and 22KHz for 30min to obtain a chitosan aqueous solution. A penetration enhancer and a stabilizer were added to the chitosan aqueous solution and stirred at 30℃ and 180rpm for 35min to obtain a coating solution. The premixed material was fed into a fluidized bed granulator, and the inlet air temperature was adjusted to 50°C. The coating liquid was sprayed onto the surface of the premixed material using a top spraying method at an atomization pressure of 0.2 MPa and a spraying rate of 5 mL / min. The mixture was dried to a moisture content of 3 wt%, and a dispersant was added. The mixture was then mixed at 20 rpm for 10 min and passed through a 20-mesh sieve to obtain a high-efficiency compound pesticide composition.

[0055] Example 3 S1. Preparation of modified chitosan Chitosan was mixed with anhydrous ethanol and ultrasonically dispersed at 250W and 30KHz for 8 min. Sodium hydroxide was added, and the mixture was microwaved at 450W and 50℃ for 30 min to obtain a chitosan dispersion. Lauric acid was added to the chitosan dispersion, and the mixture was treated at 550W and 65℃ for 28 min. Chloroacetic acid was added, and the mixture was treated at 550W and 65℃ for 35 min. The pH was adjusted to 7, the reaction was terminated, and the mixture was filtered. The precipitate was washed three times with deionized water and freeze-dried under vacuum to a water content of 2wt% to obtain modified chitosan. The weight ratio of chitosan, anhydrous ethanol, sodium hydroxide, lauric acid, and chloroacetic acid is 10:30:5:3:6.

[0056] S2. Weighing Accurately weigh the following components by weight: 8 parts tetrazolium amide, 8 parts plant-derived active ingredients, 5 parts piperine butyl ether, 3 parts sulfobutyl ether-β-cyclodextrin, 8 parts modified chitosan, 2 parts penetration enhancer, 6 parts dispersant, 1.5 parts stabilizer, and 95 parts deionized water. The plant-derived active ingredients consist of azadirachtin, linalool, and pyrethrin in a weight ratio of 2.3:4:1.2; The penetration enhancer is composed of methyl oleate and limonene in a weight ratio of 3:1; The dispersant is composed of sodium lignosulfonate and sodium alkylnaphthalenesulfonate in a weight ratio of 3:2; The stabilizer is composed of triphenyl phosphite and ascorbate palmitate in a weight ratio of 3:2.

[0057] S3. Preparation of high-efficiency compound pesticide compositions Sulfobutyl ether-β-cyclodextrin was mixed with 15 parts by weight of deionized water and stirred at 50°C and 400 rpm for 12 min to obtain an aqueous cyclodextrin solution. The plant-derived active ingredient was mixed with 24 parts by weight of anhydrous ethanol solution and stirred at 32°C and 250 rpm for 22 min to obtain a plant-derived active ingredient solution. A plant-derived active ingredient solution was added to a cyclodextrin aqueous solution, stirred at 45℃ and 400rpm for 60min, concentrated, and vacuum dried to a water content of 1wt% to obtain an inclusion powder. The inclusion powder, tetrazolium amide, and piperine butyl ether were mixed to obtain a premix; The modified chitosan was mixed with the remaining deionized water and ultrasonically treated at 320W and 27KHz for 20min to obtain a chitosan aqueous solution. A penetration enhancer and a stabilizer were added to the chitosan aqueous solution and stirred at 35℃ and 250rpm for 27min to obtain a coating solution. The premixed material was fed into a fluidized bed granulator, and the inlet air temperature was adjusted to 55°C. The coating liquid was sprayed onto the surface of the premixed material using a top spray method at an atomization pressure of 0.25 MPa and a spraying rate of 8 mL / min. The mixture was dried to a moisture content of 2 wt%, and a dispersant was added. The mixture was then mixed at 20 rpm for 10 min and passed through a 40-mesh sieve to obtain a high-efficiency compound pesticide composition.

[0058] Comparative Example 1 Unlike Example 1, tetrazolium amide was removed, and the weight of the plant-derived active ingredient was adjusted to 10 parts, so that the total weight remained the same as in Example 1.

[0059] Comparative Example 2 Unlike Example 1, the plant-derived active ingredient was removed, and the weight of tetrazolium amide was adjusted to 10 parts, so that the total weight was consistent with that of Example 1.

[0060] Comparative Example 3 Unlike Example 1, piperidine was replaced with triphenyl phosphate.

[0061] Comparative Example 4 Unlike Example 1, the modified chitosan was prepared by the following method: Chitosan was mixed with anhydrous ethanol and ultrasonically dispersed at 200W and 25KHz for 10 min. Sodium hydroxide was added, and the mixture was microwaved at 400W and 48℃ for 35 min to obtain a chitosan dispersion. Lauric acid was added to the chitosan dispersion, and the mixture was treated at 500W and 60℃ for 30 min. The pH was adjusted to 6.8, the reaction was terminated, and the mixture was filtered. The precipitate was washed three times with deionized water and freeze-dried under vacuum to a water content of 2wt% to obtain modified chitosan. The weight ratio of chitosan, anhydrous ethanol, sodium hydroxide, and lauric acid was 10:25:3:2.5.

[0062] Comparative Example 5 Unlike Example 1, the modified chitosan was prepared by the following method: Chitosan was mixed with anhydrous ethanol and ultrasonically dispersed at 200W and 25KHz for 10 min. Sodium hydroxide was added, and the mixture was microwaved at 400W and 48℃ for 35 min to obtain a chitosan dispersion. Chloroacetic acid was added to the chitosan dispersion and treated at 500W and 60℃ for 40 min. The pH was adjusted to 6.8, the reaction was terminated, and the mixture was filtered. The precipitate was washed three times with deionized water and freeze-dried under vacuum to a water content of 2wt% to obtain modified chitosan. The weight ratio of chitosan, anhydrous ethanol, sodium hydroxide, and chloroacetic acid was 10:25:3:5.

[0063] Comparative Example 6 Unlike Example 1, sulfobutyl ether-β-cyclodextrin was replaced with methylated-β-cyclodextrin.

[0064] Experimental Example 1 Stability test 1. Experimental Objective This experiment aims to systematically evaluate the stability of the compound pesticide compositions prepared in Example 1 and Comparative Examples 1-6, including thermal stability, storage stability and suspension stability.

[0065] The effects of each component on the stability of the composition were clarified by detecting changes in the retention rate, appearance, and suspension rate of the active ingredients (tetrazocarpine, azadirachtin, styraxin, and pyrethrin).

[0066] 2. Experimental Samples Example 1: Highly efficient compound pesticide compositions prepared according to Comparative Examples 1-6.

[0067] 3. Experimental Procedure 3.1 Thermal stability test Sample preparation: Take 5g of each sample and place it in a sealed brown glass bottle. Set up 3 replicates in parallel.

[0068] Constant temperature treatment: The samples were placed in a constant temperature and humidity chamber, with the temperature set at 54℃ and the relative humidity at 75%, and treated for 0 days (initial), 7 days, and 14 days respectively.

[0069] Determination of active ingredient content: Accurately weigh 0.5g of sample, add 50mL of methanol, and extract by sonication for 30min (300W power, 30℃). Centrifuge (8000r / min, 10min), and filter the supernatant through a 0.22μm organic filter membrane for later use.

[0070] The contents of tetrazolium, azadirachtin, cypermethrin, and pyrethrin were determined by HPLC under the following chromatographic conditions: Chromatographic column: C18 column (4.6 mm × 250 mm, 5 μm); Mobile phase: Acetonitrile-water (60:40, v / v) was used for the detection of tetrazolium acetonitrile, with a flow rate of 1.0 mL / min; methanol-0.05 mol / L potassium dihydrogen phosphate buffer (pH=4.5, v / v 55:45) was used for the detection of plant-derived active ingredients, with a flow rate of 1.0 mL / min. Detection wavelengths: Tetrazocarpine 254nm, Azadirachtin 210nm, Cuscutin 230nm, Pyrethrin 220nm; Column temperature: 30℃; injection volume: 20μL.

[0071] Calculate the retention rate of active ingredients: Retention rate (%) = (content after treatment / initial content) × 100%.

[0072] Visual observation: Record changes in appearance of the treated sample, such as color, clumping, and moisture absorption.

[0073] The retention rate of active ingredients and appearance changes of each group of high-efficiency compound pesticide compositions are shown in Table 1.

[0074] Table 1. Retention rate of active ingredients and changes in appearance of each group of compositions.

[0075] Table 1 shows that the thermal stability of Example 1 is significantly better than that of the comparative examples. The core reason is the interaction between the stabilizer and sulfobutyl ether-β-cyclodextrin in the formulation. The stabilizer inhibits the oxidative hydrolysis of the active ingredient, while the inclusion structure of cyclodextrin reduces the volatilization and loss of plant-derived components. In Comparative Examples 4-5, the modified chitosan lacked lauric acid or chloroacetic acid grafting, disrupting the hydrophobic-hydrophilic balance, leading to moisture absorption and clumping, and accelerating the loss of active ingredients. In Comparative Example 6, after replacing the cyclodextrin, the stability of the plant-derived components decreased, confirming the inclusion protection advantage of sulfobutyl ether-β-cyclodextrin for fat-soluble components. Overall, the component combination of Example 1 achieves dual protection of chemical and physical stability.

[0076] 3.2 Storage stability test Sample preparation: Take 20g of each sample, put it into the original packaging container, seal it and store it at room temperature (25±5℃) and relative humidity 60±10% for 0 months (initial), 3 months, 6 months and 12 months respectively.

[0077] Testing indicators: Total effective ingredient retention rate: determined according to step 3 in "Thermal Stability Test"; Total effective ingredient retention rate (%) = (total mass of each effective ingredient after treatment) / (total initial mass of each effective ingredient) × 100%.

[0078] Suspension rate: Refer to GB / T 14825-2006 "Determination of Suspension Rate of Pesticides", take 5g of sample, dilute with standard hard water to 250mL, stir evenly and let stand for 30min, take the upper 9 / 10 suspension, determine the content of active ingredients, and calculate the suspension rate; Appearance: Observe the clumping and layering of the sample.

[0079] The total effective component retention rate, suspension rate and appearance changes of each group of high-efficiency compound pesticide compositions are shown in Table 2.

[0080] Table 2 Results of key indicators in storage stability experiments

[0081] Table 2 shows that after 12 months of storage, Example 1 maintained a total active ingredient retention rate of 89.57% and a suspension rate of 88.72%, while still exhibiting good dispersibility. This is due to the slow-release coating structure of the modified chitosan and the effect of the dispersant. The microcapsules formed by the modified chitosan can block oxygen and moisture, reducing the degradation of the active ingredient, while the dispersant prevents particle aggregation and maintains suspension performance. Comparative Examples 4-5, due to key component substitution or defects in the modification process, showed significant agglomeration after 6 months, with an active ingredient retention rate of only 75%-77% and a suspension rate dropping to 72%-75% after 12 months. This indicates that the coating material modification process and the selection of synergists are crucial for long-term storage stability. The storage stability data of Example 1 meet the long-term shelf-life requirements of pesticide formulations, providing a guarantee for practical application.

[0082] 3.3 Suspension stability test Sample preparation: Take 3g of each sample, dilute with standard hard water (pH=7.0, hardness 342mg / L) to 100mL, place in a 100mL stoppered graduated cylinder, and repeat in 3 parallel groups.

[0083] Observation after standing: Let the mixture stand at 25℃ for 0h, 2h, 4h, 8h, and 24h, and record the percentage of sediment volume at the bottom of the graduated cylinder; Redispersibility: After standing for 24 hours, invert the graduated cylinder 10 times and observe whether the precipitate is completely dispersed. It is considered qualified if there is no obvious particle agglomeration.

[0084] The volume percentage of sedimentation and redispersibility of each high-efficiency compound pesticide composition are shown in Table 3.

[0085] Table 3. Sedimentation volume ratio and redispersibility of each group of high-efficiency compound pesticide compositions after standing.

[0086] Table 3 shows that Example 1 exhibited excellent suspension performance with a sediment volume ratio of only 7.83% after 24 hours of settling, and was completely dispersed without particles. This is because sulfobutyl ether-β-cyclodextrin improved the water solubility of the plant-derived components, the dispersant effectively inhibited particle aggregation, and the modified chitosan coating endowed the particles with suitable density and surface properties, slowing down the sedimentation rate. Comparative Examples 4-6 showed increased sediment volume ratios and poor redispersibility. Specifically, the modified chitosan in Comparative Examples 4-5 lacked a single grafting step, resulting in an imbalance of surface hydrophilicity and hydrophobicity, making it prone to flocculation. In Comparative Example 6, the methylated-β-cyclodextrin had poor inclusion effect, leading to increased sedimentation due to the release of plant-derived components. The suspension stability of Example 1 meets the requirements for pesticide spray formulations, ensuring uniform distribution of the pesticide solution during application, avoiding excessively high or low local concentrations, and guaranteeing consistent control effects.

[0087] Experimental Example 2 Indoor pest control test 1. Experimental Objective The indoor insecticidal activity of the highly efficient compound pesticide composition of this invention against representative pests of Lepidoptera, Coleoptera, and Hemiptera was tested.

[0088] 2. Experimental Materials 2.1 Test Sample The highly efficient compound pesticide compositions prepared in Examples 1-3 and Comparative Examples 1-6 were compared with commercially available conventional pesticides (10% acetamiprid suspension concentrate) as positive controls.

[0089] 2.2 Test pests: Lepidoptera: Diamondback moth (3rd instar larva), Spodoptera litura (3rd instar larva), Bollworm (3rd instar larva); Coleoptera: Green-skinned scarab beetle (adult), longhorn beetle (larva); Hemiptera: Cotton aphid (wingless adult), Wheat long-tubed aphid (wingless adult); All pests were from an indoor artificially bred population. The breeding conditions were a temperature of 25±2℃, a relative humidity of 60±5%, a photoperiod of 16L:8D, and a 4-hour starvation treatment before the experiment.

[0090] 2.3 Experimental Apparatus Petri dishes (9cm in diameter), sprayers (50mL capacity, atomized particle size 50-100μm), electronic balances, dissecting microscopes, constant temperature and humidity incubators, insect aspirators, insect rearing boxes, etc.

[0091] 2.4 Auxiliary Materials Leaf samples from the tested crops (cabbage leaves for diamondback moth, beet armyworm, and cotton bollworm; cotton and wheat leaves for cotton aphid and wheat long-tubed aphid) and artificial feed (longhorn beetle larvae) were used.

[0092] 3 Experimental Design Concentration design: Three concentration gradients were set up: normal concentration (800 times dilution), high concentration (500 times dilution), and low concentration (1200 times dilution); the blank control was standard hard water without pesticides.

[0093] Group design: Each sample-pest-concentration combination was set up with 3 replicates. The number of insects tested in each group was: 50 larvae / group, 20 adults / group, and 100 aphids / group.

[0094] 4. Experimental Procedure 4.1 Sample Dilution Accurately weigh each test sample, dilute it with standard hard water according to the set concentration, stir evenly and let it stand for 10 minutes to ensure that the preparation is completely dispersed without precipitation.

[0095] 4.2 Processing Method Foliar spraying method (applicable to chewing and piercing-sucking pest larvae and adults): Cut fresh crop leaves into 3cm×3cm pieces, place them in a petri dish, and spray the diluted pesticide solution evenly with a sprayer. The amount of pesticide sprayed per leaf is 0.5mL. After air drying, introduce the test pests and cover the dish with a lid with ventilation holes.

[0096] Feed-mixed pesticide method (applicable to borer and underground pest larvae): Mix the diluted pesticide solution with artificial feed at a ratio of 1:10 (volume / mass), put it into the insect rearing box, introduce the test larvae, seal it, and leave a ventilation hole.

[0097] 4.3 Cultivation Conditions All treatment groups were placed in a constant temperature and humidity incubator under the following conditions: temperature 25±2℃, relative humidity 60±5%, and photoperiod 16L:8D.

[0098] 4.4 Observation and Recording The number of pest deaths was observed and recorded at 24h, 48h and 72h after treatment.

[0099] 5. Experimental Results The mortality results of each group of compositions for different pest orders are shown in Tables 4, 5 and 6.

[0100] The death counts in Tables 4, 5, and 6 are the sum of the death counts for the three repeated groups.

[0101] Table 4. Number of Lepidoptera pests killed by each combination (individuals)

[0102] Table 5. Mortality rate (%) of each group of compositions against Coleoptera pests

[0103] Table 6. Mortality rate (%) of each combination of hemiptera pests

[0104] Table 4 shows that Examples 1-3 exhibit extremely strong insecticidal activity against lepidopteran pests (diamond moth, beet armyworm, and cotton bollworm). The insecticidal effect of Example 1 is superior to the comparative examples and the positive control. This is due to the synergistic effect of tetrazolium amide and the plant-derived active ingredients: tetrazolium amide rapidly activates ryanodine receptors to kill pests, azadirachtin inhibits growth and development, terpinene enhances stomach poisoning and antifeedant effects, and pyrethrin improves rapid efficacy. The targets of action do not overlap, resulting in significant synergistic effects. Comparative examples 1-2, lacking any core insecticidal component, showed a decrease in mortality after 72 hours, indicating a loss of synergistic effect. Comparative examples 3-6, due to the replacement or modification of key auxiliary components and process defects, showed decreased activity, confirming the synergistic effect of piperine butyl ether and the protective and release-regulating functions of modified chitosan and cyclodextrin on the active ingredients. Example 1 maintained a high mortality rate even at low concentrations (1200 times), demonstrating a balance between high efficiency and economy.

[0105] Table 5 shows that the mortality rate in Examples 1-3 was significantly higher than that in the comparative and positive controls. This is because tetrazolium amide has a systemic stomach poison effect, effective against both adult and larval coleopterans. The plant-derived component, terpinene, enhances the stomach poison effect, while piperine inhibits the activity of insecticidal enzymes, increasing the accumulation of active ingredients. Comparative Examples 1-2, lacking the core insecticidal component, showed a decrease in mortality, indicating an inability to effectively control coleopteran pests. Comparative Examples 3-6, due to changes in auxiliary components or modified processes, showed a decrease in mortality, demonstrating the significant impact of synergists and formulation processes on the control efficacy against coleopteran pests. Example 1 maintained high activity against boring longhorn beetle larvae, thanks to the formulation's slow-release properties and systemic translocation efficiency, providing an effective solution for the control of underground and boring pests.

[0106] Table 6 shows that Examples 1-3 exhibited excellent insecticidal activity, superior to the positive control and higher than the comparative examples. This is because pyrethrin's neuroparalytic effect has a strong rapid effect on piercing-sucking pests, terpineol disrupts cell structure and induces stomach poison death, azadirachtin's antifeedant effect reduces damage, and tetrazolium's contact and systemic effects provide sustained killing. These active ingredients synergistically cover different growth stages of aphids. Comparative examples 1-2, lacking core components, showed decreased mortality, rapid effect, and sustained effect after 72 hours; comparative examples 3-6 showed decreased activity due to auxiliary components or process defects, highlighting the important roles of penetration enhancers in increasing pesticide penetration and stabilizers in protecting active ingredients. Example 1 showed a mortality rate close to 300 at high concentrations and maintained high activity at low concentrations, making it suitable for different insect population density scenarios. Furthermore, due to its multiple mechanisms of action, it effectively delays the development of resistance in easily resistant pests like aphids.

[0107] In addition, the composition of Example 1 maintained high insecticidal activity at low concentrations (1200 times), which is due to the synergistic effect of tetrazolium amide and plant-derived active ingredients, and the penetration enhancer improved the penetration efficiency of the active ingredients in the pests, thus compensating for the effect of reduced concentration.

[0108] Experimental Example 3 Field test A field control efficacy test of a diamondback moth 1. Experimental Objective The high-efficiency compound pesticide compositions prepared in Examples 1-3 and Comparative Examples 1-6 were tested for their control effects on diamondback moth under field conditions.

[0109] 2. Experimental Materials 2.1 Test Sample Highly efficient compound pesticide compositions prepared in Examples 1-3 and Comparative Examples 1-6; commercially available 10% acetamiprid suspension concentrate (positive control); blank control was standard hard water.

[0110] 2.2 Test Crops and Field Environment The test crop was cabbage (variety: Jingfeng No. 1), in the rosette stage, with uniform growth and no history of pest or disease control. The experimental field soil was loam, with a pH of 6.8±0.2 and an organic matter content of 1.7±0.2%, and good irrigation and drainage conditions. The field was divided into 20m sections. 2 / Community, repeated 3 times, with a 5m distance between communities, and a protective row around the perimeter to avoid cross-contamination.

[0111] 2.3 Test Pests Diamondback moth larvae in their third instar form naturally in the field. Before the experiment, the insect population density was investigated to ensure that the population was uniform in each plot.

[0112] 3 Experimental Design 3.1 Concentration Design The standard application concentration was set uniformly, i.e., diluted 800 times, with no drug applied to the blank control.

[0113] 3.2 Application time Apply pesticides during the peak period of diamondback moth infestation, when the temperature is 19-23℃, the wind force is ≤2, and there is no rainfall in the next 48 hours.

[0114] 3.3 Application Method Foliar spraying, focusing on the front and back of the cabbage leaves and the heart leaves, applying 25 kg of pesticide solution per acre, ensuring that the areas where the target pests live are fully moistened.

[0115] 4. Survey Methods and Data Calculation 4.1 Survey period One day before application (baseline before application), one day after application (rapid effect), three days, seven days, and fourteen days after application (long-lasting effect).

[0116] 4.2 Survey Methodology The five-point sampling method was used, with five points randomly selected from each plot. A 50cm×50cm sampling frame was used at each point to investigate the number of diamondback moth larvae on the cabbage plants within the frame and record the total number of larvae.

[0117] 4.3 Data Calculation Insect population reduction rate (%) = (Insect population density before pesticide application - Insect population density after pesticide application) / Insect population density before pesticide application × 100% Corrected control efficacy (%) = (Pest population reduction rate in the treatment group - Pest population reduction rate in the blank control group) / (1 - Pest population reduction rate in the blank control group) × 100%.

[0118] 5. Experimental Results The corrected control efficacy of each composition against diamondback moth is shown in Table 7.

[0119] Table 7 Corrected control efficacy (%) of each composition against diamondback moth

[0120] Table 7 shows that the corrected control efficacy of Examples 1-3 was superior to that of the comparative examples and the positive control. Example 1 showed a control efficacy of 79.52% one day after application, reaching 97.62% at seven days, and maintaining 92.40% at fourteen days, demonstrating both rapid and sustained efficacy. In the field environment, the modified chitosan coating resisted rain erosion, prolonging the effective period, while the penetration enhancer improved the wetting and spreading of the pesticide on cabbage leaves, ensuring coverage of the target area. Comparative examples 1-2, lacking a core insecticidal component, showed a control efficacy of only 68%-73% at fourteen days, with a rapid resurgence of insect populations later. Comparative examples 3-6, due to defects in auxiliary components or processing, showed a 5%-10% decrease in control efficacy at seven days, with a more significant decrease at fourteen days, indicating that the field environment amplified differences in formulation stability and the effects of auxiliary components. Example 1's field control efficacy remained above 90% fourteen days after application, reducing the number of applications, labor intensity, and environmental impact, meeting the needs of green agriculture.

[0121] Field control efficacy test of wheat aphid. 1. Experimental Objective The high-efficiency compound pesticide compositions prepared in Examples 1-3 and Comparative Examples 1-6 were tested to assess their control efficacy against wheat aphids under field conditions.

[0122] 2. Experimental Materials 2.1 Test Sample Highly efficient compound pesticide compositions prepared in Examples 1-3 and Comparative Examples 1-6; commercially available 10% acetamiprid suspension concentrate (positive control); blank control was standard hard water.

[0123] 2.2 Test Crops and Field Environment The test crop was wheat (variety: Jimai 44), which was in the jointing stage, with uniform growth and no history of pest or disease control. The experimental field soil was loam, with a pH of 6.6-7.0, an organic matter content of 1.5%-1.8%, and good irrigation and drainage conditions. The field was divided into 20m sections. 2 / Community, repeated 3 times, with a 5m distance between communities, and a protective row around the perimeter to avoid cross-contamination.

[0124] 2.3 Test Pests The wingless adult wheat aphids naturally form populations in the field. Before the experiment, the insect population density was investigated to ensure that the insect population in each plot was uniform.

[0125] 3 Experimental Design 3.1 Concentration Design The standard application concentration was set uniformly, i.e., diluted 800 times, with no drug applied to the blank control.

[0126] 3.2 Application time Apply pesticides during the peak period of wheat aphid infestation, when the temperature is 18-22℃, the wind force is ≤2, and there is no rainfall in the next 48 hours.

[0127] 3.3 Application Method Foliar spraying should focus on the underside of wheat leaves and tender shoots, applying 30 kg of pesticide solution per acre to ensure that the areas where the target pests reside are fully moistened.

[0128] 4. Survey Methods and Data Calculation 4.1 Survey period One day before application (baseline before application), one day after application (rapid effect), three days, seven days, and fourteen days after application (long-lasting effect).

[0129] 4.2 Survey Methodology The five-point sampling method was used, with five points randomly selected in each plot. Ten wheat plants were surveyed at each point, and the number of wheat aphids per plant was recorded. The total number of insects was then counted.

[0130] 4.3 Data Calculation Insect population reduction rate (%) = (Insect population density before pesticide application - Insect population density after pesticide application) / Insect population density before pesticide application × 100% Corrected control efficacy (%) = (Pest population reduction rate in the treatment group - Pest population reduction rate in the blank control group) / (1 - Pest population reduction rate in the blank control group) × 100% 5. Experimental Results The corrected control efficacy of each composition against the wheat aphid is shown in Table 8.

[0131] Table 8 Corrected control efficacy (%) of each composition against wheat aphid

[0132] Table 8 shows that Examples 1-3 exhibited excellent field application effects, with Example 1 showing the best results, significantly superior to the positive control and all comparative examples. In the wheat field environment, the suspension stability of the formulation ensured uniform coverage of the underside of the leaves (where aphids inhabit), and the penetration enhancer helped the active ingredient penetrate the leaf cuticle, achieving systemic translocation and continuous aphid killing. Comparative examples 1-2, lacking a core insecticidal ingredient, showed only 75%-80% efficacy after 14 days, failing to control the aphid population long-term; comparative examples 3-6, due to auxiliary ingredients or process defects, showed a 5%-10% decrease in efficacy and insufficient persistence. Example 1 maintained high efficacy under field conditions and was safe for wheat without phytotoxicity, making it suitable for aphid control during critical growth stages such as the wheat jointing stage, which is of great significance for ensuring wheat yield.

[0133] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A highly efficient compound pesticide composition, characterized in that, The raw materials include the following parts by weight: 3-8 parts tetrazolium amide, 3-8 parts plant-derived active ingredients, 2-5 parts piperine butyl ether, 1-3 parts sulfobutyl ether-β-cyclodextrin, 4-8 parts modified chitosan, 1-2 parts penetration enhancer, 3-6 parts dispersant, and 0.5-1.5 parts stabilizer; the plant-derived active ingredients are composed of azadirachtin, terpineol, and pyrethrin.

2. The high-efficiency compound pesticide composition according to claim 1, characterized in that, The weight ratio of azadirachtin, styraxin and pyrethrin is (1.7-2.3):(2-4):(0.8-1.2).

3. The high-efficiency compound pesticide composition according to claim 1, characterized in that, The method for preparing the modified chitosan includes: mixing chitosan, anhydrous ethanol and sodium hydroxide, microwaving, grafting with lauric acid and chloroacetic acid in sequence, washing and drying to obtain the modified chitosan.

4. The high-efficiency compound pesticide composition according to claim 3, characterized in that, The weight ratio of chitosan, anhydrous ethanol and sodium hydroxide is 10:(20-30):(2-5).

5. The high-efficiency compound pesticide composition according to claim 3, characterized in that, The microwave processing power is 350-450W, the temperature is 45-50℃, and the time is 30-40min.

6. The high-efficiency compound pesticide composition according to claim 3, characterized in that, The weight ratio of chitosan, lauric acid and chloroacetic acid is 10:(2-3):(4-6).

7. The high-efficiency compound pesticide composition according to claim 1, characterized in that, The penetration enhancer is at least one of polyether-modified trisiloxane, methyl oleate, turpentine, and limonene; the dispersant is at least one of sodium lignosulfonate, naphthalene sulfonate formaldehyde condensate, and alkyl naphthalene sulfonate; and the stabilizer is at least one of triphenyl phosphite, ascorbate palmitate, phenyl salicylate, and EDTA-2Na.

8. A method for preparing a highly efficient compound pesticide composition according to any one of claims 1-7, characterized in that, include: Sulfobutyl ether-β-cyclodextrin was mixed with water, and plant-derived active ingredients were added. The mixture was then dried to obtain an inclusion powder. The inclusion powder, tetrazolium acetamiprid, and piperine butyl ether were mixed to obtain a premix. Modified chitosan was mixed with water, and a penetration enhancer and stabilizer were added to obtain a coating solution. The coating solution was sprayed onto the surface of the premix, dried, and a dispersant was added to obtain a highly efficient compound pesticide composition.

9. The application of a highly efficient compound pesticide composition according to any one of claims 1-7 in the control of crop pests.

10. The application according to claim 9, characterized in that, The pests include those belonging to the orders Lepidoptera, Coleoptera, and Hemiptera.

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