A pesticide composition containing acerola fruit lactone and triflumizole and application thereof
The pesticide composition of Annona squamosa lactone and trifluorophenylpyrimidine solves the problems of pesticide resistance and environmental pollution, achieving efficient and low-cost pest control and environmental protection.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- ZHENJIANG AGRI SCI INST JIANGSU HILLY AREAS
- Filing Date
- 2026-03-10
- Publication Date
- 2026-06-05
AI Technical Summary
In existing technologies, pest resistance is increasing, and the increased use of pesticides leads to environmental pollution and rising costs. Trifluoropyrimidine has a single target and is prone to resistance, while custard lactone is expensive and its widespread application is limited.
Anchovy lactone and trifluorophenylpyrimidine are combined in a certain proportion to form a pesticide composition for the control of piercing-sucking pests of crops. Multiple formulations are available to suit different application scenarios, reduce dosage and delay the development of pesticide resistance in pests.
Significantly improves control efficacy, reduces pesticide costs, minimizes environmental residues, extends pesticide lifespan, and offers a variety of formulation options to enhance ease of use and efficacy stability.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of pesticide compositions and their applications, and in particular to a pesticide composition containing anechoic acid lactone and trifluorophenylpyrimidine and its applications. Background Technology
[0002] Triflumezopyrim (3,4-dihydro-2,4-dioxo-1-(pyrimidin-5-ylmethyl)-3-(α,α,α-trifluorom-tolyl)-2H-pyrido[1,2-α]pyrimidin-1-on-3-salt) is a novel metronid or zwitterionic insecticide developed by DuPont, and is also a novel pyrimidinone compound. It is highly effective, long-lasting, requires low dosage, and is environmentally friendly. It primarily controls rice planthoppers and leafhoppers, and has a different mechanism of action than neonicotinoid insecticides, having no adverse effects on pollinating insects.
[0003] Annonaceous acetogenins are a new class of compounds discovered from plants in the Annonaceae family. They exhibit a variety of significant biological activities, including antitumor, cytotoxic, insecticidal, antibacterial, and immunosuppressive effects, with cytotoxic and insecticidal activities being particularly noteworthy. They possess strong stomach poison and antifeedant effects on pests, and their insecticidal activity is much higher than that of rotenone, a globally recognized highly effective plant insecticide, and acephate, an organophosphorus pesticide. Research by the US NIH has confirmed that these compounds have very low toxicity to humans.
[0004] With years of chemical pest control, factors such as increased pesticide use and unscientific pesticide application have led to the following problems in pesticide use and application: 1) Pest resistance is intensifying, with an increasing number of resistant pests and reduced effectiveness of single pesticides; 2) High-intensity pesticide use has resulted in excessive pesticide residues in agricultural products, environmental pollution, and increased pesticide costs for farmers; 3) While trifluoropyrimidine is highly effective, its single target makes it prone to resistance with long-term use; anechoic acid lactone has a unique mechanism of action but is expensive, limiting its widespread application. Therefore, developing a pesticide composition that synergistically enhances efficacy, delays resistance development, and reduces dosage is of great significance. Summary of the Invention
[0005] Purpose of the invention: In order to solve the problems existing in the prior art, the present invention proposes a pesticide composition containing Annona squamosa lactone and trifluorophenylpyrimidine and its application. The two active ingredients have different mechanisms of action and, within a certain compound ratio range, have a significant synergistic effect on a variety of pests on crops, especially piercing-sucking pests (planthoppers, aphids, leafhoppers, etc.), thus expanding the control spectrum, while reducing the dosage of a single agent, delaying resistance development and reducing environmental residues.
[0006] Another object of the present invention is to provide the application of the pesticide composition in the control of piercing-sucking pests of crops.
[0007] Technical Solution: To achieve the above objectives, the present invention adopts the following technical solution: a pesticide composition containing Annona squamosa lactone and trifluoropyrimidine, comprising the following active ingredients: Annona squamosa lactone and trifluoropyrimidine; the mass ratio of Annona squamosa lactone to trifluoropyrimidine is 1:10-20:1; the Annona squamosa lactone is extracted from Annonaceae family, Annona genus plant (Annona squamosa). Annona squamosa The dried, mature seeds of Linn. are 1,2-dihydrofuran-type anechoic acid lactone with a purity ≥90%.
[0008] Furthermore, the mass ratio of anolyte lactone to trifluorophenylpyrimidine is 1:5-10:1.
[0009] Furthermore, the mass ratio of anolyte lactone to trifluorophenylpyrimidine is 1:2-5:1.
[0010] Furthermore, the mass ratio of anolyte lactone to trifluorophenylpyrimidine is 1:1 to 2:1.
[0011] Furthermore, the active ingredient in the pesticide composition comprises 10% to 30% by mass, with the remainder being pesticide adjuvants.
[0012] Furthermore, the dosage form is one of the following: suspension concentrate, water-in-oil emulsion, suspension seed coating agent, soluble granules, or microcapsule suspension-suspension concentrate.
[0013] Furthermore, for suspensions, the adjuvants are selected from one or more of wetting agents, dispersants, thickeners, antifreeze agents, defoamers, preservatives, pH adjusters, antioxidants, and light stabilizers; for emulsions, the adjuvants are selected from one or more of solvents, emulsifiers, thickeners, antifreeze agents, antioxidants, light stabilizers, defoamers, preservatives, and pH adjusters; for suspension seed coating agents, the adjuvants are selected from one or more of film-forming agents, binders, dispersants, wetting agents, thickeners, antioxidants, light stabilizers, pH adjusters, antifreeze agents, defoamers, preservatives, and colorants; for soluble granules, the adjuvants are selected from wetting agents, dispersants, disintegrants, binders, carriers, cosolvents, antioxidants, light stabilizers, pH adjusters, and colorants. One or more of the modifier and anti-caking agent; for microcapsule suspensions, the adjuvant is selected from one or more of the capsule wall material, emulsifier, catalyst, encapsulation aid, dispersant, anti-crystallization agent, antifreeze agent, thickener, preservative, antioxidant, light stabilizer, pH adjuster, and defoamer.
[0014] Furthermore, by weight percentage, the suspending agent comprises: 6-20% anechoic acid lactone, 4-10% trifluorophenylpyrimidine, 0.8-1.5% fatty alcohol polyoxyethylene ether (a wetting agent), 2.0-4.0% sodium comb polycarboxylate (a dispersant), 0.3-0.6% ethylene glycol (an antifreeze), 0.3-0.6% xanthan gum (a thickener), 0.4-0.8% magnesium aluminum silicate (an auxiliary thickener), 0.05-0.1% isothiazolinone (a preservative), 0.1-0.3% polydimethylsiloxane (a defoamer), 0.1-0.2% citric acid (a pH adjuster), 0.2-0.4% 2,6-di-tert-butyl-p-cresol (an antioxidant), 0.1-0.2% 2-hydroxy-4-n-octyloxybenzophenone (a light stabilizer), and deionized water to make up to 100%. The water-in-oil emulsion comprises, by weight percentage: 6-20% anechoic acid lactone, 4-10% trifluorophenylpyrimidine, 5.0-15.0% methyl oleate (solvent), 1.0-3.0% ethylene glycol monooleate (cosolvent), 2.0-4.0% phenylphenol polyoxyethylene ether (emulsifier), 0.1-0.3% xanthan gum (thickener), 2.0-4.0% ethylene glycol (antifreeze agent), 0.2-0.5% 2,6-di-tert-butyl-p-cresol (antioxidant), 0.1-0.3% 2-hydroxy-4-n-octyloxybenzophenone (light stabilizer), 0.1-0.2% citric acid (pH adjuster), 0.1-0.3% polydimethylsiloxane (defoamer), 0.05-0.12% isothiazolinone (preservative), and deionized water to make up to 100%. The suspension seed coating agent, by weight percentage, comprises: 6-20% anechoic acid lactone, 4-10% trifluorophenylpyrimidine, 3.0-6.0% acrylate-styrene copolymer as the main film-forming agent, 0.5-1.5% hydroxypropyl methylcellulose as the auxiliary film-forming agent, 0.3-0.8% polyvinylpyrrolidone as the binder, 2.5-4.5% sodium comb polycarboxylate as the dispersant, 0.8-1.5% fatty alcohol polyoxyethylene ether as the wetting agent, 1.0-2.0% basic rose extract as the colorant, 0.4-0.8% xanthan gum as the main thickener, and magnesium silicate as the auxiliary thickener. Aluminum 0.5-1.0%, antioxidant 2,6-di-tert-butyl-p-cresol 0.3-0.6%, light stabilizer 2-hydroxy-4-n-octyloxybenzophenone 0.15-0.35%, pH adjuster citric acid 0.15-0.3%, defoamer polydimethylsiloxane 0.1-0.3%, preservative isothiazolinone 0.05-0.12%, antifreeze ethylene glycol 2.0-4.0%, preservative isothiazolinone 0.06-0.12%, defoamer polydimethylsiloxane 0.1-0.4%, deionized water to 100%; The soluble granules, by weight percentage, comprise: 6-20% anechoic acid lactone, 4-10% trifluorophenylpyrimidine, 2.0-4.0% sodium comb-shaped polycarboxylate dispersant, 1.5-3.0% sodium dodecylbenzenesulfonate wetting agent, 5.0-15.0% urea (a cosolvent / disintegrant), 1.0-3.0% polyethylene glycol 6000 binder, 1.0-2.5% sodium carboxymethyl starch disintegrant, 0.3-0.6% 2,6-di-tert-butyl-p-cresol (an antioxidant), 0.15-0.35% 2-hydroxy-4-n-octyloxybenzophenone (a light stabilizer), 0.15-0.25% citric acid (a pH adjuster), 0.5-1.5% fumed silica (an anti-caking agent), and anhydrous sodium sulfate carrier to make up to 100%. By weight percentage, the microcapsule suspending agent comprises: 6-20% anechoic acid lactone, 4-10% trifluorophenylpyrimidine, 2.0-5.0% polyisocyanate (capsule wall material), 1.5-3.5% phenylphenol polyoxyethylene ether and sodium dodecylbenzenesulfonate (emulsifiers), 0.1-0.4% triethylamine (catalyst), 0.5-2.0% polyethylene glycol 4000 and glycerin (encapsulation aids), 1.0-3.0% sodium comb polycarboxylate (dispersant), 0.5-1.5% sucrose (anti-crystallization agent), and yellow (thickener). The composition comprises: raw gum 0.3-0.8%, thickener magnesium aluminum silicate 0.4-1.0%, antifreeze ethylene glycol 2.0-4.0%, antioxidant 2,6-di-tert-butyl-p-cresol 0.3-0.6%, light stabilizer 2-hydroxy-4-n-octyloxybenzophenone 0.15-0.35%, pH adjuster citric acid 0.15-0.3%, defoamer polydimethylsiloxane 0.1-0.4%, preservative isothiazolinone 0.06-0.12%, and deionized water to make up to 100%. This invention also provides the application of the described pesticide composition in controlling piercing-sucking pests of crops.
[0015] Furthermore, the present invention also provides the application of the pesticide composition in controlling piercing-sucking pests of crops, wherein the piercing-sucking pests of crops are one or more of wheat aphids, corn aphids, and brown planthoppers; the application methods include foliar spraying or seed treatment.
[0016] Beneficial effects: Compared with the prior art, the pesticide composition containing anechoic acid lactone and trifluoropyrimidine of the present invention has the following advantages: (1) Significant synergistic effect: After the combination of custard lactone and trifluoropyrimidine, the control effect on piercing-sucking pests such as wheat aphids, corn aphids and brown planthoppers is significantly improved. The co-toxicity coefficient can reach up to 176.31, which is far higher than the synergistic effect judgment standard of 120. The control effect is significantly improved compared with the single agent used alone.
[0017] (2) Reduced dosage and residue: Field trials showed that when the efficacy was >85%, the amount of chemical pesticides used was reduced by more than 20%; and the pesticide residues in agricultural products were significantly reduced. The residue of trifluoropyrimidine in rice was far below 0.2 mg / kg, which met the GB 2763-2021 standard, improved the quality of rice and reduced the cost of pesticides for farmers.
[0018] (3) Delaying the development of pesticide resistance in pests: Anchovy lactone and trifluoropyrimidine have different mechanisms of action and increased action sites, which can effectively delay the development of pesticide resistance in pests and extend the service life of pesticides.
[0019] (4) Rich and innovative dosage forms: It offers a variety of dosage form options, including new soluble granules (penetration enhancement) and microcapsule suspension-suspension (trifluoropyrimidine microencapsulation + sucrase lactone suspension), which are suitable for different use scenarios and improve the convenience of use and the stability of efficacy. Detailed Implementation
[0020] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. After reading the present invention, any modifications of the present invention in various equivalent forms by those skilled in the art will fall within the scope defined by the appended claims.
[0021] The method for preparing Annona lactone used in the examples is as follows: Anchovy (Annona squamosa), a plant of the genus Anchovy in the family Annonaceae, is used... Annona squamosa The dried mature seeds of *Annona squamosa* were mechanically pulverized and passed through a 20-mesh sieve. After drying under reduced pressure at 40°C for 12 h, 500 g of crude powder was weighed and placed in an extraction vessel. Supercritical CO2 extraction was performed at 45°C and 30 MPa. Separation was carried out at 35°C and 8 MPa for 4 h. The extract (approximately 80 g) was collected and extracted three times with 200 mL of chloroform each time. The chloroform layers were combined, filtered under reduced pressure, and the solvent was recovered under reduced pressure at 45°C. The crude Annona squamosa lactone was then obtained by drying under reduced pressure. Further purification was performed by silica gel column chromatography (eluting agent: petroleum ether-ethyl acetate = 50:1 → 1:1 gradient elution) and reversed-phase preparative liquid chromatography (column: C18, mobile phase: methanol-water = 85:15) to obtain o-ditetrahydrofuran-type Annona squamosa lactone monomer with a purity ≥90%.
[0022] Referencing the People's Republic of China Agricultural Industry Standard NY / T 1156.6-2006 "Guidelines for Indoor Bioassay Testing of Pesticides - Fungicides Part 6: Determination of Combined Effects of Mixtures". Data were statistically processed using DPS software. The median lethal concentration (LC50) was calculated. 50 ), Actual toxicity index (ATI), Theoretical toxicity index (TTI), and Co-toxicity coefficient (CTC), etc.
[0023] The calculation formula is as follows: Actual Toxicity Index (ATI) = (LC50 of Standard Agent) 50 / LC of the test reagent 50 )×100 Theoretical Toxicity Index (TTI) = Σ(Toxicity Index ATI of a drug × Percentage of the active ingredient of the drug in the mixture) Cotoxicity coefficient (CTC) = (Actual toxicity index ATI / Theoretical toxicity index TTI) × 100 Criteria for classifying combined effects: When CTC is greater than 120, it is a synergistic effect; when it is less than 80, it is an antagonistic effect; and when it is between 80 and 120, it is an additive effect.
[0024] (1) Test subjects: Wheat aphids, corn aphids and brown planthoppers were collected from conventional planting fields and reared indoors for one generation before use; custard lactone was prepared by the above method (purity ≥90%), 10% trifluoropyrimidine suspension was produced by DuPont Crop Protection Company, USA, and was directly diluted with deionized water to the required concentration of active ingredient.
[0025] (2) Test method: systemic activity test, continuous immersion method, investigation 4 days after application. The test method refers to NY / T 1154.4-2006 Pesticide Indoor Bioassay Test Guidelines Insecticide Part 4: Systemic Activity Test Continuous Immersion Method.
[0026] 1) Indoor activity determination of custard lactone and trifluorophenylpyrimidine against wheat aphids.
[0027] Table 1. Results of indoor activity assays of Annona squamosa lactone and Trifluorophenylpyrimidine against wheat aphids.
[0028] Table 1 shows that when the mass ratio of anechoic acid lactone to trifluoropyrimidine is in the range of 1:10-20:1, the systemic activity of anechoic acid lactone and trifluoropyrimidine against wheat aphids is enhanced, with a co-toxicity coefficient greater than 120. When the mass ratio of anechoic acid lactone to trifluoropyrimidine is in the range of 1:2-5:1, the systemic activity of anechoic acid lactone to trifluoropyrimidine against wheat aphids is enhanced more significantly, with a co-toxicity coefficient greater than 150. When the mass ratio of anechoic acid lactone to trifluoropyrimidine is in the range of 1:1-2:1, the synergistic effect is most prominent, with a co-toxicity coefficient greater than 160.
[0029] 2) Indoor activity determination of custard lactone and trifluorophenylpyrimidine against corn aphids.
[0030] Table 2. Results of indoor activity assays of Annona squamosa lactone and Trifluorophenylpyrimidine against maize aphids.
[0031] The results in the table above indicate that when the mass ratio of anechoic acid lactone to trifluoropyrimidine is in the range of 1:5-10:1, the systemic activity of anechoic acid lactone and trifluoropyrimidine is enhanced, with a co-toxicity coefficient greater than 120. The enhanced systemic activity of anechoic acid lactone to trifluoropyrimidine is most significant when the mass ratio is in the range of 1:1-2:1, with a co-toxicity coefficient greater than 170.
[0032] 3) Indoor activity determination of custard lactone and trifluorophenylpyrimidine against brown planthopper.
[0033] Table 3: Results of indoor activity assays of custard lactone and trifluorophenylpyrimidine against brown planthopper
[0034] The results in the table above show that when the mass ratio of anechoic acid lactone to trifluoropyrimidine is in the range of 1:10-10:1, it has a synergistic effect on the systemic activity of brown planthopper, with a co-toxicity coefficient greater than 120; when the mass ratio of anechoic acid lactone to trifluoropyrimidine is in the range of 1:2-2:1, the synergistic effect on the systemic activity of brown planthopper is more significant, with a co-toxicity coefficient greater than 150.
[0035] The concentrations of the drug solutions in the following preparation examples are based on the content of the active ingredient. For example, according to the labeled content of a commercially available 10% trifluoropyrimidine suspension, accurately weigh a formulation equivalent to the required mass of the active ingredient, dilute it with deionized water to the corresponding volume, and prepare a drug solution of the required concentration.
[0036] Preparation Example 1: Preparation of 24% Trifluoropyrimidine·Annona squamole aqueous emulsion (ratio 1:2) The following ingredients were added to a 24% trifluorophenylpyrimidine·anthocyanin emulsion: 16% anechoic acid lactone, 8% trifluorophenylpyrimidine, 15% methyl oleate, 3.5% phenylphenol polyoxyethylene ether, 1.75% calcium dodecylbenzenesulfonate, 0.5% 2,6-di-tert-butyl-p-cresol, 0.3% 2-hydroxy-4-n-octyloxybenzophenone, 3.5% ethylene glycol, 0.2% dimethylsiloxane, 0.12% isothiazolinone, 0.2% citric acid, 0.3% xanthan gum, and deionized water to make up to 100%. The above active ingredients, solvent, emulsifier, antioxidant, and light stabilizer were mixed to form an oil phase. Antifreeze, defoamer, preservative, pH adjuster, and thickener were dissolved in deionized water to form an aqueous phase. The oil phase was slowly added to the aqueous phase under high-speed shearing, and shearing continued for 30 minutes to obtain the anechoic acid·anthocyanin emulsion.
[0037] Preparation Example 2: Preparation of 24% Trifluoropyrimidine·Annona squamole suspension (ratio 1:1) Aniseol 12.0%, trifluorophenylpyrimidine 12.0%, sodium comb-shaped polycarboxylate 4.0%, fatty alcohol polyoxyethylene ether 1.5%, sucrose 1.2%, 2,6-di-tert-butyl-p-cresol 0.4%, 2-hydroxy-4-n-octyloxybenzophenone 0.2%, citric acid 0.2%, xanthan gum 0.6%, magnesium aluminum silicate 0.8%, ethylene glycol 0.6%, polydimethylsiloxane 0.3%, isothiazolinone 0.1%, deionized water to make up to 100%; mix the above active ingredients, wetting and dispersing agents, anti-crystallization agents and active ingredient protective agents evenly, add 50% deionized water, and mill until the particle size D90≤3μm to form an initial suspension; dissolve the thickener, antifreeze, defoamer and preservative in the remaining deionized water, and stir until completely dissolved to form an aqueous phase; heat in a high-speed shear machine (2500~3000) Under the action of r / min, the initial suspension was slowly added to the aqueous phase and sheared continuously for 30 minutes. After sampling and testing, the suspension rate, particle size and pH value were found to be up to standard, and a 24% trifluoropyrimidine·anthocarbamate suspension was obtained.
[0038] Preparation Example 3: Preparation of 24% Trifluoropyrimidine·Annona squamole soluble granules (ratio 2:1) Anthocyanin 8.0%, Trifluorophenylpyrimidine 16.0%, Sodium comb-shaped polycarboxylate 3.5%, Sodium dodecylbenzenesulfonate 2.5%, Urea 12.0%, Polyethylene glycol 6000 2.5% sodium carboxymethyl starch, 2.0% sodium 2,6-di-tert-butyl-p-cresol, 0.5% 2-hydroxy-4-n-octyloxybenzophenone, 0.25% citric acid, 0.2% fumed silica, and anhydrous sodium sulfate to make up to 100%; the above active ingredients, wetting and dispersing agents, disintegrants, binders, protective agents and carriers are added to a double cone mixer in the order of "carrier → adjuvants → active ingredient", and mixed for 30-40 minutes until the uniformity is ≥95%; 5%-8% deionized water is added to the mixed powder, kneaded until it can be formed into a ball by hand and easily dispersed by light kneading, and granulated by an extrusion granulator (sieve aperture 1.0-1.5mm); after granulation, it is dried at 50-60℃ until the moisture content is ≤3%, cooled and sieved (20-40 mesh) to obtain 24% trifluoropyrimidine·anthocarbamate soluble granules.
[0039] Preparation Example 4: Preparation of 16% Trifluoropyrimidine·Annona squamosa lactone suspension seed coating agent (ratio 1:1) Aniseol 8.0%, trifluorophenylpyrimidine 8.0%, acrylic acid-styrene copolymer 4.0%, hydroxypropyl methylcellulose 0.8%, polyvinylpyrrolidone 0.5%, comb-shaped sodium polycarboxylate 3.0%, fatty alcohol polyoxyethylene ether 1.0%, xanthan gum 0.5%, magnesium aluminum silicate 0.6%, 2,6-di-tert-butyl-p-cresol 0.4%, 2-hydroxy-4-n-octyloxybenzophenone 0.2%, citric acid 0.15%, ethylene glycol 2.5%, polydimethylsiloxane 0.2%, isothiazolinone 0.08%, basic rose essence 1.5%, deionized water to make up to 100%; first, mix aniseol, 2,6-di-tert-butyl-p-cresol, and 2-hydroxy-4-n-octyloxybenzophenone at high speed (800) beforehand. (r / min, 10 min), then mix with trifluoropyrimidine and pass through a 325-mesh sieve; add the ingredients in the following order: "deionized water → wetting and dispersing agent → technical powder mixture → sand milling → pH adjuster → antifreeze → defoamer → film-forming agent → thickener → preservative", sand mill until the technical particle size D90 ≤ 3 μm, and finally stir at low speed for 20 min to obtain a 16% trifluoropyrimidine·annucrabutalide suspension seed coating agent.
[0040] Preparation Example 5: Preparation of 30% Trifluoropyrimidine·Annona squamosa lactone microcapsule suspension-suspension agent (ratio 1:5) Aniseol 25.0%, Trifluorophenylpyrimidine 5.0%, Polyisocyanate 3.5%, Phenylene phenol polyoxyethylene ether and sodium dodecylbenzenesulfonate 2.5%, Triethylamine 0.3%, Polyethylene glycol 4000 and glycerin 1.5%, Sodium comb polycarboxylate 3.0%, Sucrose 1.2%, Xanthan gum 0.6%, Magnesium aluminum silicate 0.9%, 2,6-Di-tert-butyl-p-cresol 0.6%, 2-hydroxy-4-n-octyloxybenzophenone 0.35%, Citric acid 0.25%, Ethylene glycol 3.5%, Polydimethylsiloxane 0.3%, Isothiazolinone 0.12%, Deionized water to make up to 100%; 1. Microcapsule phase preparation: Trifluorophenylpyrimidine, polyisocyanate, and 60% of compound emulsifier were added to a reaction vessel and stirred at 40-50℃ to dissolve and form an oil phase; deionized water, the remaining 40% of emulsifier, and encapsulation aid were mixed evenly, and the pH was adjusted to 7-9 to form an aqueous phase; the oil phase was dropped into the aqueous phase under high-speed shear (2000-3000 r / min), triethylamine was added, and the reaction was kept at 50-60℃ for 2-3 h. After cooling to room temperature, the microcapsule phase preparation was completed. 2. Preparation of suspension phase: Aniseol lactone, 2,6-di-tert-butyl-p-cresol, 2-hydroxy-4-n-octyloxybenzophenone, comb-shaped sodium polycarboxylate, and sucrose were mixed evenly, some deionized water was added, and the mixture was milled until the particle size D90 ≤ 3 μm. Citric acid was added to adjust the pH, and the mixture was stirred evenly to form a suspension phase. 3. Dual-phase combination: The suspension phase is slowly added to the microcapsule phase and stirred at low speed (300 r / min) for 10 min. Ethylene glycol, defoamer, thickener (magnesium aluminum silicate is added first, followed by xanthan gum), and isothiazolinone are added in sequence. Deionized water is added to the total mass, and stirring is continued for 20 min. After the stability of the two phases is tested and found to be up to standard, a 30% trifluoropyrimidine·anthocarbamate microcapsule suspension-suspension agent is obtained.
[0041] Application Example 1: Referring to and slightly modifying the "Guidelines for Field Efficacy Trials of Pesticides (II) Part 79: Insecticide Control of Wheat Aphids," the 24% trifluoropyrimidine·anthocarbamate emulsifiable concentrate obtained in Preparation Example 1 and the 30% trifluoropyrimidine·anthocarbamate suspension obtained in Preparation Example 2 were used to control wheat aphids and corn aphids. Foliar spraying was used, with a spray volume of 30 L per acre. The results were assessed 7 days after application. The formula for calculating the control effect is as follows: Insect population reduction rate (%) = (Insect population before pesticide application - Insect population after pesticide application) / Insect population before pesticide application × 100 Control efficacy (%) = (Pest population reduction rate in the treated area - Pest population reduction rate in the blank control area) / (100 - Pest population reduction rate in the blank control area) × 100 The control effects of field trials on wheat aphids and corn aphids are shown in Table 4.
[0042] Table 4. Field trials of pesticide compositions prepared in Examples 1, 2, 3, and 5 on wheat and corn aphid control efficacy.
[0043] The results in Table 4 indicate that the dosage of 24% trifluoropyrimidine·anthocarbamate emulsion, suspension, and soluble granule formulations is 8-12 mL (g) / 667m. 2 30% trifluoropyrimidine·anthocarbamate microcapsule suspension - suspension formulation dosage: 6-10 mL / 667 m 2 It exhibits good control effects against both wheat aphids and corn aphids. The control efficacy against wheat aphids is above 87%, reaching a maximum of 94.68%; the control efficacy against corn aphids is above 77%, reaching a maximum of 85.46%. Compared to using trifluoropyrimidine or anechoic acid lactone alone, the dosage is reduced by more than 30% for the same control efficacy, and the control effect is more stable.
[0044] Application Example 2: The 16% trifluoropyrimidine·annulidinone suspension seed coating agent obtained in Example 4 was used for seed treatment to investigate the control effect of different dosages of the agent on rice planthoppers. Nanjing 9108 was used as the test subject, with a seed rate of 4 kg per mu. The rice seeds were first soaked in clean water in a mesh bag for 48 h, then removed from the mesh bag and allowed to drain for 12 h. The seeds from Example 6 were then treated with 5 mL, 10 mL, and 15 mL of the agent per kilogram of rice seed, mixed thoroughly, and left to stand for 6 hours before sowing. The rice seeds sown in seedling trays were then darkened for 3 days before being transferred to seedbeds for seedling cultivation. After 21 days of seedling cultivation, the seedlings were machine-transplanted into the field. Sixty days after sowing, the number of rice planthoppers in each treatment was investigated every 10 days. The method for investigating rice planthoppers was based on the "Guidelines for Field Efficacy Trials of Pesticides (I) Insecticide Control of Rice Planthoppers," with each treatment replicated 4 times. Simultaneously, seeds were treated with 10% trifluoropyrimidine suspension, seeds were treated with custard lactone, and a blank control was established without any treatment. The formula for calculating the control efficacy is as follows: Control efficacy (%) = (Number of insects in the seed-treated area - Number of insects in the blank control area) / Number of insects in the blank control area × 100 The control effect of rice planthoppers in field trials is shown in Table 5.
[0045] Table 5. Field trial results of the pesticide composition from Example 3 on the control of rice planthoppers.
[0046] Field trials showed that a 16% trifluoropyrimidine·annulodinol suspension seed coating agent, applied at a dosage of 2.5-5 mL / kg of seeds, effectively controlled rice planthoppers. Even 100 days after sowing, the control efficacy remained above 80%, comparable to that of 10% trifluoropyrimidine, while reducing the amount of chemical pesticides used. Field trials also indicated that when the control efficacy was >80%, the amount of chemical pesticides used was reduced by more than 30%, lowering operating costs and mitigating environmental pollution. Furthermore, professional testing showed that trifluoropyrimidine residues in rice were <0.01 mg / kg, meeting agricultural product safety standards.
[0047] In addition to controlling wheat aphids, corn aphids and rice planthoppers, the synergistic pesticide composition of this invention can also be used to control other piercing-sucking pests.
Claims
1. A pesticide composition containing Annona squamosa lactone and Trifluoropyrimidine, characterized in that... The active ingredients include: anomeric lactone and trifluorophenylpyrimidine; the mass ratio of anomeric lactone to trifluorophenylpyrimidine is 1:10-20:1; the anomeric lactone is extracted from the plant *Annona squamosa* (family Annonaceae). Annona squamosa The dried, mature seeds of Linn. are 1,2-dihydrofuran-type anechoic acid lactone with a purity ≥90%.
2. The pesticide composition containing anolyte lactone and trifluoropyrimidine according to claim 1, characterized in that: The mass ratio of anolyte lactone to trifluorophenylpyrimidine is 1:5-10:
1.
3. The pesticide composition containing Annona squamosa lactone and Trifluoropyrimidine according to claim 1, characterized in that: The mass ratio of anolyte lactone to trifluorophenylpyrimidine is 1:2-5:
1.
4. The pesticide composition containing Annona squamosa lactone and Trifluoropyrimidine according to claim 1, characterized in that: The mass ratio of anolyte lactone to trifluorophenylpyrimidine is 1:1 to 2:
1.
5. The pesticide composition of Annona squamosa lactone and trifluorophenylpyrimidine according to any one of claims 1-4, characterized in that: The active ingredient comprises 10% to 30% by mass in the pesticide composition, with the remainder being pesticide adjuvants.
6. The pesticide composition of Annona squamosa lactone and trifluorophenylpyrimidine according to claim 1, characterized in that: The dosage form is one of the following: suspension concentrate, water-in-oil emulsion, suspension seed coating agent, soluble granules, and microcapsule suspension-suspension concentrate.
7. The pesticide composition containing Annona squamosa lactone and Trifluoropyrimidine according to claim 6, characterized in that: For suspensions, the additives are selected from one or more of wetting agents, dispersants, thickeners, antifreeze agents, defoamers, preservatives, pH adjusters, antioxidants, and light stabilizers; For water-based emulsions, the additives are selected from one or more of solvents, emulsifiers, thickeners, antifreeze agents, antioxidants, light stabilizers, defoamers, preservatives, and pH adjusters; For suspension seed coating agents, the adjuvants are selected from one or more of the following: film-forming agents, binders, dispersants, wetting agents, thickeners, antioxidants, light stabilizers, pH adjusters, antifreeze agents, defoamers, preservatives, and colorants. For soluble granules, the adjuvant is selected from one or more of wetting agents, dispersants, disintegrants, binders, carriers, solubilizers, antioxidants, light stabilizers, pH adjusters, and anti-caking agents; For microcapsule suspensions, the additives are selected from one or more of the following: capsule wall material, emulsifier, catalyst, encapsulation aid, dispersant, anti-crystallization agent, antifreeze agent, thickener, preservative, antioxidant, light stabilizer, pH adjuster, and defoamer.
8. The pesticide composition containing anolyte lactone and trifluoropyrimidine according to claim 7, characterized in that: The suspending agent, by weight percentage, comprises: 6-20% anechoic acid lactone, 4-10% trifluorophenylpyrimidine, 0.8-1.5% fatty alcohol polyoxyethylene ether (a wetting agent), 2.0-4.0% sodium comb polycarboxylate (a dispersant), 0.3-0.6% ethylene glycol (an antifreeze), 0.3-0.6% xanthan gum (a thickener), 0.4-0.8% magnesium aluminum silicate (an auxiliary thickener), 0.05-0.1% isothiazolinone (a preservative), 0.1-0.3% polydimethylsiloxane (a defoamer), 0.1-0.2% citric acid (a pH adjuster), 0.2-0.4% 2,6-di-tert-butyl-p-cresol (an antioxidant), 0.1-0.2% 2-hydroxy-4-n-octyloxybenzophenone (a light stabilizer), and deionized water to make up to 100%. The water-in-oil emulsion comprises, by weight percentage: 6-20% anechoic acid lactone, 4-10% trifluorophenylpyrimidine, 5.0-15.0% methyl oleate (solvent), 1.0-3.0% ethylene glycol monooleate (cosolvent), 2.0-4.0% phenylphenol polyoxyethylene ether (emulsifier), 0.1-0.3% xanthan gum (thickener), 2.0-4.0% ethylene glycol (antifreeze agent), 0.2-0.5% 2,6-di-tert-butyl-p-cresol (antioxidant), 0.1-0.3% 2-hydroxy-4-n-octyloxybenzophenone (light stabilizer), 0.1-0.2% citric acid (pH adjuster), 0.1-0.3% polydimethylsiloxane (defoamer), 0.05-0.12% isothiazolinone (preservative), and deionized water to make up to 100%. The suspension seed coating agent, by weight percentage, comprises: 6-20% anechoic acid lactone, 4-10% trifluorophenylpyrimidine, 3.0-6.0% acrylate-styrene copolymer as the main film-forming agent, 0.5-1.5% hydroxypropyl methylcellulose as the auxiliary film-forming agent, 0.3-0.8% polyvinylpyrrolidone as the binder, 2.5-4.5% sodium comb polycarboxylate as the dispersant, 0.8-1.5% fatty alcohol polyoxyethylene ether as the wetting agent, 1.0-2.0% basic rose extract as the colorant, 0.4-0.8% xanthan gum as the main thickener, 0.5-1.0% magnesium aluminum silicate as the auxiliary thickener, and 2,6-di-tert-butyl-p-methyl... Phenol 0.3-0.6%, light stabilizer 2-hydroxy-4-n-octyloxybenzophenone 0.15-0.35%, pH adjuster citric acid 0.15-0.3%, defoamer polydimethylsiloxane 0.1-0.3%, preservative isothiazolinone 0.05-0.12%, antifreeze ethylene glycol 2.0-4.0%, preservative isothiazolinone 0.06-0.12%, defoamer polydimethylsiloxane 0.1-0.4%, deionized water to 100%; The soluble granules, by weight percentage, comprise: 6-20% anechoic acid lactone, 4-10% trifluorophenylpyrimidine, 2.0-4.0% sodium comb-shaped polycarboxylate dispersant, 1.5-3.0% sodium dodecylbenzenesulfonate wetting agent, 5.0-15.0% urea (a cosolvent / disintegrant), 1.0-3.0% polyethylene glycol 6000 binder, 1.0-2.5% sodium carboxymethyl starch disintegrant, 0.3-0.6% 2,6-di-tert-butyl-p-cresol (an antioxidant), 0.15-0.35% 2-hydroxy-4-n-octyloxybenzophenone (a light stabilizer), 0.15-0.25% citric acid (a pH adjuster), 0.5-1.5% fumed silica (an anti-caking agent), and anhydrous sodium sulfate carrier to make up to 100%. By weight percentage, the microcapsule suspending agent comprises: 6-20% anechoic acid lactone, 4-10% trifluorophenylpyrimidine, 2.0-5.0% polyisocyanate (capsule wall material), 1.5-3.5% phenylphenol polyoxyethylene ether and sodium dodecylbenzenesulfonate (emulsifiers), 0.1-0.4% triethylamine (catalyst), 0.5-2.0% polyethylene glycol 4000 and glycerin (encapsulation aids), 1.0-3.0% sodium comb polycarboxylate (dispersant), 0.5-1.5% sucrose (anti-crystallization agent), and yellow (thickener). Raw gum 0.3-0.8%, thickener magnesium aluminum silicate 0.4-1.0%, antifreeze ethylene glycol 2.0-4.0%, antioxidant 2,6-di-tert-butyl-p-cresol 0.3-0.6%, light stabilizer 2-hydroxy-4-n-octyloxybenzophenone 0.15-0.35%, pH adjuster citric acid 0.15-0.3%, defoamer polydimethylsiloxane 0.1-0.4%, preservative isothiazolinone 0.06-0.12%, deionized water to make up to 100%.
9. The application of a pesticide composition containing anechoic acid lactone and trifluorophenylpyrimidine as described in any one of claims 1-8 in the control of piercing-sucking pests of crops.
10. The application of a pesticide composition containing anechoic acid lactone and trifluorophenylpyrimidine as described in any one of claims 1-8 in the control of piercing-sucking pests of crops, such as wheat aphids, corn aphids, and brown planthoppers.