A pesticidal composition containing Aminopyrifen and its application

Abstract

The present invention belongs to the field of agricultural fungicides, and discloses a pesticide composition containing Aminopyrifen and its application; the active ingredients of the pesticide composition comprise ingredient A and active ingredient B; the active ingredient A is a compound shown by formula (I), and the active ingredient B is ethirimol sulfate. The pesticide composition of the present invention overcomes the deficiencies of single-agent use, has a broad-spectrum bactericidal effect, effectively reduces the usage amount and usage cost of the active ingredients, and delays the generation and development of resistance. The pesticide composition has a high control effect on various plant fungal diseases.

Description

Technical Field

[0001] The present invention relates to the field of pesticide fungicides, and specifically to a pesticide composition containing aminopyrifen and ethynol sulfonate and its application. The pesticide composition or its preparation can enhance the efficacy, reduce the dosage, and at the same time improve the rapid effect, prolong the lasting effect and delay the development of drug resistance. Background Art

[0002] Aminopyrifen is a broad-spectrum pyridine fungicide developed by Agro-kanesho, Japan. Its development code is AKD-5195. Its IUPAC chemical name is 4-phenoxybenzyl 2-amino-6-methylnicotinate and its CAS chemical name is (4-phenoxyphenyl)methyl 2-amino-6-methyl-3-pyridinecarboxylate. CAS registration number is 1531626-08-0. This agent has a high control effect on powdery mildew and gray mold of various fruit and vegetable crops. Its chemical structure is:

[0003]

[0004] Ethylpyrimidine sulfonate is a new generation of systemic fungicide, belonging to adenosine deaminase inhibitor. It can be quickly absorbed by plant stems and leaves, and transported to various parts of the plant body to inhibit the formation of pathogen spores. It has protective and therapeutic effects, and is particularly effective against powdery mildew of crops. It can be used throughout the growth period of crops, and can comprehensively and effectively control all development stages of powdery mildew pathogens, and has a good preventive, therapeutic and eradication effect. Its chemical structure is:

[0005]

[0006] Melon powdery mildew (Sphaeotheca fuliginea) is common in various melon crops in various parts of my country. It is a disease that is widely distributed and causes serious damage to this type of crop, commonly known as "hanging white ash". Melon powdery mildew can occur in melon crops such as cucumber, zucchini, pumpkin, melon, wax gourd, and watermelon throughout the growth period, and is serious in the middle and late stages. It mainly harms leaves, followed by stems and petioles. In the early stage of occurrence, small white, nearly circular powdery spots appear on both sides of the leaves. As the disease progresses, the spots gradually expand into larger white powdery spots. The edges of the spots are unclear, and most of the spots are connected, resembling a layer of white powder. In severe cases, the white powder covers the entire leaf, and then gradually turns gray or gray-brown; in the late growth stage, many small black particles may be scattered on some spots. With the continuous expansion of the planting area of melon crops, the widespread occurrence of this type of disease has caused serious economic losses to farmers.

[0007] Cucumber powdery mildew is a leaf disease caused by Podosphaera xanthii, which has a short incubation period, frequent reinfection, and strong epidemicity. It occurs commonly throughout the country, causes serious damage, and is one of the main diseases in cucumber production. It is prone to occur under high humidity conditions, mainly damaging the leaves, followed by the petioles and stems. At the initial stage of the disease, nearly round powdery white mildew appears on the leaves first, and then fuses into powdery patches. When it is severe, the leaves are covered, causing the leaves to wither or fall off, resulting in serious economic losses to the normal growth of cucumbers.

[0008] Melon powdery mildew is a common disease of melons and can cause serious damage. It can occur throughout the whole growth period of melons. At the initial stage, small white powder spots appear on the front and back of the leaves, and gradually expand into white round powdery patches. Multiple disease spots are connected to each other, covering the leaf surface with white powder. As the disease develops, the color of the powdery patches gradually turns grayish white, and occasionally small black dots appear under the powder layer in the later stage. Finally, the diseased leaves wither and die. Higher humidity is conducive to the germination and invasion of spores. It can occur at 10 - 25°C. Whether it can become epidemic depends on humidity and the growth of the host. It can germinate under low humidity, and the germination rate significantly increases under high humidity. Therefore, after rain when it is dry or with little rain, but the field humidity is high, the epidemic speed of powdery mildew accelerates. In the process of agricultural production, chemical agents are the most effective means to control diseases. Long-term continuous high-dose use of a single chemical agent easily causes a series of problems such as the generation of drug resistance in harmful bacteria and environmental pollution. Rational compounding or mixing of chemical agents has positive characteristics such as expanding the bactericidal spectrum, improving the control effect, extending the suitable application period of pesticides, reducing the dosage of pesticides, reducing phytotoxicity, reducing residues, and delaying the occurrence of drug resistance and resistance in harmful bacteria. As farmers' awareness of environmental protection concepts is getting deeper and deeper, high efficiency, low toxicity, high activity, and low residue have become an inevitable trend in the development of pesticides. Therefore, with the increasing requirements for the environment and food safety, as well as the resistance problem of agents, how to use pesticides scientifically, reduce the dosage of chemical pesticides, and improve the efficacy of pesticides has become an urgent problem to be solved in the pesticide field; in addition, there is no relevant report on the application of the pesticide composition of Aminopyrifen and ethirimol in this regard. Summary of the Invention

[0009] Based on the above situation, the purpose of the present invention is to provide a pesticide composition containing Aminopyrifen and its preparation, which is mainly used for controlling fungal diseases of fruit and vegetable crops. This composition or its preparation can enhance the efficacy of pesticides, reduce the dosage of pesticides, and at the same time can extend the effective period and delay the development of drug resistance.

[0010] To achieve the above purpose, a pesticide composition containing Aminopyrifen includes active ingredient A and active ingredient B. Active ingredient A is Aminopyrifen, and its structural formula is as follows:

[0011]

[0012] Active ingredient B is ethirimol.

[0013] Furthermore, the mass ratio of Aminopyrifen to ethirimol besylate is 50:1 to 1:50.

[0014] Furthermore, the mass ratio of Aminopyrifen to ethirimol besylate is 20:1 to 1:20.

[0015] Furthermore, based on the total weight of the pesticide composition being 100 wt%, the sum of the contents of active ingredient A and active ingredient B in the pesticide composition is 1 to 95 wt%, preferably 5 to 80 wt%, more preferably 10 to 60 wt%;

[0016] Furthermore, the pesticide composition further comprises adjuvants, and the adjuvants are selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreezing agents, defoaming agents, solvents, preservatives, stabilizers, synergists or carriers.

[0017] Furthermore, the dosage form of the pesticide composition can be any one of emulsifiable concentrates, emulsifiable suspensions, microemulsions, suspensions, wettable powders or water dispersible granules;

[0018] Furthermore, the dosage form of the preparation is a microemulsion or an emulsifiable suspension.

[0019] Furthermore, the application of the pesticide composition in controlling plant diseases.

[0020] Furthermore, the plant diseases are plant diseases caused by fungi or bacteria; preferably, the plant diseases are plant diseases caused by fungi; more preferably, the fungi are Sphaerotheca cucurbitae (Jacz) Z.Y.Zhao and Erysiphe cucurbitacearum Zheng & Chen which belong to the genus Sphaerotheca or the genus Erysiphe of the phylum Ascomycota.

[0021] Preferably, the plant diseases are diseases of cucurbitaceous plants; more preferably, the cucurbitaceous plants are cucumber and melon.

[0022] Detailed description of the present invention

[0023] A pesticide composition containing Aminopyrifen, comprising active ingredient A and active ingredient B, where active ingredient A is Aminopyrifen, and the structural formula is as follows:

[0024]

[0025] Active ingredient B is ethirimol besylate.

[0026] Further, the mass ratio of Aminopyrifen to ethirimol sulfate is 50:1, 20:1, 10:1, 5:1, 3:1, 1:1, 1:3, 1:5, 1:10, 1:20 or 1:50.

[0027] Further, the mass ratio of Aminopyrifen to ethirimol sulfate is 20:1 to 1:20.

[0028] Further, based on the total weight of the pesticide composition being 100 wt%, the sum of the contents of active ingredient A and active ingredient B in the pesticide composition is 1 - 95 wt%, preferably 5 - 80 wt%, more preferably 10 - 60 wt%;

[0029] In an embodiment, the sum of the contents of Aminopyrifen and ethirimol sulfate in the pesticide composition is 10 - 60 wt%. For example, the sum of the contents of Aminopyrifen and ethirimol sulfate is 20 wt%, 25 wt%, 30 wt% and 40 wt%.

[0030] By optimizing the content of the active ingredients in the pesticide composition, the present invention enables a better balance between toxicity and residue, enhances the pesticidal efficacy, reduces the dosage of the pesticide, and lowers the cost.

[0031] According to a pesticide composition containing Aminopyrifen provided by the present invention, further, the pesticide composition further comprises adjuvants, and the adjuvants are selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreezing agents, defoaming agents, solvents, preservatives, stabilizers, synergists or carriers.

[0032] The wetting agent is selected from one or more of alkylbenzene sulfonates, alkylnaphthalene sulfonates, lignin sulfonates, sodium dodecyl sulfate, sodium dioctyl sulfosuccinate, α - olefin sulfonates, alkylphenol polyoxyethylene ethers, castor oil polyoxyethylene ethers, alkylphenol ethoxylates, fatty alcohol ethoxylates, fatty alcohol polyoxyethylene ether sulfates, silkworm excrement, sophora flavescens powder, sapindus powder, SOPA, detergent, emulsifier 2000 series and wetting penetrant F; and / or

[0033] The dispersant is selected from one or more of lignin sulfonates, alkylnaphthalene sulfonate formaldehyde condensates, naphthalene sulfonates, triphenylvinylphenol ethoxylate phosphates, fatty alcohol ethoxylates, alkylphenol polyoxyethylene ethers, alkylphenol polyoxyethylene ether methyl ether condensate sulfates, fatty amine polyoxyethylene ethers, glycerol fatty acid ester polyoxyethylene ethers, polycarboxylates, polyacrylates, phosphates, EO - PO block copolymers and EO - PO graft copolymers; and / or

[0034] The emulsifier is selected from one or more of calcium dodecylbenzenesulfonate, alkylphenol formaldehyde resin polyoxyethylene ether, phenylethylphenol polyoxyethylene polyoxypropylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, styrylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, and alkylphenol ether phosphate; and / or

[0035] The thickener is selected from one or more of xanthan gum, organic bentonite, gum arabic, sodium alginate, magnesium aluminum silicate, carboxymethyl cellulose, and silica white; and / or

[0036] The disintegrant is selected from one or more of sodium sulfate, ammonium sulfate, aluminum chloride, sodium chloride, ammonium chloride, bentonite, glucose, sucrose, starch, cellulose, urea, sodium carbonate, sodium bicarbonate, citric acid, and tartaric acid; and / or

[0037] The antifreeze is selected from one or more of alcohols, alcohol ethers, chlorinated hydrocarbons, and inorganic salts; and / or

[0038] The defoamer is selected from one or more of C 10 -C 20 saturated fatty acid compounds, silicone oils, silicone compounds, C8-C 10 fatty alcohols; and / or

[0039] The solvent is selected from one or more of benzene, toluene, xylene, durene, methanol, ethanol, isopropanol, n-butanol, dimethyl sulfoxide, dimethylformamide, cyclohexanone, alkylene carbonate, diesel oil, solvent naphtha, vegetable oil, vegetable oil derivatives, and water; and / or

[0040] The preservative is selected from one or more of propionic acid, sodium propionate, sorbic acid, sodium sorbate, potassium sorbate, benzoic acid, sodium benzoate, sodium p-hydroxybenzoate, methyl p-hydroxybenzoate, Kathon, and 1,2-benzisothiazolin-3-one; and / or

[0041] The stabilizer is selected from one or more of disodium hydrogen phosphate, oxalic acid, succinic acid, adipic acid, borax, 2,6-di-tert-butyl-p-cresol, triethanolamine oleate, epoxidized vegetable oil, kaolin, bentonite, attapulgite, silica white, talc powder, montmorillonite, and starch; and / or

[0042] The synergist is selected from synergistic phosphorus and synergistic ether; and / or

[0043] The carrier is selected from one or more of ammonium salts, ground natural minerals, ground artificial minerals, silicates, resins, waxes, solid fertilizers, water, organic solvents, mineral oils, vegetable oils, and vegetable oil derivatives.

[0044] The present invention provides a pesticidal composition containing Aminopyrifen and its applications. Further, the dosage form of the pesticidal composition is selected from emulsifiable concentrates, emulsifiable oil in water, microemulsions, suspension concentrates, wettable powders, water-dispersible granules; preferably, the dosage form of the preparation is selected from microemulsions and emulsifiable oil in water.

[0045] An emulsifiable concentrate is a liquid prepared by dissolving a high-concentration active ingredient in a solvent and adding an emulsifier. Most emulsifiers use a mixture of non-ionic and anionic surfactants. The preparation of emulsifiable concentrates is relatively simple and convenient, and the biological effect is relatively high. However, the raw material cost is high, and the cost of the preparation is too high, increasing the manufacturing cost of the preparation.

[0046] An emulsifiable oil in water is a preparation in which a liquid pesticide technical or a liquid obtained by mixing with a solvent is dispersed in water in the form of small droplets with a size of 0.5 - 1.5 microns, and the appearance is a milky white liquid. In addition to the active ingredient and the solvent, an emulsifiable oil in water also adds auxiliary agents such as an emulsifier, a dispersant, an antifreeze agent, etc. to improve the stability of the emulsifier.

[0047] A microemulsion is composed of a liquid pesticide, a dispersant, water, a stabilizer, etc. The pesticide particles are 0.01 - 0.1 microns. Using water as the medium, it contains little or no organic solvent, has little environmental pollution, strong permeability to target organisms, and good adhesion. It is an environmentally friendly green pesticide preparation.

[0048] A suspension concentrate refers to a composition that is mixed with a suitable surfactant, water or organic solvent in a certain proportion, and is pulverized to D 90 (the particle size of 90% of the particles) < 10 μm using glass beads and a sand mill to obtain a pulverized slurry, and then thickeners, dispersants, anti-settling agents, defoamers, antifreeze agents and deionized water, etc. are added to the pulverized slurry and mixed. Suspension concentrates are divided into water suspension concentrates and oil suspension concentrates. They have small particle sizes, high biological activities, no problem of dust flying, and are not flammable or explosive.

[0049] A wettable powder refers to a composition in which the technical material of the composition is pre-pulverized and mixed evenly with a dispersant, a wetting agent, a filler, etc. in a certain proportion, and then pulverized by an air-flow pulverizer to meet the requirement that at least 98 wt% passes through a 45 μm test sieve. A wettable powder is a preparation that can be evenly dispersed in water. In addition to the active substance and the inert substance, it also contains a certain amount of anionic or non-ionic surfactants. Wettable powders do not use solvents and emulsifiers, are relatively safe for plants, are not prone to causing phytotoxicity, and are environmentally safe.

[0050] The water dispersible granule is obtained by regranulating the wettable powder or suspension into a water dispersible granule. The composition is mixed with a suitable surfactant and inert substances (kaolin, diatomaceous earth, clay, etc.) powder in a certain proportion to form a mixture, and then granulated by fluidized bed granulation, spray granulation or pan granulation. During the mixing process, the raw materials are pulverized by air flow to make the fineness of the powder particles meet the requirements, and a double - helix mixer and a plow - blade mixer are used for multiple mixings to make the product evenly mixed. This dosage form has good fluidity, is convenient to use, has no dust flying, and is safe and reliable.

[0051] The present invention provides a pesticide composition containing Aminopyrifen. Preferably, the application of the pesticide composition in controlling plant diseases. Preferably, the plant diseases are plant diseases caused by fungi or bacteria; more preferably, the plant diseases are plant diseases caused by fungi; still more preferably, the fungi are Sphaerotheca cucurbitae (Jacz) Z.Y.Zhao and Erysiphe cucurbitacearum Zheng & Chen belonging to the genus Sphaerotheca or Erysiphe of the phylum Ascomycota; still more preferably, the plant diseases are diseases of cucurbitaceae plants; even more preferably, the cucurbitaceae plants are cucumber and melon.

[0052] Compared with the prior art, the beneficial effects of the technical solution of the present invention are as follows:

[0053] (1) By compounding Aminopyrifen with ethirimol besylate, the bactericidal activity is increased and the application range is expanded;

[0054] (2) Safe and environmentally friendly, with broad development prospects, reducing the amount of pesticide used and lowering the agricultural cost;

[0055] (3) Ultra - efficient, with a broad bactericidal spectrum, capable of delaying the generation of pathogen resistance and prolonging the efficacy of the medicament. Detailed implementation manners

[0056] To make the technical solution, purpose and advantages of the present invention clearer, the present invention is illustrated by the following specific examples, but the present invention can be implemented in various forms and should not be limited by the embodiments described herein.

[0057] The implementation examples refer to the Guidelines for Pesticide Bioassay in the Laboratory, Part 11, Potted Plant Method for Controlling Powdery Mildew of Cucurbitaceae, NT / T 1156.11 - 2008; Part 7: Determination of Joint Action of Mixed Formulations, NT / T 1154.7 - 2008.

[0058] Experimental instruments and equipment: electronic balance (sensitivity 0.01mg), artificial climate chamber, pipette, small sprayer, etc.

[0059] Example 1

[0060] Toxicity determination of aminopyrifen and ethirimol blasticidin S against powdery mildew

[0061] Test crops and strains

[0062] Test crops: Cucumbers, potted. When the seedlings grow to 2 - 4 true leaves, they are numbered and reserved for use.

[0063] Test pathogen: Powdery mildew (Sphaeotheca fuliginea), collected from the diseased leaves of cucumbers (variety: Jinyou No. 1) in Nancun Town, Pingdu, Qingdao. The diseased leaves are washed with distilled water at 4°C to wash off the powdery mildew spores on the leaf surface, and a suspension (concentration: 1×10 5 spores / mL) is prepared and stored in a refrigerator at 4°C for later use.

[0064] Formulation of medicaments:

[0065] The original drugs of aminopyrifen and ethirimol blasticidin S are provided by the Research Center of Hailir Group Co., Ltd.

[0066] The original drugs of aminopyrifen and ethirimol blasticidin S are first dissolved in DMF and then diluted with a 0.1% Tween - 80 aqueous solution. Single - agent mother liquors are prepared respectively, and 5 groups of ratios are designed according to the purpose of mixing and the activity of the medicaments. Each single agent and the mixed agents of each group are configured into 5 series of mass concentrations according to the geometric - ratio method.

[0067] Application method: The application equipment is a small sprayer with a capacity of 250 ml and a spray hole diameter of 1 mm. The medicaments are evenly sprayed onto the leaves by the spraying method (it is appropriate to have a water film on the leaves), and then left to dry naturally. Each treatment has no less than 4 replicates, 5 pots for each treatment, 2 plants in each pot, and a treatment without medicaments (including all organic solvents and emulsifiers) is set as a blank control.

[0068] Data statistics and analysis:

[0069] The fresh spore suspension is sprayed onto the inoculated leaves, and the medicaments are sprayed 24 h after artificial inoculation, and then cultured under suitable conditions.

[0070] After application, the disease incidence of each treatment is investigated by grading, and the disease grades are recorded in detail. When the disease leaf rate of the blank control reaches more than 80%, the disease incidence of each treatment is investigated by grading. The grading method is as follows:

[0071] Grade 0: Disease - free

[0072] Grade 1: There are only a small number of small disease spots on the leaves, and the disease spots account for less than 5% of the leaf area;

[0073] Level 3: The diseased spots on the leaves account for 6% - 15% of the leaf area;

[0074] Level 5: The diseased spots on the leaves account for 16% - 25% of the leaf area;

[0075] Level 7: The diseased spots on the leaves account for 26 - 50% of the leaf area;

[0076] Level 9: The diseased spots on the leaves account for 51 - 75% of the leaf area;

[0077] Level 11: The diseased spots on the leaves account for more than 75% of the leaf area.

[0078] According to the survey data, calculate the disease index and control effect of each treatment. Calculate according to formulas (1) and (2), and the calculation results are retained to two decimal places:

[0079]

[0080] X - Disease index;

[0081] N i - Number of diseased leaves at each level;

[0082] i - Relative level value;

[0083] N - Total number of leaves surveyed.

[0084]

[0085] P - Control effect, in percentage (%);

[0086] CK - Disease index of the blank control;

[0087] PT - Disease index of the medicament treatment.

[0088] Use the method of probit analysis to process the data. It can be analyzed with the IBM SPSS Statistics 2.0 statistical analysis system to obtain the EC of the toxicity regression line 50 value, its 95% confidence limit and the correlation coefficient r, and evaluate the activity of the test medicament on the biological test materials.

[0089] Sun Yunpei method: Evaluate the synergistic effect of medicament mixtures according to the co-toxicity coefficient (CTC). A co-toxicity coefficient CTC ≥ 120 for the mixture indicates a synergistic effect; CTC ≤ 80 indicates an antagonistic effect; 80 < CTC < 120 indicates an additive effect. The co-toxicity coefficient (CTC value) of the mixture is calculated according to formulas (3), (4), and (5):

[0090]

[0091] Where:

[0092] ATI——Actual measured toxicity index of the mixture;

[0093] S——EC of the standard fungicide 50 , with the unit of milligram per liter (mg / L);

[0094] M——EC of the mixture 50 , with the unit of milligram per liter (mg / L).

[0095] TTI = TI A *P A +TI B *P B ·······(4)

[0096] In the formula:

[0097] TTI——Theoretical toxicity index of the mixture;

[0098] TI A ——Toxicity index of agent A;

[0099] P A ——Percentage content of agent A in the mixture, with the unit of percentage (%);

[0100] TI B ——Toxicity index of agent B;

[0101] P B ——Percentage content of agent B in the mixture, with the unit of percentage (%).

[0102]

[0103] In the formula:

[0104] CTC——Coefficient of co-toxicity;

[0105] ATI——Actual measured toxicity index of the mixture;

[0106] TTI——Theoretical toxicity index of the mixture.

[0107] Results and analysis:

[0108] It can be seen from Table 1 that: Both the single agents of Aminopyrifen and ethirimol besylate and their compound agents have good bactericidal activities against powdery mildew. The EC 50 value of the single agent of Aminopyrifen is 12.378 mg / L, and the EC 50 value of the single agent of ethirimol besylate is 6.272 mg / L. The EC 50 value of the compound agent of Aminopyrifen and ethirimol besylate at a ratio of 1:5 is the smallest, which is 5.851 mg / L.

[0109] Table 1 Joint Toxicity Determination of Different Ratios of Aminopyrifen and Bupirimate against Powdery Mildew

[0110]

[0111]

[0112]

[0113] It can be seen from Table 2 that both the single agents of Aminopyrifen and bupirimate and their compound agents showed additive or synergistic effects against powdery mildew. The compound agents of Aminopyrifen and bupirimate at ratios of 1:10 to 20:1 all showed synergistic effects. Among them, the co-toxicity coefficient value of the compound agent of Aminopyrifen and bupirimate at a ratio of 5:1 was the largest, being 153.36 > 120.

[0114] Table 2 Determination Results of Synergistic Effects of Different Ratios of Aminopyrifen and Bupirimate against Powdery Mildew

[0115] Test agents <![CDATA[EC 50 > Coefficient of co-toxicity Synergistic effect Biopesticide (mg / L) (ATI) (TTI) (CTC) Aminopyrifen 12.387 100 / / / Bupirimate 6.272 197.49 / / / Aminopyrifen: Bupirimate = 1:50 7.700 160.87 195.58 82.25 Additive effect Aminopyrifen: Bupirimate = 1:20 6.669 185.74 192.85 96.31 Additive effect Aminopyrifen: Bupirimate = 1:10 6.258 197.94 188.63 104.93 Additive effect Aminopyrifen: Bupirimate = 1:5 5.851 211.71 181.24 116.81 Additive effect Aminopyrifen: Bupirimate = 1:3 5.989 206.83 173.12 119.47 Additive effect Aminopyrifen: Bupirimate = 1:1 6.900 179.53 148.74 120.69 Synergistic effect Aminopyrifen: Bupirimate = 3:1 7.200 172.04 124.37 138.33 Synergistic effect Aminopyrifen: Bupirimate = 5:1 6.948 178.28 116.24 153.36 Synergistic effect Aminopyrifen: Bupirimate = 10:1 7.914 156.52 108.86 143.78 Synergistic effect Aminopyrifen: Bupirimate = 20:1 8.753 141.52 104.64 135.24 Synergistic effect Aminopyrifen: Bupirimate = 50:1 10.586 117.01 101.91 114.82 Additive effect

[0116] Preparation Example 1: 20wt% Aminopyrifen·Bupirimate Emulsion in Water

[0117] Dissolve 15 g of Aminopyrifen technical and 5 g of bupirimate technical in a compound solvent composed of 10 g of cyclohexanone and 15 g of 150# solvent oil, and then mix well with 3 g of castor oil polyoxyethylene ether and 3 g of EO-PO block copolymer to obtain the oil phase; mix 5 g of ethylene glycol, 0.2 g of silicone defoamer and 43.8 g of water evenly to obtain the water phase; under high-speed shearing (5000 revolutions per minute), drop the water phase into the oil phase and continue shearing for 10 minutes. The oil phase particles are small droplets with a size of 0.5 - 1.5 microns, and an Aminopyrifen·Bupirimate emulsion in water with an active ingredient mass content of 20wt% is prepared.

[0118] Preparation Example 2: 25wt% Aminopyrifen·Bupirimate Microemulsion

[0119] Dissolve 20 g of the original drug of aminopyrifen and 5 g of the original drug of ethirimol besylate in a compound solvent composed of 10 g of cyclohexanone and 15 g of 150# solvent oil, and then mix well with 3 g of castor oil polyoxyethylene ether and 3 g of EO-PO block copolymer to obtain an oil phase; mix 5 g of ethylene glycol, 0.2 g of silicone defoamer and 38.8 g of water evenly to obtain an aqueous phase; drop the aqueous phase into the oil phase under high-speed shearing (5000 revolutions per minute), and continue shearing for 10 minutes. The oil phase particles are small droplets with a size of 0.01 - 0.1 microns, and a microemulsion of aminopyrifen·ethirimol besylate with an active ingredient mass content of 25 wt% is prepared.

[0120] Preparation Example 3: 30 wt% aminopyrifen·ethirimol besylate aqueous emulsion

[0121] Dissolve 15 g of the original drug of aminopyrifen and 15 g of the original drug of ethirimol besylate in a compound solvent composed of 10 g of cyclohexanone and 15 g of 150# solvent oil, and then mix well with 3 g of castor oil polyoxyethylene ether and 3 g of EO-PO block copolymer to obtain an oil phase; mix 5 g of ethylene glycol, 0.2 g of silicone defoamer and 33.8 g of water evenly to obtain an aqueous phase; drop the aqueous phase into the oil phase under high-speed shearing (5000 revolutions per minute), and continue shearing for 10 minutes. The oil phase particles are small droplets with a size of 0.5 - 1.5 microns, and an aqueous emulsion of aminopyrifen·ethirimol besylate with an active ingredient mass content of 30 wt% is prepared.

[0122] Preparation Example 4: 40 wt% aminopyrifen·ethirimol besylate microemulsion

[0123] Dissolve 30 g of the original drug of aminopyrifen and 10 g of the original drug of ethirimol besylate in a compound solvent composed of 10 g of cyclohexanone and 15 g of 150# solvent oil, and then mix well with 3 g of castor oil polyoxyethylene ether and 3 g of EO-PO block copolymer to obtain an oil phase; mix 5 g of ethylene glycol, 0.2 g of silicone defoamer and 23.8 g of water evenly to obtain an aqueous phase; drop the aqueous phase into the oil phase under high-speed shearing (5000 revolutions per minute), and continue shearing for 10 min. The oil phase particles are small droplets with a size of 0.01 - 0.1 microns, and a microemulsion of aminopyrifen·ethirimol besylate with an active ingredient mass content of 40 wt% is prepared.

[0124] Example 2

[0125] Field experiment on controlling cucumber powdery mildew

[0126] Test scheme

[0127] Test crops: Cucumber (Cucumis sativus L)

[0128] Test object: Powdery mildew

[0129] The experiment was conducted in a cucumber plantation in Nancun Town, Pingdu City, Shandong Province. The cucumber variety was Dutch cucumber. The soil fertility of the experimental plot was medium, the terrain was flat, the fertility was uniform, and the irrigation conditions were good. The cultivation conditions (soil type, fertilization, tillage, row spacing, etc.) of all experimental plots were uniform and consistent with the local agricultural cultivation practice (GAP). The preparation treatment, control treatment, and blank control were arranged in random blocks, and the plot area was 10m 2 (4 rows), the plots were arranged in random blocks, and buffer rows were set between adjacent plots, which was repeated 4 times.

[0130] The application time was mid-July and early August. At the early stage of the disease, the pesticide was applied once every 7 days for 3 consecutive times. The weather was good during the experiment. On the day of the first application, the average daily temperature was 25℃, the highest temperature was 32℃, and the lowest temperature was 21℃.

[0131] The pesticide application equipment is a WS-16D Guardian electric sprayer, the nozzle is a single fan-shaped mist nozzle, the working pressure is 0.15-0.4Mpa, according to the dosage requirements of the drug, according to the area of the plot, accurately measure the dosage. When dispensing the drug, first add one-third of the actual water consumption to the sprayer, add a little water to a small measuring cup to stir the drug evenly, pour it into the sprayer, and finally add the remaining water and mix it. When applying the drug, spray the control first, and then proceed from low concentration to high concentration in sequence, using the constant spray method, and spray evenly at a constant speed according to the calculated pace. When changing different drugs, first clean the sprayer three times and spray out all the water in the spray rod.

[0132] Survey method: Before spraying, the disease index of the plot was investigated at fixed points and plants. 20 plants were randomly investigated in each plot, and 5 leaves of each plant were investigated from top to bottom. The disease level was recorded respectively, and the disease leaf rate and disease index were calculated. The disease situation of each plot was investigated before spraying, 7 days after the first spraying, 7 days after the second spraying, and 7 days after the third spraying, and the disease index and control effect were calculated, and data analysis was performed.

[0133] Using 9-level grading method

[0134] Level 0: no lesions;

[0135] Level 1: The lesion area accounts for less than 5% of the entire leaf area;

[0136] Level 3: The lesion area accounts for 6% to 10% of the entire leaf area;

[0137] Level 5: The lesion area accounts for 11% to 20% of the entire leaf area;

[0138] Level 7: The lesion area accounts for 21% to 50% of the entire leaf area;

[0139] Grade 9: The lesion area accounts for more than 50% of the entire leaf area.

[0140] The drug efficacy is calculated according to formulas (1) and (2):

[0141] (1) Disease index = ∑{(number of diseased leaves at each level * relative level value) / total number of leaves surveyed * 9} * 100

[0142] (2) Control effect (%) = {1 - (disease index before treatment in blank control area * disease index after treatment in treatment area) / (disease index after treatment in blank control area * disease index before treatment in treatment area)} * 100

[0143] Or control effect (without base number before application) % = (disease index in blank control area - disease index in treatment area) / disease index in blank control area * 100

[0144] Test results of cucumber powdery mildew control with each treatment agent

[0145] Table 3 Field test results of different test agents on cucumber powdery mildew

[0146]

[0147] Note: The control effect (%) in the above table is the average value of each repetition. Lowercase letters represent significant differences at the 5% level, and uppercase letters represent significant differences at the 1% level.

[0148] As can be seen from Table 3, cucumber powdery mildew in the experimental plots was in the initial stage of disease, with disease indices ranging from 4.36 to 5.39. Seven days after the first application, the control efficacies of each compound formulation were above 77.01%, and the control efficacy of 20% Aminopyrifen aqueous emulsion was 74.89%, showing good quick-acting properties. The experimental data were processed by the Duncan's new multiple range method using IBM SPSS data processing software. The results of variance analysis showed that there was no difference between 30% Aminopyrifen·ethirimol sulfate aqueous emulsion and 40% Aminopyrifen·ethirimol sulfate microemulsion at the 0.05 and 0.01 levels. The experimental results showed that 30% Aminopyrifen·ethirimol sulfate aqueous emulsion had high quick-acting properties, with a control efficacy of 79.15%, and there were significant differences between each compound formulation and the control single agent. As the application time increased, the control efficacies of most agents of 40% Aminopyrifen·ethirimol sulfate microemulsion increased 7 days after the second application, with the maximum control efficacy being 84.06%. The control efficacies of 25% Aminopyrifen·ethirimol sulfate microemulsion, 30% Aminopyrifen·ethirimol sulfate aqueous emulsion, and 40% Aminopyrifen·ethirimol sulfate microemulsion were 81.09%, 83.95%, and 84.06% respectively. The control efficacy of 25% ethirimol sulfate microemulsion decreased with the increase of application time, being 60.96%. The results of variance analysis showed that 25% ethirimol sulfate microemulsion was significantly different from other treatments at the 0.05 and 0.01 levels, 7 days after the first application and 7 days after the second application. Seven days after the third application, 30% Aminopyrifen·ethirimol sulfate aqueous emulsion was the highest, being 91.43%. The control efficacies of the four compound formulations of 20% Aminopyrifen·ethirimol sulfate aqueous emulsion, 25% Aminopyrifen·ethirimol sulfate microemulsion, 30% Aminopyrifen·ethirimol sulfate aqueous emulsion, and 40% Aminopyrifen·ethirimol sulfate microemulsion were above 83.69%, and there was no difference between the two agents at the 0.05 and 0.01 levels, and there were significant differences from the single agent. Through the experiment, it was found that cucumber powdery mildew was prone to occur under high humidity conditions, mainly damaging the leaves, followed by the petioles and stems. When initially diseased, nearly circular powdery white mildew appears on the leaves first, and then fuses into powdery patches. When severe, the leaves are covered, causing the leaves to wither or fall off, resulting in serious economic losses to the normal growth of cucumbers. The key to the control of cucumber powdery mildew lies in mastering the best control period, and during the disease epidemic period, continuous control is carried out 2 - 3 times.

[0149] Example 3

[0150] Field experiment on the control of melon powdery mildew

[0151] Experimental scheme

[0152] Test crop: Melon (Cucumis melo L)

[0153] Test object: Powdery mildew

[0154] The experiment was conducted in mid-July at a melon plantation in Weifang, Shandong Province. The melon variety was Emerald No. 2. The soil fertility of the experimental field was medium, the terrain was flat, the fertility was uniform, and the irrigation conditions were good. The cultivation conditions (soil type, fertilization, tillage, row spacing, etc.) of all experimental plots were uniform and consistent with the local agricultural cultivation practice (GAP). The preparation treatment, control treatment, and blank control were arranged in random blocks, and the plot area was 20m 2 , the cells were arranged in random blocks, and buffer rows were set between adjacent cells, which was repeated 4 times.

[0155] The pesticide was applied in late July. At the initial stage of the disease, the pesticide was applied once every 7 days for 3 consecutive times. The weather was good during the test. On the day of the first application, the average daily temperature was 23°C, the highest temperature was 31°C, and the lowest temperature was 19°C.

[0156] The pesticide application equipment is a WS-16D Guardian electric sprayer, the nozzle is a single fan-shaped mist nozzle, the working pressure is 0.15-0.4Mpa, according to the dosage requirements of the drug, according to the area of the plot, accurately measure the dosage. When dispensing the drug, first add one-third of the actual water consumption to the sprayer, add a little water to a small measuring cup to stir the drug evenly, pour it into the sprayer, and finally add the remaining water and mix it. When applying the drug, spray the control first, and then proceed from low concentration to high concentration in sequence, using the constant spray method, and spray evenly at a constant speed according to the calculated pace. When changing different drugs, first clean the sprayer three times and spray out all the water in the spray rod.

[0157] Survey method: Before spraying, the disease index of each plot was investigated at fixed points and plants. Ten plants were randomly investigated in each plot, and five leaves were investigated for each plant. The disease level was recorded and the disease leaf rate and disease index were calculated. The disease situation of each plot was investigated before spraying, 7 days after the first spraying, 7 days after the second spraying, and 7 days after the third spraying, and the disease index and control effect were calculated, and data analysis was performed.

[0158] Using 9-level grading method

[0159] Level 0: no lesions;

[0160] Level 1: The lesion area accounts for less than 5% of the entire leaf area;

[0161] Level 3: The lesion area accounts for 6% to 10% of the entire leaf area;

[0162] Level 5: The lesion area accounts for 11% to 20% of the entire leaf area;

[0163] Grade 7: The lesion area accounts for 21% - 50% of the entire leaf area;

[0164] Grade 9: The lesion area accounts for more than 50% of the entire leaf area.

[0165] The drug efficacy is calculated according to formulas (1) and (2):

[0166] (1) Disease index = ∑{(number of diseased leaves at each level * relative level value) / total number of leaves surveyed * 9} * 100

[0167] (2) Control effect (%) = {1 - (disease index before treatment in blank control area * disease index after treatment in treatment area) / (disease index after treatment in blank control area * disease index before treatment in treatment area)} * 100

[0168] Or control effect (without base number before applying medicine) % = (disease index in blank control area - disease index in treatment area) / disease index in blank control area * 100

[0169] Test results of the control of powdery mildew on melons by each treatment agent

[0170] Table 4 Field test results of different test agents on powdery mildew of melons

[0171]

[0172]

[0173] Note: The control effect (%) in the above table is the average value of each repetition. Lowercase letters represent significant differences at the 5% level, and uppercase letters represent significant differences at the 1% level.

[0174] The test results showed that, as can be seen from Table 4, powdery mildew of melons occurred severely in the test plots and was in the disease stage, with the disease index ranging from 8.61 to 10.17. Seven days after the first application of pesticides, the control effects of each compound pesticide were above 49.65%. The control effect of 20% Aminopyrifen aqueous emulsion was 49.73%, and the control effect of 25% ethirimol besylate microemulsion was 52.38%, with relatively poor control effects. As time went by, the control effects increased. Seven days after the second application of pesticides, the control effect of 30% Aminopyrifen·ethirimol besylate aqueous emulsion was 64.77%, the control effect of 40% Aminopyrifen·ethirimol besylate microemulsion was 64.50%, the control effect of 20% Aminopyrifen·ethirimol besylate aqueous emulsion was 62.62%, and the control effect of 30% Aminopyrifen·ethirimol besylate aqueous emulsion was 62.41%. The control effects of the four compound pesticides were higher than those seven days after the first application of pesticides. The test data were processed by the Duncan's new multiple range method using IBM SPSS data processing software. The results of variance analysis showed that there were no differences among the four compound pesticides at the 0.05 and 0.01 levels. Seven days after the third application of pesticides, the control effect of 30% Aminopyrifen·ethirimol besylate aqueous emulsion was the highest, at 81.76%; the control effect of 20% Aminopyrifen·ethirimol besylate aqueous emulsion was the second, at 80.28%. The control effect of 25% ethirimol besylate microemulsion was 66.00%, and the control effect of 20% Aminopyrifen aqueous emulsion was 70.10%, which was significantly higher than that of 25% ethirimol besylate microemulsion. Powdery mildew of melons is a common disease of melons and can cause serious harm. It can occur throughout the whole growth period of melons. At the initial stage, small white powder spots appear on the front and back of the leaves, and gradually expand into white round powder spots. Multiple disease spots are connected to each other, covering the leaf surface with white powder. As the disease develops, the color of the powder spots gradually turns grayish white, and occasionally small black dots appear under the powder layer in the later stage. Finally, the diseased leaves wither and die. Higher humidity is conducive to the germination and invasion of spores. It can occur at 10 - 25°C. Whether it can prevail depends on the humidity and the growth of the host. Spores can germinate in low humidity, and the germination rate increases significantly in high humidity. Therefore, after rain or in less rainy weather, but with high field humidity, the epidemic speed of powdery mildew accelerates. It was found through the test that the control of powdery mildew of melons should be carried out at the initial stage of the disease. During the epidemic period of the disease, continuous control for 2 - 3 times will result in better control effects.

[0175] Through indoor toxicity determination and field trials, the pesticide composition obtained by compounding Aminopyrifen and ethirimol besylate according to the present invention shows good control effects against fungal diseases (cucumber powdery mildew, melon powdery mildew) of fruit and vegetable crops. The control effect of the pesticide composition or its preparation obtained by compounding according to the present invention is remarkable, and it is superior to the single agent in delaying the generation of drug resistance and prolonging the drug persistence. And no phytotoxicity to crops was found in the tests, indicating that under the condition of improved bactericidal synergistic effect of the obtained pesticide composition or preparation, the production cost and use cost can be reduced, and it is safe for crops.

[0176] Although the present invention has been described in detail with general descriptions and specific embodiments above, based on the present invention, some modifications or improvements can be made, which are obvious to those skilled in the art. Therefore, these modifications or improvements made without departing from the spirit of the present invention all fall within the scope of protection required by the present invention.

Claims

1. A pesticide composition containing Aminopyrifen, characterized in that: It comprises active ingredient A and active ingredient B. Active ingredient A is Aminopyrifen, and its structural formula is as follows: Active ingredient B is ethirimol besylate. The mass ratio of Aminopyrifen to ethirimol besylate is 1:1 to 20:

1.

2. The pesticidal composition according to claim 1, wherein, Based on the total weight of the pesticide composition being 100 wt%, the sum of the contents of active ingredient A and active ingredient B in the pesticide composition is 1 to 95 wt%.

3. The pesticide composition according to claim 2, wherein, The sum of the contents of active ingredient A and active ingredient B in the pesticide composition is 5 to 80 wt%.

4. The pesticide composition according to claim 3, wherein, The sum of the contents of active ingredient A and active ingredient B in the pesticide composition is 10 to 60 wt%.

5. The pesticidal composition according to claim 1, characterized in that, The pesticide composition further comprises adjuvants, and the adjuvants are selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreezing agents, defoaming agents, solvents, preservatives, stabilizers, synergists or carriers.

6. The pesticide composition according to claim 1, wherein The dosage form of the pesticide composition can be any one of emulsifiable concentrates, emulsifiable concentrates, microemulsions, suspensions, wettable powders or water-dispersible granules.

7. The pesticidal composition according to claim 6, characterized in that, The dosage form of the pesticide composition is microemulsion or emulsifiable concentrate.

8. Use of the pesticide composition according to any one of claims 1-7 in controlling plant diseases.

9. The application according to claim 8, characterized in that, The plant diseases are plant diseases caused by fungi or bacteria.

10. The application according to claim 9, characterized in that, The plant diseases are plant diseases caused by fungi.

11. The application according to claim 10, wherein The fungi are Sphaerotheca cucurbitae (Jacz) Z.Y.Zhao and Erysiphe cucurbitacearum Zheng & Chen, which belong to the genus Sphaerotheca or the genus Erysiphe in the phylum Ascomycota.

12. The application according to claim 8, characterized in that, The plant diseases are diseases of cucurbitaceous plants.

13. The application according to claim 12, wherein The cucurbitaceous plants are cucumber and melon.

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