A bactericidal composition and its use
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- QINGDAO HAILIER BIOTECHNOLOGY CO LTD
- Filing Date
- 2025-04-08
- Publication Date
- 2026-07-03
AI Technical Summary
[0007]近年来,随着辣椒种植面积的逐年扩大,引进的品种逐年增多,加上长期连作,使得辣椒炭疽病发病面积不断扩大,导致属于次要病害的炭疽病上升为主要病害,造成辣椒减产,给生产带来巨大损失
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Abstract
Description
Technical Field
[0001] This invention relates to the field of pesticides and fungicides, specifically to a fungicidal composition and its application. Background Technology
[0002] Compound (I) is a quinoline carboxamide fungicide developed by Syngenta. It has a broad spectrum of control, is safe and highly effective, and can effectively control a variety of fungal diseases. CAS Registry Number: 2132414-06-1 (racemic 2132414-04-9), English chemical name: N-(2R)-[1,3-dimethyl-1-(phenylmethyl)butyl]-8-fluoro-3-quinolinecarboxamide, and its chemical structure is as follows:
[0003]
[0004] Bromhizobium is a broad-spectrum, highly effective, and low-toxicity fungicide that can inhibit and eliminate the growth of fungi, bacteria, and algae, and has a good control effect on crop diseases.
[0005] Cyazofamid is a 2-cyanoacrylate fungicide. It is a selective fungicide with a unique mode of action. It is effective against diseases caused by Fusarium. Cyazofamid is absorbed through the roots and has an upward transport effect on the leaves.
[0006] Imazalil is a broad-spectrum fungicide with acrotropic translocation activity. Its mechanism of action is to inhibit the biosynthesis of ergosterol, thereby disrupting the cell membrane function of fungi. It has significant preventive effects against diseases caused by ascomycetes and deuteromycetes in various crops.
[0007] In recent years, with the continuous expansion of chili pepper planting area and the increasing number of introduced varieties, coupled with long-term continuous cropping, the affected area of chili pepper anthracnose has been expanding, causing anthracnose, once a minor disease, to rise to a major one, resulting in reduced chili pepper yields and significant production losses. Chili pepper anthracnose is caused by the pathogen *Colletotrichum*, a fungus belonging to the Deuteromycetes. It has a wide distribution in my country, develops rapidly, causes significant damage to crops, and results in substantial economic losses. Furthermore, it has developed resistance to many fungicides, and the effectiveness of conventional chemical control has been gradually declining in recent years. Chemical pesticides remain the mainstay of crop disease control; however, prolonged use of pesticides can lead to cross-resistance, resulting in a gradual decrease in efficacy. Combining two or more pesticides to create a synergistic effect and improve efficacy is the main approach to solving this problem. Developing new fungicides is expensive and time-consuming. In contrast, the development and research of highly efficient, low-toxicity, and low-residue compound and mixed fungicides has attracted attention both domestically and internationally due to its lower investment and shorter development cycle, leading to increased research efforts. No combination of compound (I) with bromodiphenyl ether, cyazofamid, or imazalil has been reported. Summary of the Invention
[0008] Based on the above, the present invention aims to provide a fungicidal composition and its formulation, mainly used for the prevention and control of plant fungal diseases. The composition or its formulation can enhance efficacy, reduce dosage, prolong the duration of effect, and delay the development of resistance.
[0009] To achieve the above objectives, the following technical solution is provided: a bactericidal composition comprising active ingredient A and active ingredient B, wherein active ingredient A is a compound of formula (I):
[0010] Active ingredient B is any one of bromochlorothalonil, cyazofamid, and prochloraz;
[0011] Furthermore, the mass ratio of active ingredient A to active ingredient B is 1:36 to 34:1.
[0012] Furthermore, the mass ratio of the compound of formula (I) to bromodiphenyl ether is 1:32 to 32:1;
[0013] Furthermore, the mass ratio of the compound of formula (I) to bromodiphenyl ether is 1:32, 1:24, 1:10, 1:6, 1:3, 1:1, 3:1, 6:1, 10:1, 18:1, or 32:1;
[0014] Furthermore, the mass ratio of the compound of formula (I) to bromodiphenyl ether is 1:24 to 32:1;
[0015] Furthermore, the mass ratio of the compound of formula (I) to bromodiphenyl ether is 1:24, 1:10, 1:6, 1:3, 1:1, 3:1, 6:1, 10:1, 18:1, or 32:1;
[0016] Furthermore, the mass ratio of the compound of formula (I) to cyazofamid is 1:30 to 25:1;
[0017] Furthermore, the mass ratio of the compound of formula (I) to cyazofamid is 1:30, 1:25, 1:18, 1:12, 1:8, 1:5, 5:4, 5:1, 10:1, 15:1, or 25:1.
[0018] Furthermore, the mass ratio of the compound of formula (I) to cyazofamid is 1:25 to 25:1;
[0019] Furthermore, the mass ratio of the compound of formula (I) to cyazofamid is 1:25, 1:18, 1:12, 1:8, 1:5, 5:4, 5:1, 10:1, 15:1, or 25:1.
[0020] Furthermore, the mass ratio of the compound of formula (I) to imazalil is 1:36 to 34:1;
[0021] Furthermore, the mass ratio of the compound of formula (I) to imazalil is 1:36, 1:25, 1:15, 2:11, 3:8, 2:1, 8:3, 11:2, 10:1, 20:1, or 34:1;
[0022] Furthermore, the mass ratio of the compound of formula (I) to imazalil is 1:25 to 20:1;
[0023] Furthermore, the mass ratio of the compound of formula (I) to imazalil is 1:25, 1:15, 2:11, 3:8, 2:1, 8:3, 11:2, 10:1, or 20:1;
[0024] Furthermore, based on a total weight of 100 wt% of the bactericidal composition, the sum of the contents of active ingredient A and active ingredient B in the bactericidal composition is 1 to 90 wt%.
[0025] Furthermore, based on the total weight of the bactericidal composition being 100 wt%, the sum of the contents of active ingredient A and active ingredient B in the bactericidal composition is preferably 5 to 80 wt%.
[0026] Furthermore, the bactericidal composition, in addition to containing the active ingredient, also contains agriculturally permissible auxiliary ingredients, which are selected from one or more of the following: wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoamers, solvents, preservatives, stabilizers, synergists, binders, or carriers.
[0027] Further, the wetting agent is selected from one or more of alkylbenzene sulfonates, alkylnaphthalene sulfonates, lignin sulfonates, sodium dodecyl sulfate, sodium dioctyl succinate sulfonate, α-olefin sulfonates, alkylphenol polyoxyethylene ethers, castor oil polyoxyethylene ethers, alkylphenol ethoxylates, fatty alcohol ethoxylates, sodium fatty alcohol polyoxyethylene ether sulfate, silkworm excrement, soapberry powder, soapberry powder, SOPA, detergents, emulsifiers 2000 series, and wetting and penetrating agents F; and / or
[0028] Further, the dispersant is selected from one or more of the following: lignin sulfonate, alkyl naphthalene sulfonate formaldehyde condensate, naphthalene sulfonate, tristyrylphenol ethoxylate phosphate, fatty alcohol ethoxylate, alkylphenol polyoxyethylene ether, alkylphenol polyoxyethylene ether methyl ether condensate sulfate, fatty amine polyoxyethylene ether, glycerol fatty acid ester polyoxyethylene ether, polycarboxylates, polyacrylic acids, phosphates, EO-PO block copolymers, and EO-PO graft copolymers; and / or
[0029] Further, the emulsifier is selected from one or more of the following: calcium dodecylbenzenesulfonate, alkylphenol formaldehyde resin polyoxyethylene ether, phenethylphenol polyoxyethylene polyoxypropylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, styrene-phenol polyoxyethylene ether, castor oil polyoxyethylene ether, and alkylphenol ether phosphate; and / or
[0030] Furthermore, the thickener is selected from one or more of xanthan gum, organobentonite, gum arabic, sodium alginate, magnesium aluminum silicate, carboxymethyl cellulose, and silica; and / or
[0031] Further, 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
[0032] Furthermore, the antifreeze is selected from one or more of alcohols, alcohol ethers, chlorinated hydrocarbons, and inorganic salts; and / or
[0033] Furthermore, the defoamer is selected from C 10 -C 20 Saturated fatty acid compounds, silicone oil, silicone compounds, C8-C 10 One or more of the fatty alcohols; and / or
[0034] Further, the solvent is selected from one or more of benzene, toluene, xylene, mesitylene, methanol, ethanol, isopropanol, n-butanol, dimethyl sulfoxide, dimethylformamide, cyclohexanone, hydrocarbon carbonates, diesel oil, solvent oil, vegetable oil (soybean oil, corn oil, rapeseed oil, palm oil, etc.), vegetable oil derivatives, and water; and / or
[0035] Further, 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
[0036] Further, the stabilizer is selected from one or more of the following: disodium hydrogen phosphate, oxalic acid, succinic acid, adipic acid, borax, 2,6-di-tert-butyl-p-methylphenol, triethanolamine oleate, epoxidized vegetable oil, kaolin, diatomaceous earth, bentonite, attapulgite, silica, talc, montmorillonite, and starch; and / or
[0037] Furthermore, the synergist is selected from synergistic phosphorus, synergistic ether; and / or
[0038] Furthermore, the carrier is selected from one or more of the following: ammonium salts, ground natural minerals, ground artificial minerals, silicates, resins, waxes, solid fertilizers, water, organic solvents, mineral oils, vegetable oils, and vegetable oil derivatives.
[0039] Furthermore, the dosage form of the bactericidal composition is selected from solid dosage forms and / or liquid dosage forms and / or seed treatment formulations;
[0040] The solid dosage forms include powders, granules, balls, tablets, strips, wettable powders, oil-dispersible powders, emulsion powders, water-dispersible granules, emulsion granules, water-dispersible tablets, soluble powders, soluble tablets, or soluble granules.
[0041] The liquid formulations include soluble agents, colloids, oils, spreading oils, emulsifiable concentrates, latexes, dispersible liquids, ointments, water emulsions, oil emulsions, microemulsions, lipids, suspensions, microcapsule suspensions, oil suspensions, dispersible oil suspensions, suspensions, microcapsule suspension-suspensions, microcapsule suspension-water emulsions, or microcapsule suspension-suspension emulsions.
[0042] Furthermore, the powder is a free-flowing powdered preparation containing active ingredients suitable for spraying or spreading;
[0043] Furthermore, the granules are granular preparations containing active ingredients that are free-flowing and have a certain particle size range;
[0044] Furthermore, the spherical agent is a spherical preparation containing active ingredients (generally with a diameter greater than 6 mm);
[0045] Furthermore, the tablet is a tablet-shaped preparation containing active ingredients with a certain shape and size (usually having two planes or convex surfaces, with the distance between the two surfaces being less than the diameter);
[0046] Furthermore, the strip preparation is a strip or rod-shaped preparation containing active ingredients (generally a few centimeters long and a few millimeters wide / diameter, i.e., the length is greater than the diameter / width);
[0047] Furthermore, the wettable powder is a powdered preparation in which the active ingredient is dispersed in water to form a suspension;
[0048] Furthermore, the oil-dispersible powder is a powdered preparation in which the active ingredient is dispersed in an organic solvent to form a suspension;
[0049] Furthermore, the aforementioned milk powder is a powdered preparation in which the active ingredient is dissolved in an organic solvent, encapsulated in a soluble or insoluble inert component, and dispersed in water to form an oil-in-water emulsion.
[0050] Furthermore, the water-dispersible granules are granular formulations that disintegrate in water and disperse the active ingredients into a suspension;
[0051] Furthermore, the emulsion granules are granular formulations in which the active ingredient is dissolved in an organic solvent, encapsulated in a soluble or insoluble inert component, and dispersed in water to form an oil-in-water emulsion.
[0052] Furthermore, the water-dispersible tablets are tablet formulations that disintegrate in water and disperse the active ingredients into a suspension;
[0053] Furthermore, the soluble powder is a powdered preparation in which the active ingredient forms a true solution in water, and may contain inert components that are insoluble in water;
[0054] Furthermore, the soluble granules are granular preparations in which the active ingredient forms a true solution in water, and may contain inert components that are insoluble in water;
[0055] Furthermore, the soluble tablets are tablet-shaped preparations in which the active ingredient forms a true solution in water, and may contain inert components that are insoluble in water;
[0056] Furthermore, the soluble agent is a transparent or translucent liquid preparation containing active ingredients that is diluted with water, and may contain inert components that are insoluble in water;
[0057] Furthermore, the soluble agent is a gel-like preparation containing effective ingredients that is diluted with water to form a true solution;
[0058] Furthermore, the oil is a homogeneous liquid preparation containing active ingredients, diluted (or undiluted) with an organic solvent;
[0059] Furthermore, the spreading oil is an oil containing effective ingredients that automatically diffuses into an oil film on the water surface;
[0060] Furthermore, the emulsifiable concentrate is a homogeneous liquid formulation containing active ingredients that is diluted and dispersed in water into an emulsion.
[0061] Furthermore, the latex is a latex preparation containing effective ingredients that is diluted and dispersed in water into an emulsion.
[0062] Furthermore, the dispersible liquid is a homogeneous liquid formulation containing active ingredients that is diluted and dispersed in water to form a suspension;
[0063] Furthermore, the ointment is a water-based ointment preparation containing effective ingredients that can form a film, and is generally used directly;
[0064] Furthermore, the water-in-water emulsion is a formulation in which the active ingredient (or its organic solution) forms an emulsion liquid in water;
[0065] Furthermore, the oil emulsion is a formulation in which the active ingredient (or its aqueous solution) forms an emulsion liquid in oil;
[0066] Furthermore, the microemulsion is a microemulsion liquid formulation in which the active ingredient is transparent or translucent in water, and can be used directly or after dilution with water;
[0067] Furthermore, the liposome is an oil or fat-based viscous preparation containing active ingredients, which is generally used directly;
[0068] Furthermore, the suspending agent is a stable suspension of active ingredients dispersed in water as solid particles, and is generally diluted with water before use;
[0069] Furthermore, the microcapsule suspension is a stable suspension formulation in which microcapsules containing active ingredients are dispersed in a liquid.
[0070] Furthermore, the oil suspension is a stable suspension formulation in which the active ingredient is dispersed in a liquid as solid particles, and is generally diluted with an organic solvent before use;
[0071] Furthermore, the dispersible oil suspension is a stable suspension formulation in which the active ingredient is dispersed as solid particles in a non-aqueous medium, and is generally diluted with water before use;
[0072] Furthermore, the suspension emulsion is a heterogeneous liquid formulation in which the active ingredients are stably dispersed in a continuous aqueous phase in the form of solid microparticles and water-insoluble microdroplets.
[0073] Furthermore, the microcapsule suspension-suspension agent is a stable suspension liquid formulation in which the active ingredients are dispersed in water as microcapsules and solid particles;
[0074] Furthermore, the microcapsule suspension-water emulsion is a heterogeneous liquid formulation in which the active ingredient is stably dispersed in a continuous aqueous phase in the form of microcapsules and tiny droplets.
[0075] Furthermore, the microcapsule suspension-emulsion is an active ingredient that is stably dispersed in a continuous aqueous phase in the form of microcapsules, solid particles and tiny droplets to form a heterogeneous liquid formulation.
[0076] Furthermore, the bactericidal composition can be prepared into a pesticide-acceptable formulation, wherein the formulation is a microemulsion, water-in-oil emulsion, suspension, dispersible oil suspension, soluble concentrate, emulsifiable concentrate, suspension emulsion, microcapsule suspension, water-dispersible granules, wettable powder, granules, seed treatment suspension, or seed treatment dry powder.
[0077] Furthermore, the formulation is a microemulsion, emulsifiable concentrate, suspension concentrate, water emulsion, water-dispersible granules, wettable powder, or seed treatment suspension.
[0078] The present invention also discloses the application of the bactericidal composition described above in the prevention and control of plant diseases;
[0079] Compound (I) used in combination with bromodiphenyl ether, cyazofamid, and imazalil is effective against *Blumiria*, *Erysiphe*, *Gibberella*, *Sclerotinia*, *Botryotinia*, *Puccinia*, *Tilletia*, *Gymnosporzngium*, *Phakopsora*, *Ustilago*, and *Rhizoctonia*. It has synergistic effects with species such as Verticillium, Alternaria, Pyriculara, Botrytis, Cercospora, Fusarium, Colletotrichum, Rhizoctonia, and Sclerotium, especially with Colletotrichum in the mass ratio range of 1:32 to 30:1.
[0080] Furthermore, the plant disease is a plant disease caused by fungi or bacteria;
[0081] Furthermore, the plant disease is a plant disease caused by fungi;
[0082] Furthermore, the plant disease caused by the fungus is anthracnose of pepper.
[0083] The present invention has the following beneficial effects:
[0084] 1) This bactericidal composition increases bactericidal activity and has a synergistic effect on the target at a certain mass ratio, which can reduce the amount of pesticides used, reduce the cost of use and reduce the environmental burden.
[0085] 2) This bactericidal composition is safe and efficient, and is safe for crops, non-target organisms, beneficial organisms and natural enemies, and has the effect of increasing yield and ensuring harvest. Detailed Implementation
[0086] To make the technical solution, objectives and advantages of the present invention clearer, the present invention is described with reference to the following specific embodiments. However, the present invention can be implemented in various forms and should not be limited to the embodiments described herein.
[0087] Indoor bioassay for anthrax in peppers
[0088] Test basis: Refer to the Agricultural Industry Standard of the People's Republic of China, Indoor Bioassay Test Guidelines for Pesticides, Part 2: Test for Inhibition of Mycelial Growth of Pathogenic Fungi, Plate Method NY / T 1156.2-2006.
[0089] Test strain: Anthracnose was isolated from anthracnose lesions exhibiting typical symptoms on chili pepper fruits from Shouguang, Weifang. The strain was isolated, purified, cultured, and preserved using conventional tissue isolation methods, and identified as *Colletotrichum nigrum*, the causal agent of black anthracnose. Before the experiment, the strain was transferred to PDA medium for large-scale culture at 26–27°C for approximately 5 days.
[0090] Test reagents: 95% bromuconazole technical, 95% cyazofamid technical, 95% imazalil technical, and compound (I) technical. All of the above reagents were provided by the Group's R&D Center.
[0091] Reagent preparation: Dissolve the test drug in acetone first, then dilute with 0.1% Tween 80 aqueous solution. Prepare single-agent stock solutions separately, and set 5 series of mass concentrations according to the purpose of mixing and the drug activity.
[0092] Melt the PDA medium in a microwave oven and cool it to about 50°C. Following the principle of starting from low concentration and gradually increasing the concentration, take 1 mL of the prepared test solution and 9 mL of PDA medium and add them to a 9 cm diameter petri dish. Mix well to prepare a drug-containing plate of the corresponding concentration.
[0093] Inoculation: Under aseptic conditions, the activated pathogenic fungus was punched into a fungal cake using a 6mm diameter punch. After the drug-containing culture medium solidified, the fungal cake was placed in the center of the culture medium. Finally, the culture dish was sealed with sealing film and placed in an incubator at 27℃ and 70% relative humidity for cultivation. A blank control without the drug was set up. Each treatment was repeated 3 times.
[0094] Investigation: The growth of pathogenic fungal hyphae was investigated based on the growth of hyphae in blank control culture dishes. After 5 days of culture, the diameter of the colonies was measured with calipers in millimeters (mm). The diameter of each colony was measured vertically once using the cross-sectional method, and the average value was taken.
[0095] Calculate the mycelial growth inhibition rate using the following formula, expressed as a percentage (%), and retain the result to two decimal places.
[0096] D = D1 - D2
[0097] D – Colony growth diameter;
[0098] D1—colony diameter;
[0099] D2 – Diameter of the mushroom cake.
[0100] I = (D0 - D) t ) / D0*100
[0101] In the formula:
[0102] I – Mycelial growth inhibition rate;
[0103] D0—Correlation diameter of the blank control group;
[0104] D t — Diameter of colonies grown after chemical treatment.
[0105] Statistical analysis: Regression analysis (using DPS statistical analysis software) was performed based on the logarithmic values of each agent concentration and the corresponding mycelial growth inhibition probability values to calculate the EC50 of each agent. 50 Equivalent value, correlation coefficient R, is used to evaluate the activity of the test reagent on the biological sample.
[0106] Sun Yunpei's method: The synergistic effect of drug mixtures is evaluated based on the co-toxicity coefficient (CTC). A CTC ≥ 120 indicates a synergistic effect; a CTC ≤ 80 indicates an antagonistic effect; and a CTC < 120 indicates an additive effect.
[0107] The co-toxicity coefficient (CTC value) of the mixture is calculated using the following formula:
[0108]
[0109] In the formula:
[0110] ATI – Actual Measured Toxicity Index of Mixtures;
[0111] S – EC of standard bactericides 50 The unit is milligrams per liter (mg / L);
[0112] M – EC of the mixture 50 The unit is milligrams per liter (mg / L).
[0113] TTI = TI A *P A +TI B *P B
[0114] In the formula:
[0115] TTI – Theoretical Toxicity Index of Mixtures;
[0116] TI A —A. Toxicity index of drug A;
[0117] P A —Percentage content of drug A in the mixture, expressed as percentage (%);
[0118] TI B —Toxicity index of drug B;
[0119] P B —Percentage content of agent B in the mixture, expressed as percentage (%).
[0120]
[0121] In the formula:
[0122] CTC – Cotoxicity Coefficient;
[0123] ATI – Actual Measured Toxicity Index of Mixtures;
[0124] TTI – Theoretical Toxicity Index of Mixtures.
[0125] Results of indoor bioactivity assay:
[0126] Table 1 shows the results of compound (I) controlling EC anthracnose in peppers. 50 The concentration of bromuconazole was 2.9582 mg / L, which was effective in controlling EC50 anthracnose in peppers. 50 It is 0.2862 mg / L.
[0127] Compound (I) mixed with bromodiphenyl ether in a mass ratio of 1:32 to 32:1 exhibits additive or synergistic effects. Specifically, when the mass ratio is 1:18 to 32:1, the co-toxicity coefficient is >120, demonstrating a synergistic effect. The co-toxicity coefficient of compound (I) mixed with bromodiphenyl ether at a ratio of 1:1 is the highest, at 191.9480, EC50. 50 The concentration was 0.2719 mg / L, indicating a significant synergistic effect.
[0128] Table 1 shows the synergistic effect of different ratios of compound (I) with bromodiphenyl ether on anthracnose in peppers.
[0129]
[0130]
[0131] Table 2 shows that compound (I) controls EC anthracnose in peppers. 50 The concentration of cyazofamid in controlling EC of pepper anthracnose was 3.0029 mg / L. 50 The concentration was 25.9952 mg / L. When the mass ratio of compound (I) to cyazofamid was 1:30 to 25:1, the co-toxicity coefficient was >120, indicating a synergistic effect. The co-toxicity coefficient of compound (I) with cyazofamid at a ratio of 1:5 was the highest, at 188.1187, EC50. 50 The concentration was 6.0715 mg / L, indicating a significant synergistic effect.
[0132] Table 2 shows the synergistic effect of compound (I) with different ratios of cyazofamid on anthracnose in peppers.
[0133]
[0134] Table 3 shows that compound (I) controls EC anthracnose in peppers. 50 The concentration of prochloraz was 3.0090 mg / L, which is effective in controlling EC50 anthracnose in peppers. 50 The concentration was 10.3421 mg / L. Compound (I) mixed with imazalil in a mass ratio of 1:36 to 34:1 showed additive or synergistic effects. Among these, the co-toxicity coefficient was >120 at a mass ratio of 1:25 to 20:1, indicating a synergistic effect. The co-toxicity coefficient of compound (I) with imazalil at a ratio of 2:1 was the highest, at 185.7448, EC50. 50 The concentration was 3.0722 mg / L, indicating a significant synergistic effect.
[0135] Table 3 shows the synergistic effect of different ratios of compound (I) with imazalil on anthracnose in peppers.
[0136]
[0137] Formulation Examples
[0138] Preparation Example 1:
[0139] 40% Formula (I) Compound·Bromoxynil Wettable Powder (20:20)
[0140] Formulation: 20% of compound (Ⅰ), 20% of bromodiphenyl ether, 5% of sodium polycarboxylate, 5% of dispersant NNO, 5% of sodium alkyl polyoxyethylene ether sulfonate, 3.5% of sodium dodecyl sulfate, 5% of bentonite, and kaolin to make up the balance;
[0141] Preparation method: The active ingredients, other functional additives and fillers are mixed according to the formula ratio, stirred evenly in a stirring tank, and then pulverized and mixed evenly multiple times by an air jet mill to prepare the wettable powder of the composition of the present invention.
[0142] Preparation Example 2:
[0143] 14% Formula (I) compound bromodiphenyl ether emulsifiable concentrate (7:7)
[0144] Preparation formula: 7% of compound (Ⅰ), 7% of bromodiphenyl ether, 1.5% of BHT, 5% of epoxidized soybean oil, 10% of propylene carbonate, 15% of acetophenone, 5% of cyclohexanone, 3.5% of calcium dodecylbenzenesulfonate, 10% of fatty alcohol polyoxyethylene ether, and methyl oleate to make up the balance.
[0145] Preparation method: Add the active ingredients to the cosolvent according to the formulation ratio of the example, and add surfactants and other functional additives thereto. Stir and mix evenly in a stirring mixing tank to obtain emulsifiable oil.
[0146] Preparation Example 3:
[0147] 14% Formula (I) Compound·Iprodione Water Emulsion (10:4)
[0148] Formula: 10% of compound (I), 4% of imazalil, 12% of trimethylbenzene, 10% of cyclohexanone, 1% of calcium dodecylbenzenesulfonate, 0.5% of sodium fatty alcohol polyoxyethylene ether sulfate, 5% of EO / PO block copolymer, 5% of glycerol, 1.5% of glycerin, 0.1% of silicone defoamer, 0.2% of xanthan gum, 0.1% of sodium benzoate, and deionized water to make up the balance;
[0149] Preparation method: According to the formulation ratio in the example, the active ingredient is dissolved in the solvent and an emulsifier is added to form a homogeneous oil phase. Deionized water and antifreeze are mixed together to form a homogeneous aqueous phase. Under high-speed shearing, the aqueous phase is added to the oil phase to form a well-dispersed water-emulsion formulation.
[0150] Preparation Example 4:
[0151] 25% Formula (I) compound·bromodiphenyl ether suspension (15:10)
[0152] Formulation: 15% of compound (Ⅰ), 10% bromobenzoic acid, 3% naphthalene sulfonate formaldehyde condensation, 2% lignin sulfonic acid, 2% sodium lignin sulfonate, 1% sodium dioctyl succinate sulfonate, 1% magnesium aluminum silicate, 0.5% fumed silica, 0.5% polyvinylpyrrolidone, 0.25% xanthan gum, 5% ethylene glycol, 0.02% benzisothiazolinone, 0.5% organosilicon defoamer, and deionized water to make up the balance;
[0153] Preparation method: According to the formula ratio, the active ingredients, surfactants and other functional additives are placed in the reaction vessel in sequence, water is added and mixed evenly, and then subjected to high-speed shearing, wet sand milling and finally homogenization filtration to obtain the suspension.
[0154] Preparation Example 5:
[0155] 28% Formula (I) Compound·Cypermethrin Suspension Concentrate (24:4)
[0156] Formulation: 24% of compound (Ⅰ), 4% of cyazofamid, 1.5% of isomeric alcohol polyoxyethylene ether, 4% of polyether, 3% of styrene-phenol polyoxyethylene ether phosphate, 1% of sodium polycarboxylate, 1% of magnesium aluminum silicate, 0.25% of xanthan gum, 5% of ethylene glycol, 0.02% of benzisothiazolinone, 0.5% of organosilicon defoamer, and deionized water to make up the balance;
[0157] Preparation method: Same as in preparation example 4.
[0158] Preparation Example 6:
[0159] 30% Formula (I) Compound·Iprodione Suspension (20:10)
[0160] Formulation: 10% of compound (Ⅰ), 10% of imazalil, 1% of isomeric alcohol polyoxyethylene ether, 3% of sodium lignosulfonate, 1% of sodium polycarboxylate, 3.5% of sodium naphthalenesulfonic acid formaldehyde condensate, 1% of magnesium aluminum silicate, 0.25% of xanthan gum, 0.5% of fumed silica, 0.5% of polyvinylpyrrolidone, 5% of ethylene glycol, 0.02% of benzisothiazolinone, 0.5% of organosilicon defoamer, and deionized water to make up the balance;
[0161] Preparation method: Same as in preparation example 4.
[0162] Field efficacy trials
[0163] Field efficacy trial of anthracnose in peppers
[0164] Test location: Qingzhou City, Weifang City, Shandong Province;
[0165] Test crop: Chili pepper (long pepper), grown in the open field; the planting environment, water and fertilizer conditions, and growth status of chili peppers in the field were all consistent, making them relatively susceptible to disease. The conditions met the requirements for field trials.
[0166] Experiment date: July 5, 2023. Anthracnose of pepper was treated by uniform spraying of the plant stems and leaves at the early stage of the disease.
[0167] Test reagents and dosages:
[0168] Table 4. Comparison of pesticide dosage in field trials
[0169] deal with medicine <![CDATA[Dosage g a.i / hm 2 > A1 40% Formula (I) Compound·Bromoxynil Wettable Powder (20:20) 100 A2 28% Formula (I) Compound·Cypermethrin Suspension Concentrate (24:4) 100 A3 30% Formula (I) Compound·Iprodione Suspension (20:10) 100 A4 30% Formula (I) Compound Suspension 200 A5 25% bromocyanide wettable powder 180 A6 25% imazalil emulsifiable concentrate 250 A7 25% Cyazofamid suspension 300 A8 Water comparison /
[0170] Experimental treatments included a single-agent treatment and a water control. Two applications were administered 7 days apart, and each treatment was repeated four times. The plots were divided into 20m² areas. 2 Randomized block designation. Ensure application is protected from rain, strong winds, and extreme temperatures. The application equipment is a 3WBD-18L backpack electric sprayer with a spray volume of 700L / hm². 2 .
[0171] Investigation Methods: Disease incidence was investigated before the first application, 7 days after the first application, and 7 days after the last application. The number of diseased fruits and relative severity scores were recorded. The grading method followed GB / T 17980.33-2000 "Guidelines for Field Efficacy Tests of Pesticides (I) - Control of Anthracnose in Peppers with Fungicides," and the specific grading is as follows:
[0172] There are 9 levels in total:
[0173] Level 0, no symptoms reported;
[0174] Grade 1: Diseased spots cover ≤2% of the fruit area;
[0175] Grade 3, with lesions covering 3% to 8% of the fruit area;
[0176] Grade 5, with lesions covering 9%–15% of the fruit area;
[0177] Grade 7, with lesions covering 16%–25% of the fruit area;
[0178] Grade 9, with lesions covering more than 25% of the fruit area;
[0179] Methods for calculating disease severity index and drug efficacy:
[0180]
[0181] The experimental data were analyzed using the Duncan's New Multiple Range Method (DMRT) biostatistical analysis with DPS software, and the significance of differences was evaluated.
[0182] Results of field efficacy trials:
[0183] The results showed that 40% of compound (I)·bromodiflubenzuron wettable powder (20:20), 28% of compound (I)·cypermethrin suspension (24:4), and 30% of compound (I)·prochloraz suspension (20:10) had good control effects on anthracnose of pepper. Seven days after the first application, their control efficacies were 83.24%, 81.35%, and 78.91%, respectively. The mixed formulations showed significant differences compared with other single agents.
[0184] Table 5. Results of field efficacy trials (7 days after the first application)
[0185]
[0186] Note: Data in the table are the average of four replicates; lowercase letters indicate that the differences between treatments are statistically significant (p < 0.05).
[0187] The results showed that 40% of compound (I)·bromodiflubenzuron wettable powder (20:20), 28% of compound (I)·cypermethrin suspension (24:4), and 30% of compound (I)·prochloraz suspension (20:10) had good control effects on anthracnose of pepper. Seven days after the last application, their control efficacies were 85.39%, 84.55%, and 82.26%, respectively. The mixed formulations showed significant differences compared with other single agents.
[0188] Table 6. Results of field efficacy trials (7 days after the last application)
[0189]
[0190] Note: Data in the table are the average of four replicates; lowercase letters indicate that the differences between treatments are statistically significant (p < 0.05).
[0191] No phytotoxicity or impact on crop growth and development was recorded during the experiment, indicating that the tested pesticide was safe for crops within the recommended dosage range. No effects on non-target organisms were found within the dosage range. No extreme weather events such as heavy rainfall or strong winds were recorded during the experiment.
[0192] Field efficacy trials showed that the compound shown in formula (I), in combination with bromodiphenyl ether, cyazofamid, and prochloraz, exhibited high control efficacy in the treatment of anthracnose in peppers. It not only reduced the disease incidence and disease index, demonstrating significant control effects, but also had little impact on yield. Furthermore, post-treatment observations showed that pepper growth in all treatment areas was normal, with no phytotoxicity observed, indicating that each pesticide was safe for pepper growth at the dosages used in this experiment.
[0193] Through indoor toxicity testing and field trials, the compound shown in formula (I) of this invention, combined with any one of bromodiphenyl ether, cyazofamid, or prochloraz, exhibited excellent control effects against anthracnose in peppers. The fungicidal composition or formulation obtained by this invention demonstrates significant efficacy, exhibiting high efficiency, broad spectrum, low residue, long-lasting effect, and strong systemic properties. Furthermore, no phytotoxicity was observed in the experiments, indicating that the enhanced synergistic effect of the obtained fungicidal composition or formulation reduces production and usage costs while ensuring crop safety.
[0194] Although the present invention has been described in detail above with general description and specific embodiments, some modifications or improvements can be made to it based on the present invention, which will be obvious to those skilled in the art. Therefore, all such modifications or improvements made without departing from the spirit of the present invention are within the scope of protection claimed by the present invention.
Claims
1. A bactericidal composition, characterized in that: It contains active ingredient A and active ingredient B, wherein active ingredient A is a compound of formula (I): (I) Active ingredient B is bromodiphenyl ether, and the mass ratio of the compound of formula (I) to bromodiphenyl ether is 1:24~32:
1.
2. The bactericidal composition according to claim 1, characterized in that, The mass ratio of the compound of formula (I) to bromodiphenyl ether is 1:24, 1:10, 1:6, 1:3, 1:1, 3:1, 6:1, 10:1, 18:1, or 32:
1.
3. The bactericidal composition according to claim 1, characterized in that, Based on a total weight of 100 wt% of the bactericidal composition, the sum of the contents of active ingredient A and active ingredient B in the bactericidal composition is 1 to 90 wt%.
4. The bactericidal composition according to claim 1, characterized in that, Based on a total weight of 100 wt% of the bactericidal composition, the sum of the contents of active ingredient A and active ingredient B in the bactericidal composition is 5-80 wt%.
5. The bactericidal composition according to claim 1, characterized in that, In addition to the active ingredient, the bactericidal composition contains agriculturally permissible auxiliary ingredients, which are selected from one or more of the following: wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoamers, solvents, preservatives, stabilizers, synergists, binders, or carriers.
6. The bactericidal composition according to claim 5, characterized in that, The dosage form of the bactericidal composition is selected from solid dosage forms and / or liquid dosage forms, wherein the dosage form is a microemulsion, emulsifiable concentrate, suspension concentrate, water emulsion, water-dispersible granules, wettable powder, or seed treatment suspension.
7. The application of the bactericidal composition according to any one of claims 1-6 in the prevention and control of plant diseases, characterized in that, The plant disease mentioned is a plant disease caused by fungi; the plant disease caused by fungi is anthracnose of pepper.