A bactericidal composition

By combining fluopyram, prothioconazole, and chlorothalonil to prepare fungicidal compositions in different formulations, the problems of narrow fungicidal spectrum and high cost of existing fungicides are solved, achieving a broad-spectrum, efficient, and low-cost fungicidal effect.

CN118383371BActive Publication Date: 2026-02-17HAILIR PESTICIDES & CHEM GRP
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Patent Information

Application Number
CN202410496219.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-04-24
Publication Date
2026-02-17
Estimated Expiration
2044-04-24

AI Technical Summary

Technical Problem

Existing fungicides have problems such as narrow fungicidal spectrum, insignificant synergistic effect, and high cost when controlling plant diseases.

Method used

Fluopyram, prothioconazole, and chlorothalonil, which have different mechanisms of action, are compounded to form fungicidal compositions. Their mass ratios are optimized, and appropriate agriculturally permissible auxiliary ingredients are added to prepare different formulations.

Benefits of technology

It significantly improved bactericidal activity, broadened the bactericidal spectrum, reduced drug costs, prolonged the duration of drug efficacy, and reduced the development of drug resistance in harmful bacteria.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention belongs to the field of pesticide fungicides and discloses a fungicidal composition. The active ingredients of the fungicidal composition include active ingredient A, active ingredient B, and active ingredient C. Active ingredient A is fluopyram, active ingredient B is prothioconazole, and active ingredient C is chlorothalonil. The mass ratio of active ingredient A, active ingredient B, and active ingredient C is (1-20):(1-20):(10-100). The fungicidal composition of this invention can be used to control plant diseases caused by Basidiomycetes or Mitotic spore-forming fungi, and has good control effects. It features a broad fungicidal spectrum, low dosage, and significant synergistic effect.
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Description

TECHNICAL FIELD

[0001] The present application relates to the field of fungicide, in particular to a fungicide composition and application thereof. BACKGROUND

[0002] Pydiflumetofen is a succinate dehydrogenase inhibitor fungicide developed by Syngenta Crop Protection AG. It is suitable for a variety of crops, especially the highest activity on leaf spot and powdery mildew, and is highly effective on diseases caused by pathogenic fungi such as grapevine, sclerotinia and claviceps, etc. Pydiflumetofen also breaks through the prevention and treatment of diseases caused by fusarium in cereals. The chemical name is 3-(difluoromethyl)-N-methyl-N-[1-methyl-2-(2,4,6-trichlorophenyl)ethyl]-1H-pyrazole-4-formamide, and the chemical structure is as follows:

[0003]

[0004] Prothioconazole is a new triazole sulfone fungicide developed by Bayer in 2004. It inhibits the demethylation of lanosterol, a precursor of sterol, and interferes with the biosynthesis of sterol, thereby playing a fungicidal role. It has good systemicity, unique mechanism of action, excellent protection, treatment and eradication activity, and wide fungicidal spectrum. It is mainly used in cereal crops such as wheat, barley, rice, peanut, rapeseed and legumes, etc. to prevent and treat various diseases.

[0005] Chlorothalonil is a broad-spectrum, protective fungicide that can interact with glycerol phosphate dehydrogenase in pathogenic fungi cells, bind to proteins containing cysteine in the enzyme, thereby destroying the activity of the enzyme, disrupting the metabolism of pathogenic fungal cells and losing vitality. Chlorothalonil has no systemic conductive effect, but after being sprayed on the plant body, it has good adhesion on the surface and is not easily washed off by rain, so the drug efficacy period is longer.

[0006] The applicant accidentally found that the combination of pydiflumetofen, prothioconazole and chlorothalonil with different mechanisms of action for preventing and treating plant diseases has a significant synergistic effect. SUMMARY

[0007] Based on the above, the present application aims to provide a fungicide composition, wherein the active ingredients of the fungicide composition comprise pydiflumetofen, prothioconazole and chlorothalonil. The fungicide composition has good control effect, wide fungicidal spectrum, significant synergistic effect, low drug cost, high safety to crops and other characteristics.

[0008] Another object of the present application is to provide a fungicidal composition containing fluoxastrobin, prothioconazole and chlorothalonil.

[0009] Another object of the present application is to provide a fungicidal composition containing fluoxastrobin, prothioconazole and chlorothalonil for preventing and treating plant diseases.

[0010] To achieve the above object, the following technical solution is provided: a fungicidal composition, wherein the active ingredients of the fungicidal composition comprise active ingredient A, active ingredient B and active ingredient C, the active ingredient A is fluoxastrobin, the active ingredient B is prothioconazole, and the active ingredient C is chlorothalonil.

[0011] Further, the mass ratio of the active ingredient A, the active ingredient B and the active ingredient C is (1-20):(1-20):(10-100).

[0012] Further, the mass ratio of the active ingredient A, the active ingredient B and the active ingredient C is (1-10):(1-10):(20-50) or any value between the above values.

[0013] Further, the mass ratio of the active ingredient A, the active ingredient B and the active ingredient C is:

[0014]

[0015]

[0016] Further, the mass ratio of the active ingredient A, the active ingredient B and the active ingredient C is:

[0017] mass ratio active ingredient A active ingredient B active ingredient C A:B:C 1 1 22.5 A:B:C 1 1 25 A:B:C 1 1 30 A:B:C 2 3 40 A:B:C 2 3 50 A:B:C 2 3 60 A:B:C 5 8 100 A:B:C 5 8 125 A:B:C 5 8 150 A:B:C 1 2 10 A:B:C 1 2 25 A:B:C 1 2 30 A:B:C 5 12 80 A:B:C 2 5 75

[0018] Further, the mass ratio of the active ingredient A, the active ingredient B and the active ingredient C is:

[0019] A:B:C mass ratio active ingredient A active ingredient B active ingredient C 1 1 22.5 A:B:C 1 1 25 A:B:C 1 1 30 A:B:C 2 3 40 A:B:C 2 3 50 A:B:C 2 3 60 A:B:C 5 8 100 A:B:C 5 8 125 A:B:C 5 8 150 A:B:C 1 2 10 A:B:C 1 2 25 A:B:C A:B:C 1 2 30

[0020] Further, the total content of the active ingredients in the fungicidal composition is 1-90wt% based on 100wt% of the total weight of the fungicidal composition.

[0021] Further, the total content of the active ingredients in the fungicidal composition is 5-80wt%.

[0022] Further, the total content of the active ingredients in the fungicidal composition is 22wt%, 28wt%, 45wt%, 49wt%, 55wt%, 69wt%, 76wt%.

[0023] Further, the fungicidal composition comprises, in addition to the active ingredient, an agriculturally acceptable auxiliary ingredient selected from one or more of wetting agents, dispersants, emulsifiers, thickening agents, disintegrants, antifreezing agents, antifoaming agents, solvents, preservatives, stabilizers, synergists, or carriers;

[0024] The wetting agent is selected from one or more of alkylbenzene sulfonate, alkylnaphthalene sulfonate, lignin sulfonate, sodium dodecyl sulfate, dioctyl sulfosuccinate sodium, alpha olefin sulfonate, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol ethoxylate, fatty alcohol ethoxylate, fatty alcohol polyoxyethylene ether sulfate sodium, silkworm excrement, soap nut, soapberry, SOPA, detergent, emulsifier 2000 series, and wetting penetrant F; and / or

[0025] The dispersant is selected from one or more of lignin sulfonate, alkylnaphthalene sulfonate formaldehyde condensate, naphthalene sulfonate, tristyrylphenol ethoxylate phosphate, fatty alcohol ethoxylate, alkylphenol polyoxyethylene ether, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, fatty amine polyoxyethylene ether, glycerol fatty acid ester polyoxyethylene ether, polycarboxylate, polyacrylate, phosphate, EO-PO block copolymer, and EO-PO graft copolymer; and / or

[0026] 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

[0027] The thickening agent is selected from one or more of xanthan gum, organobentonite, gum arabic, sodium alginate, magnesium aluminum silicate, carboxymethyl cellulose, and white carbon black; and / or

[0028] 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

[0029] The antifreezing agent is selected from one or more of alcohols, alcohol ethers, chlorinated hydrocarbons, and inorganic salts; and / or

[0030] The antifoaming agent is selected from one or more of C 10 -C 20 saturated fatty acid compound, silicone oil, silicone compound, C8-C 10 fatty alcohol; and / or

[0031] the solvent is selected from one or more of benzene, toluene, xylene, mesitylene, methanol, ethanol, isopropanol, n-butanol, dimethyl sulfoxide, dimethyl formamide, cyclohexanone, alkylene carbonate, diesel oil, solvent oil, vegetable oil, vegetable oil derivative, and water; and / or

[0032] 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, carboxin, and 1,2-benzisothiazolin-3-one; and / or

[0033] 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, white carbon black, talc, montmorillonite, and starch; and / or

[0034] the synergist is selected from phosphorus synergist and ether synergist; and / or

[0035] the carrier is selected from one or more of ammonium salt, ground natural mineral, ground artificial mineral, silicate, resin, wax, solid fertilizer, water, organic solvent, mineral oil, vegetable oil, and vegetable oil derivative;

[0036] Further, the fungicidal composition can be prepared into an agriculturally allowable formulation form selected from solid formulation and / or liquid formulation.

[0037] The solid formulation includes powder, granule, pellet, tablet, strip, wettable powder, oil dispersible powder, emulsion powder, water dispersible granule, emulsion granule, water dispersible tablet, soluble powder, soluble tablet, or soluble granule.

[0038] The liquid formulation includes soluble liquid, soluble gel, oil, spreadable oil, emulsion, emulsion concentrate, dispersible liquid, paste, water emulsion, oil emulsion, microemulsion, lipid, suspension, microcapsule suspension, oil suspension, dispersible oil suspension, suspoemulsion, microcapsule suspension-suspension, microcapsule suspension-water emulsion, or microcapsule suspension-suspoemulsion.

[0039] Further, the solid formulation is selected from wettable powder and water dispersible granule; and the liquid formulation is selected from suspension and dispersible oil suspension.

[0040] The present application also discloses the use of the fungicidal composition as described above for preventing and treating plant diseases.

[0041] Further, the plant is crop, vegetable, or fruit tree.

[0042] Further, the plant disease is caused by Basidiomycetes or Mitosporic fungi.

[0043] Furthermore, the basidiomycete fungi are *Puccinia* and *Phakopsora*; the mitotic spore fungi are *Pyricularia*, *Drechslera*, *Exserohilum*, *Cercospora*, *Rhizoctonia*, and *Corynespora*.

[0044] Furthermore, the plant diseases mentioned are wheat leaf rust (Puccinia recondita f.sp.tritici), wheat stripe rust (Puccinia striiformis f.sp.tritici), soybean rust fungus (Phakopsorapachyrhizi), rice blast (Pyricularia oryzae), maize large leaf spot (Exserohilum turcicum), soybean gray leaf spot (Cercospora sojina), rice sheath blight fungus (Rhizoctonia solani), and cucumber target spot fungus (Corynespora cassiicola).

[0045] A method of using a bactericidal composition, wherein the bactericidal composition or its formulation is applied at an effective dose to a disease or its growth medium that needs to be controlled.

[0046] Compared with the prior art, the beneficial effects of the technical solution of the present invention are as follows:

[0047] 1) By combining bactericides with different mechanisms of action, the bactericidal activity was increased, and the synergistic effect was significant;

[0048] 2) Safe and environmentally friendly, with broad development prospects, reducing the amount of pesticides used and lowering agricultural costs;

[0049] 3) It is highly efficient, has a broad bactericidal spectrum, and can delay the development of drug resistance in harmful bacteria and prolong the duration of drug efficacy. Detailed Implementation

[0050] 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.

[0051] Specific preparation example:

[0052] Preparation Example 1:

[0053] 49% Fluopyram·Prothioconazole·Chlorothalonil Suspension Concentrate (6+6+37)

[0054] Formula composition: Fluopyram hydroxylamine 6%, Prothioconazole 6%, Chlorothalonil 37%, Fatty alcohol polyoxyethylene ether 1.2%, Sodium polycarboxylate 1%, Styrene-phenol polyoxyethylene ether phosphate 1%, Xanthan gum 0.1%, Glycerin 5%, Benzo[a]isothiazolinone 0.01%, Silicone oil 0.5%, Deionized water to make up the balance;

[0055] Preparation method: Water, dispersant and wetting agent are mixed evenly. Defoamer and antifreeze are added in sequence under stirring. The mixture is then mixed evenly by high-speed shearing. Then the original drug is added and shearing is continued. The mixture is then ground in a horizontal sand mill to control the particle size of the material to be below 90% of 5μm. Finally, thickener is added and sheared evenly to obtain the suspension of the present invention.

[0056] Preparation Example 2:

[0057] 28% Fluopyram·Prothioconazole·Chlorothalonil Suspension Concentrate (1.5+1.5+25)

[0058] Formula composition: Fluopyram hydroxylamine 1.5%, Prothioconazole 1.5%, Chlorothalonil 25%, Fatty alcohol polyoxyethylene ether 1.5%, Sodium polycarboxylate 1.2%, Styrene-phenol polyoxyethylene ether phosphate 0.5%, Isothiazol polyoxyethylene ether 0.5%, Xanthan gum 0.2%, Glycerin 5%, Benzo[a]isothiazolinone 0.01%, Dimethyl silicone oil 0.4%, Deionized water to make up the balance;

[0059] Preparation method: Same as in preparation example 1.

[0060] Preparation Example 3:

[0061] 28% Fluopyram·Prothioconazole·Chlorothalonil Dispersible Oil Suspension (1+2+25)

[0062] Formula composition: fluopyram hydroxylamine 1%, prothioconazole 2%, chlorothalonil 25%, tristyrene-phenylphenol polyoxyethylene ether 7%, alkylphenol polyoxyethylene ether 7%, sodium dodecylbenzenesulfonate 2.5%, organobentonite 1.5%, methyl oleate to make up 100%;

[0063] Preparation method: Methyl oleate and wetting and dispersing agent are stirred evenly, then the original drug and structural stabilizer are added and sheared and stirred evenly. Then, the mixture is ground in a horizontal sand mill, and the particle size of the material is controlled to be below 5 μm for 90% of the particles. Finally, the mixture is evenly mixed to obtain the dispersible oil suspension of the present invention.

[0064] Preparation Example 4:

[0065] 22% Fluopyram·Prothioconazole·Chlorothalonil Dispersible Oil Suspension (2+2.5+17.5)

[0066] Formula composition: Fluopyram hydroxylamine 2%, Prothioconazole 2.5%, Chlorothalonil 17.5%, Tristyrene-phenylphenol polyoxyethylene ether 7%, Alkylphenol polyoxyethylene ether 7%, Calcium dodecylbenzenesulfonate 2%, Organic bentonite 1%, Methyl oleate to make up 100%;

[0067] Preparation method: Same as in preparation example 3.

[0068] Preparation Example 5:

[0069] 55% Fluopyram·Prothioconazole·Chlorothalonil Wettable Powder (2+3+50)

[0070] Formula composition: Fluopyram hydroxylamine 2%, Prothioconazole 3%, Chlorothalonil 50%, Naphthalenesulfonate formaldehyde condensate 5%, Sodium lignosulfonate 10%, Sodium dodecyl sulfate 2%, Kaolin to make up the balance;

[0071] Preparation method: The active ingredient fluopyram is mixed with prothioconazole, chlorothalonil, dispersant, wetting agent and filler, and stirred evenly in a stirring tank. The mixture is then pulverized and mixed evenly multiple times by an air jet mill to prepare the wettable powder of the composition of the present invention.

[0072] Preparation Example 6:

[0073] 45% Fluopyram·Prothioconazole·Chlorothalonil Wettable Powder (2+3+40)

[0074] Formula composition: Fluopyram hydroxylamine 2%, Prothioconazole 3%, Chlorothalonil 40%, Naphthalenesulfonate formaldehyde condensate 5%, Sodium lignosulfonate 10%, Sodium dodecyl sulfate 1%, Starch 0.5%, Kaolin to make up the balance;

[0075] Preparation method: Same as in preparation example 5.

[0076] Preparation Example 7:

[0077] 69% Fluopyram·Prothioconazole·Chlorothalonil Water Dispersible Granules (2.5+4+62.5)

[0078] Formula composition: fluopyram hydroxylamine 2.5%, prothioconazole 4%, chlorothalonil 62.5%, sodium dodecyl sulfate 2%, naphthalene sulfonate formaldehyde condensate 8.5%, sodium polycarboxylate 3.5%, white sugar 4.5%, kaolin to make up the balance;

[0079] Preparation method: Mix the active ingredients, dispersant, wetting agent and filler, stir evenly in a stirring tank, pulverize by air jet, add 10-25% water, and then knead, granulate, dry and sieve to obtain water-dispersible granules; or spray water, granulate and dry the pulverized powder in a fluidized bed granulator, and then sieve to obtain the product.

[0080] Preparation Example 8:

[0081] 76% Fluopyram·Prothioconazole·Chlorothalonil Water Dispersible Granules (8+8+60)

[0082] Formula composition: fluopyram hydroxylamine 8%, prothioconazole 8%, chlorothalonil 60%, sodium dodecyl sulfate 2%, naphthalene sulfonate formaldehyde condensate 9%, sodium polycarboxylate 5%, white sugar 5%, kaolin to make up the balance;

[0083] Preparation method: Same as in preparation example 7.

[0084] Indoor test targets:

[0085] Rice sheath blight fungus (Rhizoctonia solani) - broad bean leaf method, soybean rust fungus (Phakopsorapachyrhizi) - pot method, cucumber target spot fungus (Corynespora cassiicola) - petri dish method.

[0086] Indoor toxicity testing

[0087] Indoor combined action test of fluopyram, prothioconazole and chlorothalonil on plant diseases

[0088] Test reagents: 98% fluopyram technical grade, 95% prothioconazole technical grade, and 98.5% chlorothalonil technical grade. The above technical grades were provided by the Group's R&D Center.

[0089] The mixing test should be conducted in accordance with NY / T 1156.6-2006, "Guidelines for Indoor Bioassay Testing of Pesticides - Part 6: Determination of Combined Effects of Mixtures of Fungicides".

[0090] Wadley method: Evaluating the synergistic effect of drug combinations based on the synergistic coefficient (SR).

[0091] The performance enhancement factor (SR) is calculated using the following formula:

[0092]

[0093] In the formula:

[0094] X1 – EC of the mixture 50 Theoretical value, in milligrams per liter (mg / L);

[0095] P A —The percentage content of A in the mixture, expressed as a percentage (%);

[0096] P B —The percentage content of B in the mixture, expressed as a percentage (%);

[0097] P C—The percentage content of C in the mixture, expressed as a percentage (%);

[0098] A—EC of A in the mixture 50 Value, in milligrams per liter (mg / L);

[0099] B—EC of B in the mixture 50 Value, in milligrams per liter (mg / L);

[0100] C—EC of C in the mixture 50 Value, in milligrams per liter (mg / L);

[0101]

[0102] In the formula:

[0103] SR – Synergistic effect coefficient of the mixture;

[0104] X1 – Mixture EC 50 Theoretical value, in milligrams per liter (mg / L);

[0105] X2 – Mixture EC 50 Measured values, in milligrams per liter (mg / L).

[0106] The synergistic effect coefficient (SR) of the mixture was calculated using the Wadley method. SR ≥ 1.5 indicates a synergistic effect; SR ≤ 0.5 indicates an antagonistic effect; and 0.5 < SR < 1.5 indicates an additive effect.

[0107] Methods for determining toxicity:

[0108] Broad bean leaf method:

[0109] Test basis: The test references NT / T 1156.5-2006 "Guidelines for Indoor Bioassay Tests of Pesticides - Fungicides Part 5: Tests on Inhibition of Rice Sheath Blight Fungicide - Broad Bean Leaf Method".

[0110] Materials preparation: Select a potted broad bean variety susceptible to disease, cut off the second leaf with a petiole that is growing at the same rate, and place it in a 9cm diameter humidified petri dish for later use.

[0111] Humidified Petri Dishes: Dissolve 1g of agar in 100mL and pour it into a 9cm diameter Petri dish. Pour 100mL of 1% agar solution into approximately 8 plates. After it solidifies, place a 9cm diameter sterile filter paper on top.

[0112] Reagent preparation: Dissolve the test drug in acetone first, then dilute with 0.05% 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.

[0113] Application method: Immerse the leaves thoroughly in the pre-prepared solution for 5 seconds, drain off excess solution, allow to air dry naturally, and then incubate under moist conditions according to the treatment label. A control group without the pesticide was included.

[0114] 24 hours after the treatment, use an inoculator to inoculate the mycelial side of a 5mm diameter mycelial cake onto the center of the treated leaf. Inoculate 30 leaves per treatment.

[0115] After inoculation, the cells were placed in an artificial climate incubator and cultured at a temperature controlled at 26±1℃ and a relative humidity of 80% to 90%.

[0116] Based on the disease incidence in the blank control group, the length and width of the lesion at each inoculation point were measured and recorded using calipers, and the lesion diameter (unit: mm) was expressed as the average of the length and width.

[0117] Data statistics and analysis:

[0118] Based on the survey data, the prevention and control effect is calculated using the following formula, with the unit being percentage (%), and the result is rounded to three decimal places.

[0119] P = (D0 - D1) / D0 * 100

[0120] In the formula:

[0121] P—Prevention and control effect;

[0122] D0—Diameter of lesions in the blank control group;

[0123] D1 – Diameter of the lesion treated with the drug.

[0124] Potted plant method:

[0125] Materials preparation: Select potted seedlings of soybean varieties susceptible to disease that are growing uniformly (2 true leaves) and set aside.

[0126] Reagent preparation: Dissolve the test drug in acetone first, then dilute with 0.05% 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.

[0127] Application method: Spray treatment; 24 hours after treatment, inoculate with spore suspension at a concentration of 5 × 10⁻⁶. 5 cells / mL

[0128] After inoculation, the cells were placed in an artificial climate incubator with 100% humidity and in the dark for the first 24 hours. After 24 hours, the cells were cultured at a temperature of 25±1℃ and a relative humidity of 80% to 90%, with a light / dark ratio of 12h / 12h, for 12 to 15 days.

[0129] Disease classification is based on GB / T 17980.89-2004 "Field Efficacy Trial Guidelines (II) Fungicides Part 89: Fungicide Control of Soybean Rust", and the control effect is calculated using the disease index.

[0130] Specifically:

[0131] Grading Standards

[0132] Level 0: No disease;

[0133] Grade 1: The lesion area accounts for less than 5% of the total leaf area;

[0134] Grade 3: Lesions cover 6% to 25% of the total leaf area;

[0135] Level 5: The lesion area accounts for 26% to 50% of the total leaf area;

[0136] Level 7: Lesions cover 51% to 75% of the total leaf area;

[0137] Level 9: The lesion area accounts for more than 76% of the total leaf area;

[0138] Methods for calculating drug efficacy:

[0139]

[0140]

[0141] Plate method:

[0142] Test basis: The test referenced NY / T 1156.2-2006 "Guidelines for Indoor Bioassay Tests of Pesticides - Fungicides Part 2: Plate Test for Inhibition of Mycelial Growth of Pathogenic Fungi";

[0143] 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. The final content of organic solvent shall not exceed 2%.

[0144] 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.

[0145] Inoculation: Under aseptic conditions, the activated pathogenic fungi were 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℃ for incubation. A blank solution without the drug was set up as a blank control. Each treatment was repeated 4 times.

[0146] Investigation: After 12 days of cultivation, 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.

[0147] Data statistics and analysis: The growth of pathogenic mycelia was investigated based on the growth of bacteria in the blank control culture dishes. The colony diameter was measured using the cross-crossing method.

[0148] Based on the survey results, the inhibition rate of mycelial growth of the tested target bacteria by each treatment concentration was calculated as a percentage (%), and the calculation results were retained to two decimal places.

[0149] D = D1 - D2

[0150] In the formula:

[0151] D – Colony growth diameter;

[0152] D1—colony diameter;

[0153] D2 – Diameter of the mushroom cake.

[0154]

[0155] I – Mycelial growth inhibition rate;

[0156] D0—Correlation diameter of the blank control group;

[0157] D t — Diameter of colonies grown after chemical treatment.

[0158] Experimental statistics: Data were processed using probability value analysis. The DPS statistical analysis system was used to analyze the data and determine the toxicity regression line, R, and EC. 50 The value is used to evaluate the activity of the test reagent on the biological sample.

[0159] Indoor toxicity example 1:

[0160] Broad bean leaf method: Rhizoctonia solani, collected from severely affected rice leaves in Hubei.

[0161] The test results are shown in the table below:

[0162] Indoor activity tests showed (see Table 1) that fluopyram, prothioconazole, and chlorothalonil were effective against EC50 of sheath blight. 50The concentrations were 0.455 mg / L, 0.737 mg / L, and 1.476 mg / L, respectively. Mixtures of fluopyram, prothioconazole, and chlorothalonil in ratios of 1:1:25, 1:1:30, 2:3:40, 2:3:50, 2:3:60, 5:8:100, 5:8:125, and 1:2:30 all showed a synergistic effect (SR) greater than 1.5 in their control of sheath blight.

[0163] Table 1. Results of indoor combined action test of fluopyram, prothioconazole and chlorothalonil against *Rhizoctonia solani*.

[0164]

[0165]

[0166] Indoor toxicity example 2:

[0167] Pot cultivation method: Soybean rust fungus (Phakopsora pachyrhizi).

[0168] The test results are shown in the table below:

[0169] Indoor activity tests showed (see Table 2) that fluopyram, prothioconazole, and chlorothalonil were effective against soybean rust EC. 50 The concentrations were 0.086 mg / L, 0.149 mg / L, and 4.547 mg / L, respectively. Mixtures of fluopyram, prothioconazole, and chlorothalonil in ratios of 1:1:25, 1:1:30, 2:3:40, 2:3:50, 2:3:60, 5:8:100, 5:8:125, and 1:2:30 all showed a synergistic effect (SR) greater than 1.5 in controlling soybean rust.

[0170] Table 2. Results of the indoor combined effect test of fluopyram, prothioconazole, and chlorothalonil on soybean rust.

[0171]

[0172] Indoor toxicity example 3:

[0173] Plate test: Cucumber target spot pathogen (Corynespora cassiicola).

[0174] The test results are shown in the table below:

[0175] Indoor activity tests showed (see Table 3) that fluopyram, prothioconazole, and chlorothalonil were effective against cucumber target spot disease EC. 50The concentrations were 0.059 mg / L, 0.544 mg / L, and 84.969 mg / L, respectively. Mixtures of fluopyram, prothioconazole, and chlorothalonil in ratios of 1:1:22.5, 1:1:30, 2:3:40, 2:3:50, 2:3:60, 5:8:100, 5:8:125, and 5:8:150 all showed a synergistic effect (SR) greater than 1.5 in controlling cucumber target spot disease.

[0176] Table 3. Results of the indoor combined effect test of fluopyram, prothioconazole, and chlorothalonil on cucumber target spot disease.

[0177]

[0178] Field efficacy trials

[0179] Soybean rust fungus (Phakopsora pachyrhizi) and corn leaf blight (Exserohilum turcicum).

[0180] Field Example 1

[0181] Field efficacy trials of a combination of fluopyram, prothioconazole, and chlorothalonil against soybean rust.

[0182] Test basis: Refer to GB / T 17980.89-2004 "Field Efficacy Test Guidelines (II) Fungicides Part 89: Fungicides for the Control of Soybean Rust".

[0183] Experimental crop: Soybean (Fengshou 24)

[0184] Experimental site: Soybean field in Qingzhou City. The previous crop was wheat. The soil fertility was moderate and the plants grew uniformly.

[0185] Conditions at the experimental site: Scattered lesions were initially observed on soybean leaves.

[0186] Experimental design: The experimental cells were randomly arranged in blocks, with a cell area of ​​30m². 2 Each cell was repeated 4 times.

[0187] Application time: The soybean plants were evenly sprayed using a Gongnong 16 backpack sprayer, with a pesticide solution volume of 45 kg / mu. The experiment was conducted with the first application in mid-May 2022, followed by a second application at 7-day intervals, for a total of two applications.

[0188] Experimental treatment and dosage:

[0189] Table 4. Test reagents and dosages

[0190]

[0191]

[0192] Experimental investigation: The disease baseline was investigated before the first application of the drug, and the disease index was investigated before the second application (i.e., 7 days after the first application) and 10 days after the second application, and the control effect was calculated. A total of 3 investigations were conducted.

[0193] Survey method: Five sampling points were used in each plot, with four plants sampled at each point, and 5-10 leaves were sampled from top to bottom on each plant.

[0194] Specifically:

[0195] Grading Standards

[0196] Level 0: No disease;

[0197] Grade 1: The lesion area accounts for less than 5% of the total leaf area;

[0198] Grade 3: Lesions cover 6% to 25% of the total leaf area;

[0199] Level 5: The lesion area accounts for 26% to 50% of the total leaf area;

[0200] Level 7: Lesions cover 51% to 75% of the total leaf area;

[0201] Level 9: The lesion area accounts for more than 76% of the total leaf area;

[0202] Methods for calculating drug efficacy:

[0203]

[0204]

[0205] Security survey:

[0206] During the experiment, soybeans in each treatment plot grew well, and none of the pesticides at the tested concentrations caused phytotoxicity to soybean plants or other non-target organisms.

[0207] The results of the field efficacy trials are shown in the table below:

[0208] Field efficacy results (see Table 5): Under the same environmental conditions, the overall control efficacy of different treatments for soybean rust ranged from 68.46% to 83.15% 7 days after the first application. Among them, the two ternary mixtures of 28% fluopyram·prothiophanate-methyl·chlorothalonil oil dispersible suspension (1+2+25) and 69% fluopyram·prothiophanate-methyl·chlorothalonil water dispersible granules (2.5+4+62.5) showed good control effects, with control efficacies of 82.69% and 83.15%, respectively. They were superior to the conventional agent 250 g / L azoxystrobin suspension and the control agents (20% fluopyram·chlorothalonil suspension (2:1), 25% fluopyram·prothiophanate-methyl (10+15) oil dispersible suspension, 72% prothiophanate-methyl·chlorothalonil water dispersible granules (12+60), 200 g / L fluopyram suspension, 480 g / L prothiophanate suspension, and 75% chlorothalonil wettable powder).

[0209] Table 5. Results of field efficacy trials of different treatment combinations against soybean rust 7 days after the first application.

[0210]

[0211] Note: Lowercase letters represent significant differences at the 5% level, and uppercase letters represent significant differences at the 1% level.

[0212] Field efficacy results (see Table 6): Ten days after the second application, the overall control efficacy of all treatments increased, ranging from 70.93% to 86.67%. 28% fluopyram·prothiophanate-methyl·chlorothalonil oil dispersible suspension (1+2+25) and 69% fluopyram·prothiophanate-methyl·chlorothalonil water dispersible granules (2.5+4+62.5) showed good residual efficacy, with control efficiencies of 85.53% and 86.67%, respectively.

[0213] Table 6. Results of field efficacy trials of different treatment combinations against soybean rust 10 days after the second application.

[0214]

[0215]

[0216] Note: Lowercase letters represent significant differences at the 5% level, and uppercase letters represent significant differences at the 1% level.

[0217] Through indoor toxicity testing and field trials, the pesticide composition of fluopyram, prothioconazole and chlorothalonil described in this invention showed good control effect against soybean rust.

[0218] Field Example 2

[0219] Field efficacy trials of a combination of fluopyram, prothioconazole, and chlorothalonil against maize leaf spot disease.

[0220] Test basis: Refer to GB / T 17980.89-2004 "Field Efficacy Test Guidelines (II) Fungicides Part 107: Fungicides for the Control of Large and Small Leaf Spots in Maize".

[0221] Experimental crop: Maize (Xianyu 335)

[0222] Experimental location: Cornfield in Dazhouzhuang Village, Henan Province. The soil fertility is moderate. The corn is planted in contiguous areas with good management, and the plants grow uniformly.

[0223] Experimental method: Spraying was carried out in the early stage of corn growth, that is, when the large leaf spot disease was just about to occur. Spraying was carried out once every 7 days, and the treatment was carried out for 2 consecutive times.

[0224] Experimental design: The experimental cells were randomly arranged in blocks, with a cell area of ​​45m². 2 Each cell was repeated 4 times.

[0225] Experimental treatment and dosage:

[0226] Table 7. Test reagents and dosages

[0227]

[0228]

[0229] In a randomized block design, since maize leaf spot conidia can be spread by wind, rain and air currents, a reasonable isolation zone was arranged between the control and other experimental areas.

[0230] Experimental investigation: Disease index was investigated 7 days after the first application and 7 days after the second application, and the control effect was calculated.

[0231] Survey method: 5 sampling points per plot, 5 plants per point, and all leaves of each plant were surveyed.

[0232] Grading standards for the severity of maize leaf spot disease:

[0233] Level 0: No disease;

[0234] Grade 1: The lesion area accounts for less than 5% of the total leaf area;

[0235] Grade 3: The lesion area accounts for 6% to 10% of the total leaf area;

[0236] Level 5: The lesion area accounts for 11% to 25% of the total leaf area;

[0237] Level 7: Lesions cover 26% to 50% of the total leaf area;

[0238] Level 9: The lesion area accounts for more than 51% of the total leaf area;

[0239] Methods for calculating drug efficacy:

[0240]

[0241]

[0242] Security survey:

[0243] During the experiment, the maize plants in each treatment plot grew well, and none of the pesticides at the tested concentrations caused phytotoxicity to maize plants or other non-target organisms.

[0244] The results of the field efficacy trials are shown in the table below:

[0245] Field efficacy results (see Table 8): Under the same environmental conditions, the overall control efficacy of different treatments for corn leaf blight ranged from 69.31% to 83.66% 7 days after the first application. Among them, the two ternary mixtures of 28% fluopyram·prothiophanate-methyl·chlorothalonil oil dispersible suspension (1+2+25) and 69% fluopyram·prothiophanate-methyl·chlorothalonil water dispersible granules (2.5+4+62.5) showed good control effects, with control efficiencies of 81.37% and 83.66%, respectively. They were superior to the conventional agents 25% pyraclostrobin suspension and the control agents (20% fluopyram·chlorothalonil suspension (2:1), 25% fluopyram·prothiophanate-methyl (10+15) oil dispersible suspension, 72% prothiophanate-methyl·chlorothalonil water dispersible granules (12+60), 200 g / L fluopyram suspension, 480 g / L prothiophanate suspension, and 75% chlorothalonil wettable powder).

[0246] Table 8. Results of field efficacy trials of different treatment combinations against maize leaf spot disease 7 days after the first application.

[0247]

[0248] Note: Lowercase letters represent significant differences at the 5% level, and uppercase letters represent significant differences at the 1% level.

[0249] Field efficacy results (see Table 9): Ten days after the second application, the overall control efficacy of all treatments increased, ranging from 71.69% to 88.66%. 28% fluopyram·prothiophanate-methyl·chlorothalonil oil dispersible suspension (1+2+25) and 69% fluopyram·prothiophanate-methyl·chlorothalonil water dispersible granules (2.5+4+62.5) showed good residual efficacy, with control efficiencies of 86.92% and 88.66%, respectively.

[0250] Table 9. Results of field efficacy trials of different treatment combinations against maize leaf spot disease 7 days after the second application.

[0251]

[0252] Note: Lowercase letters represent significant differences at the 5% level, and uppercase letters represent significant differences at the 1% level.

[0253] Through indoor toxicity testing and field trials, the pesticide composition of fluopyram, prothioconazole and chlorothalonil described in this invention showed good control effect against maize leaf spot.

[0254] The pesticide compositions or formulations obtained by this invention exhibit significant preventive effects, demonstrating superior efficacy compared to single agents in delaying the development of resistance and extending the duration of action. Furthermore, no phytotoxicity was observed in the experiments with the compounded pesticides, indicating that the enhanced synergistic bactericidal effect of the resulting pesticide compositions or formulations can reduce production and usage costs while ensuring crop safety.

[0255] 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: The bactericidal composition comprises active ingredients A, B, and C. Active ingredient A is fluopyram, active ingredient B is prothioconazole, and active ingredient C is chlorothalonil. The mass ratio of active ingredients A, B, and C is 1:1:22.5, 1:1:25, 1:1:30, 2:3:40, 2:3:50, 2:3:60, 5:8:100, 5:8:125, or 5:8:

150.

2. 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 the active ingredients in the bactericidal composition is 1 to 90 wt%.

3. The bactericidal composition according to claim 2, characterized in that: The total content of the active ingredients in the bactericidal composition is 5-80 wt%.

4. The bactericidal composition according to claim 1, characterized in that: In addition to the active ingredient, the bactericidal composition also includes agriculturally acceptable auxiliary ingredients, which are selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoamers, solvents, preservatives, stabilizers, synergists or carriers.

5. The bactericidal composition according to claim 1, characterized in that: The bactericidal composition is prepared into an agriculturally permissible formulation, wherein the formulation is selected from solid dosage forms and / or liquid dosage forms; the solid dosage forms are selected from wettable powders and water-dispersible granules; and the liquid dosage forms are selected from suspension concentrates and dispersible oil suspensions.

6. The application of the bactericidal composition according to any one of claims 1-5 for the prevention and control of plant diseases, characterized in that: The plant diseases mentioned are rice sheath blight, soybean rust, cucumber target spot, and corn leaf blight.

7. The application according to claim 6, characterized in that: The bactericidal composition is applied in an effective dose to the disease or its growth medium that needs to be controlled.

Citation Information

Patent Citations

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  • Pesticide composition containing pydiflumetofen and chlorothalonil, and application thereof

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