A bactericidal composition containing prothioconazole and its application

Abstract

The present invention belongs to the field of pesticide sterilization technology and discloses a sterilization composition. The active ingredients of the sterilization composition include active ingredient A, active ingredient B, and active ingredient C. Active ingredient A is fluopyraclostrobin, active ingredient B is prothioconazole, and active ingredient C is difenoconazole. The sterilization composition of the present invention has good sterilization efficacy and significant synergistic effects against various pathogens.

Description

Technical Field

[0001] The invention belongs to the technical field of pesticide sterilization and discloses a sterilization composition containing prothioconazole and application thereof. Background Art

[0002] Difenoconazole is a triazole systemic fungicide with the characteristics of high efficiency, broad spectrum, safety, long lasting effect and strong systemic properties. It mainly prevents the growth of pathogenic fungi by inhibiting the biosynthesis of sterols in the cell walls. It has good preventive and control effects on leaf spot, black spot, powdery mildew and blight on a variety of vegetables and fruit trees.

[0003] Prothioconazole, a triazolethione fungicide discovered, developed, and produced by Bayer CropScience, is a sterol demethylation inhibitor with excellent systemic activity. It exhibits excellent protective, curative, and eradicative activity against a wide range of diseases, with a long-lasting effect and crop safety. Prothioconazole is primarily used in cereals, soybeans, rapeseed, rice, peanuts, sugar beets, and vegetables. It has a broad spectrum of activity and is highly effective against nearly all fungal diseases of cereals.

[0004] Flupyraclostrobin, a bifenthionyl fungicide developed by BASF, is a major player in the global grain and soybean fungicide market. Like other SDHI fungicides, it has a single site of action and a high level of resistance. Therefore, the International Fungicide Resistance Committee (FRAC) recommends combining this fungicide with other fungicides with different mechanisms of action or using it in rotation.

[0005] In order to effectively delay the emergence and development of resistance, the applicant formulated the product with a variety of fungicide products. The final research found that compounding flupyraclopram with difenoconazole and prothioconazole in a suitable ratio can not only effectively slow down the emergence and development of drug resistance problems, but also improve the prevention and control effect, expand the fungicide spectrum and ensure crop safety. Summary of the Invention

[0006] Based on the above situation, the object of the present invention is to provide a fungicide composition containing prothioconazole, which has excellent prevention and control effects on plant diseases caused by various pathogenic bacteria, a broad fungicidal spectrum, significant synergistic effects, and good safety for crops.

[0007] Another object of the present invention is to provide a formulation of a fungicide composition containing prothioconazole, difenoconazole, and fluopyraclostrobin;

[0008] Another object of the present invention is to provide a fungicidal composition containing prothioconazole, difenoconazole and fluopyraclostrobin for use in preventing and controlling plant diseases caused by various pathogenic bacteria.

[0009] In order to achieve the above object, the present invention adopts the following technical solution: a fungicide composition containing prothioconazole, the fungicide composition comprising active ingredient A, active ingredient B and active ingredient C, the active ingredient A is flupyraclostrobin, the active ingredient B is prothioconazole, and the active ingredient C is difenoconazole;

[0010] Furthermore, the mass ratio of the active ingredient A to the active ingredient B to the active ingredient C is (1-10):(1-10):(1-20), or any value within the above numerical ranges;

[0011] Furthermore, the mass ratio of the active ingredient A to the active ingredient B to the active ingredient C is (1-10):(1-10):(1-15), or any value within the above numerical range;

[0012] Furthermore, the mass ratio of the active ingredient A to the active ingredient B to the active ingredient C is (1-8):(1-9):(1-15), or any value within the above numerical ranges;

[0013] Furthermore, the mass ratio of the active ingredient A to the active ingredient B to the active ingredient C is 2:1:1, 1:1:1, 1:2:1, 1:2:2, 1:2:3, 2:3:4, 2:3:5, 6:8.4:11, 8:9:15, 2:5:10, 2:5:15, 3:2:1, or any value between the above values;

[0014] Furthermore, the mass ratio of the active ingredient A to the active ingredient B to the active ingredient C is 1:2:1, 1:2:2, 1:2:3, 2:3:4, 2:3:5, 6:8.4:11, 8:9:15, 2:5:10, or any value between the above values;

[0015] Furthermore, based on the total weight of the bactericidal composition being 100%, the sum of the active ingredients accounts for 1% to 80% of the total weight of the bactericidal composition;

[0016] Furthermore, the fungicide composition contains, in addition to the active ingredient, other auxiliary ingredients on the pesticide, wherein the auxiliary ingredients are selected from one or more of a wetting agent, a dispersant, an emulsifier, a thickener, a disintegrant, an antifreeze agent, a defoaming agent, a solvent, a preservative, a stabilizer, a synergist or a carrier;

[0017] Furthermore, the wetting agent is selected from one or more of alkylbenzene sulfonate, alkylnaphthalene sulfonate, lignin sulfonate, sodium lauryl sulfate, sodium dioctyl sulfosuccinate, α-olefin sulfonate, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol ethoxylate, fatty alcohol ethoxylate, fatty alcohol polyoxyethylene ether sodium sulfate, silkworm feces, soapberry powder, soapberry powder, SOPA, detergent, emulsifier 2000 series and wetting penetrant F; and / or

[0018] 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 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

[0019] 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

[0020] The thickener 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

[0021] 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

[0022] The antifreeze agent is selected from one or more of alcohols, alcohol ethers, chlorinated hydrocarbons and inorganic salts; and / or

[0023] Defoaming agent selected from C 10 -C 20 Saturated fatty acid compounds, silicone oil, silicone compounds, C8-C 10 One or more of fatty alcohols; and / or

[0024] 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, solvent oil, vegetable oil, vegetable oil derivatives and water; and / or

[0025] The preservative is selected from one or more of propionic acid, sodium propionic acid, sorbic acid, sodium sorbic acid, potassium sorbic acid, benzoic acid, sodium benzoic acid, sodium p-hydroxybenzoic acid, methyl p-hydroxybenzoate, kasone and 1,2-benzisothiazolin-3-one; and / or

[0026] 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

[0027] Synergists are selected from synergist, piperonyl butoxide; and / or

[0028] 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.

[0029] The present invention optimizes the content of active ingredients and adjuvants in the bactericidal composition to achieve a better balance between toxicity and residue, thereby enhancing efficacy, reducing dosage and lowering costs.

[0030] Furthermore, the bactericidal composition can be prepared into a solid preparation or a liquid preparation, wherein the solid preparation is a wettable powder or a wettable powder, and the liquid preparation is a suspension, an emulsion in water or an emulsifiable concentrate;

[0031] The invention also discloses the use of the above-mentioned fungicide composition for preventing and controlling plant diseases.

[0032] Furthermore, the plant disease is caused by Corynespora, Cercospora, Cylindrosporium, Puccinia, Puccinia, Helminthosporium or Powdery Mildew.

[0033] Furthermore, the plants are crops, vegetables or fruit trees; the crops are wheat, soybeans, cotton or corn, and the vegetables are tomatoes or cucumbers.

[0034] Furthermore, the plant diseases are soybean purple spot, soybean rust, soybean powdery mildew, cotton gray spot, cotton white spot, corn gray spot, corn large spot, corn small spot, cucumber target disease, wheat rust, wheat powdery mildew or tomato brown spot.

[0035] The beneficial effects of the present invention are:

[0036] 1) The fungicide composition of the present invention has reasonable components, and prothioconazole, difenoconazole and fluopyraclostrobin are compounded in an appropriate mass ratio, which has a significant synergistic effect on plant diseases caused by various pathogens, expanding the fungicidal spectrum while improving the control effect;

[0037] 2) The fungicidal composition of the present invention has good quick-acting properties and a long lasting effect, reduces the amount of pesticides used, is environmentally friendly, and is safe for target plants. DETAILED DESCRIPTION

[0038] In order to make the beneficial effects and technical solutions of the present invention more clearly understood, the present invention is further explained using the following preparation examples and specific embodiments.

[0039] Preparation example:

[0040] Preparation Example 1: 20% fluopicolide, prothioconazole, and difenoconazole water dispersible granules (4% + 6% + 10%) (2:3:5)

[0041] Formula composition: 4% flupyraclostrobin, 6% prothioconazole, 10% difenoconazole, 6% polycarboxylic acid sodium salt, 2.5% lakai powder BX, 8% naphthalenesulfonic acid formaldehyde condensate sodium salt, 5% ammonium sulfate, and kaolin makes up the balance.

[0042] Preparation method: The active ingredient, dispersant, wetting agent and filler are mixed, stirred evenly in a stirred tank, and after air flow grinding, 10-25% water is added, and then kneading, granulation, drying and screening are carried out to obtain a water-dispersible granule product; or the pulverized powder is sprayed with water in a boiling granulator, granulated, dried, and then sieved to obtain the product.

[0043] Preparation Example 2: 25.4% fluopicolide, prothioconazole, and difenoconazole water dispersible granules (6% + 8.4% + 11%) (6:8.4:11)

[0044] Formula composition: 6% fluopicolide, 8.4% prothioconazole, 11% difenoconazole, 10% sodium lignin sulfonate, 2.5% lakai powder BX, 5% sodium polycarboxylate, 8% glucose, and starch makes up the balance.

[0045] Preparation method: Same as Preparation Example 1.

[0046] Preparation Example 3: 32% fluopicolide·prothioconazole·difenoconazole wettable powder (8%+9%+15%) (8:9:15)

[0047] Formula composition: 8% fluopicolide, 9% prothioconazole, 15% difenoconazole, 5% naphthalenesulfonic acid formaldehyde condensate sodium salt, 8% sodium lignin sulfonate, 2% sodium lauryl sulfate, kaolin makes up the balance;

[0048] Preparation method: The active ingredients, dispersant, wetting agent and filler are mixed, stirred evenly in a stirring kettle, and pulverized and mixed evenly for multiple times in a jet mill to prepare the wettable powder of the composition of the present invention.

[0049] Preparation Example 4: 27% fluopicolide·prothioconazole·difenoconazole wettable powder (6%+9%+12%) (2:3:4)

[0050] Formula composition: 6% fluopicolide, 9% prothioconazole, 12% difenoconazole, 6% naphthalenesulfonate formaldehyde condensate, 10% sodium ligninsulfonate, 2% sodium lauryl sulfate, 5% starch, and kaolin makes up the balance;

[0051] Preparation method: Same as Preparation Example 3.

[0052] Preparation Example 5: 24% fluopicolide·prothioconazole·difenoconazole suspension concentrate (4%+8%+12%) (1:2:3)

[0053] Formula composition: 4% flupyraclostrobin, 8% prothioconazole, 12% difenoconazole, 2% Guerbet alcohol polyoxyethylene ether, 1% naphthalenesulfonate formaldehyde condensate, 3% tristyrylphenol ethoxylate phosphate, 2% alkylaryl polyoxyethylene ether polyoxypropylene ether, 0.25% xanthan gum, 1% magnesium aluminum silicate, 5% ethylene glycol, 0.3% sodium benzoate, 0.5% silicone oil, and deionized water to make up the balance;

[0054] Preparation method: According to the formula ratio, the active ingredients, surfactants and other functional additives are placed in a reactor in sequence, water is added and mixed evenly, and the suspension product is obtained by high-speed shearing, wet sand grinding, and finally homogenization filtration.

[0055] Preparation Example 6: 17.5% fluopicolide·prothioconazole·difenoconazole suspension concentrate (3.5%+7%+7%) (1:2:2)

[0056] Formula composition: 3.5% flupyraclostrobin, 7% prothioconazole, 7% difenoconazole, 1% fatty alcohol polyoxyethylene ether, 2% isotridecyl polyoxyethylene ether, 2% alkylphenol polyoxyethylene ether phosphate, 1% sodium salt of polycarboxylate, 1% magnesium aluminum silicate, 0.2% carboxyethyl cellulose, 1% sodium sorbate, 5% glycerol, 0.5% silicone oil, and deionized water to make up the balance;

[0057] Preparation method: Same as Preparation Example 5.

[0058] Preparation Example 7: 17.6% fluopicolide·prothioconazole·difenoconazole dispersible oil suspension concentrate (4.4%+8.8%+4.4%) (1:2:1)

[0059] Formula composition: 4.4% flupyraclostrobin, 8.8% prothioconazole, 4.4% difenoconazole, 2% lignin sulfonate, 12% castor oil polyoxyethylene ether, 2% isotridecyl alcohol polyoxyethylene ether, 2% calcium dodecylbenzene sulfonate, 1% silicon dioxide, 1% organic bentonite, 18% 200# solvent oil, and methyl oleate makes up the balance;

[0060] Preparation method: According to the formula ratio, the active ingredients, surfactants and other functional additives are placed in the reactor in sequence, oil is added and mixed evenly, and the dispersible oil suspension product is obtained by high-speed shearing, wet sand grinding, and finally homogenization filtration.

[0061] Preparation Example 8: 30% fluopicolide, prothioconazole, and difenoconazole dispersible oil suspension concentrate (6% + 9% + 15%) (2:3:5)

[0062] Formula composition: 6% flupyraclostrobin, 9% prothioconazole, 15% difenoconazole, 4% alkylphenol polyoxyethylene ether, 10% glycerol fatty acid ester polyoxyethylene ether, 1% calcium dodecylbenzenesulfonate, 1% sodium polycarboxylate, 20% 200# solvent oil, 1% organic bentonite, and soybean oil makes up the balance;

[0063] Preparation method: Same as Preparation Example 7.

[0064] Indoor activity experiment

[0065] Example 1: Indoor activity test - plate method

[0066] Test basis: The test refers to NY / T 1156.2-2006 "Guidelines for Indoor Bioassay Tests of Pesticides - Fungicides Part 2: Inhibition of Pathogenic Fungal Mycelial Growth Test Plate Method" and NY / T 1156.6-2006 "Guidelines for Indoor Bioassay Tests of Pesticides - Fungicides Part 6: Determination of the Combined Effect of Mixtures".

[0067] Test targets: Cercospora kikuchii, Cercospora zeae-maydis Tehon & Daniels, and Corynespora cassiicola (Berk & Curt) Wei.

[0068] Test agents: 98% fluopicolide technical, 95% prothioconazole technical, 95% difenoconazole technical, provided by the group's R&D center

[0069] Preparation: Dissolve the test stock drug in acetone and then dilute with 0.05% Tween 80 aqueous solution. Prepare single-dose stock solutions and set five concentration series based on the mixing purpose and drug activity.

[0070] Test culture medium and culture conditions of each pathogen:

[0071]

[0072] Drug Treatment: Under aseptic conditions, add pre-thawed sterilized PDA culture medium to a sterile Erlenmeyer flask according to the test treatment. Aspirate the drug solution in ascending order, adding it to the flask and shaking thoroughly. Pour equal amounts into 9 cm diameter Petri dishes to prepare drug-containing plates of the corresponding concentration. A treatment without drug was used as a blank control. Each treatment was replicated four times.

[0073] Inoculation: Use a sterile puncher with a diameter of 6 mm to cut the cultured pathogen from the edge of the colony under sterile conditions. Use a sterilized inoculator to inoculate the cake into the center of the drug-containing plate, cover it with a cap, and place it in a suitable incubator for culture.

[0074] Experimental investigation: Investigate the growth of pathogenic fungi hyphae based on the growth of bacteria in the blank control culture dish, measure the diameter of the colony with a caliper, and measure the diameter of each colony vertically once using the cross method, and take the average value.

[0075] According to the survey results, the mycelial growth inhibition rate of each treatment concentration on the target bacteria was calculated in percentage (%), and the calculation results were rounded to two decimal places.

[0076] D=D1-D2

[0077] Where:

[0078] D——colony growth diameter;

[0079] D1 - colony diameter;

[0080] D2——diameter of mushroom cake.

[0081]

[0082] I——hyphae growth inhibition rate;

[0083] D0——blank control colony growth diameter;

[0084] D t ——The growth diameter of the colony after treatment with chemicals.

[0085] Use DPS statistical analysis system to analyze and calculate the toxicity regression line, R, EC 50 The activity of the test agent on the biological test material is evaluated by the value.

[0086] Wadley method: The synergistic effect of mixed drugs is evaluated based on the synergistic coefficient (SR).

[0087] The SR is calculated as follows:

[0088]

[0089] Where:

[0090] X1——EC of the mixture 50 Theoretical value, in milligrams per liter (mg / L);

[0091] P A ——the percentage of A in the mixture, expressed in percentage (%);

[0092] P B ——the percentage of B in the mixture, expressed as percentage (%);

[0093] P C ——the percentage of C in the mixture, expressed as percentage (%);

[0094] A——EC of A in the mixture 50 Value, in milligrams per liter (mg / L);

[0095] B——EC of B in the mixture 50 Value, in milligrams per liter (mg / L);

[0096] C——EC of C in the mixture 50 Value, in milligrams per liter (mg / L);

[0097]

[0098] Where:

[0099] SR - synergistic coefficient of mixture;

[0100] X1——Mixture EC 50 Theoretical value, in milligrams per liter (mg / L);

[0101] X2——Mixture EC 50 The measured value is in milligrams per liter (mg / L).

[0102] The synergistic effect (SR) of the mixture was calculated according to the Wadley method. SR ≥ 1.5 indicates synergism; SR ≤ 0.5 indicates antagonism; and 0.5 < SR < 1.5 indicates additive effect.

[0103] Table 1 Results of indoor biological activity test on soybean purple spot

[0104]

[0105] From the indoor activity test (see Table 1), the EC values ​​of fluopyram, prothioconazole and difenoconazole against soybean purple spot were 50The synergistic coefficients (SR) of the mixtures of flupyracodyl with prothioconazole and difenoconazole at mass ratios of 1:2:2, 1:2:3, 2:3:4, 2:3:5, 6:8.4:11, 8:9:15 and 2:5:10 against soybean purple spot disease were all greater than 1.5, showing a synergistic effect.

[0106] Table 2 Results of indoor bioactivity test on corn gray leaf spot

[0107]

[0108] From the indoor activity test (see Table 2), the EC values ​​of fluopyram, prothioconazole and difenoconazole against corn gray leaf spot were 50 The synergistic coefficients (SR) of fluopyram mixed with prothioconazole and difenoconazole at mass ratios of 2:3:4, 2:3:5 and 6:8.4:11 against corn gray leaf spot were all greater than 1.5, showing a synergistic effect.

[0109] Table 3 Results of indoor bioactivity test on cucumber target spot

[0110]

[0111] From the indoor activity test (see Table 3), the EC values ​​of fluopyram, prothioconazole and difenoconazole against cucumber target spot were 50 The synergistic coefficients (SR) of fluopyram mixed with prothioconazole and difenoconazole at mass ratios of 1:2:3, 2:3:4, 2:3:5, 6:8.4:11 and 8:9:15 against cucumber target spot disease were all greater than 1.5, showing a synergistic effect.

[0112] Example 2: Indoor biological activity test on soybean rust

[0113] Test reference: NY / T 1156.6-2006 "Guidelines for Indoor Bioassay of Pesticides - Fungicides - Part 6: Determination of the Combined Action of Mixtures".

[0114] Test target: Phakopsora pachyrhizi.

[0115] Test agents: 98% fluopicolide technical, 95% prothioconazole technical, 95% difenoconazole technical, provided by the group's R&D center

[0116] Material preparation: Select potted soybean seedlings with two leaves and one heart in the same growth stage and set aside.

[0117] Preparation: Dissolve the test stock drug in acetone and then dilute with 0.05% Tween 80 aqueous solution. Prepare single-dose stock solutions and set five concentration series based on the mixing purpose and drug activity.

[0118] Application method: Place soybean seedlings on the turntable of the bio-test spray tower for spraying. For every 3 pots of soybeans to be treated, spray 30mL of the solution. Place them indoors to dry naturally after application. 24 hours after treatment, apply the prepared 5×10 6 Soybean leaves were inoculated with spores / mL of inoculum, allowed to air dry, and then incubated in the dark at 25°C, 100% humidity for 24 hours. After 24 hours, the leaves were incubated in a 25±1°C incubator with a light / dark ratio (L:D) of 12 hours / 12 hours and a relative humidity of 60% to 80%.

[0119] When the blank control disease was stable, the activity of different pesticides against soybean rust was investigated. The disease classification was based on the reference of GB / T17980.89-2004 "Guidelines for Field Efficacy Tests (II) Fungicides Part 89: Fungicides for Control of Soybean Rust", and the control effect was calculated using the disease index.

[0120] Specifically:

[0121] Grading standards

[0122] Level 0: no disease;

[0123] Level 1: The lesion area accounts for less than 5% of the entire leaf area;

[0124] Level 3: The lesion area accounts for 6% to 25% of the entire leaf area;

[0125] Level 5: The lesion area accounts for 26% to 50% of the entire leaf area;

[0126] Level 7: The lesion area accounts for 51% to 75% of the entire leaf area;

[0127] Level 9: The lesion area accounts for more than 76% of the entire leaf area;

[0128] Calculation method of drug efficacy:

[0129]

[0130]

[0131] Use DPS statistical analysis system to analyze and calculate the toxicity regression line, R, EC 50 The activity of the test agent on the biological test material is evaluated by the value.

[0132] Wadley method: The synergistic effect of mixed drugs is evaluated based on the synergistic coefficient (SR).

[0133] The SR is calculated as follows:

[0134]

[0135] Where:

[0136] X1——EC of the mixture 50 Theoretical value, in milligrams per liter (mg / L);

[0137] P A ——the percentage of A in the mixture, expressed in percentage (%);

[0138] P B ——the percentage of B in the mixture, expressed as percentage (%);

[0139] P C ——the percentage of C in the mixture, expressed as percentage (%);

[0140] A——EC of A in the mixture 50 Value, in milligrams per liter (mg / L);

[0141] B——EC of B in the mixture 50 Value, in milligrams per liter (mg / L);

[0142] C——EC of C in the mixture 50 Value, in milligrams per liter (mg / L);

[0143]

[0144] Where:

[0145] SR - synergistic coefficient of mixture;

[0146] X1——Mixture EC 50 Theoretical value, in milligrams per liter (mg / L);

[0147] X2——Mixture EC 50 The measured value is in milligrams per liter (mg / L).

[0148] The synergistic effect (SR) of the mixture was calculated according to the Wadley method. SR ≥ 1.5 indicates synergism; SR ≤ 0.5 indicates antagonism; and 0.5 < SR < 1.5 indicates additive effect.

[0149] Table 4 Indoor bioactivity test of soybean rust

[0150]

[0151] From the indoor activity test (see Table 4), the EC values ​​of fluopyram, prothioconazole and difenoconazole against soybean rust were 50 The synergistic coefficients (SR) of fluopyram mixed with prothioconazole and difenoconazole at mass ratios of 1:2:2, 1:2:3, 2:3:4, 2:3:5, 6:8.4:11, 8:9:15 and 2:5:10 against soybean rust were all greater than 1.5, showing a synergistic effect.

[0152] Example 3: Indoor biological activity test on wheat powdery mildew

[0153] Test basis: The test refers to the "Guidelines for Indoor Bioassay of Pesticides - Fungicides Part 4: Pot Method for Control of Wheat Powdery Mildew".

[0154] Test target: Blumeria graminis f.sp.tritici, a wheat-specific fungus of the Poaceae family.

[0155] Test agents: 98% fluopicolide technical, 95% prothioconazole technical, 95% difenoconazole technical, provided by the group's R&D center.

[0156] Test method:

[0157] Select susceptible wheat varieties and plant them in pots until the seedlings grow to the 2-3 leaf stage. Dissolve the original drug in acetone and dilute it with a 0.1% Tween 80 aqueous solution. Set five mass concentration gradients based on the drug's activity.

[0158] The test agent was evenly sprayed on the spare wheat seedlings by spraying and allowed to dry naturally. A treatment without the agent was set up as a blank control.

[0159] 24 hours after the treatment with the agent, the fresh spores of powdery mildew produced on the diseased wheat leaves within 24 hours were evenly shaken off and inoculated on the wheat seedlings in the 2-3 leaf stage pot. Each treatment had 4 pots, 10 plants in each pot, and they were cultured under appropriate conditions.

[0160] A graded survey was conducted based on the incidence of the blank control group, using the following grading method:

[0161] Level 0: no disease;

[0162] Level 1: The lesion area accounts for less than 5% of the entire leaf area;

[0163] Level 3: The lesion area accounts for 6% to 15% of the entire leaf area;

[0164] Level 5: The lesion area accounts for 16% to 25% of the entire leaf area;

[0165] Level 7: The lesion area accounts for 26% to 50% of the entire leaf area;

[0166] Level 9: The lesion area accounts for more than 50% of the entire leaf area;

[0167] Calculation method of drug efficacy:

[0168]

[0169]

[0170] Use DPS statistical analysis system to analyze and calculate the toxicity regression line, R, EC 50 The activity of the test agent on the biological test material is evaluated by the value.

[0171] Wadley method: The synergistic effect of mixed drugs is evaluated based on the synergistic coefficient (SR).

[0172] The SR is calculated as follows:

[0173]

[0174] Where:

[0175] X1——EC of the mixture 50 Theoretical value, in milligrams per liter (mg / L);

[0176] P A ——the percentage of A in the mixture, expressed in percentage (%);

[0177] P B ——the percentage of B in the mixture, expressed as percentage (%);

[0178] P C ——the percentage of C in the mixture, expressed as percentage (%);

[0179] A——EC of A in the mixture 50 Value, in milligrams per liter (mg / L);

[0180] B——EC of B in the mixture 50 Value, in milligrams per liter (mg / L);

[0181] C——EC of C in the mixture 50 Value, in milligrams per liter (mg / L);

[0182]

[0183] Where:

[0184] SR - synergistic coefficient of mixture;

[0185] X1——Mixture EC 50 Theoretical value, in milligrams per liter (mg / L);

[0186] X2——Mixture EC 50 The measured value is in milligrams per liter (mg / L).

[0187] The synergistic effect (SR) of the mixture was calculated according to the Wadley method. SR ≥ 1.5 indicates synergism; SR ≤ 0.5 indicates antagonism; and 0.5 < SR < 1.5 indicates additive effect.

[0188] Table 5 Indoor biological activity test of wheat powdery mildew

[0189]

[0190] From the indoor activity test (see Table 5), the EC values ​​of fluopyram, prothioconazole and difenoconazole against wheat powdery mildew are 50 The synergistic coefficients (SR) of the mixtures of flupyracodyl with prothioconazole and difenoconazole at mass ratios of 1:2:2, 1:2:3, 2:3:4, 2:3:5, 6:8.4:11, 8:9:15 and 2:5:10 against wheat powdery mildew were all greater than 1.5, showing a synergistic effect.

[0191] Field efficacy trials

[0192] Example 4: Field efficacy test on cucumber target spot disease

[0193] The trial was conducted in a cucumber field in Changlu Village, Guan County, Shandong Province. The site was flat, with moderate soil fertility and good irrigation and drainage conditions. Cultivation conditions across all plots were uniform and consistent with local agricultural practices (GAP).

[0194] Test target: cucumber target spot disease.

[0195] Test agents: 25.4% fluopicolide, prothioconazole, difenoconazole water dispersible granules (6% + 8.4% + 11%) (6:8.4:11), 30% fluopicolide, prothioconazole, difenoconazole dispersible oil suspension (6% + 9% + 15%) (2:3:5), 27% fluopicolide, prothioconazole, difenoconazole wettable powder (6% + 9% + 12%) (2:3:4), 17.5% fluopicolide Amine·prothioconazole·difenoconazole suspension concentrate (3.5%+7%+7%) (1:2:2), 15% fluopicolide·prothioconazole water-dispersible granules (2:3), 14% fluopicolide·difenoconazole suspension concentrate (7:5), 24% prothioconazole·difenoconazole suspension concentrate (3:5), 300 g / L fluopicolide suspension concentrate, 480 g / L prothioconazole suspension concentrate, 10% difenoconazole water-dispersible granules, and clean water control.

[0196] Experimental design: The experiment set up 11 treatments, each treatment was repeated 4 times, and the area of ​​the plot was 25m. 2 , protection rows are set up between each experimental plot.

[0197] Application time: The first application of pesticides was conducted on July 17, 2022, and the second application was conducted 7 days later. The pesticide solution was prepared according to the experimental concentration and sprayed with a manual backpack sprayer.

[0198] Experimental investigation: The control effect investigation was carried out 10 days after the last application of the pesticide. The investigation time adopted the random sampling method. Sampling was carried out at 5 points in each plot, 2 plants were investigated at each point, and 5 leaves of each plant were investigated at the upper, middle and lower parts. The disease degree of each leaf of each plant was recorded, and the disease index and control effect were calculated according to the disease grading standard.

[0199] The grading method is:

[0200] Level 0: no disease;

[0201] Level 1: The lesion area accounts for less than 5% of the entire leaf area;

[0202] Level 3: The lesion area accounts for 6% to 25% of the entire leaf area;

[0203] Level 5: The lesion area accounts for 26% to 50% of the entire leaf area;

[0204] Level 7: The lesion area accounts for 51% to 75% of the entire leaf area;

[0205] Level 9: The lesion area accounts for more than 76% of the entire leaf area;

[0206] Calculation method of drug efficacy:

[0207]

[0208]

[0209] Table 6 Field efficacy test results of cucumber target spot disease

[0210]

[0211]

[0212] Field efficacy showed (see Table 6): 10 days after the second application, the overall control efficacy of the three-way combination treatment in the field showed good persistence, with control efficiencies of 91.19%, 87.70%, 85.44% and 84.47% respectively.

[0213] Example 5: Field efficacy test on soybean rust

[0214] Test basis: The test was conducted with reference to GB / T 17980.89-2004 "Guidelines for Field Efficacy Tests of Pesticides (II) Part 89: Fungicides for Control of Soybean Rust".

[0215] The test site was the soybean field in Sujiatun, Shenyang, Liaoning Province. Soybean rust has occurred in the test site for many years. The cultivation conditions of all test plots were uniform and consistent with local scientific agricultural practices.

[0216] Test target: soybean rust.

[0217] Test agents: 20% fluopoxam·prothioconazole·difenoconazole water dispersible granules (4%+6%+10%) (2:3:5), 32% fluopoxam·prothioconazole·difenoconazole wettable powder (8%+9%+15%) (8:9:15), 24% fluopoxam·prothioconazole·difenoconazole suspension concentrate (4%+8%+12%) (1:2:3), 17.6% fluopoxam·prothioconazole·difenoconazole Meconazole dispersible oil suspension concentrate (4.4%+8.8%+4.4%) (1:2:1), 15% fluopicolide·prothioconazole water dispersible granules (2:3), 14% fluopicolide·fenpropimorph suspension concentrate (7:5), 24% prothioconazole·fenpropimorph suspension concentrate (3:5), 300 g / L fluopicolide suspension concentrate, 480 g / L prothioconazole suspension concentrate, 10% fenpropimorph water dispersible granules, and clear water control.

[0218] Experimental design: There are 11 treatments in the experiment. The experimental drug, control drug and blank control treatments are arranged in random blocks. Each plot is 30m2. 2 , each treatment was repeated 4 times.

[0219] Application time: Spray the pesticide with a manual sprayer at the beginning of the rust epidemic on August 17, 2022, and apply the pesticide for the second time after an interval of 7 days. A total of 2 applications were performed during the entire trial process.

[0220] Investigation method: The control efficacy investigation was carried out on the 14th day after the last application of the pesticide. Twenty plants were sampled at five points in each plot using the diagonal method. Four leaves each at the upper, middle and lower parts of each plant were investigated, and the total number of leaves and the number of diseased leaves at each level were recorded.

[0221] Grading method:

[0222] Level 0: no disease;

[0223] Level 1: The lesion area accounts for less than 5% of the entire leaf area;

[0224] Level 3: The lesion area accounts for 6% to 25% of the entire leaf area;

[0225] Level 5: The lesion area accounts for 26% to 50% of the entire leaf area;

[0226] Level 7: The lesion area accounts for 51% to 75% of the entire leaf area;

[0227] Level 9: The lesion area accounts for more than 76% of the entire leaf area;

[0228] Calculation method of drug efficacy:

[0229]

[0230]

[0231] Table 7 Results of field efficacy test on soybean rust

[0232]

[0233] Field efficacy (see Table 7) showed that the overall efficacy of different treatments against soybean rust ranged from 61.71% to 86.76% 14 days after the second application. Four fungicide combinations containing fluopoxam, prothioconazole, and difenoconazole exhibited the best efficacy, with efficacy rates of 86.76%, 88.30%, 83.80%, and 80.85%, respectively. These efficacy rates were superior to those of the control treatments: 15% fluopoxam-prothioconazole water-dispersible granules (2:3), 14% fluopoxam-difenoconazole suspension concentrate (7:5), 24% prothioconazole-difenoconazole suspension concentrate (3:5), 300 g / L fluopoxam suspension concentrate, 480 g / L prothioconazole suspension concentrate, and 10% difenoconazole water-dispersible granules.

[0234] Example 6: Field efficacy test on wheat powdery mildew and wheat stripe rust

[0235] Experimental location: The experiment was conducted in a wheat field in Ceshan Town, Luozhuang District, Linyi City, Shandong Province. The terrain of the experimental site was relatively flat, and the cultivation conditions of all experimental plots were uniform and consistent, in line with local scientific agricultural practices. Protective rows were set between the treatments in each plot.

[0236] Test target diseases: wheat powdery mildew and wheat stripe rust.

[0237] Test agents: 20% fluopicolide, prothioconazole, difenoconazole water dispersible granules (4% + 6% + 10%) (2:3:5), 32% fluopicolide, prothioconazole, difenoconazole wettable powder (8% + 9% + 15%) (8:9:15), 17.5% fluopicolide, prothioconazole, difenoconazole suspension concentrate (3.5% + 7% + 7%) (1:2:2), 17.6% fluopicolide, prothioconazole, Difenoconazole dispersible oil suspension concentrate (4.4% + 8.8% + 4.4%) (1:2:1), 15% fluopoxadil-prothioconazole water dispersible granules (2:3), 14% fluopoxadil-difenoconazole suspension concentrate (7:5), 24% prothioconazole-difenoconazole suspension concentrate (3:5), 300 g / L fluopoxadil suspension concentrate, 480 g / L prothioconazole suspension concentrate, 10% difenoconazole water dispersible granules, and a water control.

[0238] Experimental design: There are 11 treatments in the experiment, and each treatment plot is 30m 2 Each treatment was repeated 4 times, and the plots were arranged in random blocks.

[0239] Application method: The first application of pesticide was carried out on April 15, 2022, and the second application was carried out on May 11. During the application, a 3WBD-16 electric sprayer was used to evenly spray the wheat plants.

[0240] Investigation method: The control effect of each pesticide treatment on powdery mildew and stripe rust was investigated 20 days after the second application of pesticides. Sampling was carried out at 5 fixed points on the diagonal of each plot, 20 plants were investigated at each point, and the top 3 leaves of each plant were investigated. The disease index and control effect were calculated based on the percentage of the lesion area on each leaf to the total leaf area.

[0241] Grading method:

[0242] Level 0: no disease;

[0243] Level 1: The lesion area accounts for less than 5% of the entire leaf area;

[0244] Level 3: The lesion area accounts for 6% to 25% of the entire leaf area;

[0245] Level 5: The lesion area accounts for 26% to 50% of the entire leaf area;

[0246] Level 7: The lesion area accounts for 51% to 75% of the entire leaf area;

[0247] Level 9: The lesion area accounts for more than 76% of the entire leaf area;

[0248] Calculation method of drug efficacy:

[0249]

[0250]

[0251] Table 8 Field efficacy test results of wheat powdery mildew and wheat stripe rust

[0252]

[0253]

[0254] Field efficacy shows (see Table 8): The fungicidal composition of the present invention has good control effects on wheat rust and wheat powdery mildew. 20 days after the second application, the overall control efficacy of each treatment field is above 80%.

[0255] Example 7: Field efficacy test on corn gray leaf spot

[0256] Test location: The test was conducted in Hongta Town, Fang County, Hubei Province. The test site is flat, with deep soil and above-average soil fertility.

[0257] Test target: Corn gray leaf spot.

[0258] Test agents: 25.4% fluopicolide, prothioconazole, difenoconazole water dispersible granules (6% + 8.4% + 11%) (6:8.4:11), 32% fluopicolide, prothioconazole, difenoconazole wettable powder (8% + 9% + 15%) (8:9:15), 24% fluopicolide, prothioconazole, difenoconazole suspension concentrate (4% + 8% + 12%) (1:2:3), 17.6% fluopicolide, prothioconazole Azoles·difenoconazole dispersible oil suspension concentrate (4.4%+8.8%+4.4%) (1:2:1), 15% fluopicolide·prothioconazole water dispersible granules (2:3), 14% fluopicolide·difenoconazole suspension concentrate (7:5), 24% prothioconazole·difenoconazole suspension concentrate (3:5), 300 g / L fluopicolide suspension concentrate, 480 g / L prothioconazole suspension concentrate, 10% difenoconazole water dispersible granules, and clean water control.

[0259] Experimental design: The experimental plots were randomly arranged in blocks, with each plot covering an area of ​​30m 2 Each treatment was repeated 4 times, and the treatment area with only water was used as a blank control.

[0260] Application time: The first application was conducted on July 7, 2022, and the second application was conducted on July 17, 2022, for a total of 2 applications. The application rate was 675L / hm2. 2 The amount of liquid medicine is converted into the amount of medicine used in each plot and sprayed evenly on the front and back of the corn leaves.

[0261] Survey Method: The control efficacy survey was conducted 14 days after the second application, according to GB / T 17980.107-2004, "Guidelines for Field Efficacy of Pesticides (II) Part 107: Control of Corn Large and Small Leaf Spots with Fungicides." Five random sampling points were selected from each plot, and all leaves of five plants were surveyed at each point. Disease index and control efficacy were calculated using the following grading method, with each leaf being the survey unit.

[0262] Grading method:

[0263] Level 0: no disease;

[0264] Level 1: The lesion area accounts for less than 5% of the entire leaf area;

[0265] Level 3: The lesion area accounts for 6% to 10% of the entire leaf area;

[0266] Level 5: The lesion area accounts for 11% to 25% of the entire leaf area;

[0267] Level 7: The lesion area accounts for 26% to 50% of the entire leaf area;

[0268] Level 9: The lesion area accounts for more than 51% of the entire leaf area;

[0269] Calculation method of drug efficacy:

[0270]

[0271]

[0272] Table 9 Results of field efficacy test on corn gray leaf spot

[0273]

[0274] The field efficacy showed (see Table 9): the overall efficacy of different pesticides in controlling corn gray leaf spot was 63.05% to 89.14% 14 days after the second application of the pesticide. Among them, the four ternary fungicide compositions of 25.4% fluopicolide·prothioconazole·fenpropimorph water dispersible granules (6%+8.4%+11%), 32% fluopicolide·prothioconazole·fenpropimorph wettable powder (8%+9%+15%), 24% fluopicolide·prothioconazole·fenpropimorph suspension concentrate (4%+8%+12%) and 17.6% fluopicolide·prothioconazole·fenpropimorph dispersible oil suspension concentrate (4.4%+8.8%+4.4%) showed better control effects, with control efficiencies of 89.14%, 83.37%, 86.33% and 81.45% respectively, which were better than the control binary compound composition and single agent.

[0275] The fungicidal composition or formulation obtained by the present invention exhibits significant synergistic effects, outperforming single agents in delaying the development of drug resistance and prolonging the duration of efficacy. Furthermore, no phytotoxicity to crops was observed with the combined formulation during field efficacy trials, demonstrating that the improved synergistic fungicidal efficacy of the resulting fungicidal composition or formulation can reduce production and usage costs and is safe for crops.

[0276] Although the present invention has been described in detail above using general descriptions and specific implementation plans, it is obvious to those skilled in the art that some modifications or improvements can be made thereto based on the present invention. Therefore, these modifications or improvements made without departing from the spirit of the present invention shall fall within the scope of protection claimed by the present invention.

Claims

1. A fungicidal composition containing prothioconazole for preventing and controlling plant diseases, characterized in that: The fungicidal composition comprises active ingredient A, active ingredient B and active ingredient C, wherein the active ingredient A is fluopyrab, the active ingredient B is prothioconazole, and the active ingredient C is difenoconazole. The mass ratio of the active ingredient A to the active ingredient B to the active ingredient C is 1:2:2, 1:2:3, 2:3:4, 2:3:5, 6:8.4:11, 8:9:15, and 2:5:

10. The plant diseases are soybean purple leaf spot, corn gray leaf spot, cucumber target leaf spot, soybean rust, and wheat powdery mildew.

2. The use according to claim 1, characterized in that Taking the total weight of the bactericidal composition as 100%, the sum of the active ingredients accounts for 1% to 80% of the total weight of the bactericidal composition.

3. The use according to claim 1, characterized in that In addition to the active ingredients, the fungicidal composition also contains other auxiliary ingredients on the pesticide, and the auxiliary ingredients are selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoaming agents, solvents, preservatives, stabilizers, synergists or carriers.

4. The use according to claim 1, characterized in that The bactericidal composition can be prepared into a solid preparation or a liquid preparation. The solid preparation is a wettable powder or a water-dispersible granule, and the liquid preparation is a suspension, an aqueous emulsion or an emulsifiable concentrate.

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