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CN115067340B - Sterilization composition, preparation method and application thereof - Google Patents

Sterilization composition, preparation method and application thereof Download PDF

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Publication number
CN115067340B
CN115067340B CN202110269432.2A CN202110269432A CN115067340B CN 115067340 B CN115067340 B CN 115067340B CN 202110269432 A CN202110269432 A CN 202110269432A CN 115067340 B CN115067340 B CN 115067340B
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Prior art keywords
bactericide
fluazinam
composition
preparation
mass
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CN115067340A (en
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李义涛
梁任龙
刘新烁
刘杨润琪
陈锦昌
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Dongguan Hec Pesticides R&d Co ltd
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Dongguan Hec Pesticides R&d Co ltd
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G13/00—Protection of plants
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G7/00—Botany in general
    • A01G7/06—Treatment of growing trees or plants, e.g. for preventing decay of wood, for tingeing flowers or wood, for prolonging the life of plants
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/647—Triazoles; Hydrogenated triazoles
    • A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles

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  • Life Sciences & Earth Sciences (AREA)
  • Environmental Sciences (AREA)
  • Wood Science & Technology (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Zoology (AREA)
  • Dentistry (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Agronomy & Crop Science (AREA)
  • Biodiversity & Conservation Biology (AREA)
  • Ecology (AREA)
  • Forests & Forestry (AREA)
  • Botany (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention relates to a bactericidal composition, a preparation method and application thereof. In particular, the present invention relates to compositions, formulations comprising fluazinam (fungicide a) and triazole sulfonamide fungicides (fungicide B), as well as methods for their preparation and use. Wherein the bactericide B is at least one or a combination of the bromacil and the cyfluconazole. The synergistic effect of fluazinam and epoxiconazole or fluazinam and cyfluconazole is utilized to enlarge the sterilization spectrum, delay the generation of drug resistance and reduce the production and use cost. The composition and the preparation of the invention are mainly used for preventing and treating late blight, downy mildew, powdery mildew, gray mold, scab, rice blast, sheath blight, scab, leaf spot and/or target spot of cereal crops, melons and fruits and/or vegetable crops.

Description

Sterilization composition, preparation method and application thereof
Technical Field
The invention relates to the technical field of pesticides, in particular to a bactericidal composition, a preparation and a preparation method and application thereof, and more particularly relates to a composition and a preparation comprising fluazinam (bactericide A) and at least one triazole sulfonamide bactericide (bactericide B) selected from bromcyclazole or cyflufenazole, and application of the composition or the preparation thereof in preventing and treating plant-related diseases caused by fungi and a method for preventing and treating plant diseases.
Background
The bromacil is triazole sulfonamide bactericide which is created by Dongyang optical pesticide research and development limited company in Dongguan city of Guangdong, has excellent prevention effect on potato late blight and cucumber downy mildew, has very high activity on free spores of germs, and is a medicament mainly for prevention. The medicine has strong lasting effect, is resistant to rain water, and has stable effect on various diseasesAnd (5) fruits. Chemical name: n (N) 3 - (3-bromobenzyl) -N 3 -cyclopropyl-N 1 ,N 1 -dimethyl-1H-1,2,4-triazole-1,3-disulfonamide, english name: n (N) 3 -(3-bromobenzyl)-N 3 -cyclopropyl-N 1 ,N 1 -dimethyl-1H-1,2,4-triazole-1,3-disulfonamide; CAS accession number: 2247022-00-8, which has the following structural formula:
the cyflufenamid is triazole sulfonamide bactericide created by Dongyang optical pesticide research and development limited company in Dongguan city of Guangdong, has excellent prevention effect on potato late blight and cucumber downy mildew, and has good lasting effect and rain resistance. Chemical name: n (N) 3 -cyclopropyl-N 1 ,N 1 -dimethyl-N 3 - (3- (trifluoromethyl) benzyl) -1H-1,2,4-triazole-1,3-disulfonamide, english name: n (N) 3 -cyclopropyl-N 1 ,N 1 -dimethyl-N 3 - (3- (trifluoromethyl) benzyl) -1H-1,2,4-triazole-1,3-disulfonamide; the structural formula is as follows:
fluazinam is a pyridine amine derivative, and dinitroaniline bactericide, and is a broad-spectrum efficient protective bactericide. Is very effective against alternaria, phytophthora, uniaxial mould, sclerotinia and black fungus. Has good effect on Botrytis cinerea of anti-benzimidazole and dicarboximide bactericides and also has good effect on rice damping-off caused by rhizopus. Fluazinam is extremely rain wash resistant and has long residual effect period. In addition, the feed additive has the function of controlling phytophagous mites. Chemical name: 3-chloro-N- (3-chloro-2, 6-dinitro-4- (trifluoromethyl) phenyl) -5- (trifluoromethyl) pyridin-2-amine; english name: 3-chloro-N- (3-chloro-2, 6-dinitr-4- (trifluoromethyl) phenyl) -5- (trifluoromethyl) pyridin-2-amine, CAS registry number: 79622-59-6, the structural formula of fluazinam is:
The chemical agent is an effective means for preventing and treating potato late blight. The current potato late blight has stronger and stronger resistance to pesticides, so that the use amount of pesticides is increased year by year, and the pollution to the environment is more and more serious.
Therefore, rational use of pesticides and preparation of formulated fungicides to expand the spectrum of fungicides and reduce disease resistance have been urgent.
Disclosure of Invention
The invention aims to provide a composition, and the pharmacodynamic active components of the composition comprise fluazinam (bactericide A) and triazole sulfonamide bactericides (bactericide B), so that the problems of overhigh dosage and insufficient control effect in the prior art are solved, and the composition has the effects of wider bactericidal spectrum, higher quick acting performance, longer lasting period and the like.
The invention also aims to provide a preparation which is wide in preparation type, can solve the problems of overhigh dosage and insufficient prevention effect in the prior art, and can achieve the effects of expanding a sterilization spectrum, improving quick acting performance and prolonging the lasting period.
In order to achieve the above object, the present invention provides the following technical solutions:
in a first aspect, the present invention provides a composition comprising a pharmaceutically active ingredient: a bactericide A and a bactericide B; wherein the bactericide A is fluazinam and the bactericide B is triazole sulfonamide bactericide.
In some embodiments, the present invention provides a composition wherein the pharmaceutically active components are bactericide a and bactericide B; wherein the bactericide A is fluazinam and the bactericide B is triazole sulfonamide bactericide.
In some embodiments, the germicide B is selected from at least one of bromconazole and cyfluconazole, or a combination thereof.
In some embodiments, the mass ratio of the bactericide A to the bactericide B in the composition is (1-20): 20-1;
preferably, the mass ratio of the bactericide A to the bactericide B in the composition is (1-15): 20-1;
preferably, the mass ratio of the bactericide A to the bactericide B in the composition is (1-15): 15-1;
preferably, the mass ratio of the bactericide A to the bactericide B in the composition is (1-10): 10-1;
preferably, the mass ratio of the bactericide A to the bactericide B in the composition is (1-10): 5-1;
preferably, the mass ratio of the bactericide A to the bactericide B in the composition is (1-5): 3-1;
more preferably, the mass ratio of the bactericide A to the bactericide B in the composition is (1-3): 2-1.
Specifically, the mass ratio of the bactericide A to the bactericide B in the composition is 1:20, 1:15, 1:10, 1:5, 1:3, 1:2, 1:1, 2:1, 3:1, 5:1, 10:1, 15:1 or 20:1. In the invention, the composition has synergistic bactericidal effect when the mass ratio of the bactericide A to the bactericide B is in the above range.
Further, the mass ratio of fluazinam to bromcycloxaprid in the composition of the invention is 1:20, 1:15, 1:10, 1:5, 1:3, 1:2, 1:1, 2:1, 3:1, 5:1, 10:1, 15:1 or 20:1; the mass ratio of fluazinam to cyflufenamid in the composition is 1:20, 1:15, 1:10, 1:5, 1:3, 1:2, 1:1, 2:1, 3:1, 5:1, 10:1, 15:1 or 20:1.
In some embodiments, the total content of germicide a and germicide B in the composition is 1 to 90 mass%;
preferably, the total content of the bactericide a and the bactericide B in the composition is 10 to 70 mass%;
preferably, the total content of the bactericide a and the bactericide B in the composition is 10 to 60 mass%;
preferably, the total content of the bactericide a and the bactericide B in the composition is 10 to 50 mass%;
more preferably, the total content of the bactericide a and the bactericide B in the composition is 12 to 50% by mass.
Specifically, the total content of the bactericide a and the bactericide B in the composition is 12 mass%, 22 mass%, 30 mass%, 32 mass%, or 50 mass%. In the present invention, when the total content of the bactericide a and the bactericide B in the composition is within the above-described range, the synergistic effect of sterilization is further enhanced.
Further, the total content of fluazinam and epoxiconazole in the composition is 12% by mass, 22% by mass, 30% by mass, 32% by mass, or 50% by mass; alternatively, the total content of fluazinam and cyflufenamid in the composition is 12% by mass, 22% by mass, 30% by mass, 32% by mass or 50% by mass.
The composition of the invention may contain, in addition to the pharmaceutically active component, an agrochemically acceptable adjuvant, which is an auxiliary substance added during the processing or use of the agrochemical formulation for improving the physicochemical properties of the pharmaceutical formulation, which itself is substantially biologically inactive but can affect the control effect. The auxiliary agent may include at least one of a wetting agent, a dispersing agent, an emulsifying agent, a thickening agent, a disintegrating agent, an antifreezing agent, an antifoaming agent, a solvent, a preservative, a stabilizer, a synergist, a carrier, and the like, and the above auxiliary agent may be appropriately added according to the needs of the composition, and may be changed according to circumstances, and is not particularly limited.
Preferably, the wetting agent is selected from one or more of alkylphenol ethoxylates (e.g., nonylphenol ethoxylate, octylphenol ethoxylate, dodecylphenol ether, dinonylphenol ether, mixed alkylphenol ether, etc.), fatty acid or fatty acid ester sulfates, alkyl naphthalene sulfonates (e.g., sodium dibutylnaphthalene sulfonate, sodium isopropylnaphthalene sulfonate), alkylbenzene sulfonates (e.g., sodium dodecylbenzene sulfonate, calcium dodecylbenzene sulfonate), alkyl sulfates and lignin sulfonates (e.g., sodium lignin sulfonate, calcium lignin sulfonate), etc. Suitable wetting agents areOTB (dioctylsulfo)Succinate salt),>EFW (alkylated naphthalene sulfonate),>BX (alkylated naphthalenesulfonate), GY-WS10 or Galoryl->804 (alkylated naphthalene sulfonate).
The dispersing agent is selected from one or more of naphthalene sulfonate, naphthalene sulfonate formaldehyde condensate, lignin sulfonate, alkylbenzene sulfonate, alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, high molecular polycarboxylate, alkylbenzene polyoxyethylene ether, ethylene oxide propylene oxide, EO-PO block copolymer, block polyether, organic phosphate and the like. For wettable powder formulations, a common dispersant is sodium lignin sulfonate (sodium lignosulphonate). For suspension concentrates, polyelectrolytes (polyelectrolytes) such as sodium naphthalene sulfonate formaldehyde condensate (sodium naphthalene sulphonate formaldehyde condensate) are used to obtain adsorption and stabilization. Tristyrylphenol ethoxylate phosphate (tristyrylphenol ethoxylate phosphate ester) was also used. Suitable dispersants are 2700、2500、2510、YUS-EP60P、SP-3498D、4894. Ufoxane NA, morwet D425, GY-900, GY-D800, antrox B/848, morwet D-425 or Ethylan NS-500LQ.
The emulsifier is selected from one or more of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene polyoxypropylene ether, fatty amine, ethylene oxide adduct of fatty amide, fatty acid polyoxyethylene ester, castor oil ethylene oxide adduct and derivatives thereof, abietic acid ethylene oxide adduct and analogues, polyalcohol fatty acid and ethylene oxide adduct thereof, polyoxyethylene polyoxypropylene block copolymer and the like. Suitable emulsifiers are lignin A, 3A high purity modified sodium ligninsulins, agro-emulsion 500#, agro-emulsion 601#, agro-emulsion 602#, agro-emulsion 700#, agro-emulsion 1601#, agro-emulsion 1602#, SP-OF3462, TERMUL2507, TERMULR 3016, EMULMON CO-360 or Ethylan 992.
The thickening agent is one or more selected from white carbon black, kaolin, bentonite, xanthan gum, acacia, polyacrylic acid, sodium carboxymethyl cellulose and the like.
The disintegrating agent is one or more selected from urea, modified starch, bentonite, aluminum chloride, ammonium sulfate, succinic acid, sodium bicarbonate and the like.
The antifreezing agent is one or more selected from glycerol, ethylene glycol, propylene glycol and the like.
The defoamer is selected from silicone defoamer (such as ETXP-40), C 8-10 One or more of fatty alcohol defoamer, polyurea, polyethylene glycol fatty acid ester, and the like.
The solvent is one or more of toluene, xylene, cyclohexanone, aromatic hydrocarbon solvent, methanol, ethyl acetate, soybean oil, epoxidized soybean oil, castor oil, corn oil, epoxidized corn oil, methyl oleate, rapeseed oil, N-octyl pyrrolidone and the like.
The preservative is one or more selected from sodium benzoate, benzoic acid, potassium sorbate, pinus koraiensis and the like.
The stabilizer is one or more selected from phosphoric acid, pyrophosphoric acid, phthalic acid, benzoic acid, triphenyl phosphite, acetic anhydride, epichlorohydrin, magnesium aluminum silicate, resorcinol, sodium citrate and the like.
The synergist has no bioactivity, but can inhibit detoxication enzyme in organism, and can greatly improve pesticide toxicity and pesticide effect when mixed with certain pesticides, such as one or more of synergistic phosphorus, synergistic ether, etc.
The carrier is selected from one or more of kaolin, clay, talc, chalk, quartz, attapulgite, montmorillonite, diatomaceous earth, silica, alumina, natural or artificial silicate, resin, wax, solid fertilizer, water, alcohol (especially butanol), organic solvent, mineral oil and vegetable oil and derivatives thereof, etc.
In addition, if appropriate, further additional components may also be present, such as protective colloids, binders, adhesives, thixotropic substances, penetrants, chelating agents, complexing agents, colorants, etc. In general, the pharmaceutically active component may be combined with any solid or liquid additive commonly used for formulation purposes.
In a second aspect, the present invention provides a formulation, wherein the formulation is prepared from the composition of the present invention.
In some embodiments, the mass ratio of the bactericide A to the bactericide B in the preparation is (1-20): 20-1;
preferably, the mass ratio of the bactericide A to the bactericide B in the preparation is (1-15): 20-1;
preferably, the mass ratio of the bactericide A to the bactericide B in the preparation is (1-15) (15-1);
preferably, the mass ratio of the bactericide A to the bactericide B in the preparation is (1-10): 10-1;
preferably, the mass ratio of the bactericide A to the bactericide B in the preparation is (1-10): 5-1;
preferably, the mass ratio of the bactericide A to the bactericide B in the preparation is (1-5): 3-1;
More preferably, the mass ratio of the bactericide A to the bactericide B in the preparation is (1-3): 2-1.
Specifically, the mass ratio of the bactericide A to the bactericide B in the preparation provided by the invention is 1:20, 1:15, 1:10, 1:5, 1:3, 1:2, 1:1, 2:1, 3:1, 5:1, 10:1, 15:1 or 20:1. In the invention, the mass ratio of the bactericide A and the bactericide B in the preparation is within the above range, and the bactericidal synergistic effect is achieved.
Further, the mass ratio of fluazinam to bromcycloxaprid in the preparation of the invention is 1:20, 1:15, 1:10, 1:5, 1:3, 1:2, 1:1, 2:1, 3:1, 5:1, 10:1, 15:1 or 20:1; alternatively, the mass ratio of fluazinam to cyflufenamid in the formulation of the invention is 1:20, 1:15, 1:10, 1:5, 1:3, 1:2, 1:1, 2:1, 3:1, 5:1, 10:1, 15:1 or 20:1.
In some embodiments, the total content of germicide a and germicide B in the formulation is 1 to 90 mass%;
preferably, the total content of the bactericide A and the bactericide B in the preparation is 10 to 70 mass%;
preferably, the total content of the bactericide A and the bactericide B in the preparation is 10 to 60 mass%;
preferably, the total content of the bactericide A and the bactericide B in the preparation is 10 to 50 mass%;
More preferably, the total content of the bactericide a and the bactericide B in the preparation is 12 to 50% by mass.
Specifically, the total content of the bactericide a and the bactericide B in the preparation is 12 mass%, 22 mass%, 30 mass%, 32 mass%, or 50 mass%. In the present invention, when the total content of the bactericide a and the bactericide B in the preparation is within the above-described range, the synergistic effect of sterilization is further enhanced.
Further, the total content of fluazinam and epoxiconazole in the formulation is 12% by mass, 22% by mass, 30% by mass, 32% by mass, or 50% by mass; alternatively, the total content of fluazinam and cyflufenamid in the formulation is 12%, 22%, 30%, 32% or 50% by mass.
In some embodiments, the compositions and/or formulations comprising bactericide a and bactericide B provided by one or more embodiments of the present invention may be used as such or in the form of their formulations or use forms prepared therefrom according to their respective physical and/or chemical properties, such as aerosols, capsule suspensions, cold fogging concentrates, hot fogging concentrates, encapsulated particles, fine particles, flowable concentrates for treating seeds, ready-to-use solutions, sprayable powders, emulsifiable concentrates, oil-in-water emulsions, water-in-oil emulsions, large particles, microparticles, oil-dispersible powders, oil-soluble flowable concentrates, oil-soluble liquids, foams, pastes, pesticide-coated seeds, suspension concentrates, suspoemulsion concentrates, soluble concentrates, suspensions, wettable powders, soluble powders, powder and granule seed coatings, dosages, smoke, water-soluble particles or tablets, water-soluble powders for treating seeds, wettable powders impregnated with active compounds, product and synthetic substances and micro-encapsulated as well as in thermally fogging formulations in natural and synthetic substances, v. Typical formulation dosage forms include powders, wettable powders, microcapsules, water dispersible granules, water aquas, suspensions, emulsifiable concentrates, microemulsions, aqueous emulsions, ultra-low volume sprays, seed coatings and/or smoke agents.
Powders (DP) are compositions to which an amount of inert powders, such as clay, kaolin, talc, etc., is added, and which are mechanically processed to a powder with a particle diameter of less than 100 μm.
Wettable Powders (WP) refer to a mixture of the composition in a certain proportion with a suitable surfactant and inert material (kaolin powder). Wettable powders are formulations which disperse homogeneously in water and which contain, in addition to the active ingredient and inert substances (kaolin powder), a certain amount of anionic or nonionic surfactants (dispersants, wetting agents).
The Microcapsule (MC) is prepared by coating the composition in an adhesive, a film forming agent and the like to form a tiny capsule preparation, and then processing the tiny capsule preparation into a required dosage form; the suspension is divided into microcapsule suspending agents (Capsule Suspensions, CS), microcapsule granules (Encapsulated Granule, CG), microcapsule dry suspending agents (Capsulated Dry Flowable, CDF) and the like.
Water-dispersible (particulate) agent (WDG) refers to a mixture of the composition in a certain proportion with a suitable surfactant and inert material (kaolin powder). The powder fineness meets the requirement by air current crushing, and the products are mixed uniformly by using a double-screw mixer and a coulter mixer for multiple times, and then the products are granulated by conventional methods such as fluidized bed granulation, spray granulation and disk granulation.
Granules (GR) refer to a mixture of the composition in a certain proportion with suitable surfactants, diluents and inert substances (kaolin powder). The granulation by a granulator, for example, a fluidized bed granulation method, is a granulation method in which a binder solution is sprayed while the powder is kept in a fluidized state, and the powder is coagulated. The method comprises the steps of mixing, kneading, granulating, drying, classifying and the like in one device, and completing the steps in a closed state for a short time.
The aqueous preparation (AS) is a liquid prepared directly from water by utilizing the characteristic that certain raw materials can be dissolved in water without decomposing.
The suspending agent (SC) is prepared by mixing the composition with proper surfactant, water or organic solvent according to a certain proportion, grinding the mixture uniformly by a colloid mill, and grinding the mixture for 1 to 2 times by a sand mill to a certain fineness.
An oil suspension (OD/OF) is a suspension liquid formulation in which a solid pesticidal active ingredient, insoluble in an oil solvent, is dispersed in a non-aqueous medium (i.e., oil) and is highly dispersed and stabilized by means OF a surfactant. The oil suspending agent is divided into water dispersion use and oil-based medium dispersion use according to the use mode. The oil suspending agent is dispersed in water and used in an OD; the oil suspension formulation for dispersion in an oil-based medium is OF.
Emulsifiable Concentrates (EC) are prepared by dissolving the composition in an organic solvent such as benzene, toluene, xylene, cyclohexanone in a certain proportion and adding a certain amount of a mixture of anionic or nonionic surfactants (emulsifiers).
Microemulsions (ME) generally consist of liquid pesticides, surfactants (emulsifiers), water, stabilizers, etc.; it is characterized by using water as medium, and containing no or less organic solvent. The droplet size in microemulsions is typically from a few nanometers to tens of nanometers, less than a quarter of the wavelength of visible light.
An aqueous Emulsion (EW) is a pesticide formulation in which a water-insoluble liquid of a crude drug or a solution of the crude drug in a water-insoluble organic solvent is dispersed in water. The aqueous emulsion is a preparation prepared by dispersing a liquid pesticide raw material prepared by mixing the aqueous emulsion with an organic solvent in water in small liquid drops of 0.5-1.5 mu m, and the appearance of the aqueous emulsion is milky milk-like liquid.
The ultra-low volume spray (ULV) is a liquid medicine sprayed on target crops, is sprayed in very fine mist drops with very low dosage, and is a special preparation for ultra-low volume spray application.
The seed coating agent (SD) is prepared by grinding and mixing the composition and the auxiliary agent, and can be directly coated on the surface of the seed or coated on the surface of the seed after dilution to form a protective film with certain strength and permeability.
Smoke agent (FU), also known as aerosol, is a medicament obtained by mixing a composition with a combustible substance or the like, and burning the mixture to gasify a pesticide and condense the gasified pesticide into smoke particles or directly disperse the pesticide into smoke particles.
Regarding the meaning of various adjuvants and various formulations, differences in understanding are caused by differences in expression. It should be understood that various adjuvants, formulations disclosed in the art are within the scope of the present invention, such as, for example, "pesticide formulation processing techniques", luoping, song Weiwei, chemical industry Press, 2015; pesticide formulation, wang Kaiyun, chinese agriculture press, 2009; modern pesticide formulation processing technical books, liu Anwen, chemical industry publishers, 2018; pesticide formulation and preparation and method of use, tu Yuqin, jindun Press, 2008; chinese pesticide, chinese pesticide industry Association; etc. as described in the foregoing. Methods of preparing the various formulations include, but are in no way limited to, those described herein.
The above-described formulations can be prepared in a known manner, for example by mixing the active compound or active compound combination with at least one additive. Suitable additives are all customary formulation auxiliaries, for example organic solvents, fillers, solvents or diluents, solid carriers and fillers, surfactants (for example adjuvants, emulsifiers, dispersants, protective colloids, wetting agents and adhesion promoters), dispersants and/or binders or fixatives, preservatives, dyes and pigments, defoamers, inorganic and organic thickeners, water repellents, if appropriate further drying and UV stabilizers, gibberellins and water and other processing aids. In each case, depending on the type of formulation to be prepared, other processing steps may be required, such as wet milling, dry milling or granulation.
The compositions of the present invention comprise not only ready-to-use compositions (which can be applied to plants or seeds with a suitable device) but also commercial concentrates (which must be diluted with water prior to use).
The above preferred formulation type composition can improve the physicochemical properties of the pharmaceutical agent, such as stability, uniformity, quick-acting property or sustained-release property, etc., and can also improve the control effect.
In a third aspect, the present invention provides the use of a composition according to the invention and/or a formulation according to the invention for controlling plant diseases caused by fungi.
Preferably, the plant disease comprises potato late blight, cucumber downy mildew, cucumber powdery mildew, cucumber gray mold, wheat scab, rice blast, rice sheath blight, pear scab, melon leaf spot and/or cucumber target spot.
Preferably, the potato late blight is caused by phytophthora infestans. The composition and/or the preparation show more remarkable synergistic effect for preventing and treating diseases caused by phytophthora infestans.
In a fourth aspect, the present invention provides a method of controlling plant diseases, the method comprising: an effective amount of the composition of the invention and/or the formulation of the invention is applied to the plant and/or plant part to be treated.
Preferably, the plant comprises cereal, melon and/or vegetable crops.
More preferably, the plant comprises potato, grape, cucumber, wheat, rice, pear, melon, corn, soybean, cotton, canola, sugar beet, sugarcane, and/or oat.
Further, the present invention provides a method for controlling plant diseases by applying the pharmaceutically active components fungicide a and fungicide B simultaneously, or separately, or sequentially to a plant or plant part to be treated.
The simultaneous application can be directly applied after uniformly mixing the pesticide active component bactericide A and the pesticide active component bactericide B, or can be applied after uniformly mixing the bactericide A and the bactericide B to prepare a preparation.
The respective applications may be performed by separately applying the pharmaceutically active component bactericide a and the pharmaceutically active component bactericide B, or may be performed by separately preparing the respective preparations of the bactericide a and the bactericide B.
The sequential administration may be performed by sequentially administering the pharmaceutically active component fungicide a and the pharmaceutically active component fungicide B, or may be performed sequentially after each of the fungicide a and the fungicide B is prepared into a formulation. In the sequential application, the bactericide a (pharmaceutically active component or formulation) may be applied first, followed by the bactericide B (pharmaceutically active component or formulation), or the bactericide B (pharmaceutically active component or formulation) may be applied first, followed by the bactericide a (pharmaceutically active component or formulation).
In practice, the compositions and/or formulations of the present invention may be used to treat all plants and/or plant parts. Plants refer to all plants and plant populations, such as desired and undesired wild plants, cultivars and plant varieties (whether or not protected by plant variety rights or plant breeding rights). Cultivars and plant varieties may be plants obtained by conventional breeding and breeding methods (assisted or complemented by one or more biotechnological methods, for example by the use of doubled haploids, protoplast fusion, random and directed mutagenesis, molecular markers or genetic markers), or by methods of biological and genetic engineering. Plant parts refer to all above-and below-ground parts and organs of plants, where for example shoots, leaves, flowers and roots, for example leaves, needles, stems, branches, flowers, fruit bodies, fruits and seeds, and roots, bulbs and rhizomes are listed. Crops as well as vegetative and generative propagation material, for example cuttings, bulbs, rhizomes, berberis and seeds, also belong to the plant parts.
In the present invention, the term "effective amount" refers to the total amount of each active ingredient in an amount sufficient to exhibit the desired control effect. Such amounts vary widely depending on the fungus to be controlled, the plant species, the climatic conditions and the compounds contained in the composition of the invention.
In the present invention, the terms "comprising," "including," or "containing" are open-ended, i.e., to include what is specified in the present invention, but not to exclude other aspects.
In the present invention, "control" means prevention and/or treatment.
The treatment of plants and/or plant parts with the compositions and/or formulations provided by the invention can be carried out directly or by acting on their surroundings, habitat or storage area using conventional treatment methods, for example by dipping, spraying, atomizing, irrigating, evaporating, dusting, atomizing, broadcasting, foaming, painting, coating, watering (pouring), instilling, and in the case of propagation material, in particular in the case of seeds, also by coating the seed with a coating or coatings, etc., treating dry seed with a powder, treating seed with a solution, treating the slurry with a water-soluble powder. The composition or formulation may also be applied to the soil.
The invention also provides a method for treating seeds. The compositions and/or formulations of the present invention may be administered directly, i.e., without the inclusion of other components and without dilution. In general, it is preferred to apply the composition of the present invention to seeds in a suitable formulation. Suitable formulations and methods for treating seeds are conventional in the art. The compositions of the present invention may be converted into conventional seed dressing formulations such as solutions, emulsions, suspensions, powders, foams, slurries or other coating materials for seeds, as well as ULV formulations.
In addition to the synergistic activity of the germicides, the compositions and/or formulations comprising germicides a and B provided by the present invention have other surprising properties which bring about effects beyond that actually expected, which properties may also be referred to as synergy in a broad sense. For example: reduced application rate, broader spectrum of activity, broader spectrum of sterilization, higher quick-acting, longer duration of action, increased activity, increased tolerance to high or low temperatures, increased tolerance to drought and/or to water and/or soil salt content, better plant growth, easier harvesting, earlier maturation, higher harvest yields, bigger fruits, more developed root systems, higher plant height, greener leaves, larger leaf area, higher flowering quality, stronger shoots, less seed demand, lower cereal toxicity, better compatibility with cereal crops, higher quality and/or higher nutritional value of the harvested products, higher sugar concentration in the fruits, better storage stability and/or processability of the harvested products; more importantly, the composition can play a role in synergy after being combined in proper proportion; meanwhile, the generation of drug resistance can be delayed, the safety of crops is improved, the drug cost is reduced due to the combination of two pesticides, and the labor force is saved.
In summary, compared with the prior art, the invention has at least one of the following technical effects:
(1) The combination of the bactericide A and the bactericide B plays a role in synergy, and has certain quick-acting property and long-acting property;
(2) The generation of drug resistance is delayed, and the safety of crops is improved;
(3) The dosage is reduced, and the cost and labor consumption are reduced;
(4) The sterilization spectrum is enlarged.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.
The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. In the following examples, the original bromconazole and the original cyfluconazole are self-made, and the bromconazole is prepared by referring to the preparation method of example 8 in PCT/CN 2018/081979; the cyflufenamid is prepared by referring to the preparation method of the example 12 in the application No. PCT/CN 2019/108170; the fluazinam crude drug was purchased from the company of pesticide industry, inc. of Liantai, shandong province. The other reagents or instruments used are not identified to the manufacturer and are conventional products prepared by methods described in the prior art or obtained by commercial purchase.
Synthesis and characterization of cyflufenamid:
will N 3 - (3- (trifluoromethyl) benzyl) -N 1 ,N 1 dimethyl-1H-1, 2, 4-triazole-1, 3-disulfonamide (0.41 g,1.0 mmol), potassium carbonate (0.28 g,2.0 mmol) and N, N-dimethylformamide (10 mL) were added to a 100mL three-necked flask, and bromocyclopropane (0.24 g,2.0 mmol) was slowly added to the reaction system and reacted at room temperature for 8 hours; quench with water (20 mL), extract with ethyl acetate (15 ml×3), wash the organic phase with saturated brine, dry over anhydrous magnesium sulfate, filter, remove the solvent under reduced pressure from the filtrate with a rotary evaporator, purify by column chromatography (ethyl acetate/petroleum ether (v/v) =1/3) to give 0.24g of white solid, yield: 53%.
1 H NMR(400MHz,CDCl 3 ):δ(ppm)8.76(s,1H),7.49-7.16(m,4H),3.82(s,2H),2.67(s,6H),1.36-1.32(m,1H),0.71-0.68(m,2H),0.22-0.19(m,2H)。
LC-MS:(M+1)m/z＝454.0。
Synthesis and characterization of bromocyclozole:
potassium carbonate (0.276 g,2.0 mmol), N 3 -cyclopropyl-N 1 ,N 1 dimethyl-1H-1, 2, 4-triazole-1, 3-disulfonamide (0.40 g,1.36 mmol), 1-bromo-3- (bromomethyl) benzene (0.48 g,2.0 mmol) and N, N-dimethylformamide (15 mL) were added to a 50mL three-necked flask, and the reaction was stirred at room temperature for 12 hours. Water (30 mL) was added, extracted with ethyl acetate (20 mL. Times.3), the organic phase was washed with saturated brine (10 mL), dried over magnesium sulfate, filtered, the solvent was removed from the filtrate under reduced pressure using a rotary evaporator, and the residue was purified by column chromatography (ethyl acetate/petroleum ether (v/v) =1/5) to give 0.287g of a white solid in 45% yield.
1 H NMR(400MHz,CDCl 3 )δ(ppm):8.63(s,1H),7.52(s,1H),7.44(d,J＝7.9Hz,1H),7.33(d,J＝7.7Hz,1H),7.21(t,J＝7.8Hz,1H),4.54(s,2H),3.08(s,6H),2.58-2.53(m,1H),0.87-0.83(m,2H),0.77-0.73(m,2H)。
LC-MS:(M+1)m/z＝464.0。
Indoor biological test
Determining the inhibition effect of different agents on potato late blight (Phytophthora infestans (Mont.) de Bary, strain source: single satellite teacher laboratory of university of North and forestry and agricultural science and technology) on hypha growth by hypha growth rate method, and calculating EC of each agent on pathogenic bacteria 50 Values.
Rye Medium (RSA) Medium: 60g of rye; 20g of sucrose; 15g of agar powder. Soaking rye in 200mL distilled water for 36h, filtering with 2 layers of gauze, and preserving filtrate; stirring rye for 2min, adding 400mL distilled water, filtering with 4 layers of gauze in water bath at 50deg.C for 3h, mixing the two filtrates, adding sucrose and agar powder, metering volume to 1000mL, and sterilizing with 121 deg.C high pressure steam for 15min.
The single dose or each composition (see Table 1 and Table 2) is dissolved in DMSO and diluted with 0.1wt% Tween 80 water to a suitable concentration gradient (5 mg/L, 2.5mg/L, 1.25mg/L, 0.625mg/L, 0.3125mg/L, 0.15625 mg/L) for use.
In an ultra-clean workbench, adding 5mL of sterilized sample (sterilization mode: ultraviolet sterilization) into 45mL of RSA culture medium (cooled to 45-50 ℃), uniformly mixing, pouring into a flat plate (diameter of 90 mm), cooling to ensure that the final concentration of the medicine contained in the flat plate is a certain gradient, and taking the RSA culture medium added with the same amount of sterile warm water as a control, wherein each treatment is repeated for 3 times.
The inoculated late blight bacteria blocks (diameter 6 mm) are picked up and placed in the center of a toxic culture plate and cultured in a constant temperature incubator at 20 ℃ for 10d. Colony diameters were measured by the crisscross method, and relative inhibition was calculated according to formulas (2.1) and (2.2).
Colony expansion diameter (mm) =colony diameter average (mm) -6 (mm) (2.1)
According toThe concentrations of each single agent and each composition and the corresponding relative inhibition rate are subjected to corresponding regression analysis to obtain the EC of each composition 50 Values and 95% confidence intervals.
The biometric score values are obtained from a look-up table based on the relative inhibition rate. And (3) taking the logarithm of the concentration as an abscissa, converting the inhibition percentage into a biological several-value according to a biological statistics machine value conversion table as an ordinate, and drawing a virulence regression equation. The mass concentration when the value of the equation is 5 is obtained to be EC 50 (Millot M,Girardot M,Dutreix L,et al..Antifungal and anti-biofilm activities of acetone lichen extracts against Candida albicans.[J].Molecules,2017,22(4):651.)。
And calculating the co-toxicity coefficient (CTC) of the mixture by adopting a co-toxicity coefficient method calculated by grand cloud Peel, and determining the synergy of the mixture.
With a single dose of the mixture as the standard agent (EC is usually selected 50 Lower), perform calculations:
toxicity index of single dose= (EC of standard dose 50 Certain single agent EC 50 )×100
Theoretical Toxicity Index (TTI) =toxicity index of a single dose×proportion of a single dose in mixture+toxicity index of B single dose×proportion of B single dose in mixture
Measured virulence index (ATI) = (EC of standard single dose 50 EC of value/mixture 50 Value) ×100
Co-toxicity coefficient (CTC) = (measured toxicity index/theoretical toxicity index) ×100
The compound has synergy (i.e., significantly improved over the simple addition of its single dose) when CTCs are greater than 120, antagonism when CTCs are less than 80, and additive effects between 80 and 120.
Table 1: determination results of co-toxicity coefficients of fluazinam and bromacil in different proportions on potato late blight
Table 2: determination results of co-toxicity coefficients of fluazinam and cyflufenamid to potato late blight in different ratios
From the results shown in tables 1 and 2, the compound bactericide taking fluazinam and epoxiconazole as the pharmaceutically active components and the compound bactericide taking fluazinam and epoxiconazole as the pharmaceutically active components have remarkable prevention and treatment effects on potato late blight when being compounded in different mass ratios. When the mass ratio of fluazinam to epoxiconazole is (1-15): 20-1, the co-toxicity coefficient is greater than 120, and the bactericidal composition has obvious synergistic effect on potato late blight; when the mass ratio of the fluazinam to the cyflufenamid is (1-15): 20-1, the co-toxicity coefficient is more than 120, and the composition has obvious synergistic effect on potato late blight, so that the composition of the fluazinam, the bromacil, the fluazinam and the cyflufenamid can be an ideal medicament for preventing and treating potato late blight.
Example 1:50% fluazinam bromocyclozole water dispersible granule (1:1)
25g of bromcyclozole original drug, 25g of fluazinam original drug, 5g of comb polycarboxylate dispersant (trade name: GY-D900, beijing Guangdong Yinong chemical Co., ltd.) 5g of calcium lignosulfonate (trade name: borderperse NA, nanjing Jie Russian technology Co., ltd.) 5g, 4g of ammonium sulfate, 0.4g of magnesium aluminum silicate, 0.1g of high-efficiency organic silicon defoamer and 100g of kaolin are added, the materials are pre-crushed and mixed uniformly, and then crushed to the required particle size through air current, and then granulated by adopting a rotary granulator, so that the fluazinam and bromcyclozole water dispersible granule with the active ingredient mass content of 50% is prepared.
Example 2:50% fluazinam-cyflufenamid water dispersible granule (1:1)
25g of cyflufenamid technical, 25g of fluazinam technical, 6g of comb polycarboxylate dispersant (trade name: HMK-D1008, beijing Han Moke chemical Co., ltd.) and 4g of sodium lignin sulfonate (trade name: ufoxane 3A, nanjing Jie Russian technology Co., ltd.), 4g of ammonium sulfate, 0.4g of magnesium aluminum silicate, 0.1g of high-efficiency organic silicon defoamer and 100g of kaolin are added, the materials are pre-crushed and mixed uniformly, and then the mixture is crushed into the required particle size by air flow, and then a rotary granulator is adopted for granulation, so that the fluazinam and cyflufenamid water dispersible granule with the active ingredient mass content of 50% is prepared.
Example 3:32% fluazinam bromocyclozole suspension (1:3)
1. Preparation of crushed pulp
Adding 2g of non-alkylphenol high-efficiency dispersant (trade name: TERSPERSE4894, huntsman) 2g, 2g of comb-structured high-molecular compound dispersant (trade name: GY-D900, beijing Guangyuan Yinong chemical Co., ltd.) 2g of wetting agent (trade name: GY-WS10, beijing Guangyuan Yinong Chemie Co., ltd.) 2g and 0.3g of high-efficiency silicone defoamer (trade name: ETXP-40, hangzhou left New Material Co., ltd.) to disperse 24g of bromcyclozole original drug and 8g of fluazinam original drug therein, usingGlass beads were wet-pulverized with a sand mill (Shenyang New micro motor plant) for 2.0 hours to obtain 80g of pulverized slurry.
2. Preparation of dispersion Medium
In 15.2g of water, 0.3g of xanthan gum (Aba Ding Shiji), 0.4g of magnesium aluminum silicate (Aba Ding Shiji), 4g of ethylene glycol (Aba Ding Shiji) and 0.1g of sodium benzoate (Aba Ding Shiji) were dispersed to obtain 20g of a dispersion medium.
3. Preparation of aqueous suspension pesticidal composition
80g of the crushed slurry and 20g of a dispersion medium were mixed to obtain 100g of an aqueous suspension-type agricultural chemical composition, and the suspension was subjected to high shear (4000 rpm) for 30 minutes in a high-speed disperser (trade name: TG25, german IKA) to obtain a fluazinam bromocyclozole suspension having an active ingredient content of 32% by mass.
Example 4:32% fluazinam-cyflufenazole suspension (1:3)
1. Preparation of crushed pulp
Adding polycarboxylate dispersant (trade name: dispersol 589, crain) 1.5g, comb-structured polymer dispersant (trade name: SP-SC3, jiangsu Qingqing chemical engineering Co., ltd.) 1.5g, wetting agent (trade name: GY-WS10, beijing Guangyuan Yinong chemical Co., ltd.) 4g and high-efficiency silicone defoamer (trade name: ETXP-40, hangzhou left New Material Co., ltd.) 0.3g into water, dispersing cyflupyrad 24g, fluazinam 8g therein, usingGlass beads were wet-pulverized with a sand mill (Shenyang New micro motor plant) for 2.0 hours to obtain 80g of pulverized slurry. />
2. Preparation of dispersion Medium
In 15.2g of water, 0.3g of xanthan gum (Aba Ding Shiji), 0.4g of magnesium aluminum silicate (Aba Ding Shiji), 4g of ethylene glycol (Aba Ding Shiji) and 0.1g of sodium benzoate (Aba Ding Shiji) were dispersed to obtain 20g of a dispersion medium.
3. Preparation of aqueous suspension pesticidal composition
80g of the crushed slurry and 20g of a dispersion medium were mixed to obtain 100g of an aqueous suspension-type agricultural chemical composition, and the suspension was subjected to high shear (4000 rpm) for 30 minutes in a high-speed disperser (trade name: TG25, german IKA) to obtain a fluazinam-cyflufenamid suspension having an active ingredient mass content of 32%.
Example 5:30% fluazinam bromocyclozole aqueous emulsion (5:1)
1. Oil phase preparation
5g of a bromcycloxaprid original drug and 25g of a fluazinam original drug are added into a mixed solvent of 9g of cyclohexanone (Aba Ding Shiji) and 7g of xylene (Aba Ding Shiji), and after being uniformly mixed by ultrasonic, 2g of an emulsifying agent (trade name: TERMOL 2507, huntsman) and 2g of castor oil polyoxyethylene ether (trade name: EMULMPON CO-360, ackerunobel) are added and slowly stirred until the mixture is completely dissolved.
2. Aqueous phase preparation
Ethylene glycol (Aba Ding Shiji) 4g, magnesium aluminum silicate (Aba Ding Shiji) 0.2g, a high-efficiency organic silicon defoamer (trade name: ETXP-40, hangzhou left soil New materials Co., ltd.) 0.1g and water 45.7g were added and stirred uniformly.
3. Pesticide composition aqueous emulsion formulation
The aqueous phase was slowly added to the oil phase and stirred until the addition was completed, and then subjected to high shear (4000 rpm) in a high speed disperser (trade name: TG25, germany IKA) for 30 minutes to prepare an aqueous emulsion of fluazinam bromocycloxaprid with an active ingredient content of 30% by mass.
Example 6:30% fluazinam-cyfluconazole aqueous emulsion (5:1)
1. Oil phase preparation
5g of cyflufenamid technical and 25g of fluazinam technical are added into a mixed solvent of 5g of cyclohexanone (Aba Ding Shiji) and 11g of a caproamide solvent (trade name: genagen 4296, kelain), and after ultrasonic mixing is carried out uniformly, 3g of an emulsifier (trade name: TERMOL 2507, huntsman) and 2g of castor oil polyoxyethylene ether (trade name: EMULMUPON CO-360, acinetobacter) are added and stirred slowly until complete dissolution is achieved.
2. Aqueous phase preparation
Ethylene glycol (Aba Ding Shiji) 4g, magnesium aluminum silicate (Aba Ding Shiji) 0.2g, a high-efficiency organic silicon defoamer (trade name: ETXP-40, hangzhou left soil New materials Co., ltd.) 0.1g and water 44.7g were added and stirred uniformly.
3. Pesticide composition aqueous emulsion formulation
The aqueous phase was slowly added to the oil phase and stirred until the addition was completed, and then subjected to high shear (4000 rpm) in a high speed disperser (trade name: TG25, germany IKA) for 30 minutes to prepare an aqueous emulsion of fluazinam-cyflufenamid having an active ingredient mass content of 30%.
Example 7:22% fluazinam bromocyclozole microemulsion (3:1)
16.5g of fluazinam active compound, 5.5g of bromocyclozole active compound, 10g of solvent xylene (Aba Ding Shiji), 5g of solvent cyclohexanone (Aba Ding Shiji), 9g of emulsifier phenethyl phenol polyoxyethylene ether (trade name: nongru 602#, chen Ji Yan Cheng chemical auxiliary Co., ltd.), 5g of emulsifier dodecylbenzene sulfonate (trade name: nongru 500#, chen Ji Yan Cheng chemical auxiliary Co., ltd.), 5g of antifreeze propylene glycol (Aba Ding Shiji) and 39g of water are weighed. And fully dissolving the cyproconazole and the fluazinam with a solvent, adding an emulsifier and an antifreezing agent, uniformly mixing, finally adding 5g of deionized water, and uniformly stirring to obtain the fluazinam and cyproconazole microemulsion with the active ingredient mass content of 22%.
Example 8:22% fluazinam-cyfluconazole microemulsion (3:1)
16.5g of fluazinam active compound, 5.5g of cyclofluconazole active compound, 12g of solvent caproamide solvent (trade name: ADMA 810, craien), 3g of solvent cyclohexanone (Aba Ding Shiji), 10g of emulsifier phenethyl phenol polyoxyethylene polyoxypropylene ether (trade name: agrocarum 1601#, chen table Yan Cheng chemical auxiliary Co., ltd.), 3g of emulsifier phenethyl phenol polyoxyethylene ether (trade name: agrocarum 500#, chen table Yan Cheng chemical auxiliary Co., ltd.), 5g of antifreeze propylene glycol (Aba Ding Shiji) and 39g of water are weighed. After the cyflufenamid and the fluazinam are fully dissolved by using a solvent, adding an emulsifier and an antifreezing agent, uniformly mixing, finally adding 6g of deionized water, and uniformly stirring to obtain the fluazinam and cyflufenamid microemulsion with the active ingredient mass content of 22%.
Example 9:12% fluazinam bromocyclozole dispersible oil suspension (2:1)
1. Preparation of the oil phase
15g OF an emulsifier (trade name: SP-OF3462, jiangsu qingyu) and 6g OF a polycarboxylate dispersant (trade name: SP-OF3498D, jiangsu qingyu chemical engineering Co., ltd.) were added to 63g OF methyl oleate (Ara Ding Shiji), and 8g OF fluazinam and 4g OF bromcycloxazole were added thereto after stirring and mixing, using Glass beads were wet-pulverized with a sand mill (Shenyang New micro motor plant) for 2.0 hours to obtain 96g of pulverized slurry.
2. Thickener composition formulation
2g of hydrophilic white carbon black (Aba Ding Shiji) and 2g of organic bentonite (Hangzhou left earth new materials Co., ltd.) are weighed and added into an oil phase to obtain 100g of oily suspension pesticide composition, and the oily suspension pesticide composition is subjected to high shear (4000 rpm) for 20 minutes by a high-speed dispersing machine (trade name: TG25, germany IKA) to obtain the fluazinam-bromconazole dispersible oil suspending agent with the active ingredient mass content of 12%.
Example 10:12% fluazinam-cyfluconazole dispersible oil suspension (2:1)
1. Preparation of the oil phase
Adding 18g of emulsifier (trade name: SUPER-3000, jinan Jinhe New Material Co., ltd.) into 63g of methyl oleate (Aba Ding Shiji), 3g of polycarboxylate dispersant (trade name: geropon Ultrasperse, sorpe vitamin), stirring and mixing, adding 8g of fluazinam original drug and 4g of cyfluconazole original drug, usingGlass beads were wet-pulverized with a sand mill (Shenyang New micro motor plant) for 2.0 hours to obtain 96g of pulverized slurry.
2. Thickener composition formulation
2g of hydrophilic white carbon black (Aba Ding Shiji) and 2g of organic bentonite (Hangzhou left earth new materials Co., ltd.) are weighed and added into an oil phase to obtain 100g of oily suspension pesticide composition, and the oily suspension pesticide composition is subjected to high shear (4000 rpm) for 20 minutes by a high-speed dispersing machine (trade name: TG25, germany IKA) to obtain the fluazinam-cyfluconazole dispersible oil suspending agent with the active ingredient mass content of 12%.
Example 11:30% fluazinam bromocycloxaprid emulsifiable concentrate (1:2)
10g of emulsifying agent (trade name: TERMULR 3016, huntsman) 10g, 10g of fluazinam raw material and 20g of bromcyclozole raw material are added into 60g of quinamide solvent (trade name: ARMID DM10, nanjun) and stirred fully in a warm water bath at 35 ℃ until the raw material is completely dissolved, thus obtaining the fluazinam-bromcyclozole emulsifiable concentrate with the active ingredient mass content of 30%.
Example 12:30% fluazinam-cyflufenamid emulsifiable concentrate (1:2)
15g of emulsifying agent (trade name: TERMULR 2507, huntsman) is added into 55g of quinamide solvent (trade name: ADMA 810, crain), 10g of fluazinam raw material, 20g of cyflufenamid raw material are fully stirred in a warm water bath at 35 ℃ until the raw material is completely dissolved, and the fluazinam-cyflufenamid emulsifiable concentrate with the mass content of the active ingredient of 30% is prepared.
Comparative example 1:50% fluazinam suspension
1. Preparation of crushed pulp
Dispersing non-alkylphenol type high-efficiency dispersant (trade name: TERSPERSE 4894, huntsman) 2g, comb-structured high-molecular compound dispersant (trade name: GY-D900, beijing Guangdong Yinong Chemie Co., ltd.) 1.5g, wetting agent (trade name: GY-WS10, beijing Guangdong Yinong Chemie Co., ltd.) 4g and high-efficiency silicone defoamer (Hangzhou left soil New Material Co., ltd.) 0.3g in water, dispersing fluazinam raw material 50g therein, using Glass beads were wet-pulverized with a sand mill (Shenyang New micro motor plant) for 1.5 hours to obtain 80g of pulverized slurry.
2. Preparation of dispersion Medium
In 15.2g of water, 0.3g of xanthan gum (Aba Ding Shiji), 0.4g of magnesium aluminum silicate (Aba Ding Shiji), 4g of ethylene glycol (Aba Ding Shiji) and 0.1g of sodium benzoate (Aba Ding Shiji) were dispersed to obtain 20g of a dispersion medium.
3. Preparation of aqueous suspension pesticidal composition
80g of the above-mentioned pulverized slurry and 20g of a dispersion medium were mixed to obtain 100g of an aqueous suspension-type agricultural chemical composition, and the mixture was subjected to high shear (4000 rpm) for 30 minutes in a high-speed disperser (trade name: TG25, german IKA). The fluazinam suspending agent with the active ingredient mass content of 50% is prepared.
Comparative example 2:50% bromcyclozole suspending agent
1. Preparation of crushed pulp
2.5G of a dispersing block copolymer dispersant (trade name: G-5000, he Ju) in 22.1G of water, 2G of a comb-structured polymer dispersant (trade name: KY555, jiangsu Kaiyuan science and technology Co., ltd.), 3G of a wetting agent (trade name: GY-WS10, beijing Guangyuan Yinong chemical Co., ltd.) and 0.4G of a high-efficiency silicone antifoaming agent (trade name: ETXP-40, hangzhou left New Material Co., ltd.) in which bromine is dispersed 50g of original cyproconazole is usedGlass beads were wet-pulverized with a sand mill (Shenyang New micro motor plant) for 1.5 hours to obtain 80g of pulverized slurry.
2. Preparation of dispersion Medium
In 15.2g of water, 0.25g of xanthan gum (Aba Ding Shiji), 0.45g of magnesium aluminum silicate (Aba Ding Shiji), 4g of ethylene glycol (Aba Ding Shiji) and 0.1g of sodium benzoate (Aba Ding Shiji) were dispersed to obtain 20g of a dispersion medium.
3. Preparation of aqueous suspension pesticidal composition
80g of the above-mentioned pulverized slurry and 20g of a dispersion medium were mixed to obtain 100g of an aqueous suspension-type agricultural chemical composition, and the mixture was subjected to high shear (5000 rpm) for 30 minutes in a high-speed disperser (trade name: TG25, germany IKA). The bromcyclozole suspending agent with the active ingredient mass content of 50% is prepared.
Comparative example 3:50% cyflufenamid suspension
1. Preparation of crushed pulp
2g of polycarboxylate dispersant (trade name: SP-27001, jiangsu Qingsu chemical technology Co., ltd.) 2.5g of comb-structured polymer dispersant (trade name: TERSPERSE 2612, huntsman) 2.5g, 3g of wetting agent (trade name: GY-WS10, beijing Guangyuan Yinong chemical Co., ltd.) and 0.4g of high-efficiency silicone defoamer (trade name: ETXP-40, hangzhou left New material Co., ltd.) were dispersed in water, 50g of cyfluxazole original drug was used Glass beads were wet-pulverized with a sand mill (Shenyang New micro motor plant) for 1.5 hours to obtain 80g of pulverized slurry.
2. Preparation of dispersion Medium
In 15.2g of water, 0.25g of xanthan gum (Aba Ding Shiji), 0.45g of magnesium aluminum silicate (Aba Ding Shiji), 4g of ethylene glycol (Aba Ding Shiji) and 0.1g of sodium benzoate (Aba Ding Shiji) were dispersed to obtain 20g of a dispersion medium.
3. Preparation of aqueous suspension pesticidal composition
80g of the above-mentioned pulverized slurry and 20g of a dispersion medium were mixed to obtain 100g of an aqueous suspension-type agricultural chemical composition, and the mixture was subjected to high shear (5000 rpm) for 30 minutes in a high-speed disperser (trade name: TG25, germany IKA). The cyflufenamid suspending agent with the active ingredient mass content of 50% is prepared.
Comparative example 4:
blank clear water control.
Field efficacy test
Cell setting: each treatment was repeated 4 times; the cell area is 30m 2 And (3) arranging random granules.
Time and method of administration: the preparation is applied in the early stage of potato late blight, and the foliage spray treatment is carried out, wherein the spraying amount is mainly no water drop. The disease number is investigated 2 times before the first administration, the administration is carried out 1 time every 7 days, the disease index is investigated 7 days after each administration, and the control effect is calculated.
The investigation method comprises the following steps: grading according to the hazard symptom degree of potato leaf sheaths and leaves, taking five samples from each cell diagonal line by taking the plants as units, taking two plants from each point, and investigating all the leaves.
The specific classification is as follows:
level 0: no disease;
stage 1: the area of the lesion accounts for 5% of the area of the whole leaf;
3 stages: the area of the disease spots accounts for 6-10% of the area of the whole leaf;
5 stages: the area of the disease spots accounts for 11% -20% of the area of the whole leaf;
7 stages: the area of the disease spots accounts for 21% -50% of the area of the whole leaf;
stage 9: the area of the disease spots accounts for more than 50% of the area of the whole leaf.
And (3) calculating the drug effect:
wherein: CK (CK) 0 -a blank control zone pre-drug disease index; CK (CK) 1 -post-drug disease index for the blank control zone;
PT 0 -pre-drug condition index in the drug treatment zone; PT (PT) 1 -index of post-drug condition in the drug treatment zone.
The test results are shown in Table 3 and Table 4.
Table 3: prevention effect of different medicaments on potato late blight
Table 4: prevention effect of different medicaments on potato late blight
Conclusion: from the results shown in tables 3 and 4, the effect of controlling potato late blight is obviously better than that of a control medicament after the fluazinam and the epoxiconazole or the fluazinam and the epoxiconazole are compounded in a certain proportion, and the two components are compounded in a certain proportion, so that the quick-acting performance is improved and the synergistic effect is achieved compared with the control medicament alone. In addition, the pesticide composition and/or the preparation of the invention are not found to generate phytotoxicity to potatoes in the application range, which indicates that the sterilization composition of the invention has good safety to crops and practical and popularization value.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the technical scope of the present invention should be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (13)

1. The bactericidal composition is characterized in that the pharmacodynamic active components of the bactericidal composition consist of a bactericide A and a bactericide B;
wherein the bactericide A is fluazinam, and the bactericide B is bromcyclazole or cyflufenamid; the mass ratio of the bactericide A to the bactericide B is (1-15) to (20-1).
2. The bactericidal composition according to claim 1, wherein the mass ratio of bactericide a to bactericide B is (1-15): 15-1.
3. The bactericidal composition according to claim 2, wherein the mass ratio of bactericide a to bactericide B is (1-10): 5-1.
4. A bactericidal composition according to claim 3, wherein the mass ratio of bactericide a to bactericide B is (1-5): 3-1.
5. The fungicidal composition according to any one of claims 1 to 4, wherein the total content of the fungicidal agent a and the fungicidal agent B in the fungicidal composition is 1 to 90% by mass.
6. The fungicidal composition according to claim 5, wherein the total content of the fungicidal agent a and the fungicidal agent B in the fungicidal composition is 10 to 70% by mass.
7. The fungicidal composition according to claim 6, wherein the total content of the fungicidal agent a and the fungicidal agent B in the fungicidal composition is 10 to 60% by mass.
8. The fungicidal composition according to claim 7, wherein the total content of the fungicidal agent a and the fungicidal agent B in the fungicidal composition is 10 to 50 mass%.
9. A formulation, characterized in that it is prepared from the bactericidal composition according to any one of claims 1 to 8.
10. The formulation of claim 9, wherein the formulation is in the form of a water dispersible granule, a suspension, a dispersible oil suspension, a cream, a microemulsion, or an emulsion in water.
11. Use of the bactericidal composition of any one of claims 1-8 or the formulation of claim 9 or 10 for controlling potato late blight.
12. A method for controlling potato late blight, characterized in that an effective amount of a bactericidal composition according to any one of claims 1-8 or a formulation according to claim 9 or 10 is applied to a plant or plant part to be treated.
13. The method of claim 12, wherein the plant is a cereal, melon, fruit, and/or vegetable crop.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106212471A (en) * 2016-07-22 2016-12-14 重庆东永植保技术有限责任公司 A kind of containing amisulbrom and the bactericidal composition of fluazinam and application
CN106577680A (en) * 2016-12-01 2017-04-26 青岛东生药业有限公司 Bactericide and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106212471A (en) * 2016-07-22 2016-12-14 重庆东永植保技术有限责任公司 A kind of containing amisulbrom and the bactericidal composition of fluazinam and application
CN106577680A (en) * 2016-12-01 2017-04-26 青岛东生药业有限公司 Bactericide and application thereof

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