CN112772663B - Composition containing fluoride phenylate amide and penconazole, preparation and application thereof - Google Patents

Composition containing fluoride phenylate amide and penconazole, preparation and application thereof Download PDF

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Publication number
CN112772663B
CN112772663B CN201911066805.5A CN201911066805A CN112772663B CN 112772663 B CN112772663 B CN 112772663B CN 201911066805 A CN201911066805 A CN 201911066805A CN 112772663 B CN112772663 B CN 112772663B
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Prior art keywords
penconazole
agent
formulation
composition
fipronamide
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CN112772663A (en
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李义涛
鲍中斌
梁任龙
刘新烁
郭文举
董江强
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Dongguan Dongyangjunyang Hydrogen Patent Pesticide Co ltd
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Dongguan Dongyangjunyang Hydrogen Patent Pesticide 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
    • A01N43/64—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
    • 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
    • A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles

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  • Life Sciences & Earth Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention relates to a composition containing fluoride phenylate amide and penconazole, a preparation and application thereof. The composition and the preparation are mainly used for preventing and treating powdery mildew, downy mildew, leaf spot, anthracnose or scab and the like.

Description

Composition containing fluoride phenylate amide and penconazole, preparation and application thereof
Technical Field
The invention relates to the technical field of pesticide compounding, in particular to a composition containing fluoride phenylate amide and penconazole, a preparation and application thereof.
Background
The fluorophenylamide (development code: Y13149) is a novel succinic dehydrogenase inhibitor, has a certain systemic conductivity, and has the advantages of rain resistance, low dosage (5-7 g/mu), low cost (less than 20 ten thousand yuan/ton) and the like. The fluoxynol amide has excellent prevention and control effects on rice sheath blight, powdery mildew, epidemic diseases of cucumbers, tomatoes and the like. The structural formula of the fluorophenylether amide is as follows:
penconazole is a systemic triazole fungicide with protection, treatment and eradication functions, is a sterol demethylation inhibitor, can be absorbed by tissues such as roots, stems, leaves and the like of crops and is conducted upwards, and the indoor activity measurement and field efficacy test results show that the penconazole has a good control effect on grape white rot. The penconazole has the structural formula:
powdery mildew is a frequently-occurring disease of grape in young fruit stage, and typical symptoms are that the fruit surface forms an ash white powdery mildew layer, the result surface of the mildew layer is wiped off and has obvious spider web black brown reticulate patterns, drought and high temperature are easy to burst, the powdery mildew belongs to intractable diseases, and the powdery mildew is difficult to thoroughly cure after occurrence.
Therefore, there is an urgent need to develop a drug or composition capable of effectively preventing and treating powdery mildew with a small dosage.
Disclosure of Invention
The invention aims to provide a composition and a preparation, the composition mainly comprises the fluophenylamide and the penconazole, the synergistic effect of the two components is utilized to improve the control effect on powdery mildew, and the dosage of the same control effect is reduced by nearly 40 percent compared with single administration.
In order to achieve the above object, the present invention provides the following technical solutions:
a composition comprising a pharmaceutically active ingredient;
the pharmacodynamic active component comprises the fluophenylamide and penconazole.
In some embodiments, the compositions of the present invention are bactericidal compositions.
In some embodiments, the pharmaceutically active component in the composition of the present invention consists only of a fluorophenylamide and penconazole.
The invention discovers that the ideal pest control effect can be achieved by using a lower dosage after the fluophenylamide and the penconazole are combined, and the invention has good quick-acting property and long-acting property. Specifically, a large number of indoor screening and field experiments show that the composition can achieve the added bactericidal effect (co-toxicity coefficient is more than 120), and the dosage of the same control effect is reduced by nearly 40% compared with single administration. Therefore, the composition containing the fluophenylamide and the penconazole is very beneficial to keeping the plants healthy and can also ensure the quality and the yield. In a similar manner, the composition comprising the fipronamide and the penconazole provided by the invention has a longer duration.
The mass ratio of the fluophenylamide to the penconazole is arbitrary.
For example, the mass ratio of fipronamide to penconazole can vary within a relatively wide range of 1-20:20-1.
In some embodiments, the mass ratio of the fipronamide to the penconazole in the composition or formulation is 1-15:15-1, 1-10:15-1, 1-5:15-1, 1-3:15-1, 1-2:15-1, 1:15-1, 1-15:10-1, 1-15:5-1, 1-15:3-1, 1-15:2-1, 1-15:1, 1-10:15-1, 1-10:10-1, 1-10:5-1, 1-10:3-1, 1-10:2-1, 1-10:1, 1-5:15-1, 1-5:10-1, 1-5:5-1, 1-5:3-1, 1-5:2-1, 1-5:1, 1-3:15-1, 1-3:10-1, 1-3:5-1, 1-3:3:1, 1-3:3-1, 1-2:3-1, 1-2:2 or 1-2:1-2.
In some embodiments, the mass ratio of fipronamide to penconazole in the composition or formulation is 20:1, 15:1, 12:23, 10:1, 9:1, 8:1, 7:1, 6:1, 5:1, 4:1, 3:1, 2:1, 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, 1:15, or 1:20.
Besides the pharmaceutically active components, the composition of the invention can also contain auxiliary agents commonly used in pesticides, wherein the auxiliary agents are auxiliary substances added in the processing or using process of pesticide preparations and are used for improving the physicochemical properties of the medicaments, and the auxiliary agents are basically inactive, but can influence 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 filler, a disintegrating agent, an antifreezing agent, an antifoaming agent, a solvent, a preservative, a stabilizer, a synergist, a carrier, and the like, and preferably includes at least one of a dispersing agent, a wetting agent, an antifoaming agent, an organic solvent, a thickening agent, a filler disintegrating agent, a stabilizer, an antifreezing agent, a preservative, and a synergist. The above auxiliary agents may be added as appropriate according to the preparation requirements, and may be changed according to the circumstances, and are not particularly limited.
Preferably, the wetting agent may be any of various wetting agents known in the field of pesticide formulation, specifically, the wetting agent may be one or more of alkylbenzene sulfonate (such as sodium dodecylbenzene sulfonate, calcium dodecylbenzene sulfonate), alkylnaphthalene sulfonate (such as sodium dibutylnaphthalene sulfonate, sodium isopropylnaphthalene sulfonate), lignin sulfonate (such as sodium lignin sulfonate, calcium lignin sulfonate), sodium Dodecyl Sulfate (SDS), dioctyl sodium succinate, dioctyl sodium sulfosuccinate, alkylphenol ethoxylates (APEO) (such as nonylphenol ethoxylate, octylphenol ethoxylate, dodecylphenol ether, dinonylphenol ether, mixed alkylphenol ether, etc.), alkylphenol ethoxylate (APES), fatty alcohol ethoxylate sodium sulfate (ethoxylated alkyl sodium sulfate, AES), nekal, silkworm excrement, saponaria, soapbone, detergent, penetrant JFC, wetting penetrant F, wetting penetrant fast T, NP-10, etc. Typical representatives of suitable wetting agents are, inter alia, GY-WS10 (nonionic compound), W2008B.
Preferably, the dispersing agent may be various dispersing agents known in the pesticide formulation field, and specifically, the dispersing agent may be one or more of sodium lignin sulfonate, sodium naphthalene sulfonate formaldehyde condensate, tristyrylphenol ethoxylate phosphate, fatty alcohol ethoxylate, alkyl ethoxylate, alkylphenol ethoxylate methyl ether condensate sulfate, fatty amine polyoxyethylene ether, glycerin fatty acid ester polyoxyethylene ether, EO-PO block copolymer, graft copolymer, and the like. Typical representatives of suitable dispersants are in particular2700、/>2500、/>4894. Ufoxane NA, GY-D900, GY-D1008, morwet D425, antrox B/848 or Ethylan NS-500LQ.
The emulsifier can be various emulsifiers known in the pesticide formulation field, and concretely, the emulsifier can be one or more than two of calcium dodecyl benzene sulfonate, sodium dodecyl sulfate, alkylphenol ethoxylates, alkylphenol ether phosphate, phenethyl phenol polyoxyethylene polyoxypropylene ether, fatty alcohol ethylene oxide-hexane copolymer, styrylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, phosphate anionic emulsifier and the like. Typical representatives of suitable emulsifiers are, inter alia, agro-milk 500#, agro-milk 601#, agro-milk 602#, agro-milk 700#, agro-milk 1601#, agro-milk 1602#, TERMUL 2507, TERMUL 200, 601P, emupon CO-360, or ethyllan 992.
Preferably, the thickener may be various thickeners known in the field of pesticide dosage forms, and specifically, the thickener may be one or more of xanthan gum, gum arabic, sodium alginate, bentonite, magnesium aluminum silicate, carboxymethyl cellulose, white carbon black, and the like.
Preferably, the disintegrating agent may be various disintegrating agents known in the field of pesticide dosage forms, and specifically, the disintegrating agent may be 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, tartaric acid, and the like.
Preferably, the antifreezing agent may be various antifreezing agents known in the pesticide formulation field, and specifically, the antifreezing agent may be one or more of methanol, ethanol, ethylene glycol, propylene glycol, glycerol, isopropanol, diethylene glycol, ethylene glycol butyl ether, propylene glycol butyl ether, ethylene glycol butyl ether acetate, dichloromethane, 1-dichloroethane, 1, 2-dichloroethane, calcium chloride, sodium acetate, magnesium chloride, and the like.
Preferably, the antifoaming agent may be various antifoaming agents known in the field of pesticide formulation, and in particular, the antifoaming agent may be an organosilicone antifoaming agent, an organosilicon antifoaming agent, C 8～10 One or more of fatty alcohol defoamers, etc.
Preferably, the solvent may be various solvents well known in the field of pesticide dosage forms, and specifically, the solvent may be one or more of toluene, xylene, methanol, ethanol, isopropanol, N-butanol, dimethyl sulfoxide, cyclohexanone, N-octyl pyrrolidone, diesel oil, solvent oil, methyl oleate, soybean oil, epoxidized soybean, castor oil, water, N-octyl pyrrolidone, and the like.
Preferably, the preservative may be various preservatives known in the field of pesticide dosage forms, and specifically, the preservative may be one or more than two of sodium benzoate, benzoic acid, potassium sorbate, sodium p-hydroxybenzoate, methyl p-hydroxybenzoate and the like.
Preferably, the stabilizer can be one or more of triphenyl phosphite, acetic anhydride, epichlorohydrin, resorcinol, sodium citrate and the like.
Preferably, the carrier (or filler) is selected from one or more of sodium sulphate, kaolin, clay, talc, chalk, quartz, attapulgite, montmorillonite, diatomaceous earth, silica, alumina, natural or artificial silicate, resin, wax, solid fertiliser, water, organic solvents (e.g. alcohols, especially butanol), mineral and vegetable oils and derivatives thereof.
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 active compounds can be combined with any solid or liquid additive commonly used for formulation purposes.
In the composition of the present invention, the total content of the pharmaceutically active component in the composition or formulation is 1 to 90wt.%.
In some embodiments, the total content of fipronamide and penconazole in the composition or formulation is 1 to 80wt.%.
In some embodiments, the total content of fipronamide and penconazole in the composition or formulation is 5 to 70wt.%.
In some embodiments, the total content of fipronamide and penconazole in the composition or formulation is 5 to 60wt.%.
In some embodiments, the total content of fipronamide and penconazole in the composition or formulation is 10 to 60wt.%.
In some embodiments, the total content of fipronamide and penconazole in the composition or formulation is 10 to 50wt.%.
In some embodiments, the total content of fipronamide and penconazole in the composition or formulation is 10 to 45wt.%.
In some embodiments, the total content of fipronamide and penconazole in the composition or formulation is 10 to 40wt.%.
In some embodiments, the total content of fipronamide and penconazole in the composition or formulation is 12 to 40wt.%.
In some embodiments, the total content of fiuorophenylamide and penconazole in the composition or formulation is 5wt.%, 10wt.%, 12wt.%, 18wt.%, 20wt.%, 25wt.%, 30wt.%, 35wt.%, 40wt.%, 45wt.%, 50wt.%, 60wt.%, 70wt.%, 80wt.%, or 90wt.%.
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 invention also provides a preparation prepared from the composition, and the preparation can be emulsifiable concentrate, wettable powder, suspending agent, granules, water dispersible granules, microemulsion, aqueous emulsion and microcapsule. The above dosage forms can be prepared by methods conventional in the art. For example:
the powder (DP) is obtained by adding a certain amount of inert powder such as clay, kaolin, talcum powder, etc. into active material, and mechanically processing into powder with particle diameter below 100 μm.
Wettable Powders (WP) refer to a mixture of the composition in proportions with suitable surfactants and inert materials (kaolin powders). 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 active substances 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 (kaolin) powder. The powder fineness meets the requirement by air current crushing, and the products are uniformly mixed by using a double-screw mixer and a coulter mixer through repeated mixing. And granulating by conventional method such as fluid bed granulation, spray granulation, and pan 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.
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. The aqueous emulsion is a preparation prepared by dispersing the liquid pesticide raw material prepared by mixing with an organic solvent in water in small liquid drops of 0.5-1.5 microns, and the appearance of the aqueous emulsion is milky milk-like liquid.
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 ultra-low volume spray is a medicine liquid sprayed on target crops, is sprayed in an extremely low dosage by extremely fine mist drops, and is a preparation for ultra-low volume spray application.
The seed coating agent (SD) is prepared by grinding and mixing the effective components 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 in which the effective components are mixed with combustible substances and the like, and the mixture is combusted to gasify the pesticide and then condense the 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 abovementioned formulations can be prepared in a manner known per se, 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, etc.
The present invention provides some preferred formulation compositions, in particular as follows:
preferably, when the preparation is water dispersible granules, the auxiliary agent comprises at least one of dispersing agent, filler and wetting agent;
the dispersing agent preferably comprises one or more of polycarboxylate and naphthalene sulfonate, and the content in the preparation is preferably 7-15 wt.%; among them, a polycarboxylate dispersant of HMK to D1008 is further preferable; further preferred naphthalene sulfonate dispersant is Morwet D425;
the filler preferably comprises at least one of sodium sulfate and kaolin, preferably in an amount of 30 to 50wt.% in the formulation;
the wetting is preferably W2008B, the content in the formulation is preferably 0.5-3 wt.%.
When the preparation is a suspending agent, the auxiliary agent comprises at least one of a dispersing agent, a wetting agent, a defoaming agent, a thickening agent, a disintegrating agent, a carrier and a preservative, and water;
the dispersant preferably comprises at least one of sulfonates and polycarboxylates, preferably in an amount of 1 to 10wt.% of the formulation; further preferred sulfonate dispersants are Morwet D425; further preferred polycarboxylate dispersant is Agrilan 788;
the wetting agent is preferably WS-01, the content in the formulation is preferably 1-5 wt.%;
the defoamer is preferably a silicone, the content in the formulation is preferably 0.1 to 1wt.%; wherein the silicone defoamer is further preferably ETXP-40;
the thickener is preferably xanthan gum, the content in the formulation is preferably 0.1 to 0.3wt.%;
the disintegrant is preferably urea, the content in the formulation preferably being 2-3 wt.%;
the carrier is preferably bentonite, the content in the formulation is preferably 0.1 to 1wt.%;
the preservative is preferably sodium benzoate, preferably in an amount of 0.1 to 0.5wt.% of the formulation.
When the preparation is wettable powder, the auxiliary agent comprises at least one of dispersing agent, thickening agent, disintegrating agent, defoaming agent and filler,
the dispersant is preferably at least one of naphthalene sulfonate polycondensate and lignin, and the content in the formulation is preferably 5 to 10wt.%; wherein further preferred naphthalene sulfonate polycondensate dispersant is Morwet D-425;
the thickener is preferably xanthan gum, and the content in the preparation is preferably 0.3-1 wt.%;
the disintegrant is preferably ammonium sulfate, the content in the formulation is preferably 1-4 wt.%;
the defoamer is preferably an organosilicone, and the content in the preparation is preferably 0.1-0.3 wt.%; wherein further preferred organosilicone defoamer is AFE-1520;
the filler is preferably kaolin, preferably in an amount of 50 to 60wt.% in the formulation.
Preferably, when the formulation is an aqueous emulsion, the adjuvant includes at least one of an organic solvent, an antifreezing agent, an emulsifying agent, and an antifoaming agent, and water;
the organic solvent preferably comprises at least one of cyclohexanone and N-octyl pyrrolidone, and the content in the preparation is preferably 20 to 30wt.%;
the antifreezing agent is preferably at least one of ethylene glycol and n-butanol, and the content in the preparation is preferably 1-5 wt.%;
the emulsifier is preferably at least one of alkylphenol block polyether copolymer emulsifier and phosphate ester anion emulsifier, and the content in the preparation is preferably 2-6 wt.%; wherein the further preferred alkylphenol block polyether copolymer emulsifier is TERMUL 200; further preferred phosphate anionic emulsifier is 601P;
the defoamer is preferably a silicone, the content in the formulation preferably being 0.1 to 0.3wt.%; of these, ETXP-40 is a further preferred silicone defoamer.
The above preferred formulation composition can improve physicochemical properties of the pharmaceutical agent, such as stability, uniformity, quick-acting property or sustained-release property, etc., and can also improve control effect.
The preparation method of the composition or the preparation is simple, and the composition or the preparation can be prepared by combining or mixing the fluophenylate amide, penconazole and one or more auxiliary agents by adopting a conventional method in the field.
The composition and the preparation provided by the invention can be used for preventing and treating powdery mildew, downy mildew, leaf spot, anthracnose or cladosporium cucumerinum, and especially for grape powdery mildew, and have remarkable effects.
In conclusion, compared with the prior art, the invention achieves the following technical effects:
(1) The bactericidal composition has good synergistic effect in a certain range, and the bactericidal effect is obviously improved compared with the simple addition of single dosage;
(2) The dosage is reduced, and the use cost is reduced;
(3) Delay the development of drug resistance of single agent;
(4) Is safe to crops and reduces the environmental pressure.
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. The raw materials, reagents or instruments used are not identified to the manufacturer and are conventional products commercially available or can be prepared according to the prior art.
Indoor biological test
The potting method is adopted indoors to measure different conditionsInhibition of the agent on the growth of powdery mildew (Uncinula necator) of grape, and calculation of EC of each agent on pathogenic bacteria 50 Values.
And (3) drug application: and selecting 1-2 potted grape seedlings with complete leaves and consistent growth vigor for experiments. The single dose or each composition (see Table 1) was dissolved in DMSO and diluted to 5mg/L, 2.5mg/L, 1.25mg/L, 0.625mg/L, 0.3125mg/L, 0.15625mg/L with 0.1wt% Tween 80 water. Spraying the stem leaves until the surfaces of the leaves are wet, and drying the test material in the shade for 24 hours. The test was carried out with no drug as a control group.
Inoculating: collecting fresh leaf, washing off grape powdery mildew spore on the leaf with water, filtering with single-layer gauze to obtain spore suspension (2-3×10) 5 CFU/ml) and then evenly spraying the inoculation on the grape leaf surface with an inoculation sprayer. After inoculation, the cells are transferred into a greenhouse for cultivation at 25-28 ℃ and classified investigation is carried out for about 7 days according to the disease condition of a blank control.
Grading standard:
level 0: no disease;
stage 1: the area of the disease spots accounts for less than 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% -25% of the area of the whole leaf;
7 stages: the area of the disease spots accounts for 26% -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:
performing corresponding regression analysis according to the concentration of each medicament and the corresponding control effect to obtain EC of each medicament 50 Values.
And calculating the co-toxicity coefficient (CTC) of the mixture by adopting a co-toxicity coefficient calculation method introduced 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:
single dose toxicity index = standard dose EC 50 Certain single agent EC 50 ×100；
Theoretical Toxicity Index (TTI) =toxicity index of a single dose×proportion of a single dose in the mixture+toxicity index of B single dose×proportion of B single dose in the mixture;
measured virulence index (ATI) =ec of standard single dose 50 EC of value/mixture 50 Value x 100
Co-toxicity coefficient (CTC) =measured/theoretical toxicity index x 100
The compound was synergistic when CTCs were greater than 120, antagonistic when CTCs were less than 80, and additive between 80 and 120.
TABLE 1 determination results of co-toxicity coefficients of Fluophenylamide and penconazole for powdery mildew of grape
The composition takes the fluophenylamide and the penconazole as the effective components, has obvious synergism on grape powdery mildew in the composition with different mass ratios, and the co-toxicity coefficient is more than 120. Therefore, the compound of the fluophenylate amide and the penconazole can become an ideal medicament for preventing and treating the powdery mildew of grape.
Preparation example
Preparation example 1 18% Fluophenylamide penconazole suspending agent
1. Preparation of crushed pulp
In 43.5g of water, 3g of a sulfonate dispersant (trade name: morwet D425, ackersinobell) and a polycarboxylate dispersant (trade name: agri were dispersedlan 788, acethunobel) 2g, a wetting agent (trade name: WS-01, beijing Guangdong Yinong) 3g and high-efficiency organosilicon defoamer (ETXP-40, hangzhou left soil New material Co., ltd.) 0.5g, into which the stock fluorophenylamide 12g and penconazole 6g are dispersed, usingZirconium beads were wet-pulverized for 2.5 hours with a sand mill to obtain 70g of pulverized slurry.
2. Preparation of dispersion Medium
In 26.26g of water, 0.24g of xanthan gum, 0.4g of bentonite, 2.8g of urea and 0.3g of sodium benzoate were dispersed to obtain 30g of a dispersion medium.
3. Preparation of aqueous suspension pesticidal composition
70g of the crushed slurry and 30g of a dispersion medium were mixed to obtain 100g of an aqueous suspension-type agricultural chemical composition, and a suspension having an active ingredient mass content of 18% was obtained.
Preparation example 2 40% fluophenylamide penconazole water dispersible granule
20g of a fipronil amide raw medicine, 20g of penconazole, 8g of a polycarboxylate dispersant (trade name: HMK-D1008, beijing Han Moke), 3g of a naphthalene sulfonate dispersant (trade name: morwet D425, across Sulbel), 2g of a low-foam wetting agent (trade name: W2008B, beijing Han Moke), 8g of sodium sulfate decahydrate and 800 mesh kaolin are added to 100g, the mixture is pre-crushed and uniformly mixed, and then crushed to the required particle size (10-15 mu m) by a jet mill, and then the mixture is granulated by a rotary granulator, so that the water dispersible granule with the active ingredient mass content of 40% is prepared.
Preparation example 3 35% wettable powder of Fluophenylamide penconazole
11.67g of a fluorophenylamide original drug, 23.33g of penconazole, 5g of naphthalene sulfonate polycondensate (trade name: morwet D-425, acinetobacter, new materials Co., ltd.) of lignin C (Hangzhou left earth Co., ltd.), 3g of ammonium sulfate 2g, 0.5g of xanthan gum, 0.2g of organic silicone (trade name: AFE-1520, DOW CORNING) and 100g of kaolin are added, and the mixture is pre-crushed and mixed uniformly, and then crushed to the required particle size (10-15 mu m) by air current, so that the wettable powder with the active ingredient mass content of 35% is prepared.
PREPARATION EXAMPLE 4 12% Fluophenylamide penconazole aqueous emulsion
1. Oil phase preparation
3g of a stock solution of a fluorophenylamide and 9g of penconazole were added to a mixed solvent of 15g of cyclohexanone and 8g of N-octyl pyrrolidone, and then 2.5g of an emulsifier (trade name: TERMOL 200, huntsman) and 1.5g of a phosphate anionic emulsifier (trade name: 601P, manufactured by the Chen Tailan Fine chemical Co., ltd.) were added and stirred slowly until completely dissolved.
2. Aqueous phase preparation
3g of ethylene glycol, 1g of n-butanol, 0.2g of high-efficiency organic silicon defoamer (ETXP-40, hangzhou left soil new material Co., ltd.) and 56.8g of water are added and stirred uniformly.
3. Pesticide composition aqueous emulsion formulation
Slowly adding the oil phase into the water phase, and stirring until the oil phase is completely added, and performing high shearing (10000 r/min) for 10 minutes by a high-speed dispersing machine to obtain the aqueous emulsion with the active ingredient mass content of 12%.
Comparative example 1 18% Fluorophenylamide suspension
1. Preparation of crushed pulp
In 43.5g of water, 3g of sulfonate dispersant (trade name: morwet D425, acinetobacter nomobel), 2g of polycarboxylate dispersant (trade name: agrilan 788, acinenomobel), 3g of wetting agent (trade name: WS-01, beijing Guangdong Kogyo Co., ltd.) and 0.5g of high-efficiency silicone defoamer (ETXP-40, hangzhou Zuo New Material Co., ltd.) were dispersed, 18g of fluorophenylamide as a raw material was usedZirconium beads were wet-pulverized for 2.5 hours with a sand mill to obtain 70g of pulverized slurry.
2. Preparation of dispersion Medium
In 26.26g of water, 0.24g of xanthan gum, 0.4g of bentonite, 2.8g of urea and 0.3g of sodium benzoate were dispersed to obtain 30g of a dispersion medium.
3. Preparation of aqueous suspension pesticidal composition
70g of the crushed slurry and 30g of a dispersion medium were mixed to obtain 100g of an aqueous suspension-type agricultural chemical composition, and a suspension having an active ingredient mass content of 18% was obtained.
Comparative example 2 40% penconazole water dispersible granule
40g of penconazole, 8g of comb-shaped structural dispersing agent (trade name: GY-D1008, beijing Han moke), 3g of naphthalene sulfonate dispersing agent (trade name: morwet D425, achromofiber), 2g of low foam wetting agent (trade name: W2008B, beijing Han moke), 8g of sodium sulfate decahydrate and 800 mesh kaolin are added to 100g, the mixture is pre-crushed and uniformly mixed, and then crushed to the required particle size (10-15 mu m) by an airflow crusher, and then the mixture is granulated by a rotary granulator, so that the water dispersible granule with the active ingredient mass content of 40% is prepared.
Comparative example 3 blank clear water
Field efficacy test
Test treatment: according to the test design of the test agents in Table 2, the amounts of the three active ingredients were set for the test agents of preparation examples 1 to 4, respectively. The control medicament is respectively a self-made 18% fluophenylamide suspending agent, a self-made 40% penconazole water dispersible granule and blank clear water.
Table 2: test agent test design
Cell setting: each cell area is 30m 2 ；
The application method comprises the following steps: the preparation is applied in the early stage of the onset of grape powdery mildew, the foliage spraying treatment is carried out, and the spraying amount is mainly no water drop;
number of times of application: 3 times, raining in windy days or within 1 hour, and no drug is applied. Disease condition number was investigated before the first administration, 1 time was followed every 7 days, and control effect was investigated 7 days after the 3 rd administration.
Investigation time and number: the cardinal number was investigated 1 day after administration, and the disease index was investigated 7 days, 14 days, and 21 days after administration.
The investigation method comprises the following steps: and grading according to the damage symptom degree of the grape leaves, taking plants as units, sampling five points on the diagonal line of each cell, surveying 5 clusters connected with each point, 25 clusters in total, and recording the total plant number, the disease plant number and the disease stage number.
The method for checking the drug effect before and after drug application comprises the following steps: randomly sampling 5 points in the test treatment area, and recording the total leaf number, the disease leaf number and the disease stage number. The grading standard method is as follows:
level 0: no disease;
stage 1: the area of the disease spots accounts for less than 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% -25% of the area of the whole leaf;
7 stages: the area of the disease spots accounts for 26% -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:
the test results are shown in Table 3.
Table 3: prevention effect of different medicaments on grape powdery mildew
From Table 3, the effect of preventing and treating grape powdery mildew after the compound of the fluophenylamide and the penconazole is obviously better than that of a control medicament, and the compound of the fluophenylamide and the penconazole has good quick-acting property and long lasting period, so that the compound of the fluophenylamide and the penconazole can show synergistic effect, the administration frequency can be reduced, the manpower and material resources are reduced, and the production benefit is improved. In addition, the pesticide composition disclosed by the invention is not found to be harmful to grapes in the application range, so that the sterilization composition disclosed by the invention is good in safety to crops and can be popularized and applied.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to 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 (16)

1. A composition comprising a pharmaceutically active ingredient;
the pharmacodynamic active component comprises the fluophenylamide and penconazole; wherein the mass ratio of the fluophenylate amide to the penconazole is 1-15:15-1.
2. The composition according to claim 1, wherein the mass ratio of the fipronamide to the penconazole is 1-5:5-1.
3. The composition according to claim 1, wherein the mass ratio of the fipronamide to the penconazole is 1-2:2-1.
4. Composition according to claim 1, characterized in that the total content of fipronamide and penconazole in the composition is 1-90 wt.%.
5. Composition according to claim 1, characterized in that the total content of fipronamide and penconazole in the composition is 5-70 wt.%.
6. Composition according to claim 1, characterized in that the total content of fipronamide and penconazole in the composition is 10-50 wt.%.
7. Composition according to claim 1, characterized in that the total content of fipronamide and penconazole in the composition is 10-40 wt.%.
8. The composition of any of claims 1-7, further comprising an adjuvant comprising at least one of a dispersant, a wetting agent, an antifoaming agent, an organic solvent, a thickener, a filler, a disintegrant, a stabilizer, an antifreeze, a preservative, and a synergist.
9. The preparation prepared from the composition of claim 8, wherein the preparation is in the form of emulsifiable concentrate, wettable powder, suspension, granule, water dispersible granule, microemulsion, aqueous emulsion or microcapsule.
10. The formulation of claim 9, wherein when the formulation is a water dispersible granule, further comprising at least one of a dispersant, a filler, a wetting agent;
the dispersing agent comprises one or more of polycarboxylate and naphthalene sulfonate;
the filler comprises at least one of sodium sulfate and kaolin;
the wetting agent includes W2008B.
11. The formulation of claim 9, wherein when the formulation is a suspending agent, further comprising at least one of a dispersant, a wetting agent, an antifoaming agent, a thickener, a disintegrant, a carrier, and a preservative, and water;
the dispersing agent comprises at least one of sulfonates and polycarboxylates;
the wetting agent is WS-01;
the defoaming agent is organic silicon;
the thickener is xanthan gum;
the disintegrating agent is urea;
the carrier is bentonite;
the preservative is sodium benzoate.
12. The formulation of claim 9, wherein the formulation is a wettable powder and further comprises at least one of a dispersant, a thickener, a disintegrant, an antifoaming agent, and a filler,
the dispersant comprises at least one of naphthalene sulfonate polycondensate and lignin;
the thickener comprises xanthan gum;
the disintegrant comprises ammonium sulfate;
the defoamer comprises an organosilicone;
the filler comprises kaolin.
13. The formulation of claim 9, wherein when the formulation is an aqueous emulsion, further comprising water and at least one of an organic solvent, an anti-freeze agent, an emulsifier, and an antifoaming agent;
the organic solvent comprises at least one of cyclohexanone and N-octyl pyrrolidone;
the antifreezing agent is at least one of ethylene glycol and n-butanol;
the emulsifier is at least one of alkylphenol block polyether copolymer type emulsifier and phosphate ester anion emulsifier;
the defoaming agent is organic silicon.
14. Use of a composition according to any one of claims 1 to 8 or a formulation according to any one of claims 10 to 13 for controlling powdery mildew of grapes.
15. A process for the preparation of a composition as claimed in any one of claims 1 to 8, comprising: the fipronamide and penconazole are combined with optional adjuvants.
16. A method of preparing a formulation as claimed in any one of claims 9 to 13, comprising: the fipronamide and penconazole are combined with one or more adjuvants.
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1226244A (en) * 1996-07-24 1999-08-18 拜尔公司 Carbanilides used as pesticides
CN101056858A (en) * 2004-09-06 2007-10-17 巴斯福股份公司 (hetero)cyclyl(thio) carboxylic acid anilides for controlling pathogenic fungi
CN104381268A (en) * 2014-12-15 2015-03-04 北京燕化永乐生物科技股份有限公司 Compound bactericide
CN104430384A (en) * 2014-12-03 2015-03-25 北京燕化永乐生物科技股份有限公司 Bactericidal composition
CN104430375A (en) * 2014-10-29 2015-03-25 北京燕化永乐生物科技股份有限公司 Fungicidal composition
CN104557709A (en) * 2013-10-23 2015-04-29 华中师范大学 Pyrazole amide compound containing diphenyl ether, and application and pesticide composition of pyrazole amide compound
CN104886073A (en) * 2015-05-21 2015-09-09 华中师范大学 Fungicide composite, and preparation and application of fungicide composite
CN107347891A (en) * 2016-05-10 2017-11-17 海利尔药业集团股份有限公司 A kind of bactericidal composition containing Difenoconazole Yu fluorobenzene ether amide

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1226244A (en) * 1996-07-24 1999-08-18 拜尔公司 Carbanilides used as pesticides
CN101056858A (en) * 2004-09-06 2007-10-17 巴斯福股份公司 (hetero)cyclyl(thio) carboxylic acid anilides for controlling pathogenic fungi
CN104557709A (en) * 2013-10-23 2015-04-29 华中师范大学 Pyrazole amide compound containing diphenyl ether, and application and pesticide composition of pyrazole amide compound
CN104430375A (en) * 2014-10-29 2015-03-25 北京燕化永乐生物科技股份有限公司 Fungicidal composition
CN104430384A (en) * 2014-12-03 2015-03-25 北京燕化永乐生物科技股份有限公司 Bactericidal composition
CN104381268A (en) * 2014-12-15 2015-03-04 北京燕化永乐生物科技股份有限公司 Compound bactericide
CN104886073A (en) * 2015-05-21 2015-09-09 华中师范大学 Fungicide composite, and preparation and application of fungicide composite
CN107347891A (en) * 2016-05-10 2017-11-17 海利尔药业集团股份有限公司 A kind of bactericidal composition containing Difenoconazole Yu fluorobenzene ether amide

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