CN112471156B - Composition containing Floreylpicolaminid and fluorophenylamine, preparation and application thereof - Google Patents

Composition containing Floreylpicolaminid and fluorophenylamine, preparation and application thereof Download PDF

Info

Publication number
CN112471156B
CN112471156B CN201910860195.XA CN201910860195A CN112471156B CN 112471156 B CN112471156 B CN 112471156B CN 201910860195 A CN201910860195 A CN 201910860195A CN 112471156 B CN112471156 B CN 112471156B
Authority
CN
China
Prior art keywords
formulation
agent
composition
preparation
stabilizer
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201910860195.XA
Other languages
Chinese (zh)
Other versions
CN112471156A (en
Inventor
李义涛
郭藤
梁任龙
刘新烁
雷志火
甘焕
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dongguan Dongyangjunyang Hydrogen Patent Pesticide Co ltd
Original Assignee
Dongguan Dongyangjunyang Hydrogen Patent Pesticide Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dongguan Dongyangjunyang Hydrogen Patent Pesticide Co ltd filed Critical Dongguan Dongyangjunyang Hydrogen Patent Pesticide Co ltd
Priority to CN201910860195.XA priority Critical patent/CN112471156B/en
Publication of CN112471156A publication Critical patent/CN112471156A/en
Application granted granted Critical
Publication of CN112471156B publication Critical patent/CN112471156B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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
    • 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

Abstract

The invention relates to a composition containing Floreylpicolaminid and fluorophenylether amide, a preparation and application thereof. The synergistic effect of Floreylpicolamid and Fluophenylamide is utilized to expand the bactericidal spectrum, delay the generation of drug resistance and reduce the production and use cost.

Description

Composition containing Floreylpicolaminid and fluorophenylamine, preparation and application thereof
Technical Field
The invention relates to the technical field of pesticide compounding, in particular to a composition containing Floreylpicoxamid and fluorophenylamide, a preparation and application thereof.
Background
The Floreylpicoxamid has the development code: x12485659, XDE-659, XR-659; IUPAC name: (1S) -2, 2-bis (4-fluorophenyl) -1-methylethyl N- { [3- (acetyloxy) -4-methoxy-2-pyridinyl]Carbonyl } -L-alanine ester; the CAS registry number is: 1961312-55-9; the molecular formula is: c (C) 27 H 26 F 2 N 2 O 6 The method comprises the steps of carrying out a first treatment on the surface of the Is a new pyridine amide (neonicolinamide) bactericide developed by the department of agricultural industry (Corteva Agriscience; kedi Hua) of Tao Shidu. Can be used for controlling powdery mildew (powdery mildew), anthracnose (anthracnose), scab (Scab), diseases caused by pathogenic bacteria such as Septoria (Septoria spp.), botrytis spp, alternaria spp, and sclerotinia spp, and can be used for multiple growth stages of crops, and can improve the yield and quality of crops, and has the following structural formula:
fluorophenylamide (development code: Y13149) is a novel succinate dehydrogenase inhibitor and has certain systemic conductivity. The fluoxynol amide has excellent prevention and control effects on rice blast and banded sclerotial blight, and has better prevention and control effects on powdery mildew, epidemic diseases of cucumbers, tomatoes and the like. The structural formula of the fluorophenylether amide is as follows:
the existing improper use of pesticides causes stronger and stronger disease resistance to pesticides, so that the use amount of pesticides is increased year by year, and the environmental pollution is more and more serious. Therefore, reasonable use of pesticides and preparation of compound bactericides to expand the bactericidal spectrum and reduce disease resistance are urgent.
Disclosure of Invention
The invention aims to provide a composition and a preparation, wherein the composition mainly comprises fluorophenylamide and Floreyl picoxamid, the synergistic effect of the two components is utilized to enlarge the sterilization spectrum, delay the generation of drug resistance and reduce the production and use cost.
In order to achieve the above object, the present invention provides the following technical solutions:
a composition comprising a pharmaceutically active ingredient;
the pharmaceutically active component comprises fluorophenylamide and florylpicolamid.
In some embodiments, the compositions of the present invention are bactericidal compositions.
In some embodiments, the pharmaceutically active component in the compositions of the present invention consists only of fluorophenylamide and florylpicolamid.
The invention discovers that the ideal pest control effect can be achieved by using a lower dosage after the combination of the fluophenylamide and the florylpicoloxamid, 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 additive bactericidal effect (co-toxicity coefficient is above 90), and the bactericidal spectrum is widened to other plant pathogens (such as plant disease resistant strains); reducing the application rate of the active compound; advantageous properties during formulation or use (e.g., grinding, sieving, emulsifying, dissolving or dispersing); enhanced storage stability and photostability; advantageous residue formation; improved toxicological and ecotoxicological profiles; improved plant characteristics such as better growth, increased harvest yields, more developed root systems, larger leaf area, greener leaves, stronger shoots, less seed requirements, lower phytotoxicity, mobilization of plant defense systems, good compatibility with plants. Therefore, the composition containing the florfenicol amide and the floryl picoxamid is very helpful for keeping the plants healthy and also can ensure the quality and the yield. In a similar manner, the compositions comprising fluorophenylamide and Floreylpicoxamid provided herein have a longer duration of time.
The mass ratio of the fluorophenylamide to the florylpicolamid in the present invention is arbitrary.
For example, the mass ratio of fluorophenyloxamid to Floreylpicoxamid may vary over a relatively wide range of from 1 to 20:20 to 1, such as from 1:20, 1:3, 5:20, 7:20, 10:20, 13:20, 15:20, 17:20, 1:1, 20:1, 20:3, 5:1, 4:1, 3:1, 2:1, 4:3, 20:17, etc., with preferred embodiments having a mass ratio of from 1 to 10:10 to 1, more preferably from 1 to 5:5 to 1, more preferably from 1 to 5:3 to 1, more preferably from 1 to 5:1, more preferably from 1 to 3:1, and more preferably from 1 to 3:1. When the mass ratio of the fluorophenylamide to the Floreylpicoxamid is 1-5:3-1, the co-toxicity coefficient reaches more than 120.
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, a defoaming 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 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 is one or more selected from sodium dodecyl sulfate, calcium dodecyl benzene sulfonate, dibutyl naphthalene sulfonate, dioctyl sodium succinate, morwet EFW, GY-WS10, etc. Typical representatives of suitable wetting agents are in particular GY-WS10 (nonionic compound).
Preferably, the dispersing agent is selected from one or more than two of naphthalene or alkyl naphthalene formaldehyde condensate sulfonate, fatty alcohol ethylene oxide adduct sulfonate, lignin and derivative sulfonate thereof, alkylphenol ethoxylate formaldehyde condensate sulfate, fatty alcohol ethoxylate sulfate, acrylic acid homopolymer sodium salt, maleic acid disodium salt and the like. Typical representatives of suitable dispersants are in particular Ufoxan NA, GY-D900, antrox B/848 or Ethylan NS-500LQ.
The emulsifier is one or more than two selected from sodium dodecyl sulfate, calcium dodecyl benzene sulfonate, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene ether formaldehyde condensate, fatty alcohol polyoxyethylene ether, triphenyl ethylphenol polyoxyethylene polyoxypropylene ether, alkyl naphthalene sulfonate, fatty acid polyoxyethylene ester, AEO series and the like. Typical representatives of suitable emulsifiers are, in particular, agro-milk 500#, agro-milk 601#, agro-milk 602#, agro-milk 700#, agro-milk 1601#, agro-milk 1602#, TERMUL 2507, emulpool-360 or ethyllan 992.
Preferably, the thickener is one or more selected from white carbon black, kaolin, bentonite, xanthan gum, sodium carboxymethyl cellulose and the like.
Preferably, the disintegrating agent is selected from one or more than two of urea, bentonite, aluminum chloride, ammonium sulfate, succinic acid, sodium bicarbonate and the like.
Preferably, the antifreezing agent is one or more selected from glycerol, ethylene glycol, propylene glycol and the like.
Preferably, the defoaming agent is one or two selected from organosilicon defoaming agents, organic silicone defoaming agents and C8-10 aliphatic alcohol defoaming agents.
Preferably, the solvent is one or more of toluene, xylene, cyclohexanone, aromatic hydrocarbon solvent, methanol, ethyl acetate, soybean oil, epoxidized soybean oil, castor oil and the like.
Preferably, the preservative is one or more selected from sodium benzoate, benzoic acid, potassium sorbate, pinocembrane and the like.
Preferably, the stabilizer is selected from one or more of triphenyl phosphite, acetic anhydride, epichlorohydrin, resorcinol, sodium citrate and the like.
Preferably, the synergist has no bioactivity, but can inhibit detoxification enzyme in organisms, and can greatly improve pesticide toxicity and pesticide effect when mixed with certain pesticides, and is selected from one or more than two of synergistic phosphorus, synergistic ether and the like.
Preferably, 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, organic solvents (e.g. alcohols, especially butanol), mineral and vegetable oils and derivatives thereof, and the like.
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 is 1 to 90wt.%, for example 1.0wt.%, 5.0wt.%, 10.0wt.%, 15.0wt.%, 20.0wt.%, 22.0wt.%, 30.0wt.%, 40.0wt.%, 50.0wt.%, 60.0wt.%, 70.0wt.%, 80.0wt.%, 90.0wt.%, etc., wherein the preferred range is 1 to 60wt.%, 10 to 60wt.%, 20 to 60wt.%, etc. When the total mass of the florfenicol amide and the floryl picoxamid in the preparation accounts for 20-60% of the total mass of the preparation, the toxicity and the residue reach better balance, and the cost is lower.
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 (encapsulated DryFlowable, 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, disintegrating agent, stabilizing agent and defoaming agent;
the dispersant preferably comprises one or more of lignin, lignin salts, ethylene oxide propylene oxide block copolymers, preferably in an amount of 7 to 11wt.% in the formulation;
the filler preferably comprises at least one of organobentonite and kaolin, preferably in an amount of 25 to 30wt.% in the formulation;
the stabilizer is preferably magnesium aluminum silicate, and the content in the preparation is preferably 0.3-0.7 wt.%;
the disintegrant is preferably ammonium sulfate, preferably in an amount of 3 to 7wt.% in the formulation;
the defoamer is preferably a silicone, and the content in the formulation is preferably 0.1 to 0.3wt.%.
Preferably, when the formulation is a suspending agent, the adjuvant includes at least one of a dispersant, a wetting agent, an antifoaming agent, a thickener, a stabilizer, an antifreezing agent, and a preservative, and water;
the dispersant preferably comprises at least one of a non-alkylphenol (e.g., TERSPERSE 4894) and a polycarboxylate (e.g., GY-D900), preferably in an amount of 2 to 4wt.%;
the wetting agent is preferably GY-WS10, and the content in the preparation is preferably 3-5 wt.%;
the defoamer is preferably a silicone, the content in the formulation is preferably 0.2 to 0.5wt.%;
the thickener is preferably xanthan gum, the content in the formulation is preferably 0.2 to 0.4wt.%;
the stabilizer is preferably magnesium aluminum silicate, and the content in the preparation is preferably 0.3-0.5 wt.%;
the antifreeze is preferably ethylene glycol, the content in the preparation is preferably 3-5 wt.%;
the preservative is preferably sodium benzoate, preferably in an amount of 0.1 to 0.2wt.% of the formulation.
Preferably, when the formulation is an aqueous emulsion, the adjuvant includes at least one of an organic solvent, an antifreezing agent, a stabilizer, an emulsifier, and an antifoaming agent, and water;
the organic solvent preferably comprises at least one of cyclohexanone and xylene, preferably in an amount of 15 to 20wt.% in the formulation;
the antifreeze is preferably ethylene glycol, the content in the preparation is preferably 3-5 wt.%;
the stabilizer is preferably magnesium aluminum silicate, and the content in the preparation is preferably 0.2-0.4 wt.%;
the emulsifier is preferably castor oil polyoxyethylene ether (such as TERMUL 2507, emupon CO-360), and the content in the preparation is preferably 1-5 wt.%;
the defoamer is preferably a silicone, and the content in the formulation is preferably 0.05 to 0.15wt.%.
Preferably, when the formulation is a microemulsion, the adjuvant includes at least one of an organic solvent, an emulsifier, and an antifreeze, and water;
the organic solvent preferably comprises at least one of cyclohexanone and xylene, preferably in an amount of 10 to 20wt.% in the formulation;
the emulsifier preferably comprises at least one of agro-emulsion 1601# and agro-emulsion 500# and the content in the preparation is preferably 12-15 wt.%;
the antifreeze is preferably propylene glycol, and the content in the formulation is preferably 3 to 7wt.%.
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 fluorophenylamide with Floreylpicolaminid and optional auxiliary agents by adopting a conventional method in the field.
The composition and the preparation can be used for preventing and treating powdery mildew, banded sclerotial blight, fusarium wilt, leaf spot, rust disease, sclerotinia, rice blast or anthracnose of fruits and vegetables of cereal crops.
In conclusion, compared with the prior art, the invention achieves the following technical effects:
(1) The two active ingredients of the fluophenylamide and the Floreylpicolamid are compounded, so that the synergistic effect is good;
(2) The sterilization spectrum is enlarged, and the application range is widened;
(3) Delay the generation of drug resistance;
(4) The production cost and the use cost are reduced;
(5) Is safe to crops.
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 inhibition effect of different agents on the growth of wheat powdery mildew (Erysiphe graminis) is measured by a potting method indoors, and the EC of each agent on pathogenic bacteria is calculated 50 Values.
And (3) drug application: potted wheat seedlings with consistent growth vigor in one leaf and one heart period are selected for experiment. The single dose or each composition (see Table 1) was dissolved in solvent DMSO and diluted to 5, 2.5, 1.25, 0.625, 0.3125, 0.15625mg/L with 0.1% Tween 80 water. And drying the test material in the shade for 24 hours after stem and leaf spraying treatment.
Inoculating: the mature wheat powdery mildew spores are gently shaken off and inoculated on wheat seedlings. The cultivated wheat seedlings after inoculation are placed in a greenhouse for low-humidity culture (15-26 ℃), and the cultivated wheat seedlings are subjected to grading investigation according to the disease condition of a blank control for about 7 days.
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:
based on the concentration of each composition and the corresponding control effect, corresponding regression analysis is performed to obtain EC of each composition 50 Values.
And calculating the co-toxicity coefficient (CTC) of the mixture by adopting a co-degree 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 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 x 100
Co-toxicity coefficient (CTC) =measured/theoretical toxicity index x 100
The mixture has synergy when the CTC is more than 120, antagonism when the CTC is less than 80, and additive effect between 80 and 120.
Table 1: determination results of wheat powdery mildew co-toxicity coefficients of different proportions of fluorophenylamide (Y13149) and Floreylpicoxamid
Conclusion: as can be seen from Table 1, the compound bactericide taking the florfenicol amide and the floryl picoxamid as the active ingredients has obvious synergism, and particularly the synergism is most obvious when the mass ratio of the florfenicol amide to the floryl picoxamid is 5-1:1-3.
Examples
Example 1:60% Floreylpicoloxamid-fluorophenylether amide water dispersible granule
30g of Floreylpicoxamid original drug, 30g of fluorophenylamide, 6g of EOPO block copolymer (trade name: antraox B/848, rhodia), 3g of lignin, 5g of ammonium sulfate, 0.5g of magnesium aluminum silicate, 0.2g of organic bentonite, 0.2g of high-efficiency organosilicon defoamer and 100g of kaolin are added, the mixture is pre-crushed and uniformly mixed, and then the mixture is crushed to the required particle size by air current, and then granulated by adopting a rotary granulator, so that the water dispersible granule with the active ingredient mass content of 60% is prepared.
Example 2:40% Floreylpicoloxamid-fluorophenylether amide suspending agent
1. Preparation of crushed pulp
Adding non-alkylphenol high-efficiency dispersant (trade name: TERSPERSE 4894, huntsman) 1.5g, comb-structured polymer dispersant (trade name: GY-D900, beijing Guangyuan Yinong) 1.5g, wetting agent (trade name: GY-WS10, beijing Guangyuan Yinong) 4g and high-efficiency silicone defoamer (Hangzhou left soil New Material Co., ltd.) 0.3g into water, dispersing Floreylpicolomimid original drug 10g and fluorophenylamine 30g, usingGlass beads were wet-pulverized for 2.0 hours with a sand mill to obtain 80g of pulverized slurry.
2. Preparation of dispersion Medium
In 15.2g of water, 0.3g of xanthan gum, 0.4g of magnesium aluminum silicate, 4g of ethylene glycol and 0.1g of sodium benzoate 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) in a high-speed disperser for 30 minutes to obtain a suspension having an active ingredient mass content of 40%.
Example 3:30% Floreylpicoloxamid-fluorophenylamine amide aqueous emulsion
1. Oil phase preparation
5g of Floreylpicolxamid original drug and 25g of fluorophenylether amide are added into a mixed solvent of 9g of cyclohexanone and 7g of dimethylbenzene, and after ultrasonic mixing is carried out uniformly, 2g of emulsifying agent (trade name: TERMOL 2507, huntsman) and 2g of castor oil polyoxyethylene ether (trade name: EMULMON CO-360, across nostebel) are added and stirred slowly until complete dissolution.
2. Aqueous phase preparation
Ethylene glycol 4g, magnesium aluminum silicate 0.2g, high-efficiency organic silicon defoamer (Hangzhou left soil new materials Co., ltd.) 0.1g and water 45.7g are added and stirred uniformly.
3. Pesticide composition aqueous emulsion formulation
Slowly adding the water phase into the oil phase, and stirring until the water phase is completely added, and preparing the aqueous emulsion with the active ingredient mass content of 30% under high shear (4000 rpm) of a high-speed dispersing machine for 30 minutes.
Example 4:22% Floreylpicoloxamid-fluorophenylether amide microemulsion
16.5g of Floreylpicolomid crude drug, 5.5g of fluorophenylamide, 10g of solvent dimethylbenzene, 5g of solvent cyclohexanone, 9g of emulsifier agro-emulsion 1601# (Chen Techn Yan Cheng chemical auxiliary Co., ltd.), 5g of emulsifier agro-emulsion 500# (Chen Techn Yan Cheng chemical auxiliary Co., ltd.), 5g of antifreeze propylene glycol and 44g of water are weighed. Fully dissolving Floreylpicoxamid and fluorophenylamide with a solvent, adding an emulsifier and an antifreezing agent, uniformly mixing, finally adding deionized water, and uniformly stirring to obtain the microemulsion with the active ingredient mass content of 22%.
Comparative example 1:50% Floreylpicoloxamid suspension
1. Preparation of crushed pulp
Dispersing non-alkylphenol type high-efficiency dispersant (trade name: TERSPERSE 4894, huntsman) 2g, comb-structured polymer dispersant (trade name: GY-900, beijing Guangdong Yinong) 1.5g, wetting agent (trade name: GY-WS10, beijing Guangdong Yinong) 4g and high-efficiency silicone defoamer (Hangzhou left soil New material Co., ltd.) 0.3g in water, dispersing Floreylpicoxamid raw material 50g therein, usingGlass beads were wet-milled for 1.5 hours with sand milling to obtain 80g of milled slurry.
2. Preparation of dispersion Medium
In 15.2g of water, 0.3g of xanthan gum, 0.4g of magnesium aluminum silicate, 4g of ethylene glycol and 0.1g of sodium benzoate 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-like pesticidal composition, and the aqueous suspension-like pesticidal composition was subjected to high shear (4000 rpm) for 30 minutes in a high-speed disperser. The suspending agent with the active ingredient mass content of 50% is prepared.
Comparative example 2:50% suspension of fluorophenylether amide
1. Preparation of crushed pulp
Dispersing non-alkylphenol type high-efficiency dispersant (trade name: TERSPERSE 4894, huntsman) 2.5g, comb-structured high-molecular compound dispersant (trade name: GY-900, beijing Guangyuan Yinong) 2g, wetting agent (trade name: GY-WS10, beijing Guangyuan Yinong) 3g and high-efficiency silicone defoamer (Hangzhou left soil New material Co., ltd.) 0.4g in water, dispersing 50g of fluorophenylamide original drug therein, usingGlass beads were wet-pulverized for 1.5 hours with a sand mill to obtain 80g of pulverized slurry.
2. Preparation of dispersion Medium
In 15.2g of water, 0.25g of xanthan gum, 0.45g of magnesium aluminum silicate, 4g of ethylene glycol and 0.1g of sodium benzoate 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. The suspending agent with the active ingredient mass content of 50% 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 examples 1 to 4, respectively. The control agents were 50% Floreylpicoxamid suspension prepared in control 1 and 50% Florethylanilide suspension prepared in control 2, respectively, and clear water blank.
Table 2: test agent test design
Cell setting: each cell area is 66.7m 2 。
The application method comprises the following steps: the preparation is applied in the early stage of wheat 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: classifying according to the damage symptom degree of leaf sheath and leaf of wheat, taking plant as unit, sampling five points on diagonal line of each cell, and investigating 5 clusters each point, 25 clusters total, and recording total plant number, disease number and disease stage number.
The method for checking the drug effect before and after drug application comprises the following steps: 5 points were randomly sampled in the test treatment area, and total leaf number, disease leaf number and disease progression were recorded. The grading standard method is as follows:
level 0: the whole plant is free from diseases;
stage 1: fourth leaf and leaf sheaths below the fourth leaf, and leaf onset (with sword leaf as the first leaf);
3 stages: the third leaf and leaf sheaths below the third leaf, and the leaf onset;
5 stages: a second leaf and leaf sheaths below the second leaf, the leaf being diseased;
7 stages: sword leaf and leaf sheaths below the sword leaf, and the leaf is ill;
stage 9: the whole plant is ill and die early.
And (3) calculating the drug effect:
the test results are shown in Table 3.
Table 3: prevention effect of different medicaments on wheat powdery mildew
From Table 3, the effect of preventing and treating wheat powdery mildew after the compound of the fluophenylamide and the Floreylpicolaminid is obviously better than that of a control medicament, and after the compound of the fluophenylamide and the Floreylpicolaminid is carried out, the quick-acting property is good, the lasting period is long, and the synergistic effect can be shown after the compound of the fluophenylamide and the Floreylpicolaminid, so that the administration frequency can be reduced. In addition, the pesticide composition does not generate phytotoxicity to wheat in the application range, which indicates that the sterilization composition has good safety to crops and can be popularized and applied.
In conclusion, the bactericidal composition provided by the invention, which takes the fluorophenylamide and the florylpicolamid as the active ingredients, has good control effects on powdery mildew of wheat, rice sheath blight disease and rice blast, and is safe to target crops. The compound preparation not only improves the control effect, but also expands the sterilization spectrum, widens the application range, reduces the cost, plays a role in treating various diseases simultaneously, reduces manpower and material resources and improves the production benefit. Therefore, the invention and popularization of the compound preparation have very important significance to society.
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 (34)

1. A composition comprising a pharmaceutically active ingredient;
the pharmacodynamic active component comprises the Fluorophenylamide and Floreylpicolaminid, and the mass ratio of the Floreylpicolaminid to the Floreylpicolaminid is 1-5:3-1.
2. The composition according to claim 1, wherein the mass ratio of the fluorophenylamide to the florylpicolamid is 1-5:1.
3. Composition according to claim 1, characterized in that the total content of fluorophenylamide and florylpicolamid in the composition is 1 to 90wt.%.
4. Composition according to claim 1, characterized in that the total content of fluorophenylamide and florylpicolamid in the composition is 1 to 60wt.%.
5. Composition according to claim 1, characterized in that the total content of fluorophenylamide and florylpicolamid in the composition is 20-60 wt.%.
6. The composition of any of claims 1-5, further comprising an adjuvant comprising at least one of a dispersant, a wetting agent, an organic solvent, a thickener, a filler, a disintegrant, a stabilizer, an antifreeze, a preservative, and a synergist.
7. The preparation prepared from the composition according to any one of claims 1 to 6, wherein the preparation is in the form of emulsifiable concentrate, wettable powder, suspension, granule, water dispersible granule, microemulsion, aqueous emulsion or microcapsule.
8. The formulation of claim 7, wherein when the formulation is a water dispersible granule, the adjuvant comprises at least one of a dispersant, a filler, a disintegrant, a stabilizer, and an antifoaming agent.
9. The formulation of claim 8, wherein when the formulation is a water dispersible granule, the dispersant comprises one or more of lignin, lignin salts, ethylene oxide propylene oxide block copolymers.
10. The formulation of claim 8, wherein when the formulation is a water dispersible granule, the filler comprises at least one of an organobentonite and a kaolin clay.
11. The formulation of claim 8, wherein when the formulation is a water dispersible granule, the stabilizer is magnesium aluminum silicate.
12. The formulation of claim 8, wherein when the formulation is a water dispersible granule, the disintegrant is ammonium sulfate.
13. The formulation of claim 8, wherein when the formulation is a water dispersible granule, the defoamer is a silicone.
14. The formulation of claim 7, wherein when the formulation is a suspending agent, the adjuvant comprises at least one of a dispersant, a wetting agent, an antifoaming agent, a thickener, a stabilizer, an antifreezing agent, and a preservative, and water.
15. The formulation of claim 14, wherein when the formulation is a suspending agent, the dispersing agent comprises at least one of a non-alkylphenol and a polycarboxylate.
16. The formulation of claim 14, wherein when the formulation is a suspension, the wetting agent is GY-WS10.
17. The formulation of claim 14, wherein when the formulation is a suspending agent, the antifoaming agent is a silicone.
18. The formulation of claim 14, wherein when the formulation is a suspending agent, the thickening agent is xanthan gum.
19. The formulation of claim 14, wherein when the formulation is a suspending agent, the stabilizer is magnesium aluminum silicate.
20. The formulation of claim 14, wherein when the formulation is a suspending agent, the antifreeze is ethylene glycol.
21. The formulation of claim 14, wherein when the formulation is a suspension, the preservative is sodium benzoate.
22. The formulation of claim 7, wherein when the formulation is an aqueous emulsion, the adjuvant comprises at least one of an organic solvent, an anti-freeze agent, a stabilizer, an emulsifier, and an antifoaming agent, and water.
23. The formulation of claim 22, wherein when the formulation is an aqueous emulsion, the organic solvent comprises at least one of cyclohexanone and xylene.
24. The formulation of claim 22, wherein when the formulation is an aqueous emulsion, the antifreeze is ethylene glycol.
25. The formulation of claim 22, wherein when the formulation is an aqueous emulsion, the stabilizer is magnesium aluminum silicate.
26. The formulation of claim 22, wherein when the formulation is an aqueous emulsion, the emulsifier is castor oil polyoxyethylene ether.
27. The formulation of claim 22, wherein when the formulation is an aqueous emulsion, the defoamer is a silicone.
28. The formulation of claim 7, wherein when the formulation is a microemulsion, the adjuvant comprises at least one of an organic solvent, an emulsifier, and an anti-freeze, and water.
29. The formulation of claim 28, wherein when the formulation is a microemulsion, the organic solvent comprises at least one of cyclohexanone and xylene.
30. The formulation of claim 28, wherein when the formulation is a microemulsion, the emulsifier comprises at least one of agro-emulsion 1601# and agro-emulsion 500#.
31. The formulation of claim 28, wherein when the formulation is a microemulsion, the antifreeze is propylene glycol.
32. Use of a composition according to any one of claims 1 to 6 or a formulation according to any one of claims 7 to 31 for controlling powdery mildew, banded sclerotial blight, wilt, leaf spot, rust, sclerotial blight, rice blast or melon and fruit vegetable anthracnose of cereal crops.
33. A process for the preparation of a composition as claimed in any one of claims 1 to 6, comprising: floreylpicolxamid and fluorophenylamine are combined with optional adjuvants.
34. A method of preparing a formulation as claimed in any one of claims 7 to 31 comprising: floreylpicolxamid and fluorophenylamide are combined with one or more adjuvants.
CN201910860195.XA 2019-09-11 2019-09-11 Composition containing Floreylpicolaminid and fluorophenylamine, preparation and application thereof Active CN112471156B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910860195.XA CN112471156B (en) 2019-09-11 2019-09-11 Composition containing Floreylpicolaminid and fluorophenylamine, preparation and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910860195.XA CN112471156B (en) 2019-09-11 2019-09-11 Composition containing Floreylpicolaminid and fluorophenylamine, preparation and application thereof

Publications (2)

Publication Number Publication Date
CN112471156A CN112471156A (en) 2021-03-12
CN112471156B true CN112471156B (en) 2023-11-03

Family

ID=74920433

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910860195.XA Active CN112471156B (en) 2019-09-11 2019-09-11 Composition containing Floreylpicolaminid and fluorophenylamine, preparation and application thereof

Country Status (1)

Country Link
CN (1) CN112471156B (en)

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019101580A1 (en) * 2017-11-21 2019-05-31 Syngenta Participations Ag Fungicidal compositions

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019101580A1 (en) * 2017-11-21 2019-05-31 Syngenta Participations Ag Fungicidal compositions

Also Published As

Publication number Publication date
CN112471156A (en) 2021-03-12

Similar Documents

Publication Publication Date Title
WO2017118193A1 (en) Fungicidal compound, fungicide composition and preparation and use thereof
CN109964940A (en) A kind of application of miticide composition and its preparation, miticide composition and preparation
CN110352967A (en) A kind of composition, preparation and its application, preparation method
CN112471156B (en) Composition containing Floreylpicolaminid and fluorophenylamine, preparation and application thereof
CN112772663B (en) Composition containing fluoride phenylate amide and penconazole, preparation and application thereof
CN109169676A (en) A kind of bactericidal composition containing Isoflucypram and methoxy acrylic bactericide
CN110856485A (en) Bactericidal composition containing fluophenyl ether amide and trifloxystrobin
CN112056318B (en) Insecticidal composition containing Oxazosulfanyl and antifeedant hydrazine
CN115067348A (en) Compound composition and application thereof in agriculture
SU612606A3 (en) Composition for regulating growth of plants
CN111280170A (en) Bactericidal composition and application thereof
CN110214783B (en) Composition, preparation method and application thereof
CN111165499A (en) Bactericidal composition containing Quinoflumelin and fluorophenylether amide and application and preparation method thereof
CN115067340B (en) Sterilization composition, preparation method and application thereof
CN111357748A (en) Bactericidal composition containing Pyriofenone and fluorobenzene ether amide or chlorobenzene ether amide
CN110859189B (en) Composition, preparation, application and preparation method thereof
CN115039776B (en) Composition containing mandipropamid and preparation method and application thereof
CN112931517A (en) Herbicide composition and application thereof
CN110810420A (en) Bactericidal composition containing fluorobenzene ether amide and myclobutanil
CN115039783B (en) Sterilization composition, preparation method and application thereof
CN110250190A (en) A kind of composition, preparation and its application, preparation method
CN112841204B (en) Composition and/or preparation containing Ipflufenoquin and ipconazole and application thereof
CN115039784B (en) Composition and application thereof in agriculture
CN112088889B (en) Composition containing Pyridachlorometyl and zinc thiazole
CN103190411A (en) Herbicide composite, preparation and application of preparation

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant