CN114467947A - Synergistic bactericidal composition containing quinolone compounds and application thereof - Google Patents

Synergistic bactericidal composition containing quinolone compounds and application thereof Download PDF

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Publication number
CN114467947A
CN114467947A CN202111248358.2A CN202111248358A CN114467947A CN 114467947 A CN114467947 A CN 114467947A CN 202111248358 A CN202111248358 A CN 202111248358A CN 114467947 A CN114467947 A CN 114467947A
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compound
bacterial
disease
bactericidal composition
rice
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CN114467947B (en
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迟会伟
赵宝修
吴建挺
牛纪胜
李文涛
邵莒南
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SHANDONG UNITED PESTICIDE INDUSTRY CO LTD
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SHANDONG UNITED PESTICIDE INDUSTRY CO LTD
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • 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
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/34—Nitriles
    • A—HUMAN NECESSITIES
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    • A01N41/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom
    • A01N41/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom containing a sulfur-to-oxygen double bond
    • 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
    • A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
    • A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
    • 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
    • A01N43/42—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 condensed with carbocyclic rings
    • 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
    • A01N43/60—1,4-Diazines; Hydrogenated 1,4-diazines
    • 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
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/74—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,3
    • A01N43/78—1,3-Thiazoles; Hydrogenated 1,3-thiazoles
    • 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
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
    • 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
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/82—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with three ring hetero atoms
    • 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
    • A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
    • 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
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
    • A01N47/18—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing a —O—CO—N< group, or a thio analogue thereof, directly attached to a heterocyclic or cycloaliphatic ring
    • 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
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16—Heavy metals; Compounds thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P3/00—Fungicides

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Abstract

The invention relates to a synergistic bactericidal composition containing quinolone compounds and application thereof. The bactericide composition comprises effective active ingredients, wherein the effective active ingredients comprise a compound I and a compound II, the compound I is 7-chloro-1-cyclopropyl-6-fluoro-4-oxo-1, 4-dihydroquinoline-3-carboxylic acid-2-methoxyethyl ester, and the compound II is at least one of antibiotic compounds, thiazole zinc, benziothiazolinone, bromothalonil, amino-oligosaccharin, emodin methyl ether, isothiazolinone and dithiocyano-methane. The synergistic bactericidal composition has the following advantages: 1) has synergistic effect and can improve the control effect; 2) the bactericidal spectrum is expanded, and the field diseases are mixed, so that the bactericidal composition has stronger effect on bacterial diseases; 3) the two effective components have different action mechanisms, and can delay the generation of drug resistance of pathogenic bacteria by mixing; 4) the application amount is reduced, the use times are reduced, and the use cost is reduced.

Description

Synergistic bactericidal composition containing quinolone compounds and application thereof
Technical Field
The invention belongs to the technical field of pesticide compounding, and particularly relates to a synergistic bactericidal composition containing quinolone compounds and application thereof.
Background
In recent years, the occurrence of various crop bacterial diseases shows a trend of increasing year by year, the occurrence area increases year by year, and great harm is brought to agricultural production, for example, bacterial leaf spot of rice in grain crops, bacterial leaf blight of rice, canker of citrus in fruit trees, bacterial wilt of solanaceae vegetables, bacterial angular leaf spot of cucumber, soft rot of brassicaceae vegetables, ginger blast and the like all cause serious loss to crops.
At present, the high-efficiency medicament for preventing and treating bacterial diseases is lacking in the market, and the unscientific medicament application, which increases the dosage or mixes the medicament randomly in order to improve the prevention and treatment effect, cannot achieve the synergistic effect, but causes the problems of pesticide waste, overproof residue, environment pollution, generation of resistance of germs to the pesticide and the like. Therefore, there is a need to develop a synergistic bactericidal composition against bacterial diseases, which can achieve the effects of expanding the control target range, reducing the dosage and delaying the generation of resistance.
In the actual process of agricultural production, the pathogenic bacteria can quickly generate drug resistance after long-term continuous and single use of the same medicament, so that the prevention effect is reduced, the use amount of pesticides is increased, and the pesticide residue of agricultural products and the damage to the ecological environment are aggravated. By compounding with the fungicide variety with completely different action mechanisms, the bactericide is an effective way for delaying the generation of drug resistance of pathogenic bacteria, expanding the bactericidal spectrum, prolonging the service life and reducing the use amount of pesticides. However, it is a difficult point to compound drugs so that the drugs can generate synergy rather than antagonism.
The chemical name of the quinolone compound is: 7-chloro-1-cyclopropyl-6-fluoro-4-oxo-1, 4-dihydroquinoline-3-carboxylic acid-2-methoxyethyl ester, which has broad-spectrum bactericidal activity, particularly higher bacterial activity, and excellent activity on both gram-positive bacteria and gram-negative bacteria. For various crop bacterial diseases, such as soft rot of various crops including soft rot of Chinese cabbage, black rot of Chinese cabbage, bacterial angular leaf spot of cucumber, angular leaf spot of sesame, west/melon fruit blotch, bacterial leaf blight of rice, bacterial leaf streak of rice, bacterial brown spot of rice, bacterial basal rot of rice, solanaceae bacterial wilt of tomato bacterial wilt, mulberry bacterial wilt, peanut bacterial wilt, ginger blast, tomato/pepper bacterial spot, pepper bacterial leaf spot, potato black shank, bacterial blight of corn, bacterial stem rot of corn, black glume of wheat, bacterial leaf blight of soybean, bacterial blight of cassava, mango angular leaf spot, citrus canker, bacterial perforation of peach tree, sunflower stem rot, peach gummosis, pear fire blight, pear rust disease, bacterial root canker of fruit tree, etc, The pathogenic bacteria such as potato ring rot, bean wilt, wheat white leaf streak, potato scab, tomato canker, and American winter green leaf blight all have excellent activity.
Zhongshengmycin, kasugamycin, benziothiazolinone, tetramycin, ethylicin, aureonucleomycin, zinc thiazole, shenqinmycin, hydromycin, bromothalonil, neophytomycin, polyoxin, agricultural streptomycin, agricultural antibiotic 120, validamycin, pyrimidine nucleoside antibiotic, ningnanmycin, cnidium lactone, oligosaccharins, amino oligosaccharins, garlicin and physcion are common medicaments for preventing and treating bacterial diseases at present, but the resistance appears to different degrees due to long-term single use, and the prevention effect is reduced.
In the prior art, no reports related to compounding and application of quinolone compounds and zhongshengmycin, kasugamycin, zinc thiazole, benziothiazolinone, tetramycin, ethylicin, shenqinmycin, aureonycin, hydromycin, bromothalonil, neophytomycin, polyoxin, agricultural streptomycin, agricultural antibiotic 120, validamycin, pyrimidine nucleoside antibiotics, ningnanmycin, cnidium lactone, oligosaccharins, amino oligosaccharins, allicin and physcion are found, and no reports related to compounding and application of similar substances are found.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a synergistic bactericidal composition containing quinolone compounds and application thereof, wherein the bactericidal composition comprises effective components, and the effective components comprise a compound I and a compound II, wherein the compound I is 7-chloro-1-cyclopropyl-6-fluoro-4-oxo-1, 4-dihydroquinoline-3-carboxylic acid-2-methoxyethyl ester, and the compound II is zhongshengmycin, kasugamycin, tetramycin, ethylicin, shenqinmycin, aureonycin, hydromycin, garlicin, amino-oligosaccharin, neophytycin, polyoxin, streptomycin for agriculture, agrimoninomycin 120, jinggangmycin, pyrimidine nucleoside antibiotic, ningnanmycin, osthole, oligosaccharin and other antibiotic compounds and zinc thiazole, At least one of benziothiazolinone, bromothalonil, physcion, isothiazolinone and methylene dithiocyanate.
The compound I and the compound II are mixed to form a synergistic bactericidal composition, the effective active ingredients comprise the compound I and the compound II, the mixture of the compound I and the compound II has obvious synergistic and complementary effects, and the compound can act on multiple sites of pathogenic bacteria by utilizing the difference of action sites and action mechanisms of the pathogenic bacteria, so that the bactericidal spectrum is expanded, the control effect is improved, the pesticide use amount is reduced, the generation of drug resistance is delayed, and the cost can be reduced.
The invention adopts the following scheme:
the bactericide composition comprises effective active ingredients, wherein the effective active ingredients comprise a compound I and a compound II, the compound I is 7-chloro-1-cyclopropyl-6-fluoro-4-oxo-1, 4-dihydroquinoline-3-carboxylic acid-2-methoxyethyl ester, and the compound II is at least one of antibiotic compounds, zinc thiazole, benziothiazolinone, bromothalonil, amino-oligosaccharin, physcion, isothiazolinone and thiocyanomethane.
According to an embodiment of the present invention, the antibiotic compound is at least one selected from the group consisting of zhongshengmycin, kasugamycin, tetramycin, ethylicin, aureomycin, shenqimycin, hydromycin, allicin, neomycin, polyoxin, streptomycin for agricultural use, 120-pesticide, validamycin, pyrimidine nucleoside antibiotics, ningnanmycin, cnidium lactone, oligosaccharins, and the like.
According to the embodiment of the invention, the mass ratio of the compound I to the compound II is 80-1: 1-80.
According to the embodiment of the invention, the mass ratio of the compound I to the compound II is 50-1: 1-50.
According to the embodiment of the invention, the mass ratio of the compound I to the compound II is 30-1: 1-30.
According to an embodiment of the invention, the mass ratio of compound I and compound II is 80:1, 75:1, 70:1, 65:1, 60:1, 55:1, 50:1, 45:1, 40:1, 35:1, 30:1, 25:1, 20:1, 15:1, 10:1, 5:1, 1:5, 1:10, 15:1, 1:20, 25:1, 1:30, 35:1, 1:40, 45:1, 1:50, 55:1, 1:60, 65:1, 1:70, 75:1, 1: 80.
According to an embodiment of the present invention, the sum of the mass of the compound I and the compound II in the bactericidal composition is 1 to 80%, preferably 20 to 60%, such as 1%, 5%, 8%, 10%, 13%, 15%, 18%, 20%, 24%, 30%, 35%, 38%, 42%, 45%, 50%, 55%, 60%, 65%, 68%, 75%, 80%, 85%, 90%, based on 100% of the total weight of the bactericidal composition.
According to an embodiment of the present invention, the germicidal composition may be prepared in a liquid formulation or a solid formulation.
According to the embodiment of the present invention, the content range of the effective active ingredient in the preparation varies according to different preparation types, and generally, the liquid preparation contains 1 to 60% by weight of the effective active ingredient, preferably 5 to 50%; the solid preparation contains 5-80% of effective active ingredients by weight, preferably 10-70%.
According to an embodiment of the present invention, the bactericidal composition further includes at least one of an emulsifier, a dispersant, a wetting agent, a thickener, an antifoaming agent, a stabilizer, a binder, a disintegrant, an anti-freeze agent, an anti-caking agent, a suspending agent, a film-forming agent, a preservative, a coloring agent, a polymeric wall material, a pH adjuster, a filler, or the like.
According to an embodiment of the present invention, the germicidal composition may be diluted or used directly by a user before use. The preparation method can be prepared by processing methods known by those skilled in the art, namely mixing the effective active ingredients with one or more of deionized water, organic solvents, emulsifiers, dispersing agents, wetting agents, thickening agents, defoaming agents, stabilizing agents, binders, disintegrating agents, anti-freezing agents, anti-caking agents, suspending agents, film forming agents, preservatives, coloring agents, high molecular capsule wall materials, pH regulators or fillers to prepare the bactericidal composition.
According to the preparation provided by the invention, the bactericidal composition can be prepared into various dosage forms, and preferably, the dosage forms comprise water dispersible granules, dispersible agents, wettable powder, suspending agents, aqueous emulsion, microemulsion, suspoemulsion, microcapsule suspending agents, microcapsule suspension-suspending agents, suspended seed coating agents, missible oil and granules.
According to the embodiment of the invention, the bactericidal composition comprises the following components in percentage by weight when prepared into wettable powder: 1-80% of compound I, 1-80% of compound II, 1-12% of dispersing agent, 1-8% of wetting agent and the balance of filler.
According to the embodiment of the invention, the composition comprises the following components in percentage by weight when prepared into water dispersible granules: 1-80% of compound I, 1-80% of compound II, 1-12% of dispersing agent, 1-8% of wetting agent, 1-10% of disintegrating agent and the balance of filler.
According to the embodiment of the invention, the composition is prepared into a suspending agent and comprises the following components in percentage by weight: 1 to 50 percent of compound I, 1 to 50 percent of compound II, 1 to 12 percent of dispersant, 1 to 10 percent of wetting agent, 0.1 to 8 percent of thickening agent, 0.1 to 8 percent of antifreeze agent and the balance of deionized water.
According to the embodiment of the invention, the composition is prepared into an aqueous emulsion and comprises the following components in percentage by weight: 1 to 50 percent of compound I, 1 to 50 percent of compound II, 1 to 60 percent of organic solvent, 1 to 12 percent of emulsifier, 0.1 to 8 percent of antifreeze agent, 0.01 to 2 percent of defoaming agent, 0.1 to 2 percent of thickening agent and the balance of deionized water.
According to the embodiment of the invention, the composition is prepared into a suspended seed coating and comprises the following components in percentage by weight: 1-50% of compound I, 1-50% of compound II, 1-12% of dispersing agent, 1-10% of wetting agent, 1-10% of antifreeze agent, 0.1-10% of anticaking agent, 0.1-5% of suspending agent, 1-10% of film forming agent, 0.1-5% of preservative, 1-30% of colorant, 0.1-5% of pH regulator, 0.1-8% of thickening agent and the balance of deionized water.
According to the embodiment of the invention, the composition is prepared into a microcapsule suspension agent and comprises the following components in percentage by weight: 1-50% of compound I, 1-50% of compound II, 1-30% of polymer capsule wall material, 2-10% of dispersing agent, 1-50% of organic solvent, 1-7% of emulsifier, 0.1-5% of pH regulator, 0.01-2% of defoaming agent, 0.1-8% of thickening agent, 0.1-8% of antifreeze agent and the balance of deionized water.
According to an embodiment of the invention, the composition is prepared into a microcapsule suspension-suspending agent and comprises the following components in percentage by weight: 1-50% of compound I, 1-50% of compound II, 1-12% of polymer capsule wall material, 1-12% of dispersant, 1-8% of wetting agent, 1-50% of organic solvent, 1-8% of emulsifier, 0.01-2% of defoamer, 0.1-8% of thickener, 0.1-5% of pH regulator, 0.1-8% of antifreeze agent and the balance of deionized water.
According to the embodiment of the invention, the composition is prepared into missible oil and comprises the following components in percentage by weight: 1-50% of compound I, 1-50% of compound II, 1-50% of organic solvent, 1-30% of emulsifier, 1-10% of antifreeze agent, 0.1-5% of stabilizer and the balance of organic solvent.
According to the embodiment of the invention, the composition is prepared into microemulsion and comprises the following components in percentage by weight: 1-50% of compound I, 1-50% of compound II, 1-50% of organic solvent, 1-30% of emulsifier, 1-10% of antifreeze agent, 0.1-5% of stabilizer and the balance of deionized water.
According to an embodiment of the invention, the composition is prepared into a dispersible agent and comprises the following components in percentage by weight: 1-50% of compound I, 1-50% of compound II, 1-30% of emulsifier, 1-10% of antifreeze agent, 0.1-5% of stabilizer and the balance of organic solvent.
According to the embodiment of the invention, the composition comprises the following components in percentage by weight when prepared into granules: 0.5-10% of compound I, 0.5-10% of compound II, 1-12% of dispersing agent, 1-10% of wetting agent, 0.1-8% of binder and the balance of filler.
According to an embodiment of the present invention, the emulsifier may be selected from one of the following: one or more of sodium lignosulfonate, agricultural emulsion, phenyl phenol polyoxyethylene ether phosphate, tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt, benzyl dimethyl phenol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether, sorbitan oleate (span-80), fatty alcohol polyoxyethylene ether, sodium alkyl naphthalene sulfonate, isooctyl alcohol succinate sodium sulfonate, nonylphenol polyoxyethylene ether phosphate and castor oil polyoxyethylene ether phosphate.
According to an embodiment of the present invention, the dispersant may be selected from: glycerol fatty acid polyoxyethylene ether, polyoxyethylene alkyl aryl ether, sodium lignosulfonate, a naphthalene sulfonate formaldehyde condensate, fatty alcohol polyoxyethylene ether sulfate, a naphthalene sulfonate formaldehyde condensate sodium salt, nonylphenol polyoxyethylene ether, polyoxyethylene lanolin alcohol, an alkylphenol polyoxyethylene ether formaldehyde condensate, fatty alcohol polyoxyethylene ether phosphate, polyoxyethylene sorbitan fatty acid ester and one or more of phosphate.
According to an embodiment of the present invention, the wetting agent may be selected from: trisiloxane polyoxyethylene ether, N-lauroyl sodium glutamate, sodium lauryl sulfate, sodium lauroyl sarcosinate, a methyl naphthalene sulfonate formaldehyde condensate, castor oil polyoxyethylene ether, triphenyl ethylphenol polyoxyethylene ether, sodium dodecyl benzene sulfonate, alkyl naphthalene sulfonate, isooctyl alcohol succinate sodium sulfonate, polyoxyethylene alkyl aryl ether, fatty alcohol polyether glycerol fatty acid polyoxyethylene ether and fatty alcohol polyoxyethylene ether.
According to an embodiment of the present invention, the binder may be selected from: xanthan gum, starch, urea-formaldehyde resin, gelatin, Arabic gum, carboxymethyl cellulose, carboxyethyl cellulose, and polyvinyl alcohol.
According to an embodiment of the invention, the disintegrant may be selected from: one or more of sodium bicarbonate, ammonium sulfate, sodium sulfate, calcium sulfate and magnesium chloride.
According to an embodiment of the present invention, the thickener may be selected from: one or more of magnesium aluminum silicate, polyvinyl acetate, xanthan gum, gelatin, arabic gum and polyvinyl alcohol.
According to an embodiment of the present invention, the defoaming agent may be selected from: one or more of silicone oil, n-octanol, silicone, butyl phosphate, isobutyl phosphate and the like.
According to an embodiment of the invention, the antifreeze agent can be selected from: one or more of propylene glycol, ethylene glycol, glycerol, and the like.
According to an embodiment of the invention, the stabilizer may be selected from: one or more of triethanolamine, epichlorohydrin, butyl glycidyl ether, triphenyl phosphite, N-soybean oil-based trimethylene diamine, dialkyl succinic acid acetate sulfonate and the like.
According to an embodiment of the present invention, the filler includes a solid filler and a liquid filler, wherein the solid filler can be selected from: one or more of kaolin, attapulgite, diatomite, white carbon black, bentonite, montmorillonite, calcium carbonate and talcum powder. The liquid filler can be one or more of soybean oil, castor oil and mineral oil.
According to an embodiment of the present invention, the organic solvent may be selected from: one or more of ethyl acetate, acetone, isopropanol, 2,2, 2-trifluoroethanol, propylene carbonate, benzene, toluene, xylene, dimethylformamide, dimethyl sulfoxide, dichloromethane, cyclohexane, cyclohexanone, N-methylpyrrolidone and solvent oil (such as No. 150 solvent oil).
The bactericidal composition is used for preventing and treating pathogenic bacteria and agricultural diseases caused by the pathogenic bacteria, and is particularly suitable for bacteria and plant bacterial diseases caused by the bacteria.
According to an embodiment of the invention, the bactericidal composition is used for controlling soft rot of crops such as soft rot of Chinese cabbage, black rot of Chinese cabbage, bacterial angular leaf spot of cucumber, sesame angular leaf spot, west/melon fruit blotch, bacterial leaf blight of rice, bacterial leaf streak of rice, bacterial brown spot of rice, bacterial brown strip disease of rice, bacterial basal rot of rice, solanaceae bacterial wilt such as tomato bacterial wilt, mulberry bacterial wilt, peanut bacterial wilt, ginger blast, tomato/pepper bacterial spot disease, pepper bacterial leaf spot disease, potato black shank, corn bacterial blight, corn bacterial stem rot, wheat black glume, soybean bacterial leaf blight, soybean bacterial blight, cassava bacterial blight, mango angular leaf spot, citrus canker, peach bacterial puncture disease, sunflower bacterial rot, peach gummosis, pear fire blight, pear bacterial blight, etc, Pear rust disease, fruit tree bacterial root cancer, potato ring rot, kidney bean wilt, wheat white leaf streak, potato scab, tomato canker, American winter green leaf blight and other pathogenic bacteria, cucumber downy mildew, cucumber target spot, rice blast, rice sheath blight, tomato virus disease and other pathogenic fungi and virus diseases.
The invention also provides a method for preventing and controlling pathogenic bacteria and agricultural diseases caused by the pathogenic bacteria, in particular bacteria and bacterial diseases of plants caused by the bacteria, which comprises applying the bactericidal composition on the plants with the diseases.
The bactericidal composition can be provided in the form of a finished preparation or a single agent, is directly mixed before use, is mixed with water to be mixed uniformly to obtain the required concentration, and can be applied to plants or crops in any mode, such as spraying, irrigating the roots of the plants, smearing and the like. For specific applications, it may also be used in combination with other agents such as insecticides, growth regulators, soil conditioners, herbicides, nematicides, and the like.
The invention has the beneficial effects that:
the synergistic bactericidal composition has the following advantages:
1) has synergistic effect and can improve the control effect; 2) the bactericidal spectrum is expanded, and the field diseases are mixed, so that the bactericidal composition has stronger effect on bacterial diseases; 3) the two effective components have different action mechanisms, and can delay the generation of drug resistance of pathogenic bacteria by mixing; 4) the application amount is reduced, the use times are reduced, and the use cost is reduced.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
The invention adopts a method combining indoor biological measurement and field test to carry out performance test on the sterilization effect of the sterilization composition. It should be understood that any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
First, preparation example:
preparation example 1: wettable powder
Figure BDA0003321861980000071
The materials are coarsely crushed according to a certain proportion and then are put into a mixer to be mixed evenly, and then the finished product is obtained after the materials are crushed by airflow.
Preparation example 2: water dispersible granule
Figure BDA0003321861980000072
The effective active ingredients and various auxiliary agents are uniformly mixed according to the proportion of the formula, powder is obtained after air flow crushing, a certain amount of water is added for mixing, extruding and granulating, and the finished product is obtained after drying and screening.
Preparation example 3: suspending agent
Figure BDA0003321861980000073
Figure BDA0003321861980000081
The effective active ingredients and various auxiliary agents are uniformly mixed according to the proportion of the formula, and the finished product is obtained after high-speed shearing and sanding.
Preparation example 4: emulsifiable concentrates
Figure BDA0003321861980000082
Mixing the raw materials in proportion to dissolve the raw materials into a uniform oil phase; and after the inspection is qualified, metering and subpackaging to obtain the finished product.
Preparation example 5: aqueous emulsion
Figure BDA0003321861980000083
According to the formula requirements, the raw materials are added into a batching kettle, uniformly mixed by a high-speed shearing machine to prepare the aqueous emulsion, and the finished product is obtained by metering and subpackaging after the inspection is qualified.
Preparation example 6: emulsifiable concentrate
Figure BDA0003321861980000084
Figure BDA0003321861980000091
Mixing the raw materials in proportion to dissolve the raw materials into a uniform oil phase; and after the inspection is qualified, metering and subpackaging to obtain the finished product.
Preparation example 7: emulsifiable concentrate
Figure BDA0003321861980000092
Mixing the raw materials in proportion to dissolve the raw materials into a uniform oil phase; and after the inspection is qualified, metering and subpackaging to obtain the finished product.
Preparation example 8: granules
Figure BDA0003321861980000093
Fully mixing the components according to the formula proportion, crushing, adding water for wetting, fully and uniformly stirring, granulating by using a screw extrusion granulator, drying and sieving to obtain the finished product.
Second, indoor virulence determination example
(1) Pathogenic bacteria to be tested: chinese cabbage soft rot, cucumber bacterial angular leaf spot, watermelon fruit spot, rice white leaf spot, rice bacterial stripe spot, tomato bacterial wilt, potato black shank, mango angular leaf spot, citrus canker, peach bacterial perforation and potato scab.
(2) The determination method comprises the following steps:
method for measuring bacterial virulence
The pathogenic bacteria toxicity determination uses cabbage soft rot pathogen, cucumber bacterial angular leaf spot pathogen, watermelon fruit spot pathogen, rice white leaf blight pathogen, rice bacterial streak pathogen, tomato ralstonia solanacearum, potato black shank pathogen, mango angular leaf spot pathogen, citrus canker pathogen, peach tree bacterial perforation pathogen, potato scab pathogen and other bacterial diseases as test materials, and adopts an in vitro turbidity method to perform toxicity determination on the compound I, the compound II and the mixed preparation thereof.
Referring to the agricultural industry standard NY/T1156.16-2008 of the people's republic of China, the reagent (including compound I and compound II) is first prepared into 7 concentration gradients (7 concentration gradients such as compound I: 0.5,1.0,2.0,4.0,8.0,16.0,32.0 μ g/mL, etc.; compound II: 0.5,1.0,2.0,4.0, 16.0,32.0 μ g/mL, etc.) with appropriate solvents (the types of solvents are acetone, methanol, N-dimethylformamide, dimethyl sulfoxide, etc., and are selected according to the dissolving capacity of the solvents on samples), and the compound I and the compound II to be mixed are respectively prepared according to the EC of the compound I and the compound II50The values are set into a series of proportions according to mass proportion, and 7 series concentrations with final mass concentration (referring to the total mass of the compound I and the compound II) of 0.5,1.0,2.0,4.0,8.0,16.0 and 32.0 mu g/mL are prepared according to different proportions.
Under aseptic conditions, equally packaging NB (nutrient broth containing 10g of peptone, 3g of beef extract and 5g of sodium chloride per liter) culture solution into test tubes, quantitatively sucking medicinal liquid from low concentration to high concentration in sequence, respectively adding into the test tubes, shaking up, respectively adding bacterial suspension in logarithmic phase in equal amount, and repeating for 4 times each treatment. After mixing, placing the mixture in a shaking incubator at 25 ℃ for dark culture, and measuring the OD value in the logarithmic growth phase. Taking the average of effective 4 replicates as the measurement result, calculating the relative inhibition rate, converting the inhibition rate into a probability value (y), converting the drug solution concentration (. mu.g/mL) into a logarithm value (x), and obtaining the inhibition rate by the least square methodRegression equation of virulence (y ═ a + bx) and from this the EC for each agent was calculated50The value is obtained. Simultaneously, the combined Synergistic Ratio (SR) of the two medicaments in different proportions is calculated according to the Wadley method, and the SR<0.5 is antagonistic action, 0.5-1.5 is additive action, SR is>1.5 is synergistic effect. The calculation formula is as follows:
SR＝EC50(theoretical value)/EC50(actual measurement value)
EC50(theoretical value) ═ EC of (a + b)/[ (a/A)50) + (EC of B/B50)
In the formula: a is a compound I, and B is a compound II; a. b is the proportion of the compound I and the compound II in the bactericidal composition respectively;
when mixed, different varieties of pesticides often exhibit three types of action, namely additive, synergistic and antagonistic, but the specific type of action cannot be predicted. The bactericidal composition provided by the invention takes the compound I and the compound II as effective active ingredients, and biological assay examples are adopted for illustration.
Example 1: in order to verify the bacteriostatic effect of the compound I and the zhongshengmycin on the cucumber bacterial angular leaf spot germs in different proportions, the indoor toxicity of the compound I and the zhongshengmycin on the cucumber bacterial angular leaf spot germs is determined, corresponding concentrations are prepared according to the weight percentages in a table, indoor bacteriostatic tests are carried out, and the test results are as follows:
TABLE 1 toxicity test results of single dose of compound I and zhongshengmycin and its mixture for cucumber bacterial angular leaf spot
Figure BDA0003321861980000101
Figure BDA0003321861980000111
The results in Table 1 show that the compound I and the zhongshengmycin which are mixed in different proportions have obvious synergistic effect on the inhibition of the cucumber bacterial angular leaf spot germs.
Example 2: in order to verify the bacteriostatic effect of the compound I and the zhongshengmycin on the alternaria citrulli, the indoor toxicity of the compound I and the zhongshengmycin on the alternaria citrulli is determined according to different proportions, corresponding concentrations are prepared according to the weight percentages in a table, and an indoor bacteriostatic test is carried out, wherein the test result is as follows:
TABLE 2 toxicity test results of single dose of compound I and zhongshengmycin and its mixture to watermelon fruit blotch
Figure BDA0003321861980000112
Figure BDA0003321861980000121
The results in Table 2 show that the compound I and the zhongshengmycin have obvious synergistic effect on inhibiting the watermelon fruit blotch germs in different proportioning and dosage.
Example 3: in order to verify the bacteriostatic effect of the compound I and the zhongshengmycin on the citrus canker germs in different proportions, the indoor toxicity of the compound I and the zhongshengmycin on the citrus canker germs is determined, corresponding concentrations are prepared according to the weight percentages in a table, and indoor bacteriostatic tests are carried out, wherein the test results are as follows:
TABLE 3 toxicity assay results of compound I and zhongshengmycin single agent and mixture thereof on citrus canker pathogen
Figure BDA0003321861980000122
The results in table 3 show that the compound I and the zhongshengmycin have obvious synergistic effect on the inhibition of citrus canker pathogen when mixed in different proportions.
Example 4: in order to verify the bacteriostatic effect of the compound I and the zhongshengmycin on the rice bacterial blight, the indoor toxicity of the compound I and the zhongshengmycin on the rice bacterial blight is determined according to different proportions, corresponding concentrations are prepared according to the weight percentages in a table, and an indoor bacteriostatic test is carried out, wherein the test results are as follows:
TABLE 4 toxicity test results of compound I and zhongshengmycin single agent and mixture thereof on rice leaf blight germ
Figure BDA0003321861980000123
Figure BDA0003321861980000131
The results in Table 4 show that the compound I and the zhongshengmycin which are mixed according to different proportions have obvious synergistic effect on the inhibition of the rice bacterial blight.
Example 5: in order to verify the bacteriostatic effect of the compound I and the zhongshengmycin on the ralstonia solanacearum, the indoor toxicity of the compound I and the zhongshengmycin on the ralstonia solanacearum is determined according to different proportions, corresponding concentrations are prepared according to the weight percentages in a table, and an indoor bacteriostatic test is carried out, wherein the test result is as follows:
TABLE 5 toxicity test results of compound I and zhongshengmycin single dose and mixed dose on ralstonia solanacearum
Figure BDA0003321861980000132
Figure BDA0003321861980000141
The results in Table 5 show that the compound I and the zhongshengmycin have obvious synergistic effect on inhibiting the ralstonia solanacearum when mixed in different proportions.
Example 6: in order to verify the bacteriostatic effect of the compound I and the zhongshengmycin on the Chinese cabbage soft-rot fungi, the indoor toxicity of the compound I and the zhongshengmycin on the Chinese cabbage soft-rot fungi is determined according to different proportions, corresponding concentrations are prepared according to the weight percentages in a table, an indoor bacteriostatic test is carried out, and the test results are as follows:
TABLE 6 toxicity test results of compound I and zhongshengmycin single agent and mixture thereof on Chinese cabbage soft rot pathogen
Figure BDA0003321861980000142
As can be seen from the table above, the compound I, the zhongshengmycin and the mixed preparation thereof have obvious synergistic effect on inhibiting the Chinese cabbage soft rot pathogen.
Example 7: in order to verify the bacteriostatic effect of the compound I and the allicin in different proportions on the cucumber bacterial angular leaf spot germs, the indoor toxicity of the compound I and the allicin in different proportions on the cucumber bacterial angular leaf spot germs is determined, corresponding concentrations are prepared according to the weight percentages in the table, indoor bacteriostatic tests are carried out, and the test results are as follows:
TABLE 7 toxicity test results of single dose of compound I and allicin and its mixture on cucumber bacterial angular leaf spot
Figure BDA0003321861980000143
Figure BDA0003321861980000151
As can be seen from the table above, the compound I, the allicin and the mixed preparation thereof have obvious synergistic effect on the inhibition of the cucumber bacterial angular leaf spot germs.
Example 8: in order to verify the bacteriostatic effect of the compound I and the zinc thiazole on the alternaria citrulli in different proportions, the indoor toxicity of the compound I and the zinc thiazole on the alternaria citrulli is determined, corresponding concentrations are prepared according to the weight percentages in a table, and an indoor bacteriostatic test is carried out, wherein the test result is as follows:
TABLE 8 toxicity test results of compound I and zinc thiazole on watermelon fruit blotch
Figure BDA0003321861980000152
As can be seen from the table above, the compound I, the zinc thiazole and the mixed preparation thereof have obvious synergistic effect on the inhibition of the fruit blotch of watermelon.
Example 9: in order to verify the bacteriostatic effect of the compound I and the tetramycin on the rice bacterial leaf streak pathogens in different proportions, the indoor toxicity of the compound I and the tetramycin on the rice bacterial leaf streak pathogens is determined, corresponding concentrations are prepared according to the weight percentages in a table, indoor bacteriostatic tests are carried out, and the test results are as follows:
TABLE 9 toxicity test results of single dose of compound I and tetramycin and mixture thereof on rice bacterial streak germ
Figure BDA0003321861980000161
As can be seen from the table above, the compound I, the tetramycin and the mixed preparation thereof have obvious synergistic effect on inhibiting the rice bacterial leaf streak germs.
Example 10: in order to verify the bacteriostatic effect of the compound I and the benziothiazolinone in different proportions on the scab bacteria of the potatoes, the indoor toxicity of the compound I and the benziothiazolinone in different proportions on the scab bacteria of the potatoes is determined, corresponding concentrations are prepared according to the weight percentages in the table, and an indoor bacteriostatic test is carried out, wherein the test results are as follows:
TABLE 10 toxicity test results of compound I and benziothiazolinone single dose and its mixture on potato scab
Figure BDA0003321861980000162
Figure BDA0003321861980000171
As shown in the table, the compound I, the benziothiazolinone and the mixed preparation thereof have obvious synergistic effect on the inhibition of the scab bacteria of the potatoes.
Example 11: in order to verify the bacteriostatic effect of the compound I and the kasugamycin on the potato phytophthora parasitica in different proportions, the indoor toxicity of the compound I and the kasugamycin on the potato phytophthora parasitica is determined in different proportions, corresponding concentrations are prepared according to the weight percentages in a table, an indoor bacteriostatic test is carried out, and the test results are as follows:
TABLE 11 determination of potatosis virus of compound I and kasugamycin single dose and their mixture
Figure BDA0003321861980000172
As shown in the table, the compound I, the kasugamycin and the mixed preparation thereof have obvious synergistic effect on the inhibition of the potato phytophthora parasitica.
Example 12: in order to verify the bacteriostatic effect of the compound I and the neomycin on the mango angular leaf spot germs in different proportions, the indoor toxicity of the compound I and the neomycin on the mango angular leaf spot germs in different proportions is determined, corresponding concentrations are prepared according to the weight percentages in a table, indoor bacteriostatic tests are carried out, and the test results are as follows:
TABLE 12 toxicity test results of single dose of compound I and neomycin and mixed dose thereof on mango angular leaf spot
Figure BDA0003321861980000181
As shown in the table, the compound I, the neophytomycin and the mixed preparation thereof have obvious synergistic effect on the inhibition of mango angular leaf spot.
Example 13: in order to verify the bacteriostatic effect of the compound I and the aureonucleomycin on the peach bacterial leaf spot germs in different proportions, the indoor toxicity of the compound I and the aureonucleomycin in different proportions on the peach bacterial leaf spot germs is determined, corresponding concentrations are prepared according to the weight percentages in the table, indoor bacteriostatic tests are carried out, and the test results are as follows:
TABLE 13 toxicity test results of single dose of compound I and aureonucleomycin and its mixture for peach tree bacterial perforator
Figure BDA0003321861980000182
Figure BDA0003321861980000191
As shown in the table, the compound I, the aureonucleomycin and the mixed preparation thereof have obvious synergistic effect on the inhibition of the peach bacterial leaf-piercing bacteria.
Third, field drug effect examples
In order to determine the control effects of single agents and mixed agents of the compound I and the compound II on bacterial angular leaf spot of cucumber, citrus canker, watermelon fruit blotch, tobacco wildfire, ginger blast, kiwifruit canker, pear fire blight, fruit tree bacterial root cancer, corn bacterial stem rot, citrus yellow dragon disease, tomato canker, corn bacterial wilt, tomato bacterial wilt, rice bacterial blight and other bacterial diseases, a plurality of pesticide effect tests are carried out in different regions in China.
The reagents in the following examples were prepared as described in the above preparations 1 to 8, and illustratively, the wettable 10% compound I · zhongshengmycin powder of example 1 was prepared in the same manner as in preparation 1, wherein compound II was selected from zhongshengmycin, and the wettable 10% compound I · zinc thiazole powder of example 8 was prepared in the same manner as in preparation 1, wherein compound II was selected from zinc thiazole, and similarly, other examples were prepared by referring to the above preparations 1 to 8.
The reagents of the respective proportions described below were prepared in the same manner as described in the above-mentioned preparation examples 1 to 8, except that the active ingredient content may vary, and that the formulation was filled to 100% with filler or water. For example, the preparation method of the 10% compound I water dispersible granule of the comparative example 1 refers to the preparation example 2, wherein 10% compound I replaces 20% compound I and 10% compound II in the preparation example 2, and the difference of the content is filled by the filler. For another example, the wettable powder of 3% Zhongshengmycin of comparative example 2 was prepared by referring to preparation example 1, in which 3% Zhongshengmycin was substituted for 5% Compound I and 5% Compound II in preparation example 1, and the difference in the contents was filled by the filler.
Field efficacy test of cucumber bacterial angular leaf spot (developed in Shandong chatting Guangxian county):
the test method comprises the following steps: according to the medicine application method specified in the national standard GB/T17980.110-2004 of the people's republic of China, the medicine is applied when scabs are seen at first, the medicine is applied for the 2 nd time after 7 days, the medicine is applied for two times, and the times are repeated for 4 times.
The investigation method comprises the following steps: according to the investigation method specified in the national standard GB/T17980.110-2004 of the people's republic of China, the control effect is investigated 7 days and 14 days after the 2 nd application. The diagonal of each cell was sampled at 3 points, and 5 plants at each point were examined for all leaves, and the lesion area per leaf was graded as a percentage of the total leaf area.
The grading method comprises the following steps:
no disease spot at level 0; grade 1, the lesion area accounts for less than 5% of the whole leaf area; grade 3, the lesion area accounts for 6 to 10 percent of the whole leaf area; grade 5, the lesion area accounts for 11 to 20 percent of the whole leaf area; 7 grade, the lesion area accounts for 21 to 50 percent of the whole leaf area; grade 9, the lesion area accounts for more than 51 percent of the whole leaf area.
TABLE 14 field test of efficacy of Compound I in combination with Zhongshengmycin against cucumber bacterial angular leaf spot
Figure BDA0003321861980000201
Note: different letters after the same column of data indicate significant differences at a P <0.05 level as tested by Duncan's new double-pole-difference method, the same below.
The determination results in the table show that when the compound I is used for preventing and treating the cucumber bacterial angular leaf spot, compared with the compound preparation of the zhongshengmycin and the single preparation, under the same effective component dosage, the compound preparation of the compound I and the zhongshengmycin has the effect of preventing the cucumber bacterial angular leaf spot for 7 days and the effect of preventing the cucumber bacterial angular leaf spot for 14 days which are obviously higher than the single preparation. Wherein the control effect can still reach more than 78.5 percent in 14 days, and the lasting period is longer.
TABLE 15 field test of the efficacy of Compound I in combination with Zinc thiazole on cucumber bacterial angular leaf spot
Figure BDA0003321861980000202
The determination results in the table show that when the compound I and the zinc thiazole are compounded and a single agent are used for preventing and treating the cucumber bacterial angular leaf spot, the compound I and the zinc thiazole have obviously higher 7-day prevention effect and 14-day prevention effect on the cucumber bacterial angular leaf spot than the single agent under the same effective component dosage. Wherein the control effect can still reach more than 80.6 percent in 14 days, and the lasting period is longer.
TABLE 16 field test of the efficacy of Compound I in combination with kasugamycin on cucumber bacterial angular leaf spot
Figure BDA0003321861980000203
Figure BDA0003321861980000211
The determination results in the table show that when the compound I and the kasugamycin are compounded and compared with a single preparation, the compound I and the kasugamycin have obviously higher 7-day control effect and 14-day control effect on the cucumber bacterial angular leaf spot than the single preparation under the same effective component dosage. Wherein the control effect can still reach more than 78.9 percent in 14 days, and the lasting period is longer.
Field drug effect test of rice bacterial leaf blight (developed in south Beijing of Jiangsu):
the test method comprises the following steps: according to the medicine application method specified in the national Standard GB/T17980.19-2000 of the people's republic of China, the medicine is applied when scabs are seen at first, the medicine is applied for the 2 nd time after 7 days, the medicine is applied for two times, and the times are repeated for 4 times.
The investigation method comprises the following steps: according to the investigation method specified in the national standard GB/T17980.19-2000 of the people's republic of China, the control effect is investigated 7 days and 14 days after the 2 nd application.
Prevalence of bacterial blight disease (by visual grading):
grade 0, no disease; grade 1, sporadic onset or central cluster; 3, the disease area accounts for about one fourth of the total area; grade 5, the disease area accounts for about one third of the total area; 7, the disease area accounts for about one half of the total area; and 9 grades, the disease incidence area accounts for more than three quarters of the total area.
TABLE 17 field drug effect test of compounding compound I with Zhongshengmycin on bacterial leaf blight of rice
Figure BDA0003321861980000212
According to the determination results, when the compound I is used for preventing and treating the bacterial leaf blight of rice, compared with the compound preparation and the single preparation of the zhongshengmycin, under the same effective component dosage, the 7-day control effect and the 14-day control effect of the compound I and the zhongshengmycin on the bacterial leaf blight of rice are obviously higher than those of the single preparation. Wherein the control effect can still reach more than 80.5 percent in 14 days, and the lasting period is longer.
TABLE 18 field drug effect test of compound I and tetramycin in combination on bacterial leaf blight of rice
Figure BDA0003321861980000221
According to the determination result, when the compound I is used for preventing and treating the bacterial leaf blight of rice, compared with the tetramycin compound and the single preparation, under the same effective component dosage, the compound I + tetramycin compound has a 7-day control effect and a 14-day control effect on the bacterial leaf blight of rice which are obviously higher than those of the single preparation. Wherein the control effect can still reach more than 78.6 percent in 14 days, and the lasting period is longer.
Field efficacy test for citrus canker (carried out in waring, guangxi):
according to the pesticide application method specified in the pesticide field efficacy test guidelines (GB/T17980.103-2004), the first spray is used before the first flowering, and the second spray is used after the disease appears. The application is carried out twice in total, the area of each treatment cell is 3 adult fruit trees, and the repetition times are 4 times. The application times, the application date and the growth period of the fruit trees are recorded.
The investigation method comprises the following steps: according to an investigation method specified in the pesticide field efficacy test guidelines (GB/T17980.103-2004), two plants are investigated for each cell 7d and 14d after the second pesticide application, each plant is sampled according to five points in east, west, south and north, and all the leaves on two tips are investigated at each point, and the prevention and control effects are calculated.
The leaf grading method comprises the following steps:
level 0: no disease; level 1: 1-5 scabs are formed on each leaf; and 3, level: each leaf has 6-10 spots; and 5, stage: each leaf has 11-15 scabs; and 7, stage: each leaf has 15-20 scabs; and 9, stage: each leaf has more than 21 scabs;
TABLE 19 field drug effect test of compound I compounded with Zhongshengmycin on citrus canker
Figure BDA0003321861980000222
Figure BDA0003321861980000231
According to the determination result, when the compound I is used for preventing and treating the citrus canker, compared with the compound preparation of the zhongshengmycin and the single preparation, under the same effective component dosage, the compound preparation of the compound I and the zhongshengmycin has obviously higher 7-day control effect and 14-day control effect on the citrus canker than the single preparation. Wherein the control effect can still reach more than 78.5 percent in 14 days, and the lasting period is longer.
TABLE 20 field test of efficacy of compound I in combination with shenqinmycin on citrus canker
Figure BDA0003321861980000232
According to the determination result, when the compound I is used for preventing and treating the citrus canker, compared with the compound and single preparation of the shenqinmycin, the compound and the shenqinmycin have obviously higher 7-day control effect and 14-day control effect on the citrus canker than the single preparation under the same effective component dosage. Wherein the control effect still can reach over 79.3 percent in 14 days, and the lasting period is longer.
Watermelon fruit spot field efficacy test (conducted in Changle county in Weifang city):
the test method comprises the following steps: according to the medicine application method specified in national Standard GB/T17980.110-2004 of the people's republic of China, the medicine is applied when scabs are first seen, the medicine is applied 2 times after 7 days, the medicine is applied twice in total, and the times of application are repeated 4 times.
The investigation method comprises the following steps: the control effect is investigated 7 days and 14 days after the 2 nd application according to an investigation method specified in national standard GB/T17980.110-2004 of the people's republic of China.
The diagonal of each cell was sampled at 3 points, and 5 plants at each point were examined for all leaves, and the lesion area per leaf was graded as a percentage of the total leaf area.
The grading method comprises the following steps:
no disease spot at level 0; grade 1, the lesion spot area accounts for less than 5% of the whole leaf area; grade 3, the lesion area accounts for 6 to 10 percent of the whole leaf area; grade 5, the lesion area accounts for 11 to 20 percent of the whole leaf area; 7 grade, the lesion area accounts for 21 to 50 percent of the whole leaf area; grade 9, the lesion area accounts for more than 51 percent of the whole leaf area.
TABLE 21 Compound I and Zhongshengmycin in-pairs watermelon fruit blotch field drug effect test
Figure BDA0003321861980000233
Figure BDA0003321861980000241
According to the determination result, when the compound I is used for preventing and treating the watermelon fruit blotch, compared with the compound of the zhongshengmycin and the single dose, the compound of the compound I and the zhongshengmycin has a 7-day prevention effect and a 14-day prevention effect on the watermelon fruit blotch which are obviously higher than those of the single dose under the same effective component dosage. Wherein the control effect can still reach more than 78.6 percent in 14 days, and the lasting period is longer.
TABLE 22 Compound I and allicin in-situ test for efficacy of watermelon fruit blotch
Figure BDA0003321861980000242
According to the determination result, when the compound I is used for preventing and treating the watermelon fruit blotch, compared with the compound of the allicin and the single dose, the compound of the compound I and the allicin has a 7-day prevention effect and a 14-day prevention effect on the watermelon fruit blotch which are obviously higher than those of the single dose under the same effective component dosage. Wherein the control effect still can reach more than 77.4 percent in 14 days, and the effective period is longer.
Tomato bacterial wilt field efficacy test (conducted in Changle county in Weifang city):
the test method comprises the following steps: according to a medicine application method specified in agricultural industry standard NY/T1464.32-2010 of the people's republic of China, roots are irrigated when a diseased plant is first seen, granules are spread when the diseased plant is first seen, medicine application is carried out 2 times after 7 days, medicine application is carried out twice in total, and the times of repeated medicine application are 4 times.
The investigation method comprises the following steps: according to a survey method specified in agricultural industry standard NY/T1464.32-2010 of the people's republic of China, all plants are surveyed in each cell, and the total number of plants and the number of diseased plants are recorded. The control effect was investigated 7 and 14 days after the 2 nd application.
TABLE 23 field test of Compound I in combination with Zhongshengmycin for tomato bacterial wilt
Figure BDA0003321861980000243
Figure BDA0003321861980000251
According to the determination results, when the compound I is used for preventing and treating the tomato bacterial wilt, compared with the compound preparation of the zhongshengmycin and the single preparation, under the same effective component dosage, the compound preparation of the compound I and the zhongshengmycin has the obviously higher 7-day control effect and 14-day control effect on the tomato bacterial wilt than the single preparation. Wherein the control effect can still reach more than 78.1 percent in 14 days, and the lasting period is longer.
Field efficacy test of tobacco wildfire (developed in yuxi city, Yunnan province):
the test method comprises the following steps: according to a medicine application method specified in agricultural industry standard NY/T1464.44-2012 of the people's republic of China, medicine application is carried out when scabs are first seen, medicine application is carried out 2 times after 7 days, medicine application is carried out twice in total, and the times of application are repeated 4 times.
The investigation method comprises the following steps: according to a survey method specified in agricultural industry standard NY/T1464.44-2012 of the people's republic of China, randomly surveying 5 points per cell, surveying 1 plant per point, surveying all leaves per plant, classifying by the percentage of the lesion area of each leaf to the lesion area of the whole leaf, and recording the total leaf number and the lesion leaf number of each level.
TABLE 24 field drug effect test of compounding of compound I and ethylicin on tobacco wildfire
Figure BDA0003321861980000252
According to the determination result, when the compound I is used for preventing and treating the tobacco wildfire, compared with the compound of ethylicin and the single preparation, under the same effective component dosage, the compound of the compound I and the ethylicin has obviously higher 7-day prevention effect and 14-day prevention effect on the tobacco wildfire than the single preparation. Wherein the control effect can still reach more than 77.5 percent in 14 days, and the lasting period is longer.
The field efficacy test of ginger blast (developed in Anqiu city, Shandong province):
the test method comprises the following steps: according to a medicine application method specified in agricultural industry standard NY/T1464.31-2010 of the people's republic of China, medicine application is carried out when scabs are first seen, medicine application is carried out 2 times after 7 days, medicine application is carried out twice in total, and the times of application are repeated 4 times.
The investigation method comprises the following steps: according to an investigation method specified in agricultural industry standard NY/T1464.31-2010 of the people's republic of China, 5-point investigation is carried out in each cell randomly, 10 plants are investigated in each point, symptoms of all leaves and fleshy stems are investigated in each plant, and the total plant number and all levels of diseased plant numbers are recorded and investigated.
TABLE 25 Compound I and aureonucleomycin Compound pairing ginger blast field drug Effect test
Figure BDA0003321861980000261
According to the determination result, when the ginger bacterial wilt is prevented and treated, compared with the compound of the compound I and the aureonucleomycin and the single preparation, under the same effective component dosage, the compound of the compound I and the aureonycin has obviously higher 7-day control effect and 14-day control effect on the ginger bacterial wilt than the single preparation. Wherein the control effect still can reach more than 77.9 percent in 14 days, and the effective period is longer.
Field efficacy test for pear fire blight (developed in kurler, xinjiang):
the test method comprises the following steps: the medicine is applied when the scab is initially seen, and the medicine is applied 2 times after 7 days, wherein the medicine is applied twice and repeated 4 times.
The investigation method comprises the following steps: 5 spots were surveyed randomly per cell, 10 plants per spot and 10 shoots per plant. Record and investigate the total plant number and the disease plant number of each level.
TABLE 26 field drug effect test of compound I and pyrimidine nucleoside antibiotic compound pairing for pear fire blight
Figure BDA0003321861980000262
Figure BDA0003321861980000271
According to the determination result, when the compound I and the pyrimidine nucleoside antibiotic are compounded and compared with a single preparation, under the same effective component dosage, the compound I and the pyrimidine nucleoside antibiotic have obviously higher 7-day control effect and 14-day control effect on the pear fire blight than the single preparation. Wherein the control effect still can reach more than 77.6 percent in 14 days, and the effective period is longer.
Fruit tree bacterial root cancer field efficacy test (developed on Shandong tobacco stage):
the test method comprises the following steps: irrigating roots when a diseased plant is first seen, spreading the granules when the diseased plant is first seen, applying the granules 2 times after 7 days, applying the granules twice in total, and repeating the steps for 4 times.
The investigation method comprises the following steps: all plants were investigated per cell and total and diseased plants were recorded. The control effect was investigated 7 and 14 days after the 2 nd application.
TABLE 27 field efficacy test of compounding of compound I and amino-oligosaccharin on bacterial root cancer of fruit trees
Figure BDA0003321861980000272
According to the measurement results, when the compound I is used for preventing and treating the bacterial root cancer of the fruit trees, compared with the compound preparation of the amino-oligosaccharin and the single preparation, under the same effective component dosage, the compound preparation of the compound I and the amino-oligosaccharin has obviously higher 7-day prevention effect and 14-day prevention effect on the bacterial root cancer of the fruit trees than the single preparation. Wherein the control effect can still reach more than 78.3 percent in 14 days, and the lasting period is longer.
The efficacy test of the yangtao disease field (developed in the county of pujiang province, Sichuan province) is as follows:
the test method comprises the following steps: the medicine is applied before germination, and the medicine is applied 2 times after 7 days, wherein the medicine is applied twice in total and repeated for 4 times.
The investigation method comprises the following steps: and 7d and 14d after the second pesticide application, surveying two plants in each cell, sampling each plant according to five points in east, west, south and north, surveying 20 branches in each plant, and calculating the control effect.
TABLE 28 field drug effect test of compounding of Compound I with Neophytomycin on kiwifruit canker
Figure BDA0003321861980000273
Figure BDA0003321861980000281
According to the determination result, when the compound I is used for preventing and treating the kiwifruit canker, compared with the compound of the new phytomycin and the single preparation, under the same effective component dosage, the compound of the compound I and the new phytomycin has obviously higher 7-day prevention effect and 14-day prevention effect on the kiwifruit canker than the single preparation. Wherein the control effect still can reach more than 77.7 percent in 14 days, and the effective period is longer.
Corn bacterial stem rot field efficacy test (developing in south of east China of Shanshan)
The test method comprises the following steps: spraying the granules at the time of incipient disease, broadcasting the granules at the time of incipient disease, applying the granules 2 times after 7 days, applying the granules twice in total, and repeating the application 4 times.
The investigation method comprises the following steps: all plants were investigated per cell and total and diseased plants were recorded. The control effect was investigated 7 and 14 days after the 2 nd application.
TABLE 29 field test of the efficacy of Compound I in combination with polyoxin on bacterial stalk rot of maize
Figure BDA0003321861980000282
According to the determination result, when the compound I is used for preventing and treating the corn bacterial stem rot, compared with the polyoxin compound and the single agent, under the same effective component dosage, the compound I and the polyoxin compound have obviously higher 7-day prevention effect and 14-day prevention effect on the corn bacterial stem rot than the single agent. Wherein the control effect can still reach 78.4% in 14 days, and the effective period is longer.
Citrus Huanglongbing field drug effect test (developing in Guangxi Wuming)
The test method comprises the following steps: irrigating roots when the plants are initially diseased, broadcasting granules when the plants are initially diseased, applying the granules 2 times after 7 days, applying the granules twice in total, and repeating the applying times for 4 times.
The investigation method comprises the following steps: all plants were investigated per cell and total and diseased plants were recorded. The control effect was investigated 7 and 14 days after the 2 nd application.
TABLE 30 field drug effect test of compound I compounded with validamycin on citrus Huanglongbing
Figure BDA0003321861980000291
According to the determination result, when the compound I is used for preventing and treating citrus greening disease, compared with the validamycin compound and the single preparation, under the same effective component dosage, the compound I and the validamycin compound have obviously higher 7-day control effect and 14-day control effect on the citrus greening disease than the single preparation. Wherein the control effect can still reach 79.3 percent in 14 days, and the lasting period is longer.
Tomato canker field efficacy test (developing in east China of Shanshan)
The test method comprises the following steps: spraying the granules at the time of incipient disease, broadcasting the granules at the time of incipient disease, applying the granules 2 times after 7 days, applying the granules twice in total, and repeating the application 4 times.
The investigation method comprises the following steps: all plants were investigated per cell and total and diseased plants were recorded. The control effect was investigated 7 and 14 days after the 2 nd application.
TABLE 31 field test of Compound I and oligosaccharins for treating tomato canker
Figure BDA0003321861980000292
Figure BDA0003321861980000301
According to the determination result, when the compound I is used for preventing and treating the tomato canker, compared with the compound of oligosaccharide and the single preparation, under the same effective component dosage, the compound of the compound I and oligosaccharide has obviously higher 7-day prevention effect and 14-day prevention effect on the tomato canker than the single preparation. Wherein the control effect can still reach more than 78.4 percent in 14 days, and the lasting period is longer.
A field efficacy test of the corn bacterial wilt (conducted in Changle county in Weifang City):
the test method comprises the following steps: irrigating roots when the plants are initially diseased, broadcasting granules when the plants are initially diseased, applying the granules 2 times after 7 days, applying the granules twice in total, and repeating the applying times for 4 times.
The investigation method comprises the following steps: all plants were investigated per cell and total and diseased plants were recorded. The control effect was investigated 7 and 14 days after the 2 nd application.
TABLE 32 field efficacy of Compound I in combination with Chloromycetes zeae against bacterial wilt disease
Figure BDA0003321861980000302
According to the determination result, when the corn bacterial wilt is prevented and treated, compared with the compound granules of the compound I and the hydratase mycin and the single preparation, under the same effective component dosage, the compound granules of the compound I and the hydratase mycin have obviously higher control effect on the corn bacterial wilt in 7 days and 14 days than the single preparation. Wherein the control effect can still reach 76.3 percent in 14 days, and the lasting period is longer.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. The bactericide composition comprises effective active ingredients, wherein the effective active ingredients comprise a compound I and a compound II, the compound I is 7-chloro-1-cyclopropyl-6-fluoro-4-oxo-1, 4-dihydroquinoline-3-carboxylic acid-2-methoxyethyl ester, and the compound II is at least one of antibiotic compounds, thiazole zinc, benziothiazolinone, bromothalonil, amino-oligosaccharin, emodin methyl ether, isothiazolinone and dithiocyano methane.
2. The bactericidal composition of claim 1, wherein the antibiotic compound is at least one selected from the group consisting of zhongshengmycin, kasugamycin, tetramycin, ethylicin, aureonucleomycin, shenqinmycin, hydromycin, allicin, neophytomycin, polyoxin, streptomycin for agricultural use, agroinhibin 120, validamycin, pyrimidine nucleoside antibiotics, ningnanmycin, cnidium lactone, and oligosaccharins.
3. The bactericidal composition according to claim 1 or 2, wherein the mass ratio of the compound I to the compound II is 80-1: 1-80;
preferably, the mass ratio of the compound I to the compound II is 50-1: 1-50;
preferably, the mass ratio of the compound I to the compound II is 30-1: 1-30.
4. The bactericidal composition according to any one of claims 1 to 3, wherein the sum of the mass of the compound I and the compound II in the bactericidal composition is 1 to 80% based on 100% of the total weight of the bactericidal composition.
5. The bactericidal composition according to any one of claims 1 to 4, wherein the bactericidal composition is formulated into a liquid preparation or a solid preparation.
Preferably, the liquid preparation contains 1-60% of effective active ingredients by weight; the solid preparation contains 5 to 80 percent of effective active ingredients by weight.
6. The germicidal composition of any of claims 1-5, further comprising at least one of an emulsifier, a dispersant, a wetting agent, a thickener, an anti-foaming agent, a stabilizer, a binder, a disintegrant, an anti-freezing agent, an anti-caking agent, a suspending agent, a film-forming agent, a preservative, a colorant, a polymeric wall material, a pH adjuster, or a filler.
7. The bactericidal composition according to any one of claims 1 to 6, wherein the bactericidal composition can be prepared into water dispersible granules, dispersible solutions, wettable powders, suspensions, aqueous emulsions, microemulsions, suspoemulsions, microcapsule suspensions, microcapsule suspension-suspensions, suspended seed coatings, emulsifiable concentrates and granules.
8. The bactericidal composition according to any one of claims 1 to 7 is used for controlling pathogenic bacteria and agricultural diseases caused by the pathogenic bacteria, and is particularly suitable for bacteria and bacterial diseases of plants caused by the bacteria.
9. The use of claim 8, wherein the bactericidal composition is used for controlling soft rot of crops such as soft rot of Chinese cabbage, black rot of Chinese cabbage, bacterial angular leaf spot of cucumber, sesame angular leaf spot, west/melon fruit spot, bacterial leaf blight of rice, bacterial leaf streak of rice, bacterial brown spot of rice, bacterial brown strip disease of rice, bacterial basal rot of rice, solanaceae bacterial wilt such as tomato bacterial wilt, mulberry bacterial wilt, peanut bacterial wilt, ginger blast, tomato/pepper bacterial spot disease, pepper bacterial leaf spot disease, potato black shank disease, corn bacterial wilt disease, corn bacterial stem rot disease, wheat black glume disease, soybean bacterial leaf blight, soybean bacterial blight, cassava bacterial wilt, mango angular leaf spot, citrus canker disease, peach tree perforated bacterial disease, sunflower stem rot, peach gummosis, peach stem rot disease, and the like, Pear fire blight, pear rust disease, fruit tree bacterial root cancer, potato ring rot, bean wilt, wheat white leaf streak, potato scab, tomato canker, American winter green leaf blight and cucumber downy mildew, cucumber target spot, rice blast, rice sheath blight, etc.
10. A method of controlling pathogenic bacteria and agricultural diseases caused thereby, particularly bacterial and bacterial plant diseases, comprising applying to a plant in which the disease is present a fungicidal composition according to any one of claims 1 to 7.
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