CN114467947B - 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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CN114467947B
CN114467947B CN202111248358.2A CN202111248358A CN114467947B CN 114467947 B CN114467947 B CN 114467947B CN 202111248358 A CN202111248358 A CN 202111248358A CN 114467947 B CN114467947 B CN 114467947B
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compound
bacterial
rot
bactericidal composition
rice
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CN114467947A (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
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    • 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
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    • 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
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Abstract

The invention relates to a synergistic bactericidal composition containing quinolone compounds and application thereof. The bactericide composition comprises an effective active ingredient, wherein the effective active ingredient comprises 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-methoxyl ethyl ester, and the compound II is at least one of antibiotic compounds, zinc thiazole, benziothiazolinone, bromothalonil, amino oligosaccharin, physcion, isothiazolinone and dithiomethane. The synergistic bactericidal composition has the following advantages: 1) Has synergistic effect and can improve the control effect; 2) The sterilization spectrum is enlarged, the field diseases are mixed more, and the effect on the bacterial diseases is stronger; 3) The two active ingredients have different action mechanisms, and the mixed use can delay the generation of drug resistance of pathogenic bacteria; 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, bacterial diseases of various crops tend to be increased year by year, the occurrence area is increased year by year, and huge harm is brought to agricultural production, for example, rice bacterial leaf streak disease, rice bacterial leaf blight in grain crops, citrus canker in fruit trees, bacterial wilt of vegetables in Solanaceae, cucumber bacterial angular leaf spot disease, cruciferous vegetable soft rot, ginger blast and the like cause serious losses to crops.
At present, the market lacks high-efficiency medicaments for preventing and treating bacterial diseases, farmers increase the dosage or mix medicaments at will in order to improve the preventing and treating effect, and the unscientific administration cannot achieve the synergistic effect, but rather causes the problems of pesticide waste, exceeding residues, environmental pollution, pathogen resistance to pesticides and the like. Therefore, development of a synergistic bactericidal composition for bacterial diseases is needed to achieve the effects of expanding the range of control objects, reducing the dosage and delaying the generation of resistance.
In the actual process of agricultural production, the same medicament is continuously and singly used for a long time, pathogenic bacteria can quickly generate drug resistance, so that the prevention effect is reduced, the pesticide use amount is increased, and the pesticide residue of agricultural products and the damage to ecological environment are aggravated. The bactericide variety with completely different action mechanisms is compounded, so that the bactericide is an effective way for delaying the generation of drug resistance of pathogenic bacteria, expanding a bactericidal spectrum, prolonging the service life and reducing the use amount of pesticides. However, how to compound the medicines makes the medicines generate synergy rather than antagonism is a great difficulty.
The chemical names of the quinolones are: 7-chloro-1-cyclopropyl-6-fluoro-4-oxo-1, 4-dihydroquinoline-3-carboxylic acid-2-methoxyethyl ester has broad-spectrum bactericidal activity, is particularly higher in bacterial activity, and shows excellent activity on gram-positive bacteria and gram-negative bacteria. The plant bacterial diseases such as cabbage soft rot and the like are excellent in pathogenic bacteria such as various crop soft rot diseases such as cabbage soft rot, cabbage black rot, cucumber bacterial angular leaf spot, sesame angular leaf spot, west/melon leaf spot, rice bacterial leaf blight, rice bacterial leaf streak, rice bacterial brown spot, rice bacterial brown strip, rice bacterial basal rot, tomato bacterial wilt and the like, solanaceae bacterial wilt, sang Qing blight, peanut bacterial wilt, ginger blast, tomato/pepper bacterial leaf spot, potato black shank, corn bacterial leaf blight, corn bacterial stem rot, wheat black rot, soybean bacterial leaf spot, soybean bacterial leaf blight, cassava bacterial wilt, mango angular leaf spot, citrus canker, peach bacterial leaf rot, sunflower stem rot, gummy, pear fire, pear rust water disease, fruit tree bacterial root cancer, potato ring rot, bean wilt, wheat Bai Shetiao, winter leaf rot, tomato leaf rot and American bacterial leaf rot.
The traditional Chinese medicine composition is prepared from Zhongshengmycin, kasugamycin, benziothiazolinone, tetramycin, ethylicin, aureonuclycin, zinc thiazole, shenqimycin, hydrated mycin, bromothalonil, neophytmycin, polyoxin, agricultural streptomycin, agricultural resistance 120, validamycin, pyrimidine nucleoside antibiotics, ningnan mycin, osthole, oligosaccharin, amino oligosaccharin, garlicin and physcion, and has the advantages of resistance and reduced control effect in different degrees due to single long-term use.
In the prior art, related reports about the compounding and application of quinolone compounds, zhongshengmycin, kasugamycin, zinc thiazole, benziothiazolinone, tetramycin, ethylicin, shenqimycin, aureomycin, hydrated mycin, bromoxynil, neophytmycin, polyoxin, agricultural streptomycin, agricultural antibiotic 120, validamycin, pyrimidine nucleoside antibiotics, ningnanmycin, osthole, oligosaccharin, amino oligosaccharin, garlicin and physcion are not found, and similar substances are not found for compounding.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a synergistic sterilization composition containing quinolone compounds and application thereof, wherein the sterilization composition comprises active ingredients, the 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 mesogen, kasugamycin, tetramycin, ethylicin, shengzhizycin, aureomycin, hydrated mycin, allicin, amino-oligosaccharin, neophytmycin, polyoxin, agricultural streptomycin, agricultural antibiotic 120, validamycin, pyrimidine nucleoside antibiotics, ningnanmycin, osthole, oligosaccharin and the like, and at least one of zinc thiazole, thiamycetin, bromomycins, emodin, isothiazolinone and dithiocyanmethane.
The compound I and the compound II can form a synergistic bactericidal composition, the effective active ingredients comprise the compound I and the compound II, the mixed use of the compound I and the compound II has obvious synergistic and complementary effects, and the compound can act on pathogenic bacteria at multiple sites by utilizing different pathogenic bacteria acting sites and different acting mechanisms, so that the bactericidal spectrum is enlarged, the control effect is improved, the pesticide use amount is reduced, the generation of drug resistance is delayed, and the cost is also reduced.
The invention adopts the following scheme:
the bactericidal composition comprises an effective active ingredient, wherein the effective active ingredient comprises 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-methoxyl ethyl ester, and the compound II is at least one of antibiotic compounds, thiazole zinc, benziothiazolinone, bromothalonil, amino oligosaccharin, physcion, isothiazolinone and dithiocyanmethane.
According to an embodiment of the present invention, the antibiotic compound is at least one selected from the group consisting of mesogenic fungi, kasugamycin, tetramycin, ethylicin, aureonuclycin, shenzinmycin, hydrated fungi, garlicin, neophytmycin, polyoxin, agricultural streptomycin, agricultural resistance 120, validamycin, pyrimidine nucleoside antibiotics, ningnanmycin, osthole, oligosaccharin, etc.
According to an embodiment of the invention, the mass ratio of the compound I to the compound II is 80-1:1-80.
According to an embodiment of the invention, the mass ratio of the compound I to the compound II is 50-1:1-50.
According to an 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, 1:1, 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 invention, the sum of the mass of the compound I and the mass of the compound II in the bactericidal composition is 1-80%, preferably 20-60%, 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 bactericidal composition may be prepared as a liquid formulation or a solid formulation.
According to the embodiment of the invention, the content range of the effective active ingredient in the preparation is different according to different preparation types, and generally, the liquid preparation contains 1 to 60 percent of the effective active ingredient by weight, preferably 5 to 50 percent; the solid preparation contains 5-80% by weight of effective active ingredient, preferably 10-70%.
According to an embodiment of the present invention, the bactericidal composition further comprises at least one of an emulsifier, a dispersant, a wetting agent, a thickener, a defoamer, a stabilizer, a binder, a disintegrant, an antifreeze, an anticaking agent, a suspending agent, a film forming agent, a preservative, a colorant, a polymeric wall material, a pH adjuster, a filler, or the like.
According to embodiments of the present invention, the bactericidal composition may be diluted by a user before use or used directly. The preparation can be prepared by a processing method known to a person skilled in the art, namely, the effective active ingredient is mixed with one or more of deionized water, an organic solvent, an emulsifier, a dispersing agent, a wetting agent, a thickening agent, a defoaming agent, a stabilizing agent, a binding agent, a disintegrating agent, an antifreezing agent, an anti-caking agent, a suspending agent, a film forming agent, a preservative, a coloring agent, a polymer capsule wall material, a pH regulator or a filler and the like 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 liquid, wettable powder, suspending agents, aqueous emulsion, microemulsion, suspoemulsion, microcapsule suspending agents, microcapsule suspension-suspending agents, suspension seed coating agents, emulsifiable concentrates and granules.
According to the embodiment of the invention, the bactericidal composition is prepared into wettable powder and comprises the following components in parts by weight: 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 being 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 an 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 dispersing agent, 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 parts 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 defoamer, 0.1 to 2 percent of thickener and the balance of deionized water.
According to the embodiment of the invention, the composition is prepared into a suspended seed coating agent and comprises the following components in parts 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 thickener and the balance of deionized water.
According to an embodiment of the invention, the composition is prepared into microcapsule suspending agent and comprises the following components in parts by weight: 1-50% of compound I, 1-50% of compound II, 1-30% of high molecular capsule wall material, 2-10% of dispersing agent, 1-50% of organic solvent, 1-7% of emulsifying agent, 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-suspension agent and comprises the following components in percentage by weight: 1-50% of compound I, 1-50% of compound II, 1-12% of high molecular capsule wall material, 1-12% of dispersing agent, 1-8% of wetting agent, 1-50% of organic solvent, 1-8% of emulsifying agent, 0.01-2% of defoaming agent, 0.1-8% of thickening agent, 0.1-5% of pH regulator, 0.1-8% of antifreeze agent and the balance of deionized water.
According to an embodiment of the invention, the composition is prepared into emulsifiable concentrates 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 50 percent of organic solvent, 1 to 30 percent of emulsifier, 1 to 10 percent of antifreeze agent, 0.1 to 5 percent of stabilizer and the balance of organic solvent.
According to an embodiment of the invention, the composition is prepared into a microemulsion 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 50 percent of organic solvent, 1 to 30 percent of emulsifier, 1 to 10 percent of antifreeze agent, 0.1 to 5 percent of stabilizer and the balance of deionized water.
According to an embodiment of the invention, the composition is formulated as a dispersible formulation comprising the following components and amounts: 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 an embodiment of the invention, the composition is prepared into granules and comprises the following components in percentage by weight: 0.5 to 10 percent of compound I, 0.5 to 10 percent of compound II, 1 to 12 percent of dispersing agent, 1 to 10 percent of wetting agent, 0.1 to 8 percent of adhesive and the balance of filler.
According to an embodiment of the present invention, the emulsifier may be one of the following: sodium lignin sulfonate, pesticide emulsion, phenyl phenol polyoxyethylene ether phosphate, tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt, benzyl dimethyl phenol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether, sorbitan oleic acid ester (span-80), fatty alcohol polyoxyethylene ether, sodium alkyl naphthalene sulfonate, sodium isooctyl succinate sulfonate, nonylphenol polyoxyethylene ether phosphate, castor oil polyoxyethylene ether phosphate.
According to an embodiment of the present invention, the dispersant may be selected from: one or more of glycerol fatty acid polyoxyethylene ether, polyoxyethylene alkylaryl ether, sodium lignin sulfonate, naphthalene sulfonate formaldehyde condensate, fatty alcohol polyoxyethylene ether sulfate, naphthalene sulfonate formaldehyde condensate sodium salt, nonylphenol polyoxyethylene ether, polyoxyethylene lanolin alcohol, alkylphenol polyoxyethylene ether formaldehyde condensate, fatty alcohol polyoxyethylene ether phosphate, polyoxyethylene sorbitan fatty acid ester and phosphate.
According to an embodiment of the present invention, the wetting agent may be selected from: trisiloxane polyoxyethylene ether, sodium N-lauroyl glutamate, sodium dodecyl sulfate, sodium lauroyl sarcosinate, sodium methyl naphthalene sulfonate formaldehyde condensate, castor oil polyoxyethylene ether, triphenyl ethylphenol polyoxyethylene ether, sodium dodecyl benzene sulfonate, sodium alkyl naphthalene sulfonate, sodium isooctyl succinate sulfonate, polyoxyethylene alkylaryl ether, fatty alcohol polyether glycerol fatty acid polyoxyethylene ether, fatty alcohol polyoxyethylene ether.
According to an embodiment of the present invention, the binder may be selected from: one or more of xanthan gum, starch, urea-formaldehyde resin, gelatin, acacia, carboxymethyl cellulose, carboxyethyl cellulose and polyvinyl alcohol.
According to an embodiment of the present invention, the disintegrant may be selected from: 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, acacia, and polyvinyl alcohol.
According to an embodiment of the present invention, the antifoaming agent may be selected from: silicone oil, n-octanol, silicone, butyl phosphate, isobutyl phosphate, and the like.
According to an embodiment of the invention, the antifreeze agent may be selected from: propylene glycol, ethylene glycol, glycerol, and the like.
According to an embodiment of the present 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 vinegar sulfonate, and the like.
According to an embodiment of the present invention, the filler comprises a solid filler and a liquid filler, wherein the solid filler may 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: ethyl acetate, acetone, isopropanol, 2-trifluoroethanol, propylene carbonate, benzene, toluene, xylene, dimethylformamide, dimethyl sulfoxide, dichloromethane, cyclohexane, cyclohexanone, N-methylpyrrolidone, and mineral spirits (e.g., 150# mineral spirits).
The bactericidal composition is used for preventing and controlling 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 the embodiment of the invention, the bactericidal composition is used for preventing and treating various crop soft rot diseases such as cabbage soft rot diseases, cabbage black rot, cucumber bacterial angular leaf spot, sesame angular leaf spot, west/melon fruit spot, rice bacterial leaf blight, rice bacterial streak, rice bacterial brown spot, rice bacterial basal rot, tomato bacterial wilt and the like, sang Qing bacterial wilt, peanut bacterial wilt, ginger blast, tomato/pepper bacterial spot, pepper bacterial leaf spot, potato black shank, corn bacterial leaf spot, corn bacterial stem rot, wheat black rot, soybean bacterial leaf spot, soybean bacterial blight, cassava bacterial blight, mango angular leaf spot, citrus canker, peach bacterial perforin, sunflower stem rot, peach gummy, pear fire blight, rust water rot, fruit tree bacterial root rot, potato ring rot, bean wilt Bai Shetiao, wheat leaf spot, tomato leaf spot, cucumber bacterial leaf spot, and the pathogen of the like, and the pathogen viruses such as the disease of the plant disease.
The invention also provides a method for controlling pathogenic bacteria and agricultural diseases caused by the pathogenic bacteria, especially bacterial diseases of plants caused by bacteria, which comprises the step of applying the bactericidal composition to plants with diseases.
The bactericidal composition can be provided in a finished preparation form or can be provided in a single-dose form, and can be directly mixed before use, then water is added to be uniformly mixed to prepare the required concentration, and the bactericidal composition can be applied to plants or crops in any way, such as spraying, plant root irrigation, smearing and the like. In particular application, the composition can also be mixed with other medicaments such as pesticides, growth regulators, soil regulators, 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 sterilization spectrum is enlarged, the field diseases are mixed more, and the effect on the bacterial diseases is stronger; 3) The two active ingredients have different action mechanisms, and the mixed use can delay the generation of drug resistance of pathogenic bacteria; 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 illustrative only and are not to be construed as limiting the scope of the invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; the reagents, materials, etc. used in the examples described below are commercially available unless otherwise specified.
The invention adopts a method combining indoor bioassay and field test to perform performance test on the sterilization effect of the sterilization composition. It should be noted that any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
1. Preparation example:
preparation example 1: wettable powder
The materials are coarsely crushed according to the proportion, then are mixed uniformly in a mixer, and are crushed by air flow to obtain the finished product.
Preparation example 2: water dispersible granule
Uniformly mixing the effective active ingredients, various auxiliary agents and the like according to the proportion of the formula, obtaining powder after jet milling, adding a certain amount of water, mixing, extruding and granulating, and obtaining the finished product after drying and screening.
Preparation example 3: suspending agent
The effective active ingredients and various auxiliary agents are uniformly mixed according to the proportion of the formula, sheared at high speed and sanded to obtain the finished product.
Preparation example 4: emulsifiable concentrate
Mixing the raw materials in proportion to dissolve the raw materials into a uniform oil phase; and after the inspection is qualified, metering and split charging are carried out to obtain the finished product.
Preparation example 5: aqueous emulsion
According to the formula requirement, the raw materials are added into a batching kettle, uniformly mixed by a high-speed shearing machine to prepare aqueous emulsion, and after being checked to be qualified, the aqueous emulsion is metered and split-packed to obtain the finished product.
Preparation example 6: emulsifiable concentrate
Mixing the raw materials in proportion to dissolve the raw materials into a uniform oil phase; and after the inspection is qualified, metering and split charging are carried out to obtain the finished product.
Preparation example 7: emulsifiable concentrate
Mixing the raw materials in proportion to dissolve the raw materials into a uniform oil phase; and after the inspection is qualified, metering and split charging are carried out to obtain the finished product.
Preparation example 8: granule preparation
The components are fully mixed according to the formula proportion, crushed, wetted by water, fully and uniformly stirred, granulated by a screw extrusion granulator, dried and sieved to obtain the finished product.
2. Indoor toxicity measurement example
(1) Test pathogenic bacteria: bacterial diseases such as cabbage soft rot, cucumber bacterial angular leaf spot, watermelon fruit spot, rice bacterial leaf spot, tomato bacterial wilt, potato black shank, mango angular leaf spot, citrus canker, peach bacterial perforation and potato scab.
(2) The measuring method comprises the following steps:
bacterial virulence determination method
The pathogenic bacteria virulence measurement is carried out by taking bacterial diseases such as cabbage soft rot pathogen, cucumber bacterial angular leaf spot pathogen, watermelon fruit spot pathogen, rice bacterial leaf spot pathogen, tomato bacterial wilt pathogen, potato black shank pathogen, mango angular leaf spot pathogen, citrus canker pathogen, peach bacterial perforin pathogen, potato scab pathogen and the like as test materials, and adopting an in-vitro turbidity method to carry out virulence measurement on the compound I, the compound II and a mixed preparation thereof.
Referring to agricultural industry standard NY/T1156.16-2008 of the people's republic of China, the test agent (comprising a compound I and a compound II) is firstly prepared into 7 concentration gradients (7 concentration gradients of a compound I:0.5,1.0,2.0,4.0,8.0,16.0,32.0 mug/mL and the like; 7 concentration gradients of a compound II:0.5,1.0,2.0,4.0,8.0,16.0,32.0 mug/mL and the like) by using a proper solvent (the types of the solvents are such as acetone, methanol, N-dimethylformamide, dimethyl sulfoxide and the like and are selected according to the dissolving capacity of the solvent to a sample), and the compound I and the compound II to be mixed are respectively prepared according to EC 50 The values are set into a series of proportions according to mass proportions, and 7 series of concentrations with the final mass concentration (namely the total mass of the compound I and the compound II) of 0.5,1.0,2.0,4.0,8.0,16.0,32.0 mug/mL are prepared according to different proportions.
Under aseptic operation conditions, the culture solution of NB (nutrient broth containing 10g peptone, 3g beef extract powder and 5g sodium chloride per liter) is split equally into test tubes, the liquid medicine is quantitatively sucked from low concentration to high concentration sequentially, the liquid medicine is respectively added into the test tubes, the test tubes are fully and evenly shaken, then bacterial suspension in logarithmic phase is respectively added in equal amount, and each treatment is repeated for 4 times. After mixing, placing in a shaking incubator at 25 ℃ for dark culture, and measuring OD value when the logarithmic growth phase is up. Taking the average value of the effective 4 repeats as the measurement result, calculating the relative inhibition rate, converting the inhibition rate into a mechanical rate value (y), converting the concentration of the liquid medicine (mug/mL) into a pair value (x), obtaining a toxicity regression equation (y=a+bx) by a least square method, and calculating the EC of each medicament 50 Values. Simultaneously, the combined Synergy Ratio (SR) of the two medicaments in different proportions is calculated according to the Wadley method, and the SR<0.5 is antagonism, 0.5 is equal to or more than SR is equal to or less than 1.5 is addition, SR>1.5 is synergistic effect. The calculation formula is as follows:
SR＝EC 50 (theoretical value)/EC 50 (actual measurement value)
EC 50 (theoretical value) = (a+b)/(EC of a/a) 50 ) ++ (EC of B/B) 50 )
Wherein: a is a compound I, B is a compound II; a. b is the proportion of the compound I and the compound II in the bactericidal composition respectively;
after mixing different varieties of pesticides, three types of action are usually shown, namely additive action, synergistic action and antagonistic action, but the specific action cannot be predicted. The bactericidal composition provided by the invention takes the compound I and the compound II as effective active ingredients, and is illustrated by using a bioassay example.
Example 1: in order to verify the antibacterial effect of different proportions of the compound I and the Zhongshengmycin on the bacterial angular leaf spot bacteria of the cucumber, the indoor toxicity of the different proportions of the compound I and the Zhongshengmycin on the bacterial angular leaf spot bacteria of the cucumber is measured, the corresponding concentrations are prepared according to the weight percentage in the table, and the indoor antibacterial test is carried out, wherein the test results are as follows:
TABLE 1 determination of virulence of Compound I and Zhongshengmycin Single and mixtures thereof against cucumber bacterial angular leaf spot pathogen
The results in Table 1 show that the compound I and the Zhongshengmycin have obvious synergistic effect on inhibiting the bacterial angular leaf spot bacteria of cucumber when mixed in different proportions.
Example 2: in order to verify the antibacterial effect of the compound I and the Zhongshengmycin on the watermelon fruit blotch germs, the indoor toxicity of the compound I and the Zhongshengmycin on the watermelon fruit blotch germs in different proportions is measured, the corresponding concentrations are prepared according to the weight percentages in the table, and the indoor antibacterial test is carried out, wherein the test results are as follows:
TABLE 2 determination of toxicity of Compound I and Zhongshengmycin against watermelon fruit blotch
The results in Table 2 show that the compound I and the Zhongshengmycin have obvious synergistic effect on the inhibition of the fruit blotch of the watermelon by mixing the compound I and the Zhongshengmycin in different proportions.
Example 3: in order to verify the antibacterial effect of the compound I and the Zhongshengmycin on the citrus canker, the indoor toxicity of the compound I and the Zhongshengmycin on the citrus canker is measured according to different proportions, the compound I and the Zhongshengmycin are prepared into corresponding concentrations according to the weight percentages in the table, and the indoor antibacterial test is carried out, wherein the test results are as follows:
TABLE 3 determination of toxicity of Compound I and Zhongshengmycin against citrus canker pathogen
The results in Table 3 show that the compound I and the Zhongshengmycin have obvious synergistic effect on the inhibition of the citrus canker.
Example 4: in order to verify the antibacterial effect of the compound I and the Zhongshengmycin on rice bacterial blight bacteria, the indoor toxicity of the compound I and the Zhongshengmycin on the rice bacterial blight bacteria is measured according to different proportions, the compound I and the Zhongshengmycin are prepared into corresponding concentrations according to the weight percentage in a table, and the indoor antibacterial test is carried out, wherein the test results are as follows:
table 4 results of determination of bacterial virulence of bacterial leaf blight of rice by single compound I and Zhongshengmycin and mixtures thereof
As shown in the results of Table 4, the compound I and the Zhongshengmycin have obvious synergistic effect on inhibiting bacterial blight of rice by mixing the compound I and the Zhongshengmycin in different proportions.
Example 5: in order to verify the antibacterial effect of the compound I and the Zhongshengmycin on the bacterial wilt of tomatoes, the indoor toxicity of the compound I and the Zhongshengmycin on the bacterial wilt of tomatoes is measured according to different proportions, the corresponding concentrations are prepared according to the weight percentages in the table, and the indoor antibacterial test is carried out, wherein the test results are as follows:
TABLE 5 determination of virulence of Compound I and Zhongshengmycin Single dose and mixtures thereof against Rhizoctonia solani
The results in Table 5 show that the compound I and the Zhongshengmycin have obvious synergistic effect on the inhibition of the bacterial wilt of tomatoes when mixed in different proportions.
Example 6: in order to verify the antibacterial 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 measured according to different proportions, the compound I and the Zhongshengmycin are prepared into corresponding concentrations according to the weight percentage in a table, and the indoor antibacterial test is carried out, wherein the test result is as follows:
TABLE 6 determination of the toxicity of Compound I and Zhongshengmycin against Chinese cabbage Soft rot disease by the mixture
The table shows that the compound I, the Zhongshengmycin and the mixed preparation thereof have obvious synergistic effect on inhibiting the soft rot disease bacteria of the Chinese cabbage.
Example 7: in order to verify the antibacterial effect of the compound I and the allicin on the bacterial angular leaf spot bacteria of the cucumber, the indoor toxicity of the compound I and the allicin on the bacterial angular leaf spot bacteria of the cucumber is measured according to different proportions, the compound I and the allicin are prepared into corresponding concentrations according to the weight percentages in the table, and the indoor antibacterial test is carried out, wherein the test results are as follows:
TABLE 7 determination of virulence of Compound I and allicin Single dose and their mixtures against cucumber bacterial angular leaf spot pathogen
The table shows that the compound I and the allicin and the mixed preparation thereof have obvious synergistic effect on inhibiting the bacterial angular leaf spot bacteria of the cucumber.
Example 8: in order to verify the antibacterial effect of the compound I and the thiazole zinc on the watermelon fruit blotches, the indoor toxicity of the compound I and the thiazole zinc on the watermelon fruit blotches is measured according to different proportions, the compound I and the thiazole zinc are prepared into corresponding concentrations according to the weight percentages in the table, and the indoor antibacterial test is carried out, wherein the test results are as follows:
table 8 results of toxicity measurements of Compound I and Zinc thiazole on watermelon fruit blotch
The table shows that the compound I, the zinc thiazole and the mixed preparation thereof have obvious synergistic effect on the inhibition of the watermelon fruit blotch.
Example 9: in order to verify the antibacterial effect of the compound I and tetramycin on rice bacterial leaf spot germs in different proportions, the indoor toxicity of the compound I and tetramycin on the rice bacterial leaf spot germs in different proportions is measured, the compound I and tetramycin are prepared into corresponding concentrations according to the weight percentages in the table, and the indoor antibacterial test is carried out, wherein the test results are as follows:
table 9 results of toxicity determination of Compound I and tetramycin Single dose and mixtures thereof on Rice bacterial Pyricularia strip
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As shown in the table above, the compound I and tetramycin and the mixed preparation thereof have obvious synergistic effect on inhibiting rice bacterial strip spot bacteria.
Example 10: in order to verify the antibacterial effect of the compound I and the benziothiazolinone on potato scab germs, the indoor toxicity of the compound I and the benziothiazolinone on potato scab germs is measured according to different proportions, the compound I and the benziothiazolinone are prepared into corresponding concentrations according to weight percentages in a table, and an indoor antibacterial test is carried out, wherein the test results are as follows:
table 10 results of toxicity determination of Compound I and Thiomolone alone and in combination on Potato scab pathogen
The table shows that the compound I and the benziothiazolinone and the mixed preparation thereof have obvious synergistic effect on inhibiting potato scab bacteria.
Example 11: in order to verify the antibacterial effect of the compound I and the kasugamycin on the potato black shank bacteria, the indoor toxicity of the compound I and the kasugamycin on the potato black shank bacteria in different proportions is measured, the compound I and the kasugamycin are prepared into corresponding concentrations according to the weight percentage in the table, and the indoor antibacterial test is carried out, wherein the test result is as follows:
table 11 results of toxicity determination of Compound I and kasugamycin Single and its mixture on potato Blackleg pathogen
The table shows that the compound I and the kasugamycin and the mixed preparation thereof have obvious synergistic effect on inhibiting the potato black shank bacteria.
Example 12: in order to verify the antibacterial effect of the compound I and the neomycin on the mango angular leaf spot bacteria in different proportions, the indoor toxicity of the compound I and the neomycin on the mango angular leaf spot bacteria in different proportions is measured, the compound I and the neomycin are prepared into corresponding concentrations according to the weight percentages in the table, and an indoor antibacterial test is carried out, wherein the test result is as follows:
Table 12 results of toxicity determination of Compound I and New Phytocin Single dose and Mixed dose on mango angular leaf blight bacteria
The table shows that the compound I, the new phytase and the mixed preparation thereof have obvious synergistic effect on inhibiting the mango angular leaf spot bacteria.
Example 13: in order to verify the antibacterial effect of the compound I and the aureobasidin on the bacterial perforin of the peach tree, the indoor toxicity of the compound I and the aureobasidin on the bacterial perforin of the peach tree is measured according to different proportions, the compound I and the aureobasidin are prepared into corresponding concentrations according to the weight percentage in the table, and the indoor antibacterial test is carried out, wherein the test result is as follows:
TABLE 13 determination of virulence of Compound I and aureobasidin Single and mixtures thereof against bacterial perforin of peach trees
The table shows that the compound I and the aureobasidin and the mixed preparation thereof have obvious synergistic effect on inhibiting bacterial perforin bacteria of peach trees.
3. Example of field efficacy
In order to determine the control effect of single and mixed preparations of the compound I and the compound II on bacterial diseases such as cucumber bacterial angular leaf spot, citrus canker, watermelon fruit spot, tobacco wildfire, ginger bacterial leaf spot, kiwi fruit canker, pear fire blight, bacterial root cancer of fruit trees, corn bacterial stem rot, citrus yellow dragon disease, tomato canker, corn bacterial wilt, tomato bacterial wilt, rice white leaf spot and the like, a plurality of pesticide effect tests are carried out in different domestic areas.
The preparation methods of the reagents in the following examples are as shown in the above preparation examples 1 to 8, and by way of example, the preparation method of 10% compound I-Zhongshengmycin wettable powder of example 1 is the same as in preparation example 1, wherein compound II is selected from Zhongshengmycin, the preparation method of 10% compound I-thiazole zinc wettable powder of example 8 is the same as in preparation example 1, wherein compound II is selected from thiazole zinc, and the same as in preparation example 8, and the preparation of other examples is referred to in preparation examples 1 to 8 above.
The reagents of the following comparative examples were prepared as in the above preparation examples 1 to 8, except that the content of the active ingredient therein may be varied, and accordingly, the filler or water in the formulation was used to make up the ingredient to 100%. For example, the preparation method of the 10% compound I water dispersible granule of comparative example 1 refers to preparation example 2 in which 10% compound I replaces 20% compound I and 10% compound II in preparation example 2, and the difference in content is filled by a filler. For another example, the preparation method of the 3% in-biotin wettable powder of comparative example 2 is referred to preparation example 1, in which 3% in-biotin replaces 5% of compound I and 5% of compound II in preparation example 1, and the difference in content is filled by a filler.
Cucumber bacterial angular leaf spot field efficacy test (developed in mountain eastern chat city county):
The test method comprises the following steps: according to the method of administration prescribed in national Standard of the people's republic of China GB/T17980.110-2004, the medicine is applied at the first spot, the medicine is applied at the 2 nd time after 7 days, the medicine is applied twice in total, and the times of repetition are 4 times.
The investigation method comprises the following steps: the control effect was investigated 7 days and 14 days after the 2 nd administration according to the investigation method prescribed in national Standard for the people's republic of China GB/T17980.110-2004. Sampling 3 points on the diagonal of each cell, 5 strains each, investigating all leaves, and grading the leaves according to the percentage of the disease spot area of each leaf to the whole leaf area.
The grading method comprises the following steps:
grade 0, no disease spots; stage 1, the area of the disease spots accounts for less than 5% of the whole leaf area; stage 3, the area of the lesion accounts for 6% -10% of the whole leaf area; stage 5, the area of the lesion accounts for 11% -20% of the whole leaf area; 7, the area of the lesion accounts for 21-50% of the whole leaf area; grade 9, the area of the disease spots accounts for more than 51% of the whole leaf area.
Table 14 compound I and Zhongshengmycin for field efficacy test of cucumber bacterial angular leaf spot
Note that: the different letters after the same column of data represent significant differences in P <0.05 levels as tested by Duncan's new complex polar error method, the same applies below.
As shown by the measurement results in the table, when the compound I is used for preventing and treating the bacterial angular leaf spot of the cucumber, compared with the compound of the compound I and the Zhongshengmycin and a single dose, the compound of the compound I and the Zhongshengmycin has obviously higher 7-day prevention effect and 14-day prevention effect on the bacterial angular leaf spot of the cucumber than the single dose under the condition of using the same effective components. The control effect can still reach more than 78.5% after 14 days, and the duration is long.
Table 15 Compound I and Zinc thiazole Compound field efficacy test of cucumber bacterial angular leaf spot
As shown by the measurement results in the table, when the compound I is used for preventing and treating the bacterial angular leaf spot of the cucumber, compared with the compound I and the zinc thiazole, the compound I and the zinc thiazole have obviously higher 7-day prevention effect and 14-day prevention effect on the bacterial angular leaf spot of the cucumber than the single dose under the condition of the same effective component dosage. The control effect can still reach more than 80.6% after 14 days, and the duration is long.
Table 16 Compound I and kasugamycin combination field efficacy test for cucumber bacterial angular leaf spot
As shown by the measurement results in the table, when the compound I and the kasugamycin are compounded for preventing and treating the bacterial angular leaf spot of the cucumber, compared with a single dose, the 7-day prevention effect and the 14-day prevention effect of the compound I and the kasugamycin on the bacterial angular leaf spot of the cucumber are obviously higher than those of the single dose under the condition of the same effective component dosage. The control effect can still reach more than 78.9% after 14 days, and the duration is long.
Rice bacterial leaf blight field efficacy test (developed in south Beijing of su):
the test method comprises the following steps: according to the method of drug administration prescribed in national Standard of the people's republic of China GB/T17980.19-2000, drug administration is carried out at the first spot, and the drug administration is carried out 2 nd time after 7 days, and the drug administration is carried out twice and repeated for 4 times.
The investigation method comprises the following steps: according to the investigation method specified in national Standard for the people's republic of China GB/T17980.19-2000, the control effect is investigated 7 days and 14 days after the 2 nd administration.
Bacterial leaf blight disease prevalence (rated visually):
grade 0, no disease; level 1, sporadic onset or central disease group; stage 3, the disease area occupies about one fourth of the total area; 5, the disease area occupies about one third of the total area; level 7, the disease area occupies about one half of the total area; grade 9, the disease area occupies more than three fourths of the total area.
Compound I and Zhongshengmycin of Table 17 for field efficacy test of bacterial leaf blight of rice
As shown by the measurement results, when the compound I is used for preventing and treating the bacterial leaf blight of rice, compared with the compound I and the Zhongshengmycin which are compounded and used as a single agent, the 7-day prevention effect and the 14-day prevention effect of the compound I and the Zhongshengmycin on the bacterial leaf blight of rice are obviously higher than those of the single agent under the condition of the same effective component dosage. The control effect can still reach more than 80.5% after 14 days, and the duration is long.
Compound I and tetramycin of Table 18 for field efficacy test of bacterial leaf blight of rice
As shown by the determination result, when the compound I is used for preventing and treating the bacterial leaf blight of rice, compared with tetramycin compound and single dose, the compound I+tetramycin compound has obviously higher 7-day prevention effect and 14-day prevention effect on the bacterial leaf blight of rice than single dose under the condition of the same effective component dosage. The control effect can still reach more than 78.6% after 14 days, and the duration is long.
Citrus canker field efficacy test (developed in guangxi Wu Ming):
according to pesticide field efficacy test guidelines (GB/T17980.103-2004), a pesticide application method is prescribed, wherein the pesticide is applied by spraying for the first time before flowering is started, and the pesticide is applied by spraying for the second time after diseases appear. The total application is carried out twice, the area of each treatment cell is 3 plants of mature fruit trees, and the repetition times are 4 times. The application times and the application date of each time and the growth period of the fruit tree are recorded.
The investigation method comprises the following steps: according to the investigation method specified in pesticide field efficacy test criterion (GB/T17980.103-2004), two plants are investigated for each district 7d,14d after the second application, each plant is sampled according to five points in the north and south of the east and west, all the leaves on two tips are investigated at each point, and the control and prevention effects are calculated.
Leaf classification method:
level 0: no disease; stage 1: 1 to 5 lesions are arranged on each leaf; 3 stages: 6-10 lesions are formed on each leaf; 5 stages: each leaf has 11 to 15 disease spots; 7 stages: 15-20 lesions are formed on each leaf; stage 9: more than 21 disease spots exist on each leaf;
table 19 Compound I and Zhongshengmycin for field efficacy test of citrus canker
As shown by the determination result, when the compound I is used for preventing and treating the citrus canker, compared with the compound I and the Zhongshengmycin which are compounded and used as single agents, the 7-day prevention effect and the 14-day prevention effect of the compound I and the Zhongshengmycin on the citrus canker are obviously higher than those of the single agents under the condition of the same dosage of the effective components. The control effect can still reach more than 78.5% after 14 days, and the duration is long.
Table 20 Compound I and Shenqinmycin combination field efficacy test for citrus canker
As shown by the determination result, when the compound I is used for preventing and treating the citrus canker, compared with the compound I and the shenzinomycin and the single dose, the compound I and the shenzinomycin are compounded to have the 7-day prevention effect and the 14-day prevention effect on the citrus canker which are obviously higher than those of the single dose under the condition of the same dosage of the effective components. The control effect can still reach more than 79.3% after 14 days, and the lasting period is longer.
The field efficacy test of watermelon fruit blotch (developed in Changle county, weifang, city):
the test method comprises the following steps: the method for applying the medicine is specified by referring to national Standard GB/T17980.110-2004 of the people's republic of China, the medicine is applied when the disease spots are seen at first, the medicine is applied for the 2 nd time after 7 days, the medicine is applied twice in total, and the times of repetition are 4 times.
The investigation method comprises the following steps: the control effect was investigated 7 days and 14 days after the 2 nd administration, referring to the investigation method prescribed in national Standard for the people's republic of China GB/T17980.110-2004.
Sampling 3 points on the diagonal of each cell, 5 strains each, investigating all leaves, and grading the leaves according to the percentage of the disease spot area of each leaf to the whole leaf area.
The grading method comprises the following steps:
grade 0, no disease spots; stage 1, the area of the disease spots accounts for less than 5% of the whole leaf area; stage 3, the area of the lesion accounts for 6% -10% of the whole leaf area; stage 5, the area of the lesion accounts for 11% -20% of the whole leaf area; 7, the area of the lesion accounts for 21-50% of the whole leaf area; grade 9, the area of the disease spots accounts for more than 51% of the whole leaf area.
Compound I and Zhongshengmycin of Table 21 for field efficacy test of watermelon fruit blotch
The test result shows that when the compound I is used for preventing and treating the watermelon fruit blotch, compared with the compound and the single dose of the Zhongshengmycin, the compound I and the Zhongshengmycin have obviously higher 7-day prevention effect and 14-day prevention effect on the watermelon fruit blotch than the single dose of the compound I and the Zhongshengmycin under the condition of the same dosage of effective components. The control effect can still reach more than 78.6% after 14 days, and the duration is long.
Compound I of table 22 and garlicin for field efficacy test of watermelon fruit blotch
The test result shows that when the compound I is used for preventing and treating the watermelon fruit blotch, compared with the garlicin compound and a single dose, the compound I and the garlicin compound have obviously higher 7-day prevention effect and 14-day prevention effect on the watermelon fruit blotch than the single dose under the same dosage of the effective components. The control effect can still reach more than 77.4% after 14 days, and the lasting period is longer.
Tomato bacterial wilt field efficacy test (developed in the city of the Weifang, changle county):
the test method comprises the following steps: the method for applying the pesticide is specified by referring to the national agricultural industry standard NY/T1464.32-2010 of the people's republic of China, root irrigation is carried out when a disease plant is seen at first, the granule is applied by broadcasting when the disease plant is seen at first, the pesticide is applied for the 2 nd time after 7 days, and the pesticide is applied twice in total and repeated for 4 times.
The investigation method comprises the following steps: and (3) referring to a investigation method specified in the agricultural industry standard NY/T1464.32-2010 of the people's republic of China, investigating all plants in each district, and recording the total plant number and the disease plant number. The control effect was investigated 7 days and 14 days after the 2 nd application.
Table 23 Compound I and Zhongshengmycin combination field efficacy test for tomato bacterial wilt
The determination result shows that when the compound I is used for preventing and treating tomato bacterial wilt, compared with the compound and the single dose of the Zhongshengmycin, the compound I and the Zhongshengmycin have obviously higher 7-day prevention effect and 14-day prevention effect on tomato bacterial wilt than the single dose of the compound I and the Zhongshengmycin under the same dosage of active ingredients. The control effect can still reach more than 78.1% after 14 days, and the duration is long.
Tobacco wildfire field efficacy test (developed in Yuxi city of Yunnan province):
the test method comprises the following steps: the method for applying the pesticide is specified by referring to the national agricultural industry standard NY/T1464.44-2012 of the people's republic of China, and the pesticide is applied at the first spot, and is applied for 2 nd times after 7 days, and the pesticide is applied twice in total and is repeated for 4 times.
The investigation method comprises the following steps: and 5 points are randomly surveyed in each district, 1 plant is surveyed in each district, all leaves are surveyed in each plant, the leaf spot area of each plant occupies the percentage of the leaf spot area of the whole leaf, and the total leaf number and the leaf number of each stage are recorded according to the survey method specified in the agricultural industry standard NY/T1464.44-2012 of the people's republic of China.
Table 24 Compound I and ethylicin compound field efficacy test for tobacco wildfire disease
As shown by the determination result, when the tobacco wildfire is prevented and treated, compared with the ethylicin compound and a single dose, the 7-day prevention effect and the 14-day prevention effect of the ethylicin compound and the compound of the compound I on the tobacco wildfire are obviously higher than those of the single dose under the same effective component dosage. The control effect can still reach more than 77.5% after 14 days, and the lasting period is longer.
Field efficacy test of ginger bacterial wilt disease of ginger (developed in Anchu city of Shandong province):
the test method comprises the following steps: the method for applying the pesticide is specified by referring to the national agricultural industry standard NY/T1464.31-2010 of the people's republic of China, and the pesticide is applied at the first spot, and is applied for the 2 nd time after 7 days, and is applied twice in total and repeated for 4 times.
The investigation method comprises the following steps: and 5 points are randomly investigated per cell, 10 plants are investigated per point, all leaf and fleshy stem symptoms are investigated per plant, and the total plant number and the plant number of each stage of diseases are recorded and investigated by referring to an investigation method specified in the agricultural industry standard NY/T1464.31-2010 of the people's republic of China.
Compound I of Table 25 and aureobasidin for field efficacy test of ginger distemper
The test result shows that when the compound I is used for preventing and treating the ginger blast, compared with the aureonucleomycin compound and a single dose, the compound I and the aureonucleomycin compound have obviously higher 7-day prevention effect and 14-day prevention effect on the ginger blast than the single dose under the same effective component dosage. The control effect can still reach more than 77.9% after 14 days, and the lasting period is longer.
Pear fire epidemic disease field efficacy test (developed in kurla, xinjiang):
the test method comprises the following steps: the medicine is applied at the first spot, the medicine is applied for the 2 nd time after 7 days, the medicine is applied twice together, and the times of repetition are 4 times.
The investigation method comprises the following steps: 5 spots were investigated randomly per cell, 10 plants per spot, 10 shoots per plant. The total number of plants and the number of plants with each stage of diseases were recorded and investigated.
Table 26 Compound I and pyrimidine nucleoside antibiotics compound drug efficacy test for Pyricularia fields
As shown by the determination result, when the pear fire disease is prevented and treated, compared with the pyrimidine nucleoside antibiotics and the single dose, the compound of the compound I and the pyrimidine nucleoside antibiotics has obviously higher 7-day prevention effect and 14-day prevention effect on the pear fire disease than the single dose under the condition of the same effective component dosage. The control effect can still reach more than 77.6% after 14 days, and the lasting period is longer.
Field efficacy test of bacterial root cancer disease of fruit tree (developed in Shandong tobacco stand):
the test method comprises the following steps: root irrigation is carried out when the disease plants are seen at first, the granules are broadcast when the disease plants are seen at first, the 2 nd medicine is applied after 7 days, the medicine is applied twice together, and the repetition time is 4.
The investigation method comprises the following steps: all plants were investigated per cell and total and sick plant numbers were recorded. The control effect was investigated 7 days and 14 days after the 2 nd application.
Compound I of Table 27 and amino-oligosaccharin for field efficacy test of bacterial root cancer disease of fruit tree
The determination result shows that when the compound I is used for preventing and treating the bacterial root cancer of the fruit trees, compared with the compound of the amino-oligosaccharin and a single dose, the compound 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 dose under the condition of the same dosage of the effective components. The control effect can still reach more than 78.3% after 14 days, and the duration is longer.
The field efficacy test of the macaque canker disease (developed in Pujiang county, sichuan province):
the test method comprises the following steps: the preparation is applied before germination, and is applied for 2 times after 7 days, and the preparation is applied twice and repeated for 4 times.
The investigation method comprises the following steps: after the second application, 7d and 14d survey two plants in each district, each plant is sampled according to five points in the north and south of the east, 20 branches are surveyed in each plant, and the control and prevention effect is calculated.
Table 28 Compound I and Xinzhimamycin combination field efficacy test for kiwi canker
The test result shows that when the compound I is used for preventing and treating kiwi fruit canker, compared with the compound of the new phytomycin and a single dose, the 7-day prevention effect and the 14-day prevention effect of the compound I and the new phytomycin on kiwi fruit canker are obviously higher than those of the single dose under the condition of the same effective component dosage. The control effect can still reach more than 77.7% after 14 days, and the lasting period is longer.
Corn bacterial stalk rot field efficacy test (developed in Shandong Jinan)
The test method comprises the following steps: spraying at the first occasion of the disease, broadcasting the granule at the first occasion of the disease, and applying the medicine for the 2 nd time after 7 days, wherein the medicine is applied twice together, and the repeated times are 4 times.
The investigation method comprises the following steps: all plants were investigated per cell and total and sick plant numbers were recorded. The control effect was investigated 7 days and 14 days after the 2 nd application.
Compound I and polyoxin of Table 29 for testing field efficacy of corn bacterial stem rot
The test result shows that when the compound I is used for preventing and treating the bacterial stem rot of corn, compared with the polyoxin compound and a single dose, the 7-day control effect and the 14-day control effect of the compound I and the polyoxin compound on the bacterial stem rot of corn are obviously higher than those of the single dose under the condition of the same effective component dosage. The control effect can still reach 78.4% after 14 days, and the duration is long.
Citrus yellow dragon disease field efficacy test (developed in Guangxi Wu Ming)
The test method comprises the following steps: root irrigation is carried out when the disease plants are seen at first, the granules are broadcast when the disease plants are seen at first, the 2 nd medicine is applied after 7 days, the medicine is applied twice together, and the times of repetition are 4 times.
The investigation method comprises the following steps: all plants were investigated per cell and total and sick plant numbers were recorded. The control effect was investigated 7 days and 14 days after the 2 nd application.
Table 30 Compound I and validamycin A field efficacy test of citrus yellow longdisease
The test result shows that when the compound I is used for preventing and treating the citrus yellow dragon disease, compared with the validamycin compound and a single dose, the compound I and the validamycin compound have obviously higher 7-day prevention effect and 14-day prevention effect on the citrus yellow dragon disease than the single dose under the condition of the same effective component dosage. The control effect can still reach 79.3% after 14 days, and the duration is long.
Tomato canker field efficacy test (developed in Shandong Jinan)
The test method comprises the following steps: spraying at the first occasion of the disease, broadcasting the granule at the first occasion of the disease, and applying the medicine for the 2 nd time after 7 days, wherein the medicine is applied twice together, and the repeated times are 4 times.
The investigation method comprises the following steps: all plants were investigated per cell and total and sick plant numbers were recorded. The control effect was investigated 7 days and 14 days after the 2 nd application.
Table 31 Compound I and oligosaccharin for field efficacy test of tomato canker
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The test result shows that when the compound I is used for preventing and treating tomato canker, compared with the compound and the oligosaccharin, the compound I and the oligosaccharin have obviously higher 7-day prevention effect and 14-day prevention effect than the single dosage under the condition of the same dosage of the active ingredients. The control effect can still reach more than 78.4% after 14 days, and the duration is long.
Corn bacterial wilt field efficacy test (developed in Changle county, city of Weifang):
the test method comprises the following steps: root irrigation is carried out when the disease plants are seen at first, the granules are broadcast when the disease plants are seen at first, the 2 nd medicine is applied after 7 days, the medicine is applied twice together, and the times of repetition are 4 times.
The investigation method comprises the following steps: all plants were investigated per cell and total and sick plant numbers were recorded. The control effect was investigated 7 days and 14 days after the 2 nd application.
Table 32 Compound I and hydrated mycin combination field efficacy test for bacterial blight of corn
As shown by the measurement results, when the compound I is used for preventing and treating the bacterial wilt of corn, compared with the compound granule and single dosage of the compound I and the hydrated mycin, the compound I and the hydrated mycin have obviously higher 7-day prevention effect and 14-day prevention effect on the bacterial wilt of corn than the single dosage of the compound I and the hydrated mycin under the same dosage of effective components. The control effect can still reach 76.3% after 14 days, and the duration is long.
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, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (12)

1. The bactericidal composition comprises an effective active ingredient, wherein the effective active ingredient comprises 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 one of mesogenic fungi, kasugamycin, tetramycin, ethylicin, aureonuclycin, shenzinomycin, hydrated fungi, garlicin, neophytmycin, polyoxin, pyrimidine nucleoside antibiotics, validamycin, oligosaccharins, zinc thiazole, benziothiazolin and amino oligosaccharins;
The mass ratio of the compound I to the compound II is 80-1:1-80.
2. The bactericidal composition according to claim 1, wherein the mass ratio of the compound I to the compound II is 50-1:1-50.
3. The bactericidal composition according to claim 1, wherein the mass ratio of the compound I to the compound II is 30-1:1-30.
4. The bactericidal composition according to claim 1, wherein the sum of the mass of the compound I and the mass of the compound II in the bactericidal composition is 1-80% based on 100% of the total weight of the bactericidal composition.
5. The bactericidal composition of claim 1, wherein the bactericidal composition is prepared in a liquid formulation or a solid formulation.
6. The bactericidal composition according to claim 5, wherein the liquid preparation contains 1% -60% by weight of effective active ingredient; the solid preparation contains 5-80% by weight of effective active ingredients.
7. The antiseptic composition of any of claims 1-6, further comprising at least one of an emulsifier, a dispersant, a wetting agent, a thickener, an antifoaming agent, a stabilizer, a binder, a disintegrant, an antifreeze agent, an anticaking agent, a suspending agent, a film former, a preservative, a colorant, a polymeric wall material, a pH adjuster, or a filler.
8. The bactericidal composition of claim 1, wherein the bactericidal composition is formulated as water dispersible granules, dispersible solutions, wettable powders, suspensions, emulsions in water, microemulsions, suspoemulsions, microencapsulated suspension-suspensions, suspended seed coatings, emulsifiable concentrates, granules.
9. Use of the fungicidal composition according to any one of claims 1 to 8 for controlling pathogenic bacteria and agricultural diseases caused thereby.
10. The use according to claim 9, wherein the agricultural disease is a bacterial and bacterially-induced plant bacterial disease.
11. The use according to claim 9, wherein the fungicidal composition is used for controlling crop soft rot, chinese cabbage black rot, cucumber bacterial angular leaf spot, sesame angular leaf spot, west/melon leaf spot, rice bacterial leaf blight, rice bacterial streak, rice bacterial brown spot, rice bacterial brown streak, rice bacterial basal rot, solanaceae bacterial wilt, sang Qing wilt, peanut wilt, ginger blast, tomato/pepper bacterial leaf spot, potato black shank, corn bacterial wilt, corn bacterial stem rot, wheat black rot, soybean bacterial leaf spot, soybean bacterial blight, cassava bacterial wilt, mango angular leaf spot, citrus canker, peach bacterial perforin, sunflower stem rot, peach gummy, pear fire, pear rust water disease, fruit tree bacterial root rot, potato ring rot, bean wilt, wheat Bai Shetiao, winter rot, tomato leaf rot, cucumber leaf rot, rice blast, rice rot, american rice rot.
12. A method of controlling pathogenic bacteria and agricultural diseases caused thereby, comprising applying the fungicidal composition as claimed in any one of claims 1 to 8 to plants in which the diseases are present.
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