CN114766483B - Sterilization composition containing bronopol and application thereof - Google Patents

Sterilization composition containing bronopol and application thereof Download PDF

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Publication number
CN114766483B
CN114766483B CN202210548727.8A CN202210548727A CN114766483B CN 114766483 B CN114766483 B CN 114766483B CN 202210548727 A CN202210548727 A CN 202210548727A CN 114766483 B CN114766483 B CN 114766483B
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active ingredient
bronopol
agent
test
composition
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CN114766483A (en
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葛家成
杨志鹏
刘金玲
刘桂娟
隋书婷
王玉
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Qingdao Hailier Biotechnology Co ltd
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Qingdao Hailier Biotechnology 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
    • A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
    • A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
    • A01N33/18—Nitro compounds
    • A01N33/20—Nitro compounds containing oxygen or sulfur attached to the carbon skeleton containing the nitro group
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G13/00—Protecting plants
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles

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

Abstract

The invention belongs to the technical field of pesticides, and discloses a bactericidal composition containing bronopol and application thereof, wherein the bactericidal composition comprises an active ingredient A and an active ingredient B, the active ingredient A is bronopol, the active ingredient B is selected from any one of fluoxastrobin, isopyrazam or penflufen, and the mass ratio of the active ingredient A to the active ingredient B is 1:35-35:1. The bactericidal composition has higher activity on diseases on various crops, has remarkable synergistic effect, is superior to a single dose in quick-acting property and lasting effect, reduces the dosage of the medicament in agricultural production, reduces the medicament residue of agricultural products, delays the generation of medicament resistance of pathogenic bacteria, and is beneficial to comprehensive treatment of agricultural diseases.

Description

Sterilization composition containing bronopol and application thereof
Technical Field
The invention relates to the technical field of pesticide sterilization compositions and application thereof, in particular to a sterilization composition containing bronopol and application thereof.
Background
Bronitol, chemical name: 2-bromo-2-nitro-1, 3-propanediol, also known as bronopol, and the like. Bromonitroalcohol is a bromonitroalcohol broad-spectrum fungicide. The bronopol has good control effect on plant fungi and bacterial diseases, especially on bakanae disease of rice, and has certain control effect on angular leaf spot of cotton and scab of wheat.
Fluxapyroxad hydroxylamine, ISO common name: pydifumetofen, chemical name: 3- (difluoromethyl) -N-methoxy-1-methyl-N- [ (RS) -1-methyl 2- (2, 4, 6-trichlorophenyl) ethyl ] pyrazole-4-carboxamide, CAS accession No.: 1228284-64-7. The fluxapyroxad hydroxylamine is pyridine amide fungicide which is developed by the company Neida and acts on succinic dehydrogenase, and mainly affects the respiratory chain electron conduction system of pathogenic bacteria, and the junction succinic dehydrogenase which is used for connecting oxidative phosphorylation and electron transfer in the pathogenic bacteria, so that tricarboxylic acid circulation is blocked, the energy metabolism is blocked, the growth of the pathogenic bacteria is further inhibited, and the pathogenic bacteria are killed, so that the purpose of preventing and treating diseases is achieved. The fluxapyroxad hydroxylamine has the characteristics of broad spectrum and high efficiency, and is suitable for a plurality of crops, such as corn, small grain, soybean, peanut, rapeseeds, quinoa and the like.
Isopyrazam, ISO common name: isopyrazam, CAS accession number: 881685-58-1. The isopyrazam is a succinic dehydrogenase inhibitor (SDHI), has both prevention and treatment effects, is mainly used for preventing and treating cereal leaf diseases, and can be used for preventing and treating powdery mildew, eye spots and the like. Besides the common pyrazole ring in the SDHI bactericide, the isopyrazam also contains a unique benzo bridge ring, and the two ring structures enable the isopyrazam to be strongly combined with the binding site on the mitochondrial membrane SDHI enzyme and the waxy layer on the surface of the blade, so that the isopyrazam has higher activity, and the high-efficiency disease control effect and longer lasting period of the isopyrazam in the field are ensured. In addition, the isopyrazam has the remarkable effect of keeping the health of crops, so that the photosynthesis of the crops is greatly improved, the yield is improved, and meanwhile, the harvesting time of the crops can be remarkably prolonged.
Penflufen, ISO common name: penflufen, chemical name: n- [2- (1, 3-dimethylbutyl) phenyl ] -5-1, 3-dimethyl-1H-pyrazole-4-carboxamide, CAS accession no: 494793-67-8. The penflufen is a pyrazole amide fungicide developed by Bayer, has good activity on various plant pathogenic fungi, is a succinic dehydrogenase inhibitor, and mainly acts on a respiratory chain electron transfer complex II to block energy metabolism. The penflufen has systemic, preventive and therapeutic effects and long lasting period. It is mainly used as a bactericidal seed treatment agent, and after seed treatment, the agent is permeated into germinated seeds and is conducted to the whole plant through the xylem of young plants, so that the grown seedlings are protected.
Succinate dehydrogenase inhibitor (SDHI) bactericide acts on respiratory chain succinate dehydrogenase of pathogenic fungi, and blocks electron transfer to interfere with fungal energy metabolism to perform sterilization. The SDHI bactericide has a single action site and a broad bactericidal spectrum, and has good control effect on various plant pathogenic fungi. However, due to the wide high frequency of use, resistant strains have emerged in the field, leading to a wide range of resistance and reduced field efficacy. Due to the single site of action, FRAC classifies SDHI-based bactericides as medium to high resistance risk agents, and problems of resistance development, reduced efficacy, etc. are unavoidable with the wide development and frequent use of such products. In order to delay the occurrence and development of resistance and improve the control effect, effective resistance management measures must be adopted in agricultural production. Therefore, the inventor finds that the bromonitrol is compounded with the SDHI bactericide (any one of the triflumizole acyl hydroxylamine, the isopyrazam or the penflufen through a large amount of experimental researches, so that the prevention and control effect is improved, the prevention and control spectrum is enlarged, and the generation of pathogenic bacteria resistance is delayed.
Disclosure of Invention
Based on the above circumstances, the invention aims to provide a bactericidal composition containing bronopol, which is effective for plant pathogenic bacteria, can obviously enhance the drug effect, is superior to a single dose in quick-acting and lasting effects, reduces the dosage of the drug in agricultural production, slows down the development of drug resistance of pathogenic bacteria, reduces the drug residue of agricultural products, and is beneficial to the comprehensive treatment of agricultural diseases.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the bactericidal composition containing the bronopol comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is the bronopol, the active ingredient B is selected from any one of fluoxastrobin, isopyrazam or penflufen, and the mass ratio of the active ingredient A to the active ingredient B is 1:35-35:1;
further, the active ingredient B is fluxapyroxad hydroxylamine, and the mass ratio of the active ingredient A to the active ingredient B is 1:30-30:1;
further, the mass ratio of the active component A to the active component B is 1:15-20:1;
further, the active ingredient B is isopyrazam, and the mass ratio of the active ingredient A to the active ingredient B is 1:30-30:1;
further, the mass ratio of the active component A to the active component B is 1:20-30:1;
further, the active ingredient B is penflufen, and the mass ratio of the active ingredient A to the active ingredient B is 1:25-25:1;
further, the mass ratio of the active component A to the active component B is 1:15-25:1.
Further, the total weight of the bactericidal composition is 1-80% of the total weight of the bactericidal composition based on 100 wt%;
further, the bactericidal composition comprises other auxiliary components besides the active components, wherein the auxiliary components are selected from one or more of wetting agents, dispersing agents, emulsifying agents, thickening agents, disintegrating agents, antifreezing agents, antifoaming agents, solvents, preservatives, stabilizers, warning colors, film forming agents, synergists and carriers;
the wetting agent is selected from one or more of alkylbenzene sulfonate, alkyl naphthalene sulfonate, lignin sulfonate, sodium dodecyl sulfate, dioctyl sodium sulfosuccinate, alpha-olefin sulfonate, alkylphenol ethoxylate, castor oil polyoxyethylene ether, alkylphenol ethoxylate, fatty alcohol polyoxyethylene ether sodium sulfate, silkworm excrement, spina gleditsiae powder, soapberry powder, SOPA, detergent, emulsifier 2000 series and wetting penetrating agent F; and/or
The dispersing agent is selected from one or more of lignosulfonate, alkyl naphthalene sulfonate formaldehyde condensate, naphthalene sulfonate, tristyrylphenol ethoxylate phosphate, fatty alcohol ethoxylate, alkylphenol ethoxylate methyl ether condensate sulfate, fatty amine ethoxylate, glycerin fatty acid ester polyoxyethylene ether, polycarboxylate, polyacrylic acid, phosphate, EO-PO block copolymer and EO-PO graft copolymer; and/or
The emulsifier is one or more selected from calcium dodecyl benzene sulfonate, alkylphenol formaldehyde resin polyoxyethylene ether, phenethyl phenol polyoxyethylene polyoxypropylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, styrylphenol polyoxyethylene ether, castor oil polyoxyethylene ether and alkylphenol ether phosphate; and/or
The thickener is one or more selected from xanthan gum, organic bentonite, gum arabic, sodium alginate, magnesium aluminum silicate, carboxymethyl cellulose and white carbon black; and/or
The disintegrating agent is one or more selected from sodium sulfate, ammonium sulfate, aluminum chloride, sodium chloride, ammonium chloride, bentonite, glucose, sucrose, starch, cellulose, urea, sodium carbonate, sodium bicarbonate, citric acid and tartaric acid; and/or
The antifreezing agent is one or more selected from alcohols, alcohol ethers, chlorinated hydrocarbons and inorganic salts; and/or
The defoamer is selected from C 10 -C 20 Saturated fatty acid compound, silicone oil, silicone compound, C 8 -C 10 One or more of the fatty alcohols; and/or
The solvent is selected from one or more of benzene, toluene, xylene, durene, methanol, ethanol, isopropanol, n-butanol, dimethyl sulfoxide, dimethylformamide, cyclohexanone, alkylene carbonate, diesel oil, solvent oil, vegetable oil derivatives and water; and/or
The preservative is selected from one or more of propionic acid, sodium propionate, sorbic acid, sodium sorbate, potassium sorbate, benzoic acid, sodium benzoate, sodium p-hydroxybenzoate, methyl p-hydroxybenzoate, pinocembrane and 1, 2-benzisothiazolin-3-one; and/or
The stabilizer is one or more selected from disodium hydrogen phosphate, oxalic acid, succinic acid, adipic acid, borax, 2, 6-di-tert-butyl-p-cresol, triethanolamine oleate, epoxidized vegetable oil, kaolin, bentonite, attapulgite, white carbon black, talcum powder, montmorillonite and starch; and/or
The warning color is selected from any one or more of blue, green, red and purple regulating colors; and/or
The film forming agent is one or more of sodium carboxymethyl starch, cellulose derivatives (sodium carboxymethyl cellulose, sodium alginate, polyvinyl alcohol) and polyacrylic acid; and/or
The synergistic agent is selected from synergistic phosphorus and synergistic ether; and/or
The carrier is selected from one or more of ammonium salt, ground natural mineral, ground artificial mineral, silicate, resin, wax, solid fertilizer, water, organic solvent, mineral oil, vegetable oil and vegetable oil derivative;
further, the bactericidal composition can be prepared into any one of agriculturally acceptable preparation formulations, wherein the preparation formulations are solid preparations, liquid preparations and/or seed treatment preparations;
further, the solid preparation is a direct-use solid preparation, a dispersible solid preparation or a soluble solid preparation;
further, the directly-used solid preparation is powder, granule, sphere, tablet or strip;
the dispersible solid preparation is wettable powder, oil dispersion powder, emulsion powder, water dispersible granule, emulsion granule or water dispersible tablet;
the soluble solid preparation is soluble powder, soluble tablets or soluble granules;
further, the liquid preparation is a solution preparation, a dispersion liquid preparation, an emulsion preparation, a suspension preparation or a multiphase preparation;
further, the solution preparation is a soluble agent, an oil agent or a film spreading oil agent;
the dispersion liquid preparation is emulsifiable concentrate, emulsion, dispersible agent or paste;
the emulsion preparation is aqueous emulsion, oil emulsion, microemulsion or fat agent;
the suspension preparation is suspending agent, microcapsule suspending agent, oil suspending agent or dispersible oil suspending agent;
the multiphase preparation is a suspension emulsion, a microcapsule suspension-suspending agent, a microcapsule suspension-water emulsion or a microcapsule suspension-suspending emulsion;
further, the seed treatment preparation comprises a seed treatment solid preparation or a seed treatment liquid preparation;
further, the seed treatment solid preparation is seed treatment dry powder or seed treatment dispersible powder;
the seed treatment liquid preparation is a seed treatment liquid, a seed treatment emulsion or a seed treatment suspending agent;
furthermore, the solid preparation is water dispersible granule and/or wettable powder, the liquid preparation is suspension agent, and the seed treatment preparation is seed treatment suspension agent.
The invention also discloses the application of the bactericidal composition and/or the preparation thereof in preventing or controlling crop pathogenic bacteria.
Further, the crop is selected from grain crops, cash crops, fruits and vegetables and/or lawn garden crops;
further, the pathogenic bacteria are Fusarium (Fusarium) pathogenic bacteria, wherein the Fusarium pathogenic bacteria comprise Fusarium oxysporum (Fusarium oxysporum), fusarium seminude (Fusarium incarnatum), fusarium layering (Fusarium proliferatum), fusarium equiseti (Fusarium equiseti), fusarium verticillatum (Fusarium verticillicides), fusarium graminearum (Fusarium graminearum) and Fusarium moniliforme (Fusarium moniliforme);
further, the fusarium pathogenic bacteria is selected from fusarium graminearum (Fusarium graminearum) and fusarium moniliforme (fusarium moniliforme).
The invention also discloses a method for preventing and controlling pathogenic bacteria of crops, wherein the bactericidal composition and/or the preparation thereof is applied to plants, plant propagation materials and plant organs, cultivation media, materials or spaces growing later by the methods of seed treatment, foliar application, stem application, soaking, instillation, casting, spraying, atomizing, powdering, scattering or fuming and the like in an effective and basically non-phytotoxic application amount.
Compared with the prior art, the invention has the advantages that:
1) The reasonable combination of bronopol and any one of the fluoxastrobin, the isopyrazam or the penflufen has remarkable synergistic effect, and the prevention and treatment effect on pathogenic bacteria is improved;
2) Any action mechanism of bronopol and fluxapyroxad hydroxylamine, isopyrazam or penflufen is different, which is beneficial to delay the development of drug resistance of pathogenic bacteria;
3) The usage amount of the pesticide in agricultural production is reduced, pesticide residue of agricultural products is reduced, and the pesticide is environment-friendly and is beneficial to comprehensive treatment of agricultural diseases.
Detailed Description
For a better understanding of the nature of the present invention, reference will now be made in detail to the following examples, which are not to be construed as limiting the invention, but are set forth in the following examples.
Preparation example:
preparation example 1:30% bronopol-penflufen seed treatment suspending agent (1:1)
The composition comprises, by weight, 15% of bronopol, 15% of penflufen, 4% of alkylphenol ethoxylates, 5% of alkylphenol ethoxylate phosphate, 3% of sodium lignin sulfonate, 2% of polyacrylic acid, 0.2% of xanthan gum, 6% of rose pigment, 5% of ethylene glycol, 1% of magnesium aluminum silicate, 0.5% of organosilicon defoamer, 1% of sodium benzoate and deionized water, and the balance.
The preparation method comprises the following steps: the active ingredients, the auxiliary agent and the water are subjected to high-shear mixing and stirring uniformly according to the proportion, and then are subjected to sand grinding for 2.5 hours by a sand grinder, so that the average particle size reaches 1-5 microns, and finally, the thickening agent and the preservative film forming agent are added for continuous shearing and stirring uniformly, so that the seed treatment suspending agent can be obtained.
Preparation example 2:24% bronopol-penflufen seed treatment suspending agent (1:3)
The weight percentages of the bromalcohol, the penflufen 18%, the tristyrylphenol polyoxyethylene ether polyoxypropylene ether 4%, the styrylphenol polyoxyethylene ether phosphate 3%, the sodium salt of the polycarboxylic acid 2%, the polyacrylic acid 1%, the xanthan gum 0.2%, the magnesium aluminum silicate 1%, the glycerol 5%, the rose pigment 5%, the methyl p-hydroxybenzoate 1%, the organosilicon defoamer 0.5% and the deionized water are the balance.
The preparation method comprises the following steps: the same as in preparation example 1.
Preparation example 3:30% bronopol-penflufen seed treatment suspending agent (5:1)
25% of bronopol, 5% of penflufen, 4% of fatty alcohol polyoxyethylene ether, 5% of glycerol fatty acid ester polyoxyethylene ether phosphate, 2% of sodium polycarboxylate, 0.2% of xanthan gum, 5% of rose pigment, 2% of sodium carboxymethyl starch, 5% of propylene glycol, 0.5% of organosilicon defoamer, 2% of sodium sorbate and deionized water, and the balance of the composition.
The preparation method comprises the following steps: the same as in preparation example 1.
Preparation example 4:28% bronopol-fluxapyroxad hydroxylamine seed treatment suspending agent (3:1)
The composition comprises, by weight, 21% bronopol, 7% fluxapyroxad hydroxylamine, 3% isomeric tridecanol polyoxyethylene ether, 3% alkylphenol polyoxyethylene ether phosphate, 2% polycarboxylic acid sodium salt, 1% polyacrylic acid, 0.2% xanthan gum, 4% rose pigment, 5% propylene glycol, 1% magnesium aluminum silicate, 3% sodium benzoate, 0.5% silicone defoamer and deionized water, wherein the balance is the composition.
The preparation method comprises the following steps: the same as in preparation example 1.
Preparation example 5:30% bronopol-fluxapyroxad hydroxylamine seed treatment suspending agent (1:1)
The composition comprises, by weight, 15% of bronopol, 15% of fluxapyroxad hydroxylamine, 2% of fatty alcohol polyoxyethylene ether, 3% of alkylphenol polyoxyethylene ether phosphate, 3% of naphthalene sulfonate formaldehyde condensate, 2% of polyvinyl alcohol, 0.3% of xanthan gum, 5% of rose pigment, 4% of ethylene glycol, 1.5% of magnesium aluminum silicate, 0.5% of an organosilicon defoamer, 0.1% of kathon and the balance of deionized water.
The preparation method comprises the following steps: the same as in preparation example 1.
Preparation example 6:32% bronopol-fluxapyroxad hydroxylamine seed treatment suspending agent (7:1)
28% of bronopol, 4% of fluxapyroxad hydroxylamine, 4% of isomeric tridecanol polyoxyethylene ether, 3% of EO/PO block copolymer, 3% of glycerin fatty acid ester polyoxyethylene ether phosphate, 3% of sodium lignin sulfonate, 2% of sodium carboxymethyl cellulose, 5% of glycerol, 0.3% of xanthan gum, 1.5% of magnesium aluminum silicate, 0.5% of organic silicon defoamer, 6% of rose pigment, 1% of potassium benzoate and the balance of deionized water.
The preparation method comprises the following steps: the same as in preparation example 1.
Preparation example 7:20% bronopol-fluxapyroxad hydroxylamine suspension (1:1)
The balance of 10 percent of bronopol, 10 percent of fluxapyroxad hydroxylamine, 2 percent of sodium dodecyl sulfate, 1 percent of alkylphenol ethoxylate, 3 percent of styrol polyoxyethylene ether phosphate, 0.2 percent of xanthan gum, 1 percent of magnesium aluminum silicate, 3 percent of ethylene glycol, 1 percent of sodium benzoate, 0.5 percent of silicone oil and deionized water.
The preparation method comprises the following steps: according to the formula proportion, the active ingredients, the surfactant and other functional auxiliary agents are sequentially placed in a reaction kettle, water is added and mixed uniformly, high-speed shearing and wet sanding are carried out, and finally, the suspending agent product is obtained through homogenizing and filtering.
Preparation example 8:36% bronopol and fluxapyroxad hydroxylamine water dispersible granule (3:1)
The weight percentages of the components are 27 percent of bronitol, 9 percent of fluxapyroxad hydroxylamine, 8 percent of sodium lignin sulfonate, 6 percent of naphthalene sulfonate formaldehyde condensate, 3 percent of nekal BX, 5 percent of white sugar and the balance of kaolin.
The preparation method comprises the following steps: according to the formula proportion of the embodiment, adding the active ingredients into a carrier, adding a surfactant and other functional additives into the carrier, mixing, adding 10-25% of water after jet milling, and then kneading, granulating, drying and screening to obtain a water dispersible granule product; or spraying water, granulating, drying, and sieving to obtain the final product.
Preparation example 9:48% bronopol-fluxapyroxad hydroxylamine wettable powder (1:5)
8% of bronopol, 40% of fluxapyroxad hydroxylamine, 12% of naphthalene sulfonate formaldehyde condensate, 3% of calcium lignosulfonate, 2% of sodium dodecyl sulfate and the balance of kaolin.
The preparation method comprises the following steps: the active ingredients, the dispersing agent, the wetting agent and the filler are mixed according to the formula proportion, uniformly stirred in a stirring kettle, and crushed and uniformly mixed for a plurality of times by a jet mill, thus obtaining the wettable powder of the composition.
Preparation example 10:30% bronopol-isopyrazam suspension (1:3)
The balance is 7.5 percent of bronopol, 22.5 percent of isopyrazam, 2 percent of fatty alcohol polyoxyethylene ether, 3 percent of alkylphenol polyoxyethylene ether phosphate, 2 percent of sodium lignin sulfonate, 0.3 percent of xanthan gum, 1.5 percent of magnesium aluminum silicate, 5 percent of propylene glycol, 0.5 percent of silicone oil, 0.01 percent of benzisothiazolinone potassium and deionized water.
The preparation method comprises the following steps: the same as in preparation example 7.
Preparation example 11:32% bronopol-isopyrazam water dispersible granule (1:1)
The balance of the composition comprises, by weight, 16% of bronitol, 16% of isopyrazam, 3% of sodium dodecyl sulfate, 6% of sodium lignin sulfonate, 10% of naphthalene sulfonate formaldehyde condensate, 10% of ammonium sulfate and starch.
The preparation method comprises the following steps: the same as in preparation example 8.
Preparation example 12:44% bronopol-isopyrazam wettable powder (1:10)
The balance is composed of 4% bronitol, 40% isopyrazam, 3% sodium polycarboxylate, 4% sodium lignin sulfonate, 6% dispersant NNO, 3% sodium dodecyl sulfate and kaolin according to weight percentage.
The preparation method comprises the following steps: same as in preparation example 9.
Indoor Activity assay:
example 1: indoor activity determination test for rice bakanae disease by compounding bronitol and any one of fluxapyroxad hydroxylamine or fluxapyroxad
The test is based on: test reference NY/T1156.2-2006 agricultural industry standard "pesticide indoor bioassay test criteria section 2 of the people's republic of China: test plate method for inhibiting growth of pathogenic bacterial hyphae.
Test strain: fusarium moniliforme (Fusarium moniliforme), offered by the Shenyang chemical institute.
Instrument apparatus: high pressure steam sterilizer, ultra clean bench, incubator, electrothermal blowing dry box, ten thousandth electronic balance, pipettor, alcohol lamp, beaker (50 mL), volumetric flask, triangular flask (100 mL), culture dish (Φ9cm), puncher (Φ0.6cm), inoculator, ruler, etc.
Test target culture conditions: fusarium moniliforme preserved at the temperature of 4 ℃ in an indoor refrigerator is transferred onto a potato dextrose agar culture medium, and is activated for standby after being placed in a 25 ℃ incubator for 5 days of dark culture.
Test agent: 95% bronopol technical, 98% fluxapyroxad hydroxylamine technical and 95% fluxapyroxad technical are provided by the research and development center of the halider pharmaceutical industry group.
Other reagents: acetone (analytically pure), tween 80 (chemically pure).
And (3) preparation of a medicament mother solution: the raw materials are respectively dissolved by acetone to prepare high-concentration mother liquor, then the mother liquor is diluted by 0.1% Tween 80 aqueous solution to respectively prepare single-dose mother liquor, different proportions are designed according to the mixing purpose and the medicament activity, and each single dose and each group of proportion mixture are prepared into the required series of mass concentrations.
Test replicates: test agents were 4 dishes per concentration, 1 dish per replicate, 4 replicates total, with 0.1% tween 80 in water without agent as a blank.
And (3) medicament treatment: under the aseptic operation condition, 5mL of liquid medicine with different concentrations is respectively added into a sterilized triangular flask which is calibrated accurately in advance by a liquid transfer device, then a culture medium which is melted and cooled to a proper temperature is added into the triangular flask, and the culture medium is poured into 4 culture dishes with equal quantity after being fully and evenly shaken, so that a tablet of the PDA containing the medicine with corresponding concentration is prepared.
Inoculating: cutting bacterial cake from colony edge with sterilized puncher under aseptic condition, inoculating bacterial cake in the center of medicated plate with inoculator, covering bacterial cover, and culturing in dark in constant temperature incubator at 25deg.C.
Data investigation: the experimental investigation was performed according to the time when colonies grew to a size of 2/3 to 4/5 of the diameter of the dish in the control treatment. Colony diameters (cm) were measured with a ruler, and each colony was measured once by the cross method, and the average value was taken.
Data statistics and analysis: according to the investigation result, the hypha growth inhibition rate of each treatment concentration on the target bacteria to be tested is calculated, wherein the unit is the calculated result of percentage (%) and two positions after decimal point are reserved.
D＝D 1 -D 2
Wherein:
d-colony growth diameter;
D 1 colony diameter;
D 2 -diameter of the bacterial cake.
Wherein:
i, hypha growth inhibition rate;
D 0 -the control colony increased in diameter;
D T -the agent-treated colonies increased in diameter.
And processing the data by adopting a probability value analysis method. Analyzing by IBM SPSS Statistics statistical analysis system to obtain virulence regression line and EC 50 Value and correlation coefficient R 2 The activity of the test agent on the biological test material was evaluated.
Grand cloud Pei method: evaluating the synergistic effect of the mixed medicaments according to the co-toxicity coefficient (CTC), wherein the compounded co-toxicity coefficient CTC is more than or equal to 120 and shows the synergistic effect; ctc.ltoreq.80 shows antagonism; 80 < CTC < 120 shows additive effect.
Co-toxicity coefficient (CTC value) of the blend was calculated:
wherein:
ati—actual measured virulence index of the mixture;
S-EC of Standard Agents 50 Milligrams per liter (mg/L);
M-EC of mixture 50 Units are milligrams per liter (mg/L).
TTI＝TI A *P A +TI B *P B
Wherein:
TTI-the theoretical toxicity index of the mixture;
TI A -a medicament virulence index;
P A -the percentage of agent a in the mix, in percent (%);
TI B -B agent virulence index;
P B the percentage of the B medicament in the mixture is expressed as percentage (%).
Wherein:
ctc—co-toxicity coefficient;
ati—actual measured virulence index of the mixture;
TTI-the theoretical toxicity index of the mixture.
The test results are shown in the following table:
TABLE 1 results of indoor Activity test of bronopol and penflufen against bakanae disease in rice
Table 2 results of indoor Activity test of Bromonitrol and Fluoxazoyl hydroxylamine on Rice bakanae disease
As shown in the indoor activity tests in tables 1 and 2, the compound of bronopol and any one of fluxapyroxad hydroxylamine or fluxapyroxad aniline has good control effect on bakanae disease of rice.
From the test results of Table 1As can be seen, the test agents bronopol and penflufen have better control effect on bakanae disease germs of rice, and EC thereof 50 The mass ratio of the bronopol to the penflufen is greater than 120 in the range of 1:35-35:1, and the bronopol and the penflufen have synergistic effects on the bakanae disease of the rice, wherein the maximum co-toxicity coefficient is achieved when the bronopol and the penflufen are compounded according to the mass ratio of 1:1, and the synergistic effects are most remarkable.
As shown in the test results in Table 2, the test agent fluxapyroxad hydroxylamine has high toxicity to bakanae disease of rice, EC 50 The mass ratio of bromonitrol to fluxapyroxad hydroxylamine is 0.053mg/L, the mass ratio is in the range of 1:35-35:1, the co-toxicity coefficient is more than 80, the bromonitrol and fluxapyroxad hydroxylamine have different addition or synergism effects on the bakanae disease of rice, the mass ratio of bromonitrol to fluxapyroxad hydroxylamine is in the range of 1:15-25:1, the co-toxicity coefficient is more than 120, and the synergistic effect is shown on the bakanae disease of rice.
Example 2: indoor activity determination test for wheat scab by compounding bronopol with any one of fluxapyroxad hydroxylamine or isopyrazam
The test is based on: test reference NY/T1156.2-2006 agricultural industry standard "pesticide indoor bioassay test criteria section 2 of the people's republic of China: test plate method for inhibiting growth of pathogenic bacterial hyphae.
Test target: fusarium graminearum (Fusarium graminearum) is obtained from the wheat test field of Shandong university of agriculture, and the disease plants are isolated, identified and stored by Shandong university of agriculture laboratory.
Instrument apparatus: a wet heat sterilization pot, an ultra-clean workbench, a constant temperature illumination incubator, an electric heating drum windproof drying box, a ten thousandth electronic balance, a pipetting gun, an alcohol lamp, a small beaker, a volumetric flask, a triangular flask, a culture dish (phi 9 cm), a puncher, an inoculator (phi 0.6 cm), a ruler and the like.
Test target culture conditions: fusarium graminearum stored at 4 ℃ in an indoor refrigerator is transferred onto a potato dextrose agar culture medium, and is activated for standby after being placed in a 26 ℃ incubator for 4 days of dark culture.
Test agent: 95% of bronopol technical, 98% of fluxapyroxad hydroxylamine technical and 92% of isopyrazam technical are provided by the research and development center of the halider pharmaceutical industry group.
Other reagents: solvent acetone (analytically pure), emulsifier tween 80 (chemically pure).
And (3) preparation of a medicament mother solution: the raw materials are respectively dissolved by acetone to prepare high-concentration mother liquor, then the mother liquor is diluted by 0.1% Tween 80 aqueous solution to respectively prepare single-dose mother liquor, different proportions are designed according to the mixing purpose and the medicament activity, and each single dose and each group of proportion mixture are prepared into the required series of mass concentrations.
Test replicates: test agents were 4 dishes per concentration, 1 dish per replicate, 4 replicates total, with 0.1% tween 80 in water without agent as a blank.
And (3) medicament treatment: under the aseptic operation condition, the PDA culture medium which is melted and sterilized in advance is quantitatively added into an aseptic conical flask according to the test treatment, 10mL of each prepared treatment liquid medicine is quantitatively sucked from low concentration to high concentration in sequence, the prepared treatment liquid medicines are respectively added into the conical flask, the conical flask is fully and uniformly shaken, and then the mixed liquid medicines are poured into 4 culture dishes with the diameter of 9cm in equal quantity to prepare a medicine-containing flat plate with the corresponding concentration. The test set up was run with a blank of 0.1% tween 80 in water without the addition of the agent, and 4 replicates per treatment.
Inoculating: cutting bacterial cake from colony edge with sterilized puncher under aseptic condition, inoculating bacterial cake in the center of medicated plate with inoculator, covering bacterial cover, and culturing in dark in constant temperature illumination incubator at 26deg.C.
Data investigation: the growth of pathogenic hyphae was investigated according to the growth of hyphae in a blank culture dish. Colony diameters were measured in centimeters (cm) using a ruler, diameters were measured once per colony using the cross-over method, averages were taken, and raw data was recorded for each treatment in duplicate.
Data statistics and analysis: according to the investigation result, the hypha growth inhibition rate of each treatment concentration on the target bacteria to be tested is calculated, wherein the unit is the calculated result of percentage (%) and two positions after decimal point are reserved.
D＝D 1 -D 2
Wherein:
d-colony growth diameter;
D 1 colony diameter;
D 2 -diameter of the bacterial cake.
Wherein:
i, hypha growth inhibition rate;
D 0 -the control colony increased in diameter;
D T -the agent-treated colonies increased in diameter.
And processing the data by adopting a probability value analysis method. Analyzing by IBM SPSS Statistics statistical analysis system to obtain virulence regression line and EC 50 Value and correlation coefficient R 2 The activity of the test agent on the biological test material was evaluated.
Grand cloud Pei method: evaluating the synergistic effect of the mixed medicaments according to the co-toxicity coefficient (CTC), wherein the compounded co-toxicity coefficient CTC is more than or equal to 120 and shows the synergistic effect; ctc.ltoreq.80 shows antagonism; 80 < CTC < 120 shows additive effect.
Co-toxicity coefficient (CTC value) of the blend was calculated:
wherein:
ati—actual measured virulence index of the mixture;
S-EC of Standard Agents 50 Milligrams per liter (mg/L);
M-EC of mixture 50 Units are milligrams per liter (mg/L).
TTI＝TI A *P A +TI B *P B
Wherein:
TTI-the theoretical toxicity index of the mixture;
TI A -a medicament virulence index;
P A -the percentage of agent a in the mix, in percent (%);
TI B -B agent virulence index;
P B the percentage of the B medicament in the mixture is expressed as percentage (%).
Wherein:
ctc—co-toxicity coefficient;
ati—actual measured virulence index of the mixture;
TTI-the theoretical toxicity index of the mixture.
The test results are shown in the following table:
table 3 results of indoor Activity test of Bromonitrol and Fluoxazoyl hydroxylamine on wheat scab
Table 4 results of indoor Activity test of Bromonitrol and isopyrazam on wheat scab
As shown in the indoor activity tests in tables 3 and 4, the compound of bronopol and any one of fluxapyroxad hydroxylamine or isopyrazam shows good control effect on wheat scab.
As shown in the test results in Table 3, the test reagent fluxapyroxad hydroxylamine has good control effect on wheat scab and EC thereof 50 The mass ratio of the bronopol and the fluxapyroxad hydroxylamine is 0.079mg/L, the co-toxicity coefficient is more than 120 in the range of 1:35-35:1, and the synergistic effect is achieved on wheat scab, wherein the bronopol and the fluxapyroxad are used for preparing the compositionThe hydroxylamine has the greatest co-toxicity coefficient and the most obvious synergistic effect when compounded according to the mass ratio of 1:1.
As shown in the test results in Table 4, the test agents including bronopol and isopyrazam have good control effect on wheat scab, EC 50 6.572mg/L and 4.221mg/L respectively, the bronopol and the isopyrazam are compounded, the mass ratio is in the range of 1:30-30:1, the co-toxicity coefficient is more than 120, and the synergistic effect is shown on wheat scab.
And (3) field efficacy test:
example 3: test of drug effect of compound preparation in field for preventing and controlling bakanae disease of rice
The test is based on: the test is described in GB/T17980.104-2004 section 104 of pesticide field efficacy test criterion (II): bactericide for controlling bakanae disease of rice.
Test target: bakanae disease of rice.
Test crop: rice (Hubei province 17).
Test site: white lotus river village in Luo field county of Huanggao province. The bakanae disease of the rice is a common disease in the rice production in the region, and the bakanae disease of the rice in the test field in 2018 slightly occurs. The soil in the test land is the latent rice soil, the pH value is 5.5, the organic matter content is 1.5%, and the soil fertility is moderate.
And (3) water and fertilizer management in a test land: 50kg of 30% (15-7-8) of compound fertilizer is applied to each mu of the paddy rice (5 months and 8 days) before transplanting, 12kg of 46.4% urea is applied to each mu of the paddy rice (5 months and 17 days) as a base fertilizer, and 6kg of 46.4% urea is applied to each mu of the paddy rice (7 months and 1 day) as a secondary additional fertilizer.
Weather data: the weather of the current day 2019 and 31 of the application is cloudy, the temperature is 5-19 ℃, and severe weather affecting the test result does not appear in the test period.
Cell arrangement: cell treatments with test, control and blank control agents used a randomized block arrangement.
Cell area: area of each test cell 24m 2 The cells are provided with guard rows, each processing being repeated 4 times.
Dosage of the medicament: the test agents and the dosage are shown in the following table:
table 4 test agent for field efficacy test of bakanae disease of rice and dosage thereof
Numbering device Medicament name Dosage of active ingredient (g/100 kg seed)
1 30% bronopol-penflufen seed treatment suspending agent (1:1) 50
2 32% bronopol-fluxapyroxad hydroxylamine seed treatment suspending agent (7:1) 50
3 28% bronopol-fluxapyroxad hydroxylamine seed treatment suspending agent (3:1) 50
4 24% bronopol-penflufen seed treatment suspending agent (1:3) 50
5 200 g/L fluxapyroxad hydroxylamine suspension 100
6 22.4% penflufen seed treatment suspending agent 60
7 20% bronopol wettable powder 85
8 Blank control -
The application method comprises the following steps: coating is carried out before sowing the rice. Weighing each treated seed according to the seed quantity per mu, filling into a sealing bag for standby, fully stirring each treatment liquid medicine and the seeds according to a test scheme until the liquid medicine is uniformly distributed on the surfaces of the seeds, and sowing after airing.
Sowing: the seedbed is used for sowing 4 trays (55 cm x 25 cm) in each district, the seedbeds are placed in different directions of the district, and the number of seeds sown in each tray is about 3900, so that the seedling emergence rate is investigated.
Time and frequency of application: seed coating was performed on 31 days 3.2019 for a total of 1 application.
Experimental investigation: a total of 3 surveys are conducted, the first survey is conducted on the seedling emergence time and the seedling emergence rate when the seedbed seedlings emerge, 4-disc rice sown at fixed points is surveyed in each district, and 1/2 disc is surveyed in each disc; secondly, investigating the disease plant rate before transplanting rice seedlings, sampling 5 points in each district, investigating 100 plants in each point, investigating the number of disease plants and total plants in each treatment, and calculating the control effect; thirdly, the disease condition is investigated before the rice heading, 5 points are sampled in each district, 20 clusters are obtained in each point, the number of disease plants and total plants in each treatment are investigated, and the control effect is calculated.
Safety investigation: after the test, field observation is carried out, the rice in each chemical treatment area grows normally and is basically consistent with that in a blank control area, and all test chemical has no harmful effects on rice such as growth resistance, green loss, deformity and the like. In contrast to the blank, no effect of each treatment agent on the other target organisms was seen.
The drug effect calculation method comprises the following steps:
the test results are shown in the following table:
table 5 test results of the drug efficacy of the Compound formulation for controlling bakanae disease in Rice field
And (3) analyzing the pesticide effect of the field test: the compound preparation is used for coating rice seeds, and the investigation result shows that the emergence rate of each treatment of the test agent is basically consistent with or even better than that of the control treatment. Before transplanting rice seedlings, the disease rate of the rice is investigated, the average disease rate of blank control treatment reaches 8.50%, and the control effect of the compound preparation is higher than 84.12%; the investigation result of the control effect before the heading of the rice shows that the control effect of the compound preparation on the bakanae disease of the rice is between 84.71 and 94.76 percent, which is superior to that of single-dose control.
Example 4: field efficacy test of compound preparation for preventing and treating wheat scab
The test is based on: test reference NY/T1464.15-2007 section 15 of pesticide field efficacy test guidelines: the bactericide can prevent and treat wheat scab.
Test target: wheat scab.
Test crop: wheat (Jimai 22).
Test site: in a field where rice and wheat rotation is carried out in Yutai county Zhang Huangzhen Sanbeun village in Shandong province for many years, wheat scab is serious in the past, the seed consumption per mu is 20kg, the soil of a test land is clay loam, the soil fertility is moderate, the cultivation conditions of all the test communities are consistent, and the cultivation method meets the local good agricultural specifications.
Test cell arrangement: the cell treatment of test agent, control agent and blank control adopts random group arrangement, and each cell area is 20m 2 Each treatment was repeated 4 times.
Dosage of the medicament: the test agents and the dosage are shown in the following table:
table 6 test agent and dosage for wheat scab field efficacy test
Time of application: the test is carried out for 1 time in the flowering period of wheat, and a Linong HD-400 knapsack sprayer is adopted for full plant spraying, so that the mist drops are uniformly distributed. The liquid medicine application amount per mu is 35kg.
Investigation method and investigation time: the control effect is investigated once 15 days after the application (the period of wheat milk ripeness), 5 points are sampled on the diagonal line of each district during investigation, 100 ears are investigated at each point, the ears are classified by the percentage of the area of the dried ears to the whole ears, and the number of diseased ears and the total ears at each stage are recorded.
Wheat scab classification standard:
level 0: the whole spike is free from diseases;
stage 1: the area of the dried spike accounts for less than 1/4 of the area of the whole spike;
3 stages: the area of the dried spike accounts for 1/4 to 1/2 of the area of the whole spike;
5 stages: the area of the dried spike accounts for 1/2-3/4 of the area of the whole spike;
7 stages: the area of the dried spike accounts for more than 3/4 of the area of the whole spike.
The drug effect calculation method comprises the following steps:
the test results are shown in the following table:
table 5 results of field efficacy test of the formulated formulation on wheat scab
The field efficacy results show that the compound effect of the bronopol and any one of the fluoxastrobin hydroxylamine or the isopyrazam shows better control effect on wheat scab, the total control effect of each compound preparation treatment is more than 86.25%, and the total control effect is better than that of a blank control treatment group of a control single agent.
As can be seen from an indoor toxicity test and a field efficacy test, the bactericidal composition containing the bronopol has a good control effect on fusarium pathogenic bacteria, is safe to crops, delays the generation of pathogenic bacteria drug resistance, reduces the dosage of the medicament, and reduces the medicament residue of agricultural products.
While the invention has been described in detail in terms of the general description and the specific embodiments, it will be apparent to those skilled in the art that various modifications and improvements can be made thereto without departing from the spirit of the invention.

Claims (7)

1. The bactericidal composition containing the bronopol is characterized in that an active ingredient of the bactericidal composition consists of an active ingredient A and an active ingredient B, wherein the active ingredient A is bronopol, the active ingredient B is fluxapyroxad hydroxylamine, and the mass ratio of the active ingredient A to the active ingredient B is 1:30-30:1.
2. The sterilization composition according to claim 1, wherein the mass ratio of bronopol to fluxapyroxad hydroxylamine is 1:15-20:1.
3. The sterilizing composition according to claim 1, wherein the total weight of the sterilizing composition is 1% -80% of the total weight of the sterilizing composition based on 100 wt%.
4. The composition of claim 1, wherein the composition further comprises an additional component in addition to the active ingredient, wherein the additional component is selected from one or more of a wetting agent, a dispersing agent, an emulsifying agent, a thickening agent, a disintegrating agent, an antifreezing agent, an antifoaming agent, a solvent, a preservative, a stabilizer, a warning color, a film former, a synergist, and a carrier.
5. The bactericidal composition of claim 1, wherein the bactericidal composition can be prepared into any agriculturally acceptable formulation, and the formulation is water dispersible granule, wettable powder, suspension or seed treatment suspension.
6. Use of a bactericidal composition and/or formulation thereof as claimed in any of claims 1 to 5 for the prevention or control of pathogenic bacteria in crops, wherein the pathogenic bacteria are selected from the group consisting of fusarium graminearum @Fusarium graminearum) Fusarium moniliforme (F. Moniliforme)Fusarium moniliforme）。
7. The use according to claim 6, wherein the fungicidal composition and/or the formulation thereof is applied to the plant or cultivation medium in a seed treatment, foliar application, stem application, drenching, instillation, casting, spraying, dusting, scattering or fuming process.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102781233A (en) * 2010-03-04 2012-11-14 巴斯夫欧洲公司 Synergistic fungicidal mixtures
CN107494568A (en) * 2017-08-14 2017-12-22 河北省农林科学院植物保护研究所 Prevent and treat compound synergistic bactericidal composition and its application of tomato and pear tree Major Diseases
CN107926958A (en) * 2017-12-13 2018-04-20 江西中迅农化有限公司 Sterilization group composition
CN108112593A (en) * 2016-11-28 2018-06-05 陕西美邦农药有限公司 A kind of bactericidal composition containing bronopol
CN113163762A (en) * 2018-09-27 2021-07-23 0903608Bc有限公司 Synergistic pesticidal compositions for delivery of pesticidal active ingredients and methods thereof
CN114391538A (en) * 2022-03-11 2022-04-26 顺毅股份有限公司 Bactericidal composition containing bronopol

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102781233A (en) * 2010-03-04 2012-11-14 巴斯夫欧洲公司 Synergistic fungicidal mixtures
CN108112593A (en) * 2016-11-28 2018-06-05 陕西美邦农药有限公司 A kind of bactericidal composition containing bronopol
CN107494568A (en) * 2017-08-14 2017-12-22 河北省农林科学院植物保护研究所 Prevent and treat compound synergistic bactericidal composition and its application of tomato and pear tree Major Diseases
CN107926958A (en) * 2017-12-13 2018-04-20 江西中迅农化有限公司 Sterilization group composition
CN113163762A (en) * 2018-09-27 2021-07-23 0903608Bc有限公司 Synergistic pesticidal compositions for delivery of pesticidal active ingredients and methods thereof
CN114391538A (en) * 2022-03-11 2022-04-26 顺毅股份有限公司 Bactericidal composition containing bronopol

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