CN114766492B - Pesticide composition containing bixafen and application thereof - Google Patents

Pesticide composition containing bixafen and application thereof Download PDF

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Publication number
CN114766492B
CN114766492B CN202210357686.4A CN202210357686A CN114766492B CN 114766492 B CN114766492 B CN 114766492B CN 202210357686 A CN202210357686 A CN 202210357686A CN 114766492 B CN114766492 B CN 114766492B
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bixafen
active ingredient
pesticide composition
test
bupirimate
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CN114766492A (en
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葛家成
隋书婷
杨志鹏
张永芳
王玉
张凯莉
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Qingdao Hengning Biotechnology Co ltd
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Qingdao Hengning 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
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/36—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom five-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
    • 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
    • A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The pesticide composition comprises an active ingredient A and an active ingredient B, wherein the mass ratio of the active ingredient A to the active ingredient B is 1:30-30:1, the active ingredient A is bixafen, and the active ingredient B is fludioxonil or bupirimate. The pesticide composition improves the prevention and treatment effect on pathogenic bacteria, reduces the dosage of active ingredients, reduces the resistance risk and prolongs the service life of the medicament.

Description

Pesticide composition containing bixafen and application thereof
Technical Field
The invention belongs to the technical field of pesticide sterilization, and particularly relates to a pesticide composition containing bixafen and application thereof.
Background
Bixafen, international generic name: bixafen, chemical name: n- (3 ',4' -dichloro-5-fluoro [1,1' -biphenyl ] -2-yl) -3- (difluoromethyl) -1-methyl-1H-pyrazole-4-carboxamide, CAS accession No.: 581809-46-3. Bixafen is a pyrazole amide succinic dehydrogenase inhibitor developed by Bayer company, and inhibits mitochondrial function, prevents energy generation and inhibits growth of pathogenic bacteria by interfering succinic dehydrogenase on complex II in respiratory electron transfer chain of pathogenic bacteria mitochondria, and finally causes death of the pathogenic bacteria. The bixafen is a systemic bactericide, has a wide bactericidal spectrum and is special for foliar spraying.
Bupirimate, international generic name: bupirimate, CAS accession number: 41483-43-6. The bupirimate is a new generation systemic bactericide, belongs to an adenine nucleoside deaminase inhibitor, has the protection and treatment functions, can be quickly absorbed by roots, stems and leaves, can be operated to various parts in a plant body, has the protection and treatment functions, has special effects on powdery mildew of crops, and is used for preventing and treating powdery mildew of ornamental plants such as fruits, vegetables and flowers and field crops. The bupirimate belongs to bupirimate compounds, is an upgrade substitute of bupirimate, and has the characteristics of high efficiency, low toxicity, good environmental compatibility and the like.
Fludioxonil, international generic name: fluxionoil, CAS accession number: 131341-86-1, chemical name: 4- (2, 2-difluoro-1, 3-benzodioxy-4-yl) pyrrole-3-carbonitrile. Fludioxonil is a bactericide developed and produced by the North China company, and the action mechanism is to inhibit protein-activated enzyme PK-III (kinase PK-III) with a signal effect in the osmotic induction transmission process, so that the concentration of non-phosphorylation regulatory protein is increased, the secretion of osmotic sensitive cell division agent activated protease is abnormal, and finally bacteria death is caused. Because of unique action mechanism, the novel pyrrole bactericide has no resistance with the existing bactericide, and is a pyrrole bactericide with very good development prospect. It is used in seed treatment to prevent and treat seed carrier and cross resistance with other bactericide, and belongs to contact bactericide.
The pathogen is easy to generate drug resistance to the bactericide with single position, and the drug resistance can be delayed by compounding the bactericide. In order to improve the killing effect on pathogenic bacteria, two active ingredients with different action mechanisms are adopted for compounding, and multiple target sites act on pathogenic microorganisms to achieve the effect of disease prevention, so that the dosage of the active ingredients is reduced, the resistance risk is reduced, and the service life of the medicament is prolonged.
Disclosure of Invention
Based on the above circumstances, the invention aims to provide the pesticide composition containing bixafen, which is effective on various target pathogenic bacteria, can obviously enhance the efficacy, reduce the dosage of active ingredients, reduce the resistance risk, prolong the service life of the pesticide, and has obvious effects on powdery mildew, gray mold and southern blight in particular.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the pesticide composition containing bixafen and application thereof comprise an active ingredient A and an active ingredient B, wherein the mass ratio of the active ingredient A to the active ingredient B is 1:30-30:1;
further, the active ingredient A is bixafen, and the active ingredient B is any one of fludioxonil or bupirimate;
Further, the active ingredient B is bupirimate, and the mass ratio of the active ingredient A to the active ingredient B is 1:10-15:1;
Further, the mass ratio of the active ingredient A to the active ingredient B is 1:10-10:1;
further, the mass ratio of the active ingredient A to the active ingredient B is 1:10, 1:5, 1:1, 5:1 and 10:1;
Further, the mass ratio of the active ingredient A to the active ingredient B is 1:5-10:1;
Further, the mass ratio of the active ingredient A to the active ingredient B is 1:5, 1:1, 5:1 and 10:1;
further, the active ingredient B is fludioxonil, and the mass ratio of the active ingredient A to the active ingredient B is 1:10-30:1;
further, the mass ratio of the active ingredient A to the active ingredient B is 1:3-30:1;
further, the mass ratio of the active ingredient A to the active ingredient B is 1:3, 1:1, 3:1, 5:1, 6:1, 9:1, 10:1, 13:1, 16:1, 20:1, 30:1;
further, the mass ratio of the active ingredient A to the active ingredient B is 1:1-20:1;
Further, the mass ratio of the active ingredient A to the active ingredient B is 1:1, 3:1, 5:1, 6:1, 9:1, 10:1, 13:1, 16:1, 20:1;
further, the mass ratio of the active ingredient A to the active ingredient B is 1:1-13:1;
Further, the mass ratio of the active ingredient A to the active ingredient B is 1:1, 3:1, 5:1, 6:1, 9:1, 10:1 and 13:1;
Further, the sum of the contents of the active ingredient A and the active ingredient B in the pesticide composition is 0.5 to 80 percent based on 100 weight percent of the total weight of the pesticide composition;
Further, the sum of the contents of the active ingredient A and the active ingredient B in the pesticide composition is 1 to 60 percent based on 100 weight percent of the total weight of the pesticide composition;
Further, the pesticide composition also comprises auxiliary 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, stabilizers, penetrating agents and carriers;
Further, the wetting agent is selected from one or a mixture of more of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, nekal BX, wetting penetrating agent F, chinese honeylocust fruit powder, silkworm excrement or soapberry powder;
Further, the dispersing agent is selected from one or more of polycarboxylate, lignosulfonate, alkylphenol ethoxylate formaldehyde condensate sulfate, calcium alkylbenzenesulfonate, naphthalene sulfonate formaldehyde condensate sodium salt, alkylphenol ethoxylate, fatty amine ethoxylate, fatty acid ethoxylate or glycerin fatty acid ester ethoxylate;
Further, the emulsifier is selected from one or a mixture of more of calcium alkylbenzenesulfonate, OP series phosphate (nonylphenol polyoxyethylene ether phosphate), phenylphenol polyoxyethylene ether phosphate, styrene polyoxyethylene ether ammonium sulfate, alkyl diphenyl ether disulfonate magnesium salt, triethanolamine salt, benzyl dimethyl phenol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, phenethyl phenol polyoxyethylene polypropylene ether, ethylene oxide-propylene oxide block copolymer, OP series (nonylphenol polyoxyethylene ether), castor oil polyoxyethylene ether, alkylaryl polyoxyethylene polyoxypropylene ether, sorbitan monostearate, sorbitan fatty acid ester polyoxyethylene ether or fatty alcohol polyoxyethylene ether;
Further, the thickener is selected from one or more of xanthan gum, polyvinyl alcohol, bentonite, carboxymethyl cellulose or magnesium aluminum silicate;
further, the disintegrating agent is selected from one or a mixture of more of bentonite, urea, ammonium sulfate, aluminum chloride, low-substituted hydroxypropyl cellulose, lactose, citric acid, succinic acid or sodium bicarbonate;
further, the antifreezing agent is selected from one or a mixture of more of ethylene glycol, propylene glycol, glycerol or urea;
further, the defoamer is selected from one or a mixture of more of silicone oil, silicone compounds, C 10～C20 saturated fatty acid compounds or C 8～C10 fatty alcohol compounds;
further, the solvent is selected from one or more of N, N-dimethylformamide, cyclohexanone, butyl ether, dimethylbenzene, dimethyl sulfoxide, methanol, ethylene glycol, ethanol, propanol, butanol, trimethylcyclohexanone, N-octyl pyrrolidone, toluene, ethanolamine, triethanolamine, isopropylamine, N-methylpyrrolidone, diethylene glycol, ethylene glycol methyl ether, ethyl acetate or acetonitrile;
Further, the stabilizer is selected from one or a mixture of more of epoxidized soybean oil, epichlorohydrin, BHT, ethyl acetate and triphenyl phosphate;
Further, the penetrating agent is selected from one or a mixture of more of penetrating agent JFC, penetrating agent T, azone or organic silicon;
further, the carrier is one, two or three of a solvent or a filler, and water is preferably deionized water;
Further, the filler is selected from one or a mixture of more of kaolin, diatomite, bentonite, attapulgite, white carbon black, starch or light calcium carbonate;
all of the above are commercially available;
the pesticide composition can be prepared into any one of agriculturally acceptable preparation formulations according to the requirements;
further, the preparation formulation is solid preparation, liquid preparation and/or seed treatment preparation;
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;
Further, the solid preparation is water dispersible granule, and the liquid preparation is suspending agent, emulsifiable concentrate and/or emulsion in water.
The invention also discloses application of the pesticide composition containing bixafen in preventing and controlling plant diseases.
Further, the plants are cash crops and food crops;
Further, the plant diseases are southern blight, rust disease, gray mold and powdery mildew, and preferably the plant diseases are southern blight, gray mold and powdery mildew.
Compared with the prior art, the invention has the following advantages:
1) The pesticide composition is compounded by adopting two active ingredients with different action mechanisms, and the multi-target sites act on pathogenic microorganisms to achieve the disease prevention effect, so that the control effect is enhanced, and the dosage of the active ingredients is reduced;
2) The pesticide composition can prolong the duration of the medicament, reduce the times of administration, reduce the risk of resistance and prolong the service life of the medicament.
Detailed Description
The present invention will be described in more detail with reference to the following examples, but the present invention can be embodied in various forms and should not be construed as being limited to the embodiments set forth herein.
Preparation example
Preparation example 1:30% bixafen-bupirimate aqueous emulsion (1:5)
The weight percentages of the bixafen, the bupirimate 25%, the fatty alcohol polyoxyethylene ether 2%, the alkylphenol polyoxyethylene ether phosphate 4%, the styrylphenol polyoxyethylene ether 2%, the cyclohexanone 22%, the xanthan gum 0.2%, the glycerol 3%, the sodium benzoate 0.1%, the organosilicon antifoaming agent 0.1% and the deionized water are the balance.
The preparation method comprises the following steps: according to the formula proportion of the embodiment, the surfactant, the antifreezing agent and the water are mixed into a water phase, then the bixafen and the bupirimate are dissolved by using a solvent and then added into the water phase under stirring, after being stirred uniformly, the thickening agent and the preservative are added for continuously shearing for 10min, and then the antifoaming agent is added for uniformly stirring, so that the O/W type aqueous emulsion is formed.
Preparation example 2:10% bixafen-bupirimate aqueous emulsion (1:1)
The weight percentages of the bixafen, the bupirimate, the EO-PO block copolymer, the cyclohexanone, the xanthan gum, the propylene glycol, the sodium benzoate and the organosilicon defoamer are 5 percent, 6 percent, 22 percent, 0.15 percent, 4 percent, 0.5 percent and 0.1 percent, and the balance is deionized water.
The preparation method comprises the following steps: same as in preparation example 1
Preparation example 3:30% bixafen-bupirimate emulsifiable concentrate (5:1)
The balance is prepared from 25% of bixafen, 5% of bupirimate, 14% of styrylphenol polyoxyethylene ether, 20% of N-methylpyrrolidone, 3% of calcium dodecyl benzene sulfonate, 20% of propylene carbonate and the balance of xylene by weight percent.
The preparation method comprises the following steps: according to the formula proportion of the embodiment, the metered bixafen, bupirimate, solvent and cosolvent are added into a blending kettle to be stirred and dissolved, then the emulsifier is added, the rest is complemented by the residual solvent, the mixture is stirred uniformly in the stirring kettle, and the required emulsifiable concentrate is obtained after filtration.
Preparation example 4:22% bixafen-bupirimate emulsifiable concentrate (10:1)
The balance is 20 percent of bixafen, 2 percent of bupirimate, 10 percent of alkylphenol ethoxylate, 20 percent of N-methylpyrrolidone, 4 percent of calcium dodecyl benzene sulfonate, 12 percent of acetophenone and trimethylbenzene according to the weight percentage.
The preparation method comprises the following steps: the same as in preparation example 3.
Preparation example 5:20% Bispyrimidine fludioxonil suspension (3:1)
The weight percentages of the bixafen, the fludioxonil, the isomeric alcohol polyoxyethylene ether, the alkylphenol polyoxyethylene ether phosphate ester, the polycarboxylic acid sodium salt, the xanthan gum, the glycerol, the sodium benzoate, the silicone oil and the deionized water are respectively 15 percent, 5 percent, 2 percent, 4 percent, 1 percent, 0.25 percent, 5 percent, 0.1 percent and the balance.
The preparation method comprises the following steps: according to the formula proportion of the embodiment, the metered bixafen, fludioxonil, a surfactant and other functional additives 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 by homogenizing and filtering.
Preparation example 6:21% Bispyrimidine fludioxonil suspension (6:1)
According to the weight percentage, 18 percent of bixafen, 3 percent of fludioxonil, 2 percent of isomeric alcohol polyoxyethylene ether, 2 percent of alkylaryl polyoxyethylene ether polyoxypropylene ether, 1 percent of lignosulfonate, 4 percent of styrol polyoxyethylene ether phosphate, 1 percent of magnesium aluminum silicate, 0.1 percent of carboxyethyl cellulose, 1 percent of sodium sorbate, 5 percent of ethylene glycol, 0.5 percent of silicone oil and deionized water are used for the balance.
The preparation method comprises the following steps: the same as in preparation example 5.
Preparation example 7:33% bixafen and fludioxonil water dispersible granule (10:1)
The composition comprises, by weight, 30% bixafen, 3% fludioxonil, 12% lignosulfonate, 5% sodium dodecylbenzenesulfonate, 2% naphthalene sulfonate formaldehyde condensate, 30% starch, and kaolin, the balance being.
The preparation method comprises the following steps: according to the formula proportion of the embodiment, active ingredients bixafen and fludioxonil are added into a carrier, a surfactant and other functional auxiliary agents are added into the carrier, the active ingredients bixafen and fludioxonil are mixed, 10-25% of water is added after air current crushing, and then water dispersible granule products are prepared through kneading, granulating, drying and screening; or spraying water, granulating, drying, and sieving to obtain the final product.
Preparation example 8:21% bixafen and fludioxonil water dispersible granule (20:1)
The composition comprises 20% of bixafen, 1% of fludioxonil, 10% of naphthalene sulfonate formaldehyde condensate, 3% of sodium polycarboxylate, 3% of nekal BX and the balance of kaolin in percentage by weight.
The preparation method comprises the following steps: the same as in preparation example 7.
Indoor activity test:
Example 1: indoor combined action test of combining bixafen and bupirimate on powdery mildew of cucumber
The test is based on: test reference NY/T1156.11-2006 section 11. Agricultural industry Standard pesticide indoor biological assay test criteria Bactericide, PRC: potted plant method for preventing and treating powdery mildew of cucumber; ny/T1156.6-2006 agricultural industry Standard pesticide indoor biological assay test criteria section 6 of the people's republic of China: determination of the combined action of compounding.
Test agent: 98% bixafen and 97% bupirimate, and the above agents are provided by the research and development center of the halider pharmaceutical industry group.
Test target: cucumber powdery mildew (Erysiphe cichoracearum);
Preparing a test material: and (3) selecting a disease-sensitive cucumber variety (Xintaimi thorn) for potting, and keeping the seedlings for standby after 2-4 true leaf periods.
Spore suspension preparation: fresh spores on the leaves of the cucumber which are full of powdery mildew are washed out by purified water added with a small amount of Tween 80 water solution, and filtered by double-layer gauze to prepare a suspension with the spore concentration of 1 x 10 5 spores/mL for standby.
Drug configuration: the two crude drugs are respectively dissolved by acetone, diluted by 0.1% Tween 80 aqueous solution and set to the required series of mass concentrations.
And (3) medicament treatment: spraying the agent on cucumber seedling until leaf is wetted, and air drying. The test was run with no drug-containing treatment as a blank.
Inoculating and culturing: inoculating for 24 hours after medicament treatment, spraying the cucumber powdery mildew spore suspension on cucumber seedlings by adopting an inoculator, culturing for 12 hours under high humidity, and culturing under the conditions that the temperature is 20-24 ℃ and the humidity is 65-75% and the illumination ratio is L: D=12:12 hours. Each treatment was repeated 3 pots, 4 times.
Data investigation: when the leaf rate of the blank control reaches more than 80%, the disease condition of each treatment is investigated in a grading way, and at least 30 leaves are investigated for each treatment. The following classification method is adopted:
level 0: no disease spots;
stage 1: the area of the disease spots accounts for less than 5% of the area of the whole leaf;
3 stages: the area of the disease spots accounts for 5% -15% of the area of the whole leaf;
5 stages: the area of the disease spots accounts for 15% -25% of the area of the whole leaf;
7 stages: the area of the lesion accounts for 25% -50% of the area of the whole leaf;
stage 9: the area of the disease spots accounts for 50% -75% of the area of the whole leaf;
11 grades: the area of the disease spots accounts for more than 75% of the area of the whole leaf.
Data statistics and analysis:
And calculating the disease index and the prevention and treatment effect of each treatment according to the investigation data.
The disease index is calculated according to the formula (1):
X＝[∑(Ni×i)/(N×11)]×100................................(1)
Wherein:
X-disease index;
N i -leaf numbers of each stage;
i—relative grade value;
n-total leaf number was investigated.
The control effect is calculated according to the formula (2):
Wherein:
P, the prevention and treatment effect, the unit is percentage;
CK-blank disease index;
PT-agent treatment index.
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. The co-toxicity coefficient (CTC value) of the mixture is calculated according to the formulas (3), (4) and (5):
Wherein:
Ati—actual measured virulence index of the mixture;
S-EC 50 of standard bactericide in milligrams per liter (mg/L);
M-EC 50 of the mixture in milligrams per liter (mg/L).
TTI＝TIA*PA+TIB*PB·······(4)
Wherein:
TTI-the theoretical toxicity index of the mixture;
TI A A agent toxicity index;
the percentage content of the P A -A medicament in the mixture is expressed as percentage (%);
TI B -agent toxicity index;
the percentage of the P B -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.
And calculating test results by adopting DPS data processing software, respectively solving a toxicity regression equation, R, EC 50 and a 95% confidence limit of the single test medicament and the mixed medicaments with different proportions, solving co-toxicity coefficients (CTCs) of the two medicaments with different proportions, and screening out the optimal proportion of the test medicaments.
The test results are shown in the following table:
Table 1 indoor Activity test of Bispyrimidine and bupirimate Mixed pair cucumber powdery mildew
As can be seen from the indoor activity test (see Table 1), the single doses of the bixafen and the bupirimate are 4.6892mg/L and 5.6765mg/L respectively for the powdery mildew EC 50 of the cucumber, and the powdery mildew of the cucumber is more sensitive to the bixafen; the co-toxicity coefficients of the bixafen and bupirimate are all larger than 120 after being mixed according to the proportion of 1:30-30:1, and the bixafen and bupirimate have synergistic effect on preventing and treating powdery mildew of cucumber; when the mass ratio of the bixafen to the bupirimate is 1:10-10:1, the co-toxicity coefficient after mixing is greater than 140, and the synergy is remarkable; when the mass ratio of the bixafen to the bupirimate is 1:1, the co-toxicity coefficient of the bixafen to the powdery mildew of cucumber after mixing is the maximum and is 178.179.
Example 2: indoor combined action test of combining bixafen and fludioxonil on cucumber gray mold
The test is based on: test reference NY/T1156.2-2006 "agricultural industry standard pesticide indoor bioassay test criteria for the people's republic of China section 2: test plate method for inhibiting growth of pathogenic fungi; NY/T1156.6-2006, combined action determination of pesticide 6 part of the standard pesticide indoor biological determination test criteria of agricultural industry of China's name republic of China.
Test agent: 98% of bixafen and 97% of fludioxonil are provided by the research and development center of the sea li pharmaceutical industry group.
Test pathogenic bacteria: botrytis cinerea;
And (3) preparation of a medicament: the test stock was dissolved in acetone and then diluted with 0.1% tween 80 in water. The mother solution of single dose is prepared respectively, and the required series of mass concentrations are set according to the mixing purpose and the medicament activity.
Melting PDA culture medium with microwave oven, cooling to 50deg.C, taking 1mL of prepared medicinal liquid to be tested and 9mL of PDA culture medium according to the principle from low concentration to high concentration, adding into culture dish with diameter of 9cm, mixing, and making into tablet with corresponding concentration.
And (3) beating the cultured pathogenic fungi into fungus cakes by using a puncher with the diameter of 5mm under the aseptic condition, placing the fungus cakes in the central position of a culture medium after the drug-containing culture medium is solidified, sealing a culture dish by using a sealing film, culturing in an incubator at the temperature of 27 ℃, and setting a blank solution without the drug as a blank control, wherein each treatment is repeated four times.
After 7d incubation, colony diameters were measured in millimeters (mm) using calipers. The diameter of each colony was measured vertically by the cross-over method and the average value was taken.
The hypha growth inhibition rate was calculated in percent (%) according to the following formula, and the calculated result remained two bits after the decimal point.
D＝D1-D2············(1)
D-colony growth diameter;
d 1 —colony diameter;
d 2 -diameter of the fungus cake.
I＝(D0-Dt)/D0*100············(2)
Wherein:
I, hypha growth inhibition rate;
D 0 —a control colony growth diameter;
D t —agent treated colony growth diameter.
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. The co-toxicity coefficient (CTC value) of the mixture is calculated according to the formulas (3), (4) and (5):
Wherein:
Ati—actual measured virulence index of the mixture;
S-EC 50 of standard bactericide in milligrams per liter (mg/L);
M-EC 50 of the mixture in milligrams per liter (mg/L).
TTI＝TIA*PA+TIB*PB·······(4)
Wherein:
TTI-the theoretical toxicity index of the mixture;
TI A A agent toxicity index;
the percentage content of the P A -A medicament in the mixture is expressed as percentage (%);
TI B -agent toxicity index;
the percentage of the P B -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.
And calculating test results by adopting DPS data processing software, respectively solving a toxicity regression equation, R, EC 50 and a 95% confidence limit of the single test medicament and the mixed medicaments with different proportions, solving co-toxicity coefficients (CTCs) of the two medicaments with different proportions, and screening out the optimal proportion of the test medicaments.
The test results are shown in the following table:
table 2 indoor Activity test of Biflufen and fludioxonil Mixed pair cucumber gray mold
As can be seen from the indoor activity test (see Table 2), the single doses of bixafen and fludioxonil are 4.9421mg/L and 0.0403mg/L respectively for the cucumber gray mold EC 50, and the cucumber gray mold is sensitive to fludioxonil; the co-toxicity coefficients of the bixafen and fludioxonil are all larger than 120 after being mixed according to the proportion of 1:10-30:1, and the synergistic effect is shown for controlling cucumber gray mold; when the mass ratio of the bixafen to the fludioxonil is 1:3-20:1, the co-toxicity coefficient of the bixafen and the fludioxonil is more than 140 after the bixafen and the fludioxonil are mixed, and the synergistic effect is remarkable.
Example 3: indoor combined action test of bixafen and fludioxonil mixed on peanut southern blight
The test is based on: test reference NY/T1156.2-2006 "agricultural industry standard pesticide indoor bioassay test criteria for the people's republic of China section 2: test plate method for inhibiting growth of pathogenic fungi; NY/T1156.6-2006, combined action determination of pesticide part 6, standard pesticide indoor biological determination test criteria of agricultural industry of the people's republic of China.
Test agent: 98% of bixafen and 97% of fludioxonil are provided by the research and development center of the sea li pharmaceutical industry group.
Test pathogenic bacteria: sclerotium rolfsii (Sclerotium rolfsii sacc.);
And (3) preparation of a medicament: the test stock was dissolved in acetone and then diluted with 0.1% tween 80 in water. Preparing single-dose mother liquor, and setting the required series mass concentration according to the mixing purpose and the medicament activity.
Melting PDA culture medium with microwave oven, cooling to 50deg.C, taking 1mL of prepared medicinal liquid to be tested and 9mL of PDA culture medium according to the principle from low concentration to high concentration under aseptic operation condition, adding into culture dish with diameter of 9cm, mixing, and making into tablet with corresponding concentration.
And (3) beating the cultured pathogenic fungi into fungus cakes by using a puncher with the diameter of 5mm under the aseptic condition, placing the fungus cakes in the central position of a culture medium after the medicine-containing culture medium is solidified, sealing a culture dish by using a sealing film, culturing in an incubator (26+/-0.5 ℃) and setting a blank solution without a medicament as a blank control, wherein each treatment is repeated four times.
Data statistics and analysis:
The growth of pathogenic hyphae was investigated according to the growth of bacteria in a blank culture dish. Colony diameter was measured in millimeters (mm) using calipers. The diameter of each colony was measured vertically by the cross-over method and the average value was taken.
The hypha growth inhibition rate was calculated in percent (%) according to the following formula, and the calculated result remained two bits after the decimal point.
D＝D1-D2············(1)
D-colony growth diameter;
d 1 —colony diameter;
d 2 -diameter of the fungus cake.
I＝(D0-Dt)/D0*100············(2)
Wherein:
I, hypha growth inhibition rate;
D 0 —a control colony growth diameter;
D t —agent treated colony growth diameter.
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. The co-toxicity coefficient (CTC value) of the mixture is calculated according to the formulas (3), (4) and (5):
Wherein:
Ati—actual measured virulence index of the mixture;
S-EC 50 of standard bactericide in milligrams per liter (mg/L);
M-EC 50 of the mixture in milligrams per liter (mg/L).
TTI＝TIA*PA+TIB*PB·······(4)
Wherein:
TTI-the theoretical toxicity index of the mixture;
TI A A agent toxicity index;
the percentage content of the P A -A medicament in the mixture is expressed as percentage (%);
TI B -agent toxicity index;
the percentage of the P B -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.
And calculating test results by adopting DPS data processing software, respectively solving a toxicity regression equation, R, EC 50 and a 95% confidence limit of the single test medicament and the mixed medicaments with different proportions, solving co-toxicity coefficients (CTCs) of the two medicaments with different proportions, and screening out the optimal proportion of the test medicaments.
The test results are shown in the following table:
table 3 results of indoor combined action test of bixafen and fludioxonil in combination against peanut southern blight
Test agent Regression equation (y=a+bx) R EC 50 (mg/L) 95% confidence limits Co-toxicity coefficient (CTC)
Bispyrimidine (A) y＝3.8029+1.2214x 0.9993 9.5518(9.1536-9.9673) -
Fludioxonil (B) y＝5.8543+1.2019x 0.9999 0.1946(0.1918-0.1975) -
A：B(1:3) y＝5.8378+1.2203x 0.9989 0.2058(0.1951-0.2170) 125.227
A：B(1:1) y＝5.6309+1.1001x 0.9994 0.2670(0.2569-0.2775) 142.857
A：B(3:1) y＝5.3658+1.2362x 0.9996 0.5060(0.4900-0.5224) 144.973
A：B(6:1) y＝5.2122+1.2060x 0.9999 0.6669(0.6585-0.6754) 182.010
A：B(9:1) y＝4.9956+1.2846x 0.9997 1.0079(0.9831-1.0334) 163.158
A：B(13:1) y＝4.7800+1.2112x 0.9999 1.5194(1.4923-1.5470) 141.762
A：B(16:1) y＝4.6614+1.2226x 0.9994 1.8920(1.8179-1.9692) 131.867
As shown in an indoor activity test (see Table 3), the bixafen and fludioxonil are mixed to show better activity on peanut southern blight, wherein single fludioxonil dose has higher toxicity on peanut southern blight, EC 50 is 0.1946mg/L, and peanut southern blight is sensitive to fludioxonil; the co-toxicity coefficients of the bixafen and fludioxonil are all larger than 120 after being mixed according to the proportion of 1:3-16:1, and the bixafen and fludioxonil have synergistic effect on preventing and treating peanut southern blight. When the mass ratio of the bixafen to the fludioxonil is 1:1-13:1, the co-toxicity coefficient after mixing is greater than 140, and the synergistic effect is obvious; when the mass ratio of the bixafen to the fludioxonil is 6:1, the co-toxicity coefficient is the largest and is 182.010, and the control effect is best.
Field efficacy test
Example 4 field efficacy test of Bispyrimidine and bupirimate
The test is based on: the test is described in GB/T17980.30-2000 section 30 of pesticide field efficacy test criterion (one): bactericide for preventing and treating powdery mildew of cucumber.
Test site: the application time of the greenhouse in Shandong Shouguang Nan Pan Cun of Shandong province is 2021 in 3 middle of month.
Test target: powdery mildew of cucumber.
Test crops and varieties: cucumber (Xintaimi thorns).
Test agent: the test agents and dosages are shown in the following table.
And (3) test design: the cells treated by the medicament are distributed according to random groups, and protection rows are arranged around the cells. Each treatment was repeated 4 times, 20m 2 per cell. The conventional spraying method is adopted, and a worker pesticide-16 type manual sprayer is used for spraying, so that the liquid medicine is uniformly sprayed on the front and back surfaces of the blades, and the wet and non-dripping effect is achieved.
Time of application: the experiment is carried out in the initial stage of powdery mildew of cucumber, the 1 st spraying and the 2 nd spraying are carried out at intervals of 7 days, and the spraying is carried out twice. No rainfall occurs within 24 hours of pesticide application, no special bad weather exists during the test period, and conventional management is carried out in the field.
The investigation method comprises the following steps: the disease condition number is investigated before the 1 st application, powdery mildew disease conditions are investigated respectively in 7d after the 1 st application and 11d after the 2 nd application, four points are randomly taken for investigation in each cell, two plants are investigated in each spot, all leaves are investigated in each plant, each leaf is classified according to the percentage of the leaf area of the disease spots, and the disease index and the prevention and treatment effect are calculated.
Statistics and analysis:
The classification method (in units of leaves) is as follows:
level 0: no disease spots;
stage 1: the area of the disease spots accounts for less than 5% of the whole leaf area;
3 stages: the area of the lesion accounts for 6-10% of the whole leaf area;
5 stages: the area of the lesion accounts for 11-20% of the whole leaf area;
7 stages: the area of the lesion accounts for 21-40% of the whole leaf area;
Stage 9: the area of the disease spots accounts for more than 40% of the whole leaf area.
The drug effect is calculated according to the following formula:
The test results are shown in the following table:
Table 4 results of field efficacy test of Bispyrimidine and bupirimate for controlling powdery mildew of cucumber
The field efficacy shows (see Table 4), the overall prevention effect of each treatment field effect after 7 days of the first application of the pesticide on the powdery mildew of cucumber is 69.61% -84.88%, 30% of bixafen-bupirimate aqueous emulsion (1:5), 10% of bixafen-bupirimate aqueous emulsion (1:1), 30% of bixafen-bupirimate emulsifiable concentrate (5:1), 22% of bixafen-bupirimate emulsifiable concentrate (10:1) are subjected to treatment, and the prevention effect of each treatment field effect is 80.24%, 84.88%, 83.16% and 81.21% of the pesticide on the powdery mildew of cucumber is better than that of a single dose (125 g/L of bixafen emulsifiable concentrate and 25% of bupirimate microemulsion), wherein the 10% of bixafen-bupirimate aqueous emulsion (1:1) has the best prevention effect.
The overall prevention effect of each treatment field effect is 70.36-85.98%, 30% of bixafen-bupirimate aqueous emulsion (1:5), 10% of bixafen-bupirimate aqueous emulsion (1:1), 30% of bixafen-bupirimate emulsifiable concentrate (5:1) and 22% of bixafen-bupirimate emulsifiable concentrate (10:1) after the second application is superior to that of single dose, wherein the prevention effect of the treatment on cucumber powdery mildew is 81.65%, 85.98%, 83.88% and 82.27% respectively.
In the whole test process, each medicament is safe and harmless to target crops and other organisms under the test concentration.
Example 5: field efficacy test for controlling cucumber gray mold by mixing bixafen and fludioxonil
The test is based on: the test is described in GB/T17980.28-2000 section 28 of the pesticide field efficacy test criterion (one): the bactericide can prevent and treat vegetable gray mold.
Test site: the administration time of the drug is in the middle 6 th month of 2020 in the Laiyitong city of Shandong province.
Test target: gray mold of cucumber.
Test crops and varieties: cucumber (Xintaimi thorns).
Test agent: the test agents and dosages are shown in the following table.
The test method comprises the following steps: with a random block arrangement, the cell area is 25m 2, 4 replicates.
The application method and times are as follows: the application of the medicine is carried out by adopting a conventional spray method at the early stage of the occurrence of the gray mold of the cucumber, and the medicine is applied once again after 8 days of the medicine, and the total application time is 2 times;
the investigation method comprises the following steps: disease number investigation was performed before the first application and 11d control effect investigation was performed after the last application. Five samples were randomly taken per cell, 2 plants were examined per spot, and all leaves and fruits were examined per plant and recorded in stages according to the following method, respectively.
Leaf damage classification method (taking leaf as unit):
level 0: no disease spots;
stage 1: 3 disease spots are arranged on a single leaf;
3 stages: 4-6 disease spots are arranged on a single blade;
5 stages: 7-10 disease spots are arranged on a single blade;
7 stages: the single leaf has 11-20 disease spots, and part of the single leaf is densely packed into a sheet;
stage 9: the single leaf has more than one quarter of densely-occupied disease spots.
Fruit pest grading method (in fruit unit):
level 0: no disease spots;
stage 1: onset of residual flowers;
3 stages: onset of disease at the umbilicus;
5 stages: the disease length is less than 10% of the total length of melon strips;
7 stages: the disease length is less than 11-25% of the total length of the melon strips;
stage 9: the disease length is more than 26% of the total length of the melon strips.
The drug effect is calculated according to the following formula:
The test results are shown in the following table:
Table 5 field efficacy (leaves) of bixafen and fludioxonil for controlling cucumber gray mold
Table 6 field efficacy (fruit) of bixafen and fludioxonil for controlling cucumber gray mold
The field efficacy shows (see Table 5), the overall prevention effect of each treatment field effect of different treatments for preventing and treating the gray mold of the cucumber leaf is 68.75-85.14% after the last application of the pesticide, 20% of bipyramid-fludioxonil suspending agent (3:1), 21% of bipyramid-fludioxonil suspending agent (6:1), 33% of bipyramid-fludioxonil water dispersible granule (10:1), 21% of bipyramid-fludioxonil wettable powder (20:1), and the prevention effect of each treatment field effect on the gray mold of the cucumber leaf is 81.55%, 83.64%, 85.14% and 82.36% respectively, wherein the prevention effect of each treatment field effect is better than that of single agents (20% of bipyramid suspending agent and 20% of fludioxonil suspending agent), and the prevention effect of 33% of bipyramid-fludioxonil water dispersible granule (10:1) is the best.
The field efficacy shows (see Table 6), the overall prevention effect of each treatment field effect of different treatments for preventing and treating the gray mold of the cucumber fruit is 69.08-84.11% after the last application of the pesticide, 20% of bixafen-fludioxonil suspending agent (3:1), 21% of bixafen-fludioxonil suspending agent (6:1), 33% of bixafen-fludioxonil water dispersible granule (10:1), and the prevention effect of 21% of bixafen-fludioxonil wettable powder (20:1) on the gray mold of the cucumber leaf is respectively 80.46%, 81.82%, 84.11% and 79.79%, which is superior to that of single preparations (20% of bixafen suspending agent and 20% of fludioxonil suspending agent), wherein the prevention effect of 33% of bixafen-fludioxonil water dispersible granule (10:1) is the best.
In the whole test process, each medicament is safe and harmless to target crops and other organisms under the test concentration.
Example 6: field efficacy test for controlling peanut southern blight by mixing bixafen and fludioxonil
Test site: peanut test fields in Laixi City of Qingdong, shandong province are used for continuous cropping of peanuts for many years, the occurrence of peanut southern blight is serious, and the test fields are sandy loam and have moderate fertility.
Test target: sclerotium rolfsii (Sclerotium rolfsii sacc.);
Test crop: peanut (Lu Hua # 14).
Test agent: the test agents and dosages are shown in the following table.
And (3) test design: the cells treated by the medicament are distributed according to random groups, and protection rows are arranged around the cells. Each time of 4 replicates, 30m 2 per cell. The pesticide is applied by spraying and irrigating roots.
Time of application: the test was carried out with the 1 st application at the initial stage of the onset of peanut southern blight, with the 2 nd application being carried out at 15 days intervals, and the two applications being carried out together. And no special bad weather exists during the test period, and conventional management is performed in the field.
The investigation method comprises the following steps: the disease condition number is investigated before the 1 st application, the disease condition of peanut southern blight in each cell is investigated in 15 days after the last application, 5 points are randomly sampled in each cell, 20 plants are connected in each point of investigation, 100 plants are investigated in each cell, and the number of all stages of disease plants of the peanut is recorded.
Disease grading standards refer to Dongbo et al, greenhouse inoculation technology for peanut southern blight and resistance identification, disease grading standards are divided into disease grades, and the investigation grading standards are as follows:
Level 0: the plants are asymptomatic;
Stage 1: generating lesions only at the base of the stems;
2 stages: the basal part of the stem generates a constriction symptom, and less than one third of the whole plant shows systemic symptoms (withering, death, wilting and the like);
3 stages: less than two thirds of the whole plant shows systemic symptoms;
4 stages: more than two thirds of the whole plant shows systemic symptoms.
The efficacy is calculated according to the following formula:
The test results are shown in the following table:
Table 7 results of field efficacy test of bixafen and fludioxonil in combination for controlling peanut southern blight
The field efficacy shows (see Table 7), the overall prevention effect of each treatment field effect of the different treatments for preventing and treating peanut southern blight is 78.01-83.40% 15 days after the last application, and under the condition of reducing the dosage, the prevention effect of the fludioxonil suspending agent (6:1) on the peanut southern blight is 83.40% which is superior to that of single agents (20% of the fludioxonil suspending agent and 20% of the fludioxonil suspending agent).
In conclusion, through indoor toxicity measurement and field efficacy tests, the pesticide composition of bixafen has good control effect on plant pathogenic bacteria, is safe to target crops, has remarkable control effect, is superior to single dose in the aspects of delaying the generation of drug resistance and prolonging the lasting effect, and can effectively reduce the cost and reduce the medicament residue.
While the invention has been described in detail in the foregoing general description and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto, and it is therefore intended that the invention as defined in the appended claims be interpreted as broadly as possible without departing from the spirit of the invention.

Claims (9)

1. The pesticide composition containing the bixafen is characterized in that an active ingredient of the pesticide composition consists of an active ingredient A and an active ingredient B, wherein the mass ratio of the active ingredient A to the active ingredient B is 1:30-30:1, the active ingredient A is bixafen, and the active ingredient B is bupirimate.
2. The pesticide composition as set forth in claim 1, wherein the mass ratio of bixafen to bupirimate is 1:10-15:1.
3. The pesticide composition as set forth in claim 2, wherein the mass ratio of bixafen to bupirimate is 1:10-10:1.
4. The pesticide composition as set forth in claim 3, wherein the mass ratio of bixafen to bupirimate is 1:5-10:1.
5. A pesticide composition as set forth in claim 1 wherein the sum of the contents of said active ingredient a and active ingredient B in the pesticide composition is 0.5% -80% by weight based on 100% by weight of the total weight of the pesticide composition.
6. A pesticide composition as set forth in claim 5 wherein the sum of the contents of said active ingredient a and active ingredient B in the pesticide composition is 1% to 60% by weight based on 100% by weight of the total weight of the pesticide composition.
7. A pesticide composition as set forth in claim 1 further comprising an adjunct ingredient selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoamers, stabilizers, penetrants, and carriers.
8. The pesticide composition of claim 1, wherein the formulation of the pesticide composition is water dispersible granule, suspending agent, emulsifiable concentrate or emulsion in water.
9. The use of a pesticide composition as set forth in any one of claims 1 to 8 for controlling plant diseases, wherein the plant diseases are powdery mildew of cucumber.
CN202210357686.4A 2022-04-07 2022-04-07 Pesticide composition containing bixafen and application thereof Active CN114766492B (en)

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CN104957143A (en) * 2015-06-22 2015-10-07 广东中迅农科股份有限公司 Insecticide composition containing fluxapyroxad and fludioxonil
CN105532721A (en) * 2015-12-24 2016-05-04 南京华洲药业有限公司 Sterilization composition containing bixafen and ethirimol and application of sterilization composition
WO2019166252A1 (en) * 2018-02-28 2019-09-06 Basf Se Fungicidal mixtures comprising fenpropidin
EP3679792A1 (en) * 2019-01-08 2020-07-15 Bayer AG Active compound combinations

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2005034628A1 (en) * 2003-10-10 2005-04-21 Bayer Cropscience Aktiengesellschaft Synergistic fungicidal active substance combinations
CN101631465A (en) * 2007-02-05 2010-01-20 巴斯夫欧洲公司 Fungicidal mixtures comprising substituted 1-methylpyrazol-4-ylcarboxanilides
CN102715167A (en) * 2007-04-25 2012-10-10 先正达参股股份有限公司 Fungicidal compositions
CN104957143A (en) * 2015-06-22 2015-10-07 广东中迅农科股份有限公司 Insecticide composition containing fluxapyroxad and fludioxonil
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