CN114747582B - Pesticide composition containing Isoflucypram and copper quinolinate and application thereof - Google Patents

Pesticide composition containing Isoflucypram and copper quinolinate and application thereof Download PDF

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Publication number
CN114747582B
CN114747582B CN202210210366.6A CN202210210366A CN114747582B CN 114747582 B CN114747582 B CN 114747582B CN 202210210366 A CN202210210366 A CN 202210210366A CN 114747582 B CN114747582 B CN 114747582B
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pesticide composition
isoflucypram
copper
active ingredient
agent
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CN114747582A (en
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隋书婷
杨志鹏
葛家成
张凯莉
李晶
刘笑宏
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Qingdao Hailier Biotechnology Co ltd
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Qingdao Hailier Biotechnology Co ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • A01N43/42Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings condensed with carbocyclic rings
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/561,2-Diazoles; Hydrogenated 1,2-diazoles
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Abstract

The invention belongs to the field of pesticide bactericides, and discloses a pesticide composition containing Isoflucypram and copper quinolinate and application thereof; the active ingredients of the composition comprise an active ingredient A Isoflucypram and an active ingredient B copper quinoline; the mass ratio of the Isoflucypram to the copper quinolinate is 1:30-10:1. The pesticide composition overcomes the defect of single dosage, has broad-spectrum sterilization effect, effectively reduces the use amount and the use cost of active ingredients, and delays the generation and development of resistance. The pesticide composition has higher control effect on various plant fungal diseases.

Description

Pesticide composition containing Isoflucypram and copper quinolinate and application thereof
Technical Field
The invention relates to the field of pesticide bactericides, in particular to a pesticide composition containing Isoflucypram and copper quinolinate and application thereof.
Background
Isoflucypram, a succinate dehydrogenase inhibitor (SDHI) biocide developed by bayer crop science, CAS accession No.: 1255734-28-1, chemical name: n- [ (5-chloro-2-prop-2-ylphenyl) methyl ] -N-cyclopropyl-3- (difluoromethyl) -5-fluoro-1-methylpyrazole-4-carboxamide can be used for preventing and treating a plurality of diseases such as net blotch, leaf spot, leaf rust, stripe rust, leaf blight and the like, and has good prevention and treatment effects.
The quinoline-copper (quinoline-copper) is a chelated organic copper broad-spectrum bactericide, and can prevent pathogenic bacteria from infecting crops by forming a compact protective film on the surface of the crops, and can also act inside the pathogenic bacteria to inhibit the activity and conduction of main conductors of the pathogenic bacteria, thereby killing the pathogenic bacteria. The quinclorac has the effect of preventing and controlling fungi and bacterial diseases, and is suitable for preventing and controlling various diseases on various crops such as fruit trees, vegetables, melons, vegetables, tobacco and the like.
The reasonable chemical agent compounding has the positive characteristics of expanding the sterilization spectrum, improving the control effect, prolonging the application period, reducing the dosage, reducing the phytotoxicity, reducing the residue, delaying the drug resistance of harmful bacteria, delaying the occurrence of drug resistance and the like. With the deeper and deeper understanding of farmers on environmental protection, high efficiency, low toxicity, high activity and low residue become the necessary trend of pesticide development. Therefore, with the increasing requirements on environment and food safety and the problem of drug resistance, how to scientifically use drugs, reduce the dosage of chemical pesticides and improve the drug effect becomes a problem to be solved in the pesticide field; in addition, there is no report about the application of the pesticide composition of Isoflucypram and copper quinolinate.
Disclosure of Invention
Based on the above circumstances, the present invention aims to provide a pesticide composition containing Isoflucypram and copper quinolinate and a preparation thereof, which are mainly used for controlling plant fungal diseases, wherein the composition or the preparation thereof can enhance the efficacy, reduce the dosage, prolong the duration of efficacy and delay the development of drug resistance.
In order to achieve the above object, a pesticide composition containing Isoflucypram and copper quinolinate, the pesticide composition contains an active ingredient A Isoflucypram and an active ingredient B copper quinolinate;
further, the mass ratio of the Isoflucypram to the copper quinolinate is 1:30-10:1;
further, the mass ratio of the Isoflucypram to the copper quinolinate is 1:30-3:1;
further, the mass ratio of the Isoflucypram to the copper quinolinate is 1:15-3:2;
further, the mass ratio of Isoflucypram to copper quinolinate is 1:30, 1:20, 1:15, 1:10, 1:5, 1:3, 1:1, 3:2, 3:1, 5:1, 10:1;
further, the sum of the contents of the active ingredient A and the active ingredient B in the pesticide composition is 1 to 95 weight 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 5 to 80 weight 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 10 to 80 weight percent based on 100 weight percent of the total weight of the pesticide composition;
in embodiments, the sum of the amounts of Isoflucypram and copper quinolinate in the pesticide composition is from 10 to 60wt%, for example, the sum of the amounts of Isoflucypram and copper quinolinate is 30wt%, 49wt%, 50wt%, 60wt%, 72wt% and 80wt%.
Further, the pesticide composition further comprises an auxiliary agent selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreezes, defoamers, solvents, preservatives, stabilizers, synergists or 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
Disintegrating agent the disintegrating agent is selected from one or more of 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 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 formulation of the pesticide composition can be any one of emulsifiable concentrate, aqueous emulsion, microemulsion, suspending agent, wettable powder or water dispersible granule;
the emulsifiable concentrate is a liquid obtained by dissolving high-concentration active ingredients in a solvent and adding an emulsifier. Most emulsifiers use a mixture of nonionic and anionic surfactants. The emulsifiable concentrate is simple and convenient to prepare, has higher biological effect, but has high raw material cost and excessive preparation cost, and increases the preparation cost.
The aqueous emulsion is a preparation prepared by dispersing liquid or a liquid pesticide raw material prepared by mixing the aqueous emulsion with a solvent in water in small liquid drops of 0.5-1.5 mu m, and the appearance of the aqueous emulsion is milky liquid. Besides the effective components and the solvent, the aqueous emulsion can be added with auxiliary agents such as an emulsifying agent, a dispersing agent, an antifreeze agent and the like, so that the stability of the emulsifying agent is improved.
The microemulsion is composed of liquid pesticide, dispersant, water, stabilizer, etc., the pesticide particles are 0.01-0.1 μm, water is used as medium, no or little organic solvent is contained, the environmental pollution is little, the permeability to target organism is strong, the adhesive force is good, and the microemulsion is a green pesticide preparation which is friendly to environment.
The suspending agent is prepared by mixing a surfactant, water or an organic solvent according to the formula proportion, adding other functional additives, placing the mixture into a reaction kettle for uniform mixing, adding the composition raw materials, stirring and shearing uniformly, performing wet sanding until the particle size is qualified, and finally adding a thickening agent, shearing uniformly, and filtering to obtain the product. The suspending agent is divided into two types, namely an aqueous suspending agent and an oil suspending agent, and has small particle size, high biological activity, no dust flying problem and no flammability and explosiveness.
The wettable powder is prepared by uniformly mixing the composition raw materials with a dispersing agent, a wetting agent and a filler according to a certain proportion, uniformly stirring in a stirring kettle, and uniformly crushing and mixing for multiple times by using an airflow crusher. Wettable powders are formulations which are uniformly dispersible in water and which contain, in addition to the active and inert substances, a certain amount of anionic or nonionic surfactant. The wettable powder does not use solvents or emulsifying agents, is safer to plants, is not easy to produce phytotoxicity and is safe to the environment.
The water dispersible granule is prepared by adding the raw material of the composition into a carrier, adding a surfactant and other functional additives into the carrier, mixing, carrying out jet milling, adding 10-25% of water, and then kneading, granulating, drying and screening. The water dispersible granule has good fluidity, convenient use, no dust flying, safety and reliability.
The dosage form of the pesticide composition containing Isoflucypram and copper quinolinate can be any one of suspending agent, wettable powder or water dispersible granule.
The invention also discloses application of the pesticide composition containing Isoflucypram and copper quinolinate in preventing and treating plant diseases;
further, the plant disease is a plant disease caused by fungi or bacteria;
further, the plant disease is a plant disease caused by fungi;
further, the plant disease is peanut disease and/or potato disease caused by fungi;
further, the potato disease is potato early blight, and the peanut disease is peanut leaf spot;
potato early blight (Potato early blight) also called Xia Yibing and ring rot, and fungal diseases caused by two pathogenic bacteria, namely alternaria solani (Alternaria solani) and alternaria alternata (Alternaria alternata). Wherein Alternaria solani is the dominant pathogen. The plant disease has short incubation period, frequent re-infection and strong popularity, and mainly infects plant leaves and tubers in the field growth period and the storage period of potatoes, and after pathogenic bacteria invade host tissues, the plant disease can form lesions in 2-3 days, and a large number of conidia can be generated in 3-4 days, so that cyclic infestation is caused. The primary infection of bacteria occurs on the old leaves at the lower part of potato plants, and gradually spreads upwards to tender tissues. The disease leaves show small black spots with the diameter of about 1mm, black brown round or nearly round disease spots with concentric circular patterns are formed in late stage infection, the outer edges of the disease spots show yellow halos, the diameter is about 10mm, and a villus black mould layer is generated on the disease spots when the field humidity is high. When the potato tubers are infected, dark brown round or nearly round disease spots and slightly concave disease parts appear, the potato flesh under the disease spots presents brown dry rot, and the disease key boundaries are obvious. The potato early blight occurs most seriously in the fruiting period, and a great amount of nutrition of plants is transmitted to tubers in the period, so that the nutrition of leaves is reduced, and the leaves are easily infected by germs. Early blight of potato occurs in seedling emergence stage, leaf spots gradually increase in bud stage and final flowering stage, concentric ring and gray black mildew layer appear, and the leaf spots do not increase in mature stage, but the concentric ring and mildew layer are more obvious.
The peanut leaf spot comprises brown spot (Cercospora arachidicola) and black spot (Phaeoisariopsis personata), both diseases are mainly harmful leaves, and are often mixed on the same plant and even the same leaf, and the symptoms are very similar, so that the leaves die and fall off. Leaf spot disease starts from the lower leaves of peanut plants, gradually spreads to the upper leaves after symptoms appear, and gradually develops into circular or irregular shape lesions. The brown spot is large, yellow halo is arranged around the spot, the black spot is smaller, the color is lighter than that of the brown spot, the edge is tidier, and no obvious halo exists. When the weather is moist or overcast and rainy, the disease spots can be mutually combined into irregular large spots, and the leaf scorch is serious, so that photosynthesis is affected. If the black spot happens on the fruit needle, the leaf stalk and the stem, the black brown oval and brown spot can be generated when the black spot is light, and the whole stem or the fruit needle is blackened and dead when the black spot is serious. The asexual generation of pathogenic bacteria of peanut leaf spot disease belongs to the genera Deuteromycotina, cellulare, neurosporaceae, cercospora and Bremia. The sexual generation belongs to ascomycetes, and globus. The cycles of disease development are substantially similar for both types. The pathogenic bacteria only attack the peanut. The germ mainly uses the stroma, hypha and conidium to overwinter on the disease residue, or the ascove cavity can be attached to the seed shell or seed to overwinter, so as to become the primary infection source of the next year, and the hypha directly generates the conidium to spread along with wind and rain under proper conditions.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) Isoflucypram with different action mechanisms and copper quinoline are compounded, so that the bactericidal activity is increased, and the application range is enlarged;
(2) The pesticide is safe and environment-friendly, has wide development prospect, reduces the use amount of the pesticide and reduces the agricultural cost;
(3) Has the advantages of super high efficiency, broad bactericidal spectrum, and can delay the generation of drug resistance of harmful bacteria and prolong the duration of the drug.
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 1:
60% Isoflucypram-copper quinoline wettable powder (1:3)
15% of Isoflucypram, 45% of copper quinoline, 7% of sodium lignin sulfonate, 4% of dispersant NNO, 4% of nekal BX 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, evenly stirred in a stirring kettle, and crushed and mixed evenly for many times by an airflow crusher, thus obtaining the wettable powder of the composition.
Preparation example 2:
50% Isoflucypram-copper quinolinate wettable powder (1:4)
According to the weight percentage, the Isoflucypram is 10%, the copper quinolinate is 40%, the sodium dodecyl sulfate is 3%, the sodium lignosulfonate is 8%, the calcium lignosulfonate is 2%, and the kaolin is used for the balance;
the preparation method comprises the following steps: the same as in preparation example 1.
Preparation example 3:
80% Isoflucypram-quinoline copper water dispersible granule (1:7)
10% of Isoflucypram, 70% of copper quinoline, 4% of naphthalene sulfonate formaldehyde condensate, 3% of sodium dodecyl sulfate, 10% of sodium polycarboxylate and the balance of kaolin;
the preparation method comprises the following steps: according to the formula proportion of the embodiment, the active ingredients are added into a carrier, and the surfactant and other functional additives are added into the carrier, mixed, crushed by air flow, added with 10 to 25 percent of water, and then kneaded, granulated, dried and screened to prepare the water dispersible granule product.
Preparation example 4:
72% Isoflucypram-quinoline copper water dispersible granule (1:8)
The weight percentages of the components are 64% of copper quinoline, 8% of Isoflucypram, 3% of sodium dodecyl sulfate, 3% of sodium lignin sulfonate, 10% of naphthalene sulfonate formaldehyde condensate and the balance of kaolin;
the preparation method comprises the following steps: the same as in preparation example 3.
Preparation example 5:
30% Isoflucypram-quinoline copper suspension (1:5)
According to the weight percentage, the Isoflucypram comprises 5 percent of copper quinoline, 1 percent of fatty alcohol polyoxyethylene ether, 3 percent of alkylphenol polyoxyethylene phosphate, 2 percent of alkylaryl polyoxyethylene ether polyoxypropylene ether, 1 percent of polycarboxylic acid sodium salt, 1 percent of magnesium aluminum silicate, 1 percent of sodium sorbate, 5 percent of ethylene glycol, 0.5 percent of silicone oil, 0.3 percent of xanthan gum and the balance of deionized water;
the preparation method comprises the following steps: according to the formula proportion, water, a surfactant and other functional additives are sequentially placed in a reaction kettle to be uniformly mixed, then active ingredients are added, stirring and shearing are performed uniformly, wet sanding is performed until the particle size is qualified, and finally a thickening agent is added, shearing, homogenizing and filtering are performed to obtain the product.
Preparation example 6:
49% Isoflucypram-quinoline copper suspension (1:6)
According to the weight percentage, the Isoflucypram comprises 7 percent of copper quinoline, 1 percent of alkylphenol ethoxylates, 3 percent of alkylphenol ethoxylate phosphate, 2 percent of sodium lignin sulfonate, 0.25 percent of xanthan gum, 5 percent of glycerol, 1 percent of sodium benzoate, 0.5 percent of silicone oil and the balance of deionized water;
the preparation method comprises the following steps: the same as in preparation example 5.
Indoor toxicity test
Example 1: indoor combined action test of Isoflucypram and quinoline copper mixed with potato early blight
The test is based on: section 2 of the bactericide referring to the standard pesticide indoor bioassay test guidelines in the agricultural industry of the people's republic of China: test plate method NT/T1156.2-2006 for inhibiting growth of fungal hyphae.
Test agent: 92% isoflucypram stock was supplied by the marial pharmaceutical industry group development center, 33.5% quinoline copper suspension, supplied by Shandong marial chemical Co.
Test pathogenic bacteria: potato early blight germ (Alternaria solani).
And (3) preparation of a medicament: dissolving the Isoflucypram raw medicine with acetone, and diluting with 0.1% Tween 80 aqueous solution; 33.5% copper quinolinate suspension was diluted with sterile water. Preparing single-dose mother liquor, and setting a series of mass concentrations 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 5d incubation, colony diameters were measured in millimeters (mm) using calipers, and each colony was measured vertically once by the cross-over method, and the average 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=D 1 -D 2 ············(1)
D-colony growth diameter;
D 1 colony diameter;
D 2 -diameter of the bacterial cake.
I=(D 0 -D t )/D 0 *100············(2)
Wherein:
i, hypha growth inhibition rate;
D 0 -the control colony increased in diameter;
D t -the agent-treated colonies increased in diameter.
Statistical analysis: regression analysis is carried out according to the concentration log value of each medicament and the corresponding hypha growth inhibition rate value, and the EC of each medicament is calculated 50 Equivalent valueAnd (3) evaluating the activity of the test agent on the biological test material according to the correlation coefficient R.
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 of Standard bactericides 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 ·······(4)
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.
Calculating test results by adopting DPS data processing software, and respectively solving the test resultsToxicity regression equation of single medicament and mixed medicament with different proportions, R, EC 50 And EC (EC) 90 And 95% confidence limit, and calculating co-toxicity coefficients (CTCs) of the two medicaments in different proportions, and screening out the optimal proportion of the test medicaments.
Test results:
TABLE 1 results of indoor Activity test of Isoflucypram and copper quinoline mixing against potato early blight
As can be seen from the indoor activity test (see Table 1), the Isoflucypram and the copper quinolinate single dose are used for treating potato early blight EC 50 1.985mg/L and 47.308mg/L, respectively, are susceptible to the potato early blight; the co-toxicity coefficients of the Isoflucypram and the copper quinolinolate are all larger than 120 after being mixed according to the proportion of 1:30-10:1, and the synergistic effect is shown for preventing and treating potato early blight.
Example 2: indoor combined action test of Isoflucypram and quinoline copper mixed on brown spot pathogen of peanut
The test is based on: section 2 of the bactericide referring to the standard pesticide indoor bioassay test guidelines in the agricultural industry of the people's republic of China: test plate method NT/T1156.2-2006 for inhibiting growth of fungal hyphae.
Test agent: 92% isoflucypram stock was supplied by the marial pharmaceutical industry group development center, 33.5% quinoline copper suspension, supplied by Shandong marial chemical Co.
Test pathogenic bacteria: brown spot germ of peanut (Cercospora arachidicola).
And (3) preparation of a medicament: dissolving the Isoflucypram raw medicine with acetone, and diluting with 0.1% Tween 80 aqueous solution; 33.5% copper quinolinate suspension was diluted with sterile water. Preparing single-dose mother liquor, and setting a series of mass concentrations 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 9mLPDA 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=D 1 -D 2 ············(1)
D-colony growth diameter;
D 1 colony diameter;
D 2 -diameter of the bacterial cake.
I=(D 0 -D t )/D 0 *100············(2)
Wherein:
i, hypha growth inhibition rate;
D 0 -the control colony increased in diameter;
D t -the agent-treated colonies increased in diameter.
Statistical analysis: regression analysis is carried out according to the concentration log value of each medicament and the corresponding hypha growth inhibition rate value, and the EC of each medicament is calculated 50 And (5) equivalent, correlation coefficient R, and evaluating the activity of the test agent on the biological test material.
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 of Standard bactericides 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 ·······(4)
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.
Calculating test results by adopting DPS data processing software, and respectively solving virulence regression equations, R, EC of single test medicament and mixed medicaments with different proportions 50 And EC (EC) 90 And 95% confidence limit, and solving co-toxicity coefficient (CTC) of two medicaments in different proportions, and screening out test medicamentsThe optimal proportion of the agent.
Test results:
TABLE 2 results of indoor Activity test of Isoflucypram and copper quinoline for Alternaria alternata
As can be seen from the indoor activity test (see Table 2), the Isoflucypram and the copper quinolinate single dose are used for treating peanut brown spot EC 50 3.309mg/L and 41.588mg/L, respectively, peanut brown spots are more sensitive to Isoflucypram; the co-toxicity coefficients of the Isoflucypram and the copper quinolinolate are all larger than 120 after being mixed according to the proportion of 1:15-3:2, and the synergistic effect is shown for preventing and treating peanut brown spot.
Field test
Example 3: field test for preventing and treating potato early blight
Test variety: qin dasheen No. 32;
control object: early blight of potato;
test site: the administration time of the drug is 9 middle of the year 2020.
The test method comprises the following steps: with random block arrangement, cell area 20m 2 4 replicates.
The application method and times are as follows: the potato early blight is applied by a conventional spray method at the initial stage, and is applied once again 8d after the application, and the total application time is 2 times;
the investigation method comprises the following steps: the disease number is investigated before the first application, and the disease index and the control effect are calculated after the first application and the second application, wherein the investigation is carried out once for 7d and 11d respectively.
Reference to pesticide field efficacy test guidelines (one) part 34: the bactericide can be used for preventing and treating potato late blight (GB/T17980.34-2000).
Sampling 5 points on the diagonal line of each cell, taking 3 strains at each point, checking all blades, and recording according to the following grading method.
Blade grading criteria:
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% -15% of the whole leaf area;
5 stages: the area of the lesion accounts for 16% -25% of the whole leaf area;
7 stages: the area of the lesion accounts for 26% -50% of the whole leaf area;
stage 9: the area of the disease spots accounts for more than 51% of the whole leaf area.
The drug effect is calculated according to the following formula:
(1) Disease index = [ Σ (leaf number of each stage×relative stage number)/(total leaf number of investigation×9) ]×100
(2) Control effect (%) = [1- (pre-treatment area drug condition index x treatment area post-treatment area drug condition index)/(post-treatment area drug condition index x treatment area pre-treatment area drug condition index) ]x100
Results and analysis:
TABLE 3 results of field efficacy test of Isoflucypram and copper quinoline for controlling potato early blight
Field efficacy display (see table 3): the overall control effect of each treatment field effect of different treatments for controlling potato early blight is 52.17-85.64% after the first application of the medicines, 72% of isoflucypram-quinoline copper water dispersible granule (1:8), 49% of isoflucypram-quinoline copper suspending agent (1:6), 30% of isoflucypram-quinoline copper suspending agent (1:5) and 60% of isoflucypram-quinoline copper wettable powder (1:3) are sprayed, and the control effects of the medicines for controlling potato early blight are 81.39%, 82.57%, 84.15% and 85.64% respectively, which are superior to those of single-dose 20% of isoflucypram suspending agent and 33.5% of quinoline copper suspending agent, wherein the control effect of the 60% of isoflucypram-quinoline copper wettable powder (1:3) is the best.
The overall prevention effect of each treatment field effect after 11 days of the second application is 55.36% -90.78%, 72% of isoflucypram-quinoline copper water dispersible granule (1:8), 49% of isoflucypram-quinoline copper suspending agent (1:6), 30% of isoflucypram-quinoline copper suspending agent (1:5) and 60% of isoflucypram-quinoline copper wettable powder (1:3) are sprayed, and the prevention effect of each treatment field effect after the second application is 84.87%, 85.60%, 86.29% and 90.78%, which are superior to those of a single dose of 20% isoflucypram-quinoline copper suspending agent and 33.5% of quinoline copper suspending agent, wherein the prevention effect of 60% of isoflucypram-quinoline copper wettable powder (1:3) is the best.
Example 4: field test for preventing and treating leaf spot of peanut
Test variety: peanut and white sand variety are in needle setting period and have good growth vigor.
Control object: the leaf spot disease of the peanut is identified as brown spot germ (Cercospora arachidicola) and black spot germ (Phaeoisariopsis personata) of the peanut through separation.
Test site: the administration time is 8 late in 2020.
The test method comprises the following steps: random block arrangement is adopted, and the cell area is as follows: 30m 2 The method comprises the steps of carrying out a first treatment on the surface of the Number of repetitions: 4 times.
The application method and times are as follows: the preparation is applied by a conventional spray method at the early stage of the leaf spot of the peanut, and is applied once every 7d after the preparation, and the total application time is 2 times.
The investigation method comprises the following steps: disease cardinality investigation was performed prior to the first administration, followed by control investigation 7 days after the last administration for a total of 2 surveys.
Reference is made to section 85 of pesticide field efficacy test guidelines (one): bactericide for preventing and treating peanut leaf spot disease (GB/T17980.85-2004)
Five points are randomly selected for sampling in each district, 4 plants are taken at fixed points, all leaves of main stems are investigated for each plant, and total leaf numbers and leaf numbers of all stages of diseases are recorded and investigated.
The grading method comprises the following steps:
level 0: no disease;
stage 1: the area of the disease spots accounts for less than 5% of the area of the whole leaf;
3 stages: the area of the disease spots accounts for 6% -25% of the area of the whole leaf;
5 stages: the area of the disease spots accounts for 26% -50% of the area of the whole leaf;
7 stages: the area of the disease spots accounts for 51% -75% of the area of the whole leaf;
stage 9: the area of the disease spots accounts for more than 76% of the area of the whole leaf.
The drug effect is calculated according to the following formula:
(1) Disease index = [ Σ (leaf number of each stage×relative stage number)/(total leaf number of investigation×9) ]×100
(2) Control effect (%) = [1- (pre-treatment area drug condition index x treatment area post-treatment area drug condition index)/(post-treatment area drug condition index x treatment area pre-treatment area drug condition index) ]x100
Results and analysis:
TABLE 4 results of field efficacy test of Isoflucypram and copper quinoline for controlling peanut leaf spot
Field efficacy display (see table 4): the overall control effect of each treatment field effect of 7 days after the final application of the medicines for controlling the leaf spot disease of the peanuts is 66.86-91.07%, and under the condition of reduced dosage, the control effect of the sprayed 30% isoflucypram quinoline copper suspending agent (1:5) on the leaf spot disease of the peanuts is 91.07%, which is superior to that of a single 20% isoflucypram suspending agent and a 33.5% quinoline copper suspending agent.
As can be seen from indoor toxicity measurement and field experiments, the pesticide composition compounded by Isoflucypram and copper quinolinolate has good control effect on crop diseases, especially early blight of potato and leaf spot of peanut. The pesticide composition or the preparation prepared by the combination has remarkable prevention effect, and is superior to a single dose in the aspects of delaying the generation of drug resistance and prolonging the drug retention. In addition, no phytotoxicity of the compound medicament to crops is found in the test, which proves that the production cost and the use cost can be reduced and the pesticide composition or the pesticide preparation is safe to crops under the condition that the sterilization synergy of the obtained pesticide composition or the pesticide preparation is improved.
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 (14)

1. A pesticide composition containing Isoflucypram and copper quinolinate, characterized in that: the pesticide composition comprises an active ingredient A Isoflucypram and an active ingredient B copper quinoline, wherein the mass ratio of the Isoflucypram to the copper quinoline is 1:30-10:1.
2. The pesticide composition as set forth in claim 1, wherein the mass ratio of Isoflucypram to copper quinolinate is 1:30 to 3:1.
3. The pesticide composition as set forth in claim 1, wherein the mass ratio of Isoflucypram to copper quinolinate is 1:15 to 3:2.
4. A pesticide composition as set forth in claim 1 wherein the sum of the contents of the active ingredient a and the active ingredient B in the pesticide composition is 1 to 95% by weight based on 100% by weight of the total weight of the pesticide composition.
5. A pesticide composition as set forth in claim 1 wherein the sum of the contents of the active ingredient a and the active ingredient B in the pesticide composition is 5 to 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 1 wherein the sum of the contents of the active ingredient a and the active ingredient B in the pesticide composition is 10 to 80% by weight based on 100% by weight of the total weight of the pesticide composition.
7. A pesticide composition as set forth in claim 4 further comprising an adjuvant 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 synergist or a carrier.
8. A pesticide composition as set forth in claim 5 in the form of any one of emulsifiable concentrates, aqueous emulsions, microemulsions, suspensions, wettable powders or water dispersible granules.
9. A pesticide composition as set forth in claim 8 in which the formulation of the pesticide composition is any one of a suspending agent, a wettable powder or a water dispersible granule.
10. Use of the pesticidal composition of any one of claims 1 to 9 for controlling plant diseases.
11. The use according to claim 10, wherein the plant disease is a plant disease caused by fungi or bacteria.
12. The use according to claim 11, wherein the plant disease is a fungal plant disease.
13. The use according to claim 12, wherein the plant disease is a peanut disease and/or a potato disease caused by fungi.
14. The use of claim 13, wherein the potato disease is an early blight of potato and the peanut disease is a peanut leaf spot.
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