CN114586793B - Pesticide composition and application thereof - Google Patents
Pesticide composition and application thereof Download PDFInfo
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- CN114586793B CN114586793B CN202210347631.5A CN202210347631A CN114586793B CN 114586793 B CN114586793 B CN 114586793B CN 202210347631 A CN202210347631 A CN 202210347631A CN 114586793 B CN114586793 B CN 114586793B
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- ZLVSYODPTJZFMK-UHFFFAOYSA-M sodium 4-hydroxybenzoate Chemical compound [Na+].OC1=CC=C(C([O-])=O)C=C1 ZLVSYODPTJZFMK-UHFFFAOYSA-M 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
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- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 229940074404 sodium succinate Drugs 0.000 description 1
- ZDQYSKICYIVCPN-UHFFFAOYSA-L sodium succinate (anhydrous) Chemical compound [Na+].[Na+].[O-]C(=O)CCC([O-])=O ZDQYSKICYIVCPN-UHFFFAOYSA-L 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- PYODKQIVQIVELM-UHFFFAOYSA-M sodium;2,3-bis(2-methylpropyl)naphthalene-1-sulfonate Chemical compound [Na+].C1=CC=C2C(S([O-])(=O)=O)=C(CC(C)C)C(CC(C)C)=CC2=C1 PYODKQIVQIVELM-UHFFFAOYSA-M 0.000 description 1
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Classifications
-
- 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
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
Abstract
The invention discloses a pesticide composition, the effective components of which comprise an active component A and an active component B, wherein the active component A is a compound shown in a formula I
Description
Technical Field
The invention belongs to the technical field of pesticide compounding, and particularly relates to a pesticide composition and application thereof.
Background
The chemical name of the compound of the formula (I) is 3-difluoromethyl-1-methyl-N- (3 ',4',5' -trifluoro-biphenyl-2-yl) pyrazole-4-amide, which is a high-efficiency, broad-spectrum and systemic succinic dehydrogenase inhibitor developed by Basff company, and the action mode is to prevent energy metabolism and eliminate some basic chemical building blocks used for synthesis and basic constitution, thereby inhibiting the growth of pathogenic bacteria. Diseases of grains, fruit trees and vegetables caused by the genus Septoria, botrytis, erysiphe, cercospora, puccinia, rhizoctonia and Nuclear Cavity can be prevented and treated by leaf surfaces and seeds. In particular to the prevention and treatment of diseases and rust diseases and powdery mildew caused by alternaria, botrytis and septoria in soybeans. The structural formula is as follows:
The 5-ethyl-6-octyl [1,2,4] triazole [1,5-a ] pyrimidine-7-amine is a triazole pyrimidine bactericide developed by Basoff, belongs to a mitochondrial respiration inhibitor, has a control effect on fungus of the class of downy mildew and Phytophthora, and has extremely strong residual activity and rain resistance. The compound can be combined with a colistin subsite in a fungus respiratory complex III so as to inhibit the activity of fungi, and has no cross resistance with other bactericides, and the structural formula is as follows:
In the agricultural production process, the application of chemical agents is the most effective means for preventing and treating plant diseases, but the long-term continuous high-dosage use of single chemical bactericides is easy to cause the problems of agent residue, environmental pollution, development of drug-resistant fungi and the like. The reasonable chemical bactericide is compounded and has the characteristics of expanding the bactericidal spectrum, reducing the phytotoxicity, reducing the pesticide residue, improving the control effect, delaying the occurrence of the drug resistance of fungi and the like. The inventor provides a bactericidal composition on the basis of a large number of experimental researches of indoor screening and field experiments, which has obvious synergism, and no one reports about a compound bactericidal composition of an active component A (a compound shown as a formula I) and an active component B (5-ethyl-6-octyl [1,2,4] triazole [1,5-a ] pyrimidine-7-amine).
Disclosure of Invention
Based on the above circumstances, the invention aims to provide a pesticide composition and application thereof, wherein the pesticide composition is compounded by active ingredients with different action mechanisms, so that the production cost is effectively reduced. The pesticide composition can be used for preventing and treating diseases caused by various plant pathogenic bacteria.
In order to achieve the above purpose, the present invention adopts the following technical scheme: the pesticide composition comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is a compound shown in a formula I, and the structure of the compound shown in the formula I is as follows:
The component B is a triazolopyrimidine bactericide, and the chemical name of the triazolopyrimidine bactericide is 5-ethyl-6-octyl [1,2,4] triazol [1,5-a ] pyrimidine-7-amine.
Further, the mass ratio of the active ingredient A to the active ingredient B is 38:1-1:38;
Further, the mass ratio of the active ingredient A to the active ingredient B is 35:1-1:15;
Further, the mass ratio of the active ingredient A to the active ingredient B is 35:1, 26:1, 20:1, 15:1, 10:1, 6:1, 3:1, 2:1, 1:1, 1:2, 1:3, 1:6, 1:7, 1:10, 1:15;
Further, the mass ratio of the active ingredient A to the active ingredient B is 15:1-1:15;
Further, the mass ratio of the active ingredient A to the active ingredient B is 15:1, 10:1, 6:1, 3:1, 2:1, 1:1, 1:2, 1:3, 1:6, 1:7, 1:10, 1:15;
further, when the pesticide composition is used for preventing and treating downy mildew, the mass ratio of the active component A to the active component B is 26:1-30:1;
Further, when the pesticide composition is used for preventing and treating downy mildew, the mass ratio of the active ingredient A to the active ingredient B is 15:1-1:15;
further, when the pesticide composition is used for preventing and treating late blight, the mass ratio of the active ingredient A to the active ingredient B is 35:1-1:15;
Further, when the pesticide composition is used for preventing and treating late blight, the mass ratio of the active ingredient A to the active ingredient B is 15:1-1:15;
further, the total weight of the pesticide composition is calculated by 100 weight percent, and the total weight of the active component A and the active component B accounts for 0.1 to 90 percent of the total weight of the pesticide composition;
Further, the total weight of the pesticide composition is calculated by 100 weight percent, and the total weight of the active ingredient A and the active ingredient B accounts for 1-70% of the total weight of the pesticide composition;
Further, the pesticide composition comprises an agriculturally acceptable auxiliary ingredient besides an active ingredient, wherein the auxiliary ingredient is selected from one or more of wetting agents, dispersing agents, thickening agents, disintegrating agents, emulsifying agents, antifoaming agents, preservatives, stabilizers, synergists, carriers and solvents;
The wetting agent is selected from one or more of alkylbenzene sulfonate, alkyl naphthalene sulfonate, lignin sulfonate, sodium dodecyl sulfate, dioctyl sodium succinate sulfonate, 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 polyoxyethylene ether methyl ether condensate sulfate, fatty amine polyoxyethylene ether, glycerin fatty acid ester polyoxyethylene ether, polycarboxylate, polyacrylic acid, phosphate, EO-PO block copolymer and EO-PO graft copolymer; and/or
The thickener is one or more selected from xanthan gum, polyvinyl alcohol, organic bentonite, magnesium aluminum silicate and carboxymethyl cellulose; and/or
The disintegrating agent is one or more selected from sodium sulfate, ammonium sulfate, aluminum chloride, sodium chloride, ammonium chloride, bentonite, glucose, sucrose, starch, cellulose, urea, sodium carbonate, sodium bicarbonate, citric acid and tartaric acid; and/or
The emulsifier is one or more selected from fatty alcohol polyoxyethylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, phenethyl phenol polyoxyethylene polyoxypropylene ether, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, alkylbenzene sulfonate, styrylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester; and/or
The defoamer is one or more selected from silicone oil, C 10～C20 saturated fatty acid compounds, C 8～C10 fatty alcohol compounds or silicone compounds; and/or
The preservative is one or more of sorbic acid, sodium sorbate, potassium sorbate, benzoic acid, sodium benzoate, sodium p-hydroxybenzoate and methyl p-hydroxybenzoate; 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, epoxidized vegetable oil; and/or
The synergistic agent is selected from synergistic phosphorus and synergistic ether; and/or
The carrier is one or more selected from kaolin, bentonite, attapulgite, light calcium carbonate, diatomite and white carbon black; and/or
The solvent is selected from one or more of benzene, toluene, xylene, methanol, ethanol, isopropanol, N-butanol, diesel oil, N-dimethylformamide, cyclohexanone, ethyl acetate, N-methylpyrrolidone, propanol, butanol, ethylene glycol, diethylene glycol, ethylene glycol methyl ether, butyl ether, solvent oil, vegetable oil derivatives and deionized water; and/or
Further, the pesticide composition can be prepared into any agriculturally acceptable formulation;
Further, the preparation formulation is any one of a solid preparation, a liquid preparation or a seed treatment preparation;
Further, the preparation formulation is a solid preparation, a liquid preparation or a 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 granules or wettable powder, and the liquid preparation is suspending agent;
the invention also discloses application of the pesticide composition in preventing and controlling pathogenic bacteria of agricultural, forestry or gardening plants.
Further, the plant pathogenic bacteria are bacteria and/or fungi on cereal, vegetables, fruits and ornamental plants.
Further, the plant pathogenic bacteria are plant pathogenic fungi such as basidiomycetes, ascomycetes, oomycetes and the like;
the oomycetes include Phytophthora (Phytophthora), such as Phytophthora infestans (Phytophthora infestans), phytophthora sojae (Phytophthora megasperma), citrus angle rot (Phytophthora parasitica), phytophthora camphorata (Phytophthora cinnamomi) and Phytophthora cucurbitae (Phytophthora capsici); pythum species (Pythum); the family of peronosporaceae (Peronosporaceae) such as the species downy mildew (Plasmopara viticola), the species Peronospora (including the species Peronospora tabaci (Peronospora tabacina) and Peronospora parasitica (Peronospora parasitica)); pseudoperonospora (Pseudoperonospora) and pholiota (bremia lactucae); pythium species such as Pythum aphanidermatum (Pythium aphanidermatum);
The ascomycetes include Alternaria (Alternaria), such as Alternaria solani (ALTERNARIA SOLANI) and Alternaria brassicae (ALTERNARIA BRASSICAE); genus Bremia (Guignardia), such as Pythium gracile (Guignardia bidwelli); cercospora (Venturia), such as Cercospora apple (Venturia inaequalis); septoria (Septoria), such as Rhizoctonia solani (Septorianodorum) and Rhizoctonia solani (Septoriatritici); powdery mildew such as Erysiphe (Erysiphe) (including Erysiphe graminis (ERYSIPHE GRAMINIS) and Erysiphe graminis (Erysiphe polygoni)), erysiphe graminis (Uncinula necatur), erysiphe cucumeris (Sphaerotheca fuligena) (Erysiphe cichoracearum) and Erysiphe necator (Podosphaera leucotricha); botrytis species (Botrytis), such as Botrytis cinerea (Botrytis cinerea), monilinia fructicola (Monilinia fructicola); sclerotium (Sclerotinia) such as sclerotium (Sclerotinia sclerotiorum), rice blast (Magnaporthe grisea), and cladosporium cucumeris (Phomopsis viticola); vermicular bacteria (Helminthosporium) such as alternaria corn (Helminthosporium triticirepentis); anilox bacteria (Pyrenophorateres); anthracis (Colletotrichum) such as Colletotrichum (Colletotrichum graminicola) and Colletotrichum (Colletotrichum orbiculare); wheat take-all germ (Gaeumannomyces graminis);
The Basidiomycetes includes the genus Puccinia (Puccinia) such as Puccinia recondita (Puccinia recondita), puccinia striolata (Puccinia striiformis), puccinia (Puccinia hordei), puccinia (Puccinia graminis) and Puccinia (Puccinia arachidis); rust bacteria (Hemileia vastatrix) and soybean rust bacteria (Phakopsora pachyrhizi); other pathogens include Rhizoctonia (Rhizoctonia) such as Rhizoctonia solani (Rhizoctonia solani) and sclerotinia sclerotiorum (Rhizoctonia oryzae); fusarium species (Fusarium), such as Fusarium roseum, fusarium graminearum (Fusarium graminearum), and Fusarium oxysporum (Fusarium oxysporum); verticillium dahliae (Verticillium dahliae); southern blight (Sclerotiumrolfsii); the fungus (Rynchosporiumsecalis); black spot bacteria (Cercosporaarachidicola) and brown spot bacteria (Cercosporabeticola);
further, the plant pathogenic bacteria are bacteria and fungi on cereal, vegetables, fruits and ornamental plants;
The bactericidal composition of the invention is particularly suitable for controlling diseases caused by pathogenic bacteria on crops such as grains (wheat, barley, rye, oat, rice, corn, sorghum and the like), fruit trees (apples, pears, plums, peaches, almonds, bananas, grapes, strawberries, raspberries, blackberries and the like), citrus trees (oranges, lemons, oranges, grapefruits and the like), beans (beans, peas, lentils, soybeans and the like), vegetables (spinach, lettuce, asparagus, cabbage, carrots, onions, tomatoes, potatoes, eggplants, peppers and the like), cucurbitaceae (pumpkin, zucchini, cucumber, melons and the like), oleaginous plants (sunflower, rape, peanuts, castor, coconuts and the like), tobacco, coffee, tea, cocoa, beet, sugarcane, cotton and the like.
Further, the pesticidal composition is applied to the plant pathogenic bacteria and/or the environment thereof, or the plant, plant parts, plant propagation material and subsequently growing plant organs in an effective amount.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1) The pesticide composition has obvious synergism on the prevention and treatment of various plant pathogenic bacteria, and the prevention and treatment effect is obviously improved;
2) Compared with a single pesticide, the pesticide composition can effectively reduce the usage amount and the usage times of the pesticide, reduce the agricultural production cost and save time;
3) The pesticide composition can effectively control pathogenic microorganisms to generate drug resistance, reduce the risk of resistance and prolong the service life of the pesticide.
Indoor Activity test
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
24% Active ingredient A active ingredient B suspension (3:1)
The formula comprises the following components: 18% of active ingredient A, 6% of active ingredient B, 2% of sodium dodecyl sulfate, 1% of naphthalene sulfonate formaldehyde condensate, 3% of styrol polyoxyethylene ether phosphate, 0.2% of xanthan gum, 1% of magnesium aluminum silicate, 4% of propylene glycol, 0.01% of benzisothiazolinone potassium, 0.5% of silicone oil and deionized water, and the balance of the components;
the preparation method comprises the following steps: according to the formula proportion, the active ingredients, the surfactant and other functional auxiliary agents are sequentially placed in a reaction kettle, water is added and mixed uniformly, high-speed shearing and wet sanding are carried out, and finally, the suspending agent product is obtained through homogenizing and filtering.
Preparation example 2
50% Active ingredient A active ingredient B wettable powder (1:1)
According to the weight percentage, 25 percent of active ingredient A, 25 percent of active ingredient B, 4 percent of sodium lignin sulfonate, 3 percent of dispersant NNO, 4 percent of nekal BX and the balance of kaolin are complemented;
The preparation method comprises the following steps: the effective components, 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 3
49% Active ingredient A active ingredient B Water dispersible granule (6:1)
According to weight percentage, 42% of active ingredient A, 7% of active ingredient B, 7% of naphthalene sulfonate formaldehyde condensate, 3% of sodium dodecyl sulfate, 10% of sodium salt of polycarboxylic acid and kaolin are used for the balance;
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
30% Active ingredient A active ingredient B suspension (2:1)
The weight percentage of the active ingredient A is 10 percent, the weight percentage of the active ingredient B is 20 percent, the weight percentage of the active ingredient B is 3 percent, the weight percentage of the styrylphenol polyoxyethylene ether sulfate is 2 percent, the weight percentage of the lignin sulfonate is 2 percent, the weight percentage of the alkylaryl polyoxyethylene ether polyoxypropylene ether is 1 percent, the weight percentage of the magnesium aluminum silicate is 0.1 percent, the weight percentage of the xanthan gum is 1 percent, the weight percentage of the sodium sorbate is 5 percent, the weight percentage of the ethylene glycol is 0.5 percent, and the weight percentage of the silicone oil is the balance of the deionized water;
The preparation method comprises the following steps: as in example 1.
Preparation example 5
20% Active ingredient A active ingredient B Water dispersible granule (1:3)
According to the weight percentage, 5 percent of active ingredient A, 15 percent of active ingredient B, 8 percent of sodium lignin sulfonate, 5 percent of naphthalene sulfonate formaldehyde condensate, 2 percent of sodium dodecyl benzene sulfonate, 5 percent of white carbon black, 30 percent of starch and the balance of kaolin are added.
The preparation method comprises the following steps: same as in example 3.
Example 1: indoor combined toxicity test of active ingredient A (compound of formula I) and active ingredient B (5-ethyl-6-octyl [1,2,4] triazole [1,5-a ] pyrimidine-7-amine) compounded on downy mildew
The test is based on: test reference NY/T1156.7-2006 section 7. Section "pesticide indoor biological assay test guidelines: potted plant method for preventing and controlling cucumber downy mildew; ny/T1156.6-2006 section 6 of pesticide indoor bioassay test criteria section 6: determination of the combined action of compounding.
Test target: cucumber downy mildew (Pseudoperonospora cubensis).
Preparing a test material: and (3) selecting a potted plant of the infected vincristocet cucumber, and keeping the seedling for standby after the seedling grows to 6 true leaf periods.
Test agent: 98% of active ingredient A raw medicine and 98% of active ingredient B raw medicine are provided by the research and development center of the sea li pharmaceutical industry group.
Drug configuration: the raw materials are dissolved by acetone firstly, then dissolved by 0.1% Tween 80 aqueous solution, and the required series of mass concentrations are set according to the activity of the medicament.
Preparation of sporangium suspension: selecting diseased cucumber leaves, eluting sporangium of disease leaf back downy mildew bacteria with sterile water at 4 ℃, preparing sporangium suspension (1×10 5～1×107 sporangium/mL), and storing at 4 ℃ for later use.
And (3) medicament treatment: and uniformly spraying the prepared liquid medicine on two sides of the cucumber leaf until the two sides are completely wetted, and after the liquid medicine is air-dried, keeping the cucumber leaf for later use, wherein the test is provided with a treatment without the medicine as a blank control.
Inoculating and culturing: after 24h of treatment with the agent, the fresh sporangia suspension was spray inoculated on the back of the leaf. Each treatment was 5 pots, 2 plants per pot. After inoculation, the culture is carried out under the conditions of continuous illumination/darkness for 12 hours alternately, the temperature is 17-22 ℃ and the relative humidity is more than 90 percent.
Experimental investigation:
The inoculated leaves were investigated in stages according to the onset of the blank. The following classification method is adopted:
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 6-10% of the area of the whole leaf;
5 stages: the area of the disease spots accounts for 11% -25% of the area of the whole leaf;
7 stages: the area of the disease spots accounts for 26% -50% of the area of the whole leaf;
stage 9: the area of the disease spots accounts for more than 50% 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 following formula, and the calculated result retains two decimal places.
The control effect is calculated according to the following formula:
And processing the data by adopting a probability value analysis method. And (3) analyzing by using an IBM SPSS STATISTICS statistical analysis system, solving a virulence regression line, EC 50 values and a correlation coefficient R 2, and evaluating the activity of the test agent on the biological test material.
The co-toxicity coefficient (CTC value) of the blend was calculated as follows:
wherein:
Ati—actual measured virulence index of the mixture;
S-EC 50 of standard agent in milligrams per liter (mg/L);
M-EC 50 of the mixture in milligrams per liter (mg/L).
TTI＝TIA*PA+TIB*PB
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.
The compound co-toxicity coefficient CTC is more than or equal to 120 and shows synergistic effect; ctc.ltoreq.80 shows antagonism; 80 < CTC < 120 shows additive effect.
The test results are shown in the following table:
TABLE 1 results of indoor Combined toxicity test of active ingredient A and active ingredient B compounded against downy mildew
As can be seen from Table 1, the active ingredient B (5-ethyl-6-octyl [1,2,4] triazol [1,5-a ] pyrimidin-7-amine) has higher toxicity to the cucumber downy mildew, EC 50 is 3.536mg/L, the weight ratio of the active ingredient A (compound of formula I) to the active ingredient B (5-ethyl-6-octyl [1,2,4] triazol [1,5-a ] pyrimidin-7-amine) is in the range of 38:1-1:38, and the co-toxicity coefficients are all greater than 120, which indicates that the active ingredient A and the active ingredient B show synergistic effect in the weight ratio range; when the weight ratio of the active ingredient A (a compound shown as the formula I) to the active ingredient B (5-ethyl-6-octyl [1,2,4] triazole [1,5-a ] pyrimidine-7-amine) is 15:1-1:26, the co-toxicity coefficients are all more than 150, which indicates that the synergistic effect of the two is prominent in the weight range; wherein, when the weight ratio of the active ingredient A to the active ingredient B is 1:1, the co-toxicity coefficient is 194.147, and the synergy is most remarkable.
Example 2: indoor combined toxicity test of active ingredient A (compound of formula I) and active ingredient B (5-ethyl-6-octyl [1,2,4] triazole [1,5-a ] pyrimidine-7-amine) on tomato late blight bacteria
The test is based on: test reference NY/T1156.13-2008 section 13 "pesticide indoor bioassay test criteria section 13: leaf method for inhibiting late blight bacteria; ny/T1156.6-2006 section 6 of pesticide indoor bioassay test criteria section 6: determination of the combined action of compounding.
Test target: the test pathogen is Phytophthora infestans (Phytophthora infestans).
Preparing a test material: and selecting a infected tomato pot plant, numbering for standby after seedlings grow to 2-4 true leaf periods.
Test agent: 98% of active ingredient A raw medicine and 98% of active ingredient B raw medicine are provided by the research and development center of the sea li pharmaceutical industry group.
Drug configuration: the raw materials are dissolved by acetone firstly, then dissolved by 0.1% Tween-80 aqueous solution, and the required series of mass concentrations are set according to the activity of the medicament.
Preparing zoospore suspension: moisturizing and culturing diseased tomato tissues, washing spores with sterile water after sporangia are generated, filtering with double-layer gauze to prepare sporangia suspension, placing at low temperature of 4 ℃ for 2.5 hours in the dark to release zoospores, and regulating the spore concentration to 1 multiplied by 10 5 spores/L for later use.
Inoculation and medicament treatment: spraying and inoculating zoospore suspension, uniformly spraying the liquid medicine on the back of the leaf after 24 hours of inoculation, naturally airing the liquid medicine, upwards treating the back of each leaf, and discharging the leaf into a moisturizing box according to treatment marks. 10 leaves were treated each, 4 replicates, and a treatment containing only solvent and surfactant and no active ingredient was used as a blank.
Culturing: after the medicament treatment, each treatment is alternated under continuous illumination/darkness for 12 hours every day, the temperature is (20+/-1) DEG C, a water film is kept on the leaf surface within 24 hours after inoculation, and the culture is carried out for 6-7 d under the condition that the relative humidity is kept above 90% after 24 hours.
Experimental investigation: and when the leaf disease rate of the blank control reaches more than 50%, the disease conditions of all treatments are investigated in a grading way.
Grading is performed according to the following grading standard:
Level 0: does not cause disease;
stage 1: only a small amount of small disease spots are arranged on the leaves, and the disease spots occupy less than 10% of the leaf area;
3 stages: the disease spots on the leaves occupy 10 to 25 percent of leaf area;
5 stages: the disease spots on the leaves account for 25% -50% of the leaf area;
7 stages: the disease spots on the leaves occupy more than 50 percent of the leaf area;
Stage 9: whole leaves withered.
Data statistics and analysis: and calculating the disease index and the prevention and treatment effect of each treatment according to the investigation data.
The calculation method comprises the following steps:
the disease index is calculated according to the following formula, and the calculated result retains two decimal places.
The control effect is calculated according to the following formula:
And processing the data by adopting a probability value analysis method. And (3) analyzing by using an IBM SPSS STATISTICS statistical analysis system, solving a virulence regression line, EC 50 values and a correlation coefficient R 2, and evaluating the activity of the test agent on the biological test material.
The co-toxicity coefficient (CTC value) of the blend was calculated as follows:
wherein:
Ati—actual measured virulence index of the mixture;
S-EC 50 of standard agent in milligrams per liter (mg/L);
M-EC 50 of the mixture in milligrams per liter (mg/L).
TTI＝TIA*PA+TIB*PB
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.
The compound co-toxicity coefficient CTC is more than or equal to 120 and shows synergistic effect; ctc.ltoreq.80 shows antagonism; 80 < CTC < 120 shows additive effect.
The test results are shown in the following table:
TABLE 2 results of indoor Combined toxicity test of tomato late blight pathogen by compounding active ingredient A with active ingredient B
As can be seen from Table 2, the active ingredient B (5-ethyl-6-octyl [1,2,4] triazol [1,5-a ] pyrimidin-7-amine) has higher toxicity to tomato late blight, EC 50 is 1.826mg/L, the weight ratio of active ingredient A (compound of formula I) to active ingredient B (5-ethyl-6-octyl [1,2,4] triazol [1,5-a ] pyrimidin-7-amine) is in the range of 35:1-1:15, and the co-toxicity coefficients are all greater than 120, indicating that both show synergistic effect in the weight ratio range; when the weight ratio of the active ingredient A (a compound shown as the formula I) to the active ingredient B (5-ethyl-6-octyl [1,2,4] triazole [1,5-a ] pyrimidine-7-amine) is 20:1-1:15, the co-toxicity coefficients are all more than 130, which indicates that the synergistic effect of the two is outstanding in the weight range; when the weight ratio of the active ingredient A to the active ingredient B is 6:1, the co-toxicity coefficient is 197.539, and the synergy is most remarkable.
And (3) field efficacy test:
Example 3: field efficacy test of the combination of active ingredient A (Compound of formula I) and active ingredient B (5-ethyl-6-octyl [1,2,4] triazole [1,5-a ] pyrimidine-7-amine) against Peronospora Cucumidis
The test is based on: the test is referred to GB/T17980.26-2000 "pesticide field test guidelines (one) for controlling cucumber downy mildew".
Test crop: cucumber (Bonai 13).
Test object: downy mildew (Pseudoperonospora cubensi).
Test site: in the village town greenhouse in the demonstration area of Yang Ling of Shaanxi, the soil of the test land is soil, and the cultivation management is of a medium and high level.
The test agents and the amounts of agents are shown in the following table:
cell arrangement: the cells are arranged according to random block, and repeated for 4 times, and the area of each cell is 20m 2.
The application method comprises the following steps: conventional spraying was performed using a 3WBD-16B electric sprayer, with 1 number of nozzles, in the shape of a hollow cone nozzle, and a flow rate of the sprayer at the time of application was 1 liter/min. The whole plant stem and leaf is uniformly sprayed until the front and back surfaces of the leaf are uniformly sprayed and the liquid medicine begins to drop, and the water consumption is 45 kg/mu (675 kg/hectare).
Time and frequency of application: the test was carried out for the first time on month 4 and 20 of 2020, at which point cucumber downy mildew occurred sporadically, once again at 7-day intervals, for a total of 2 administrations. Investigation of the onset was performed 7 days and 15 days after the last administration.
The investigation method comprises the following steps: 4 points are randomly taken from each cell to survey, two plants are surveyed at each point, and all the leaves are surveyed for 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.
The criteria for grading leaf onset are 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% -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 50% of the whole leaf area.
The drug effect calculation method comprises the following steps:
the disease index is calculated according to the following formula, and the calculated result retains two decimal places.
The control effect is calculated according to the following formula:
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Direct impact on crops: after each application, the cucumber in each agent treatment area is consistent with the control area. The test and control agents are shown to be safe for cucumber.
The test results are shown in the following table:
TABLE 3 results of field efficacy test of the combination of active ingredient A and active ingredient B on the cucumber downy mildew
As shown in the field efficacy test of Table 3, the active ingredient A (the compound of the formula I) and the active ingredient B (5-ethyl-6-octyl [1,2,4] triazole [1,5-a ] pyrimidine-7-amine) are mixed to show good control effect on cucumber downy mildew. The control effect is improved to different degrees under the condition that the dosage is reduced compared with a single dosage, wherein the control effect is best under the condition that the weight ratio of the active component A (a compound shown in the formula I) to the active component B (5-ethyl-6-octyl [1,2,4] triazole [1,5-a ] pyrimidine-7-amine) is 1:1.
Example 4: field efficacy test of active ingredient A (Compound of formula I) and active ingredient B (5-ethyl-6-octyl [1,2,4] triazole [1,5-a ] pyrimidine-7-amine) for tomato late blight
The test is based on: the test is referred to GB/T17980.31-2000 "pesticide field test rule Bactericide for controlling tomato early blight and late blight".
Test site: in the greenhouse of Gaoyi county in Shijia village of Hebei province, tomato late blight occurs in the past year, the water and fertilizer management of the test areas belongs to the middle-upper level, the soil fertility is medium, the conditions of soil, cultivation, water and fertilizer management and the like of each test area are consistent, and the agricultural practice of local science is met.
Test crop: tomato (Ji Dali).
Test object: phytophthora infestans (Phytophthora infestans).
The test agents and the amounts of agents are shown in the following table:
cell arrangement: the cells are arranged according to random block, and repeated for 4 times, and the area of each cell is 20m 2.
The application method comprises the following steps: when late blight happens sporadically, spraying medicine by using a 3WBD-16B electric sprayer, wherein the dosage is that the front and back sides of stems and leaves are wet and mist drops are present, and the dosage of the medicine liquid is 750L/hm 2.
Time and frequency of application: the test is carried out for the first time on the 3 month and 12 days in 2020, and then the medicine is carried out once every 7 days, namely, the medicine is respectively carried out on the 19 days of 3 months and the 26 days of 3 months, the medicine is carried out for 3 times, the medicine is carried out in clear weather, and no adverse weather influence exists in the whole test period.
Investigation time and number: 7d after the last application, the onset was investigated.
The investigation method comprises the following steps: each cell was sampled at random 5 points, each point being fixed-point for 2 plants. The lower, middle and upper leaves of each plant were examined and graded as a percentage of the lesion area on each leaf over the entire leaf area.
The criteria for grading leaf onset are 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% -50% of the whole leaf area;
Stage 9: the area of the disease spots accounts for more than 50% of the whole leaf area.
The drug effect calculation method comprises the following steps:
the disease index is calculated according to the following formula, and the calculated result retains two decimal places.
The control effect is calculated according to the following formula:
direct impact on crops: each dose treated area was observed to be consistent with the control area for tomatoes after each dose. The test and control agents are shown to be safe for tomato.
The test results are shown in the following table:
TABLE 4 results of field efficacy test of active ingredient A and active ingredient B in combination on tomato late blight
As shown in the field efficacy test of Table 4, the active ingredient A (the compound of the formula I) and the active ingredient B (5-ethyl-6-octyl [1,2,4] triazole [1,5-a ] pyrimidine-7-amine) are mixed to show good prevention and treatment effects on tomato late blight. 7 days after the last administration, the control effects of 20% of active ingredient A and active ingredient B water dispersible granules (1:3), 30% of active ingredient A and active ingredient B suspending agent (2:1) and 49% of active ingredient A and active ingredient B water dispersible granules (6:1) on tomato late blight are 86.47%, 88.54% and 91.83% respectively.
In conclusion, through indoor toxicity measurement and field efficacy tests, the active ingredient A (the compound shown in the formula I) and the active ingredient B (5-ethyl-6-octyl [1,2,4] triazole [1,5-a ] pyrimidine-7-amine) have good control effects on cucumber downy mildew, tomato late blight and the like, are safe to target crops, have obvious control effects, are superior to single agents in the aspects of delaying the generation of drug resistance and prolonging the lasting effect, can effectively reduce the cost and reduce the medicament residues.
The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention are intended to be included within the scope of the present invention.
Claims (12)
1. The pesticide composition is characterized by comprising an active ingredient A and an active ingredient B, wherein the active ingredient A is a compound shown in a formula I, and the structure of the compound shown in the formula I is as follows: (I); the component B is 5-ethyl-6-octyl [1,2,4] triazole [1,5-a ] pyrimidine-7-amine, and the mass ratio of the active component A to the active component B is 38:1-1:38.
2. The pesticide composition as set forth in claim 1, wherein the mass ratio of the active ingredient a to the active ingredient B is 35:1 to 1:15.
3. The pesticide composition as set forth in claim 2, wherein the mass ratio of the active ingredient a to the active ingredient B is 15:1 to 1:15.
4. The pesticide composition of claim 1, wherein the total weight of the pesticide composition is 0.1% -90% of the total weight of the pesticide composition based on 100% by weight of the total weight of the active ingredient a and the active ingredient B.
5. The pesticide composition of claim 4, wherein the total weight of the pesticide composition is 1% -70% of the total weight of the pesticide composition based on 100% by weight of the total weight of the active ingredient a and the active ingredient B.
6. A pesticide composition as set forth in claim 1, wherein said pesticide composition comprises agriculturally acceptable auxiliary ingredients in addition to the active ingredient, said auxiliary ingredients being selected from one or more of wetting agents, dispersants, thickeners, disintegrants, emulsifiers, defoamers, preservatives, stabilizers, synergists, carriers, solvents.
7. A pesticidal composition according to claim 1, which is formulated in any agriculturally acceptable formulation.
8. The composition of claim 7, wherein the formulation is any one of a solid formulation and a liquid formulation.
9. The composition of claim 8, wherein the solid formulation is a water dispersible granule or wettable powder and the liquid formulation is a suspension.
10. Use of a pesticidal composition as defined in any one of claims 1 to 9 for controlling agricultural, forestry or horticultural plant pathogenic bacteria.
11. The use according to claim 10, wherein the phytopathogenic bacteria are bacteria and/or fungi on cereals, vegetables, fruits, ornamental plants.
12. Use according to claim 10, wherein the pesticidal composition is applied to the phytopathogenic fungi and/or their environment or to the plants in an effective amount.
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