CN114521564A - Dispersible oil suspending agent containing prothioconazole and propiconazole, preparation method and application - Google Patents
Dispersible oil suspending agent containing prothioconazole and propiconazole, preparation method and application Download PDFInfo
- Publication number
- CN114521564A CN114521564A CN202210176176.7A CN202210176176A CN114521564A CN 114521564 A CN114521564 A CN 114521564A CN 202210176176 A CN202210176176 A CN 202210176176A CN 114521564 A CN114521564 A CN 114521564A
- Authority
- CN
- China
- Prior art keywords
- propiconazole
- prothioconazole
- dispersible oil
- wheat
- suspending agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000005822 Propiconazole Substances 0.000 title claims abstract description 270
- MNHVNIJQQRJYDH-UHFFFAOYSA-N 2-[2-(1-chlorocyclopropyl)-3-(2-chlorophenyl)-2-hydroxypropyl]-1,2-dihydro-1,2,4-triazole-3-thione Chemical compound N1=CNC(=S)N1CC(C1(Cl)CC1)(O)CC1=CC=CC=C1Cl MNHVNIJQQRJYDH-UHFFFAOYSA-N 0.000 title claims abstract description 185
- 239000005825 Prothioconazole Substances 0.000 title claims abstract description 185
- STJLVHWMYQXCPB-UHFFFAOYSA-N propiconazole Chemical compound O1C(CCC)COC1(C=1C(=CC(Cl)=CC=1)Cl)CN1N=CN=C1 STJLVHWMYQXCPB-UHFFFAOYSA-N 0.000 title claims abstract description 183
- 239000000375 suspending agent Substances 0.000 title claims abstract description 79
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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
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
-
- 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a dispersible oil suspending agent containing prothioconazole and propiconazole, a preparation method and application thereof. The dispersible oil suspending agent comprises 1-40% of prothioconazole, 1-40% of propiconazole, 3-12% of emulsifier, 2-8% of dispersant, 0.5-10% of thickener, 0.5-7% of stabilizer, 0.2-2% of antifreeze, 0.2-1% of defoamer and the balance of oil-based solvent. The prothioconazole and the propiconazole are combined and processed into the dispersible oil suspending agent, the preparation has stable performance, good adhesion and rain wash resistance, can better play the drug effect of pesticide components, is beneficial to mechanical application of flying defense and the like, expands the control spectrum, reduces the drug consumption and improves the effect, and is environment-friendly and safe.
Description
Technical Field
The invention relates to the technical field of bactericides, and in particular relates to a dispersible oil suspending agent containing prothioconazole and propiconazole, a preparation method and application thereof.
Background
Wheat scab (FHB) caused by Fusarium graminearum species complex poses serious hazards to both wheat and barley worldwide. Pathogenic bacteria can infect wheat seedlings, leaves, ears and other parts, so that the growth of wheat plants is inhibited or withered, particularly the ears are seriously damaged, and the yield loss and the quality of the wheat are reduced. In addition, many fusarium toxins are produced by pathogen infestation, including: deoxynivalenol (DON) and acetylated derivatives thereof, namely 3-acetyl-deoxynivalenol (3A-DON) and 15-acetyl deoxynivalenol (15A-DON), nivalenol (nivalenol) and T2 toxins, trichothecene toxins, fumonisin (fumonisin) and zearalenone (zearalenone), bring about the food safety problem threatening the life and health of human and animals.
The cultivation of a scab-resistant variety is the most economic and effective method for preventing and treating scab, but a wheat variety which is effective in scab resistance and excellent in agronomic characters is still lacked in the world, and chemical prevention and treatment are always main measures for preventing and treating scab harm and wheat seed toxin pollution. The DON pollution of wheat grains is closely related to the severity of gibberellic disease, and the DON is also the most common fusarium toxin in grains and products thereof all over the world, once entering the bodies of people or animals, the DON can cause chronic toxicity such as immune disorder, anorexia and weight loss and acute poisoning symptoms such as diarrhea, vomiting and fever, thereby seriously harming the health of the people or animals. In view of the current severe current situation of preventing and controlling gibberellic disease and wheat grain DON, the gibberellic disease prevention and control agent needs to be optimized urgently to guarantee the continuous and stable development of wheat production and food safety.
Wheat powdery mildew caused by Blumeria graminis (DC) Speer Erysiphe graminis DC.E. graminis DC.f. sp.tritici Marchal) of the Poaceae Blumeria graminis wheat specialization type mainly damages leaves, and in severe cases, leaf sheaths, stems and spikes are all infected. When the disease condition is mild, the mildew spots are distributed dispersedly, and gradually expand into pieces as the disease condition worsens, and finally cover the whole leaves; the lower and surrounding tissues of the lesion are faded, the diseased leaves are yellow and withered early, and if the disease affects the stem and leaf sheath, the whole plant can be fallen down; the plants are short, small and weak, the ears are small, the thousand kernel weight is obviously reduced, and the wheat yield is finally influenced. The method for preventing and treating wheat powdery mildew mainly takes agricultural prevention and chemical prevention as main components, and most of common chemical prevention and treatment agents are single agents or compound agents such as triadimefon, diniconazole and the like.
The wheat rust mainly comprises stem rust, leaf rust and stripe rust, wherein the three diseases can cause large yellow spots to appear at early stages of leaf stalks, leaf sheaths, leaves and the like of wheat, the yellow spots are connected into slices along with growth to form rust-colored powdery sores, namely the appearance of summer spore aggregation, and black spots appear at the positions when the diseases enter the later stage, namely the appearance of winter spore aggregation. When the wheat plants are rusted, the rust disease can be seriously influenced, not only can the photosynthesis be reduced, but also a large amount of water of the wheat plants can be lost, the plumpness and the filling of grains can be reduced, the wheat leaves can be premature, and the yield of the wheat can be seriously reduced. The control method of the wheat rust mainly takes agricultural control and chemical control as main parts, not only strictly monitors the occurrence information of diseases, but also achieves scientific planting and scientific medicament use.
The rice blast caused by Pyricularia oryzae (Phynicularia gisea) of fungi of deuteromycotina is one of serious diseases in rice areas in the world, the yield is reduced by 40-50% in the popular years, and even no grain is produced. At present, the prevention strategy of rice blast is mainly based on planting high-yield disease-resistant varieties, taking field cultivation management enhancement as a center, and assisting with proper and timely medicament prevention. Planting disease-resistant varieties is the most economic and effective strategy for preventing and treating rice blast, but due to the influence of factors such as pathogenicity variation of rice blast germs and the like, resistance of some disease-resistant varieties begins to be gradually lost after the rice blast germs are planted in fields for 3-5 years. In the field cultivation management aspect, some measures are mainly taken aiming at the disease condition of the rice blast, and the method has a certain effect on reducing the damage of the rice blast. The prevention and control of the pesticide is an important link in the strategy of preventing and controlling the rice blast all the time, and plays a very important role all the time. False smut caused by Ustilaginoidea virens is one of the main diseases of rice, is distributed in rice production areas in the world, generally has the morbidity of 3-5 percent, seriously reaches more than 30 percent, and has the yield reduction of 20-30 percent. At present, chemical agents are mainly used for preventing and treating false smut, and the varieties of the chemical agents for preventing and treating false smut on the market are few. Therefore, the development of new false smut prevention and treatment agents is also important for safe production of rice and grain safety.
Grape anthracnose (grapevine anthracnose) caused by glomeriella cingulata (Stonem.) Spauld et Schrenk is mainly generated on grape fruits and cob, and can also damage leaves, new tips, tendrils, fruit stalks and other parts, and the yield is reduced by over 40 percent when the damage is serious. Tea anthracnose, mainly caused by colletotrichumcalae Massee, is a worldwide disease, particularly occurring in warm and humid subtropical and tropical tea areas. The disease can affect the physiological metabolism of tea trees, and causes the reduction of the yield of the tea trees and the quality of the tea leaves. Tomato leaf mold (tomato leaf mould) caused by cladosporium fulvum (cook) ciferri mainly harms tomato leaves, and when serious, also harms stems, flowers and fruits, seriously affects photosynthesis and nutrient synthesis, and reduces tomato yield and quality. The mulberry sclerotiniose mainly infects new shoots and tender shoots of female flowers, Chinese olive and early mulberry, has great harm to mulberry, particularly mulberry for fruit, and seriously affects the yield and quality of mulberry. Therefore, the research and the application of the high-efficiency new medicament for the grape anthracnose, the tea tree anthracnose, the tomato leaf mold and the mulberry sclerotinia have important significance.
Plant protection unmanned aerial vehicle is owing to have the operating efficiency height, and the operation security is high, and water conservation economizes the medicine, and the environmental protection, artifical there is not the fungible, and plant protection flies to prevent and control market demand more and more in wheat disease pest and weed control to also have higher requirement to the formulation of medicament. Dispersible Oil suspension (OD) refers to a stable liquid-solid system with high Dispersion, high suspension and flow ability, in which one or more active ingredients of a pesticide (at least one of which is a solid original drug) are uniformly dispersed in an Oil phase by grinding with a sand mill with the help of some additives in a non-aqueous Dispersion medium. The dispersible oil suspending agent has the advantages of small particle size, high suspension rate, good dispersibility, good adhesiveness, good affinity to a target, safe and environment-friendly formulation, convenience for mechanical application and the like. Therefore, the dispersible oil suspending agent is a medicament dosage form which is relatively suitable for the current plant protection flying prevention.
Disclosure of Invention
The purpose of the invention is as follows: the invention provides a dispersible oil suspending agent containing prothioconazole and propiconazole, a preparation method and application thereof, aiming at the problems of new requirements of current environmental protection and rapid development of plant protection flying prevention on medicament dosage forms and prevention and control of wheat scab, wheat powdery mildew, wheat rust, wheat seed DON toxin, rice blast, false smut, grape anthracnose, tea tree anthracnose, tomato leaf mold, mulberry sclerotinia, and the like. The preparation can exert the effect of preventing and treating various diseases by using the medicament, has obvious prevention and treatment effect and synergy, effectively prevents and treats wheat scab, wheat powdery mildew, wheat rust, rice blast, false smut, grape anthracnose, tea tree anthracnose, tomato leaf mold and mulberry sclerotinia, can also effectively reduce the DON toxin pollution of wheat grains, reduces the medicament synergism, is convenient for the mechanical application of flying prevention and the like, and is environment-friendly and safe; the invention also aims to provide application of the dispersible oil suspending agent containing prothioconazole and propiconazole in preventing and treating wheat scab, wheat powdery mildew, wheat rust, wheat grain DON toxin, rice blast, false smut, grape anthracnose, tea tree anthracnose, tomato leaf mold and mulberry sclerotinia rot.
The technical scheme is as follows: the dispersible oil suspending agent containing prothioconazole and propiconazole comprises 1-40% of prothioconazole, 1-40% of propiconazole, 3-12% of emulsifier, 2-8% of dispersant, 0.5-10% of thickener, 0.5-7% of stabilizer, 0.2-2% of antifreeze, 0.2-1% of defoamer and the balance of oil-based solvent; the emulsifier is a mixture of polyoxyethylene ether, polyvinyl alcohol and sodium dodecyl benzene sulfonate; the dispersant is alkyl naphthalene sulfonate; the thickening agent is a mixture of fumed silica and xanthan gum; the oil-based solvent is a mixture consisting of soybean oil and methyl oleate; the antifreezing agent is ethylene glycol or propylene glycol; the defoaming agent is organic silicon.
In a preferred embodiment of the present invention, the mass ratio of the mixture of polyoxyethylene ether, polyvinyl alcohol and sodium dodecylbenzenesulfonate is 1-8: 2-6: 1-4.
In a preferred embodiment of the present invention, the stabilizer is any one or more of epoxidized soybean oil, epoxidized linseed oil, 1, 2-butanediol, isopropyl phosphate, and butyl epoxystearate.
In a preferred embodiment of the present invention, the percentage content of prothioconazole and propiconazole in the dispersible oil suspending agent is 10% to 50%.
In a preferred embodiment of the invention, the oil-based solvent is a mixture of soybean oil and methyl oleate in a mass ratio of 1: 4-8.
As a preferred embodiment of the invention, the dispersible oil suspension also comprises an auxiliary material validamycin a, and the dosage of the auxiliary material validamycin a is 0.05-0.2 times of the total mass of the prothioconazole and the propiconazole.
In a preferred embodiment of the present invention, the mass ratio of the mixture of the fumed silica and the xanthan gum is 2: 1.
In a preferred embodiment of the present invention, the mass ratio of prothioconazole and propiconazole is 1-15: 1-15.
Preferably, the mass ratio of the prothioconazole to the propiconazole is 1-5: 1-10.
The preparation method of the dispersible oil suspending agent containing prothioconazole and propiconazole comprises the following steps:
step (1): adding an emulsifier and a dispersant into an oil-based solvent in sequence, and mixing and dispersing uniformly;
step (2): stirring and adding prothioconazole and propiconazole crude oil under high-speed shearing;
and (3): adding a thickening agent and a defoaming agent, and stirring and mixing;
and (4): grinding under zirconium bead medium until the particle size is less than 4 μm;
and (5): and adding a stabilizer and an antifreezing agent, and discharging after the product is detected to be qualified to obtain a finished product.
Preferably, in the step (4), the grinding conditions of the sand mill are that the mass ratio of the zirconium beads to the grinding material is 1:1, and the rotating speed is 1500 rpm.
The dispersible oil suspending agent containing prothioconazole and propiconazole is applied to prevention and treatment of wheat scab, wheat powdery mildew, wheat rust, wheat kernel deoxynivalenol toxin, rice blast, false smut, grape anthracnose, tea tree anthracnose, tomato leaf mold and mulberry sclerotinia rot.
The application method comprises the following steps: diluting the dispersible oil suspending agent with water, and spraying stem leaves.
Prothioconazole (prothioconazole) is a novel broad-spectrum triazolethione bactericide, is mainly used for preventing and treating a plurality of diseases of cereals, wheat and bean crops and the like, has low toxicity, no teratogenicity and mutation type, no toxicity to embryos and long lasting period, and has broader-spectrum bactericidal activity to be safe to people and environment compared with triazole bactericides.
Propiconazole (propiconazole) belongs to triazole bactericides in sterol inhibitors, and has an action mechanism of influencing the biosynthesis of sterol, so that the cell membrane function of pathogenic bacteria is damaged, and finally cell death is caused, thereby achieving the effects of sterilizing, preventing and treating diseases. The systemic triazole fungicide with the double functions of protection and treatment can be absorbed by roots, stems and leaves, can be quickly conducted upwards in plant bodies, and can effectively prevent and treat various fungal diseases.
In addition, the dispersible oil suspension containing prothioconazole and propiconazole can also comprise an auxiliary material validamycin A, and the auxiliary material can obviously improve the prevention and control effect of the combined use of the prothioconazole and the propiconazole only by using a small amount, and particularly improves the prevention and control effect on wheat scab, wheat powdery mildew, wheat rust, wheat kernel DON toxin, rice blast, false smut, grape anthracnose, tea tree anthracnose, tomato leaf mold and mulberry sclerotinia.
Has the advantages that: (1) the dispersible oil suspending agent is matched with effective components, realizes efficacy synergism and is beneficial to mechanized application: the prothioconazole is beige powder which is not dissolved in water and oil phase, the propiconazole is faint yellow viscous liquid (liquid crude oil), the prothioconazole and the propiconazole are compounded into a dispersible oil suspending agent, the compounded dosage forms are extremely matched, the dosage forms have stable performance and good adhesiveness, are resistant to rain wash, can better play the efficacy of pesticide components, have obvious synergy, have no dust in the production and use processes, are environment-friendly and safe, and are directly diluted by water to be beneficial to mechanical application such as flying defense; (2) the dispersible oil suspending agent provided by the invention can enlarge the prevention and treatment objects, reduce the pesticide consumption and improve the effect: prothioconazole is a broad-spectrum triazolethione bactericide, propiconazole is a systemic triazole bactericide with dual functions of protection and treatment, can be absorbed by roots, stems and leaves, can be quickly conducted upwards in plant plants, is commonly used for preventing and treating diseases caused by ascomycetes, basidiomycetes and deuteromycetes, and a dispersible oil suspending agent containing prothioconazole and propiconazole can realize that a medicament can effectively prevent and treat wheat scab, wheat powdery mildew, wheat rust, wheat kernel DON toxin, rice blast, false smut, grape anthracnose, tea tree anthracnose, tomato leaf mold and mulberry sclerotinia rot, has remarkable synergism, can reduce the application times, reduce the usage amount of pesticides, and is environment-friendly and safe; (3) the dispersible oil suspending agent delays the generation and development of drug resistance: the dispersible oil suspending agent containing prothioconazole and propiconazole provided by the invention can effectively treat the drug resistance of various pathogenic bacteria, particularly the drug resistance of fusarium graminearum to carbendazim, prochloraz, phenamacril and other medicaments, can be used alternately with various conventional medicaments, and delays the development and spread of the drug resistance of the pathogenic bacteria to the conventional medicaments; meanwhile, the potential drug resistance of pathogenic bacteria to prothioconazole and propiconazole is reduced, the service life of the medicament is prolonged, and the medicament has important significance for comprehensive treatment of diseases; (4) the product of the invention is novel and has great popularization and application value: the dispersible oil suspending agent containing prothioconazole and propiconazole provided by the invention can effectively solve the problems in the prevention and treatment of wheat scab, wheat powdery mildew, wheat rust, wheat kernel DON toxin, rice blast, false smut, grape anthracnose, tea tree anthracnose, tomato leaf mold and mulberry sclerotinia, has the advantages of drug reduction, synergism and high popularization and application value, and has important significance in various aspects such as grain safety, food safety, sustainable, stable and healthy agricultural development and the like.
Detailed Description
The present invention is further illustrated by the following examples, which are intended to be purely exemplary and are not intended to limit the scope of the invention, as various equivalent modifications of the invention will occur to those skilled in the art upon reading the present disclosure and fall within the scope of the appended claims.
Firstly, indoor activity determination test.
The single and compound preparation of prothioconazole and propiconazole has the bacteriostatic activity on fusarium graminearum:
(1) test strains: fusarium graminearum (Fusarium graminearum) is isolated, identified and stored for later use in plant protection laboratories of the institute of agricultural science in Zhenjiang city in Jiangsu hilly area. The strain was stored on Potato Sucrose Agar (PSA) slants (4 ℃).
(2) Reagent to be tested: 95.2% (W/W) prothioconazole original drug, Shandong Hailier chemical Co., Ltd; 97% (W/W) propiconazole technical material, Limin chemical Limited liability company.
(3) The test method comprises the following steps: according to the 'pesticide bioassay test criterion NY/T1156.2-2006', a hypha growth rate method is adopted to carry out indoor toxicity determination of the single reagent and the compound agents with different proportions on the fusarium graminearum.
(4) And (3) data analysis: adopts a DPS13.0 professional version data processing system to calculate the regression equation and EC of the single medicament and the compound agents with different proportions for inhibiting the growth of fusarium graminearum hyphae50And its 95% confidence limit.
The synergy coefficient (SR) was calculated according to the Wadley method. Evaluation of the type of combined action of a mixture of agents according to the potentiating factor (SR), i.e. SR<0.5 is antagonistic action, 0.5-1.5 is additive action, SR is>1.5 is synergistic effect. SR ═ EC50(Eth)/EC50(Eob)，EC50(Eth)＝(a+b)/[(a/EC50A)+(b/EC50B)]. WhereinA, B are each single doses of the agent, a and b are the proportions of the respective single doses in the mixture, EC50(Eth) as a mixture EC50Theoretical value, EC50(Eob) is EC50The measured value.
(5) Results and analysis:
TABLE 1 measurement of prothioconazole, propiconazole and their mixture on the biological activity (toxicity) of fusarium graminearum
Note: in the table, the mass ratio of prothioconazole to propiconazole is given.
Indoor determination results show that the single dose of prothioconazole and propiconazole inhibits the growth of fusarium graminearum hyphae500.0413 and 0.0833 mug/mL respectively, and the inhibition activity of the prothioconazole on the growth of fusarium graminearum hyphae is higher than that of propiconazole. The prothioconazole and the propiconazole are compounded and combined according to the mixture ratio of 15:1, 10:1, 5:1, 1:5, 1:10 and 1:15 respectively to inhibit the growth of fusarium graminearum hyphae500.0253, 0.0272, 0.0295, 0.0240, 0.0272, 0.0259, and 0.0289 μ g/mL, respectively; the synergy coefficient (SR) of 7 compound combinations such as 15:1, 10:1, 5:1, 1:5, 1:10 and 1:15 to fusarium graminearum is 1.6838, 1.5919, 1.5288, 2.3000, 2.6176, 2.9459 and 2.7093 respectively, and all the coefficients are more than 1.5. This shows that the compound combination of prothioconazole and propiconazole respectively in the mixture ratio of 15:1, 10:1, 5:1, 1:5, 1:10 and 1:15 shows synergistic effect on fusarium graminearum (table 1).
By combining the bacteriostatic activity of the prothioconazole and the propiconazole, the disease control spectrum and the results of indoor ratio screening, the preferable mass ratio of the prothioconazole and the propiconazole to be compounded is preliminarily determined to be 1-15: 1-15.
Secondly, preparation of products
Example 1: preparation of 16% prothioconazole-propiconazole OD
The dispersible oil suspending agent comprises the following components in percentage by mass: 15% of prothioconazole, 1% of propiconazole, 4% of polyoxyethylene ether (emulsifier), 3% of polyvinyl alcohol (emulsifier), 2% of sodium dodecyl benzene sulfonate (emulsifier), 6% of sodium alkyl naphthalene sulfonate (dispersant), 5% of fumed silica (thickener), 2.5% of xanthan gum (thickener), 2% of epoxidized soybean oil (stabilizer), 3% of 1, 2-butanediol (stabilizer), 0.5% of ethylene glycol (anti-freezing agent), 0.5% of organic silicon (defoaming agent), and 100% of oil-based solvent supplement with the mass ratio of soybean oil to methyl oleate of 1: 8.
The preparation method comprises the following steps: the materials are prepared according to the proportion, and the 16 percent prothioconazole-propiconazole OD is prepared by the processing and preparation method of the dispersible oil suspending agent.
Example 2: preparation of 32% prothioconazole-propiconazole OD
The dispersible oil suspending agent comprises the following components in percentage by mass: 2% of prothioconazole, 30% of propiconazole, 3% of polyoxyethylene ether (emulsifier), 3% of polyvinyl alcohol (emulsifier), 1% of sodium dodecyl benzene sulfonate (emulsifier), 4% of sodium alkyl naphthalene sulfonate (dispersant), 4% of fumed silica (thickener), 2% of xanthan gum (thickener), 1% of epoxidized soybean oil (stabilizer), 3% of epoxidized butyl stearate (stabilizer), 0.2% of propylene glycol (anti-freezing agent), 0.6% of organic silicon (defoaming agent), and 100% of oil-based solvent supplement with the mass ratio of soybean oil to methyl oleate of 1: 7.
The preparation method comprises the following steps: preparing the materials according to the proportion and preparing the 32 percent prothioconazole-propiconazole OD by the processing and preparation method of the dispersible oil suspending agent.
Example 3: preparation of 22% prothioconazole-propiconazole OD
The dispersible oil suspending agent comprises the following components in percentage by mass: 2% of prothioconazole, 20% of propiconazole, 1% of polyoxyethylene ether (emulsifier), 3% of polyvinyl alcohol (emulsifier), 2% of sodium dodecyl benzene sulfonate (emulsifier), 5% of sodium alkyl naphthalene sulfonate (dispersant), 3% of fumed silica (thickener), 1.5% of xanthan gum (thickener), 3% of epoxy linseed oil (stabilizer), 2% of isopropyl phosphate (stabilizer), 2% of propylene glycol (anti-freezing agent), 1% of organic silicon (defoaming agent), and 100% of an oil-based solvent supplement with the mass ratio of soybean oil to methyl oleate of 1: 8.
The preparation method comprises the following steps: the materials are prepared according to the proportion, and 22 percent of prothioconazole-propiconazole OD is prepared by the processing and preparation method of the dispersible oil suspending agent.
Example 4: preparation of 48% prothioconazole-propiconazole OD
The dispersible oil suspending agent comprises the following components in percentage by mass: 40% of prothioconazole, 8% of propiconazole, 2% of polyoxyethylene ether (emulsifier), 3% of polyvinyl alcohol (emulsifier), 2% of sodium dodecyl benzene sulfonate (emulsifier), 6% of sodium alkyl naphthalene sulfonate (dispersant), 4% of fumed silica (thickener), 2% of xanthan gum (thickener), 2% of epoxy linseed oil (stabilizer), 3% of 1, 2-butanediol (stabilizer), 0.7% of propylene glycol (anti-freezing agent), 0.6% of organic silicon (defoaming agent), and 100% of oil-based solvent supplement with the mass ratio of soybean oil to methyl oleate of 1: 3.
The preparation method comprises the following steps: the materials are prepared according to the proportion, and the 48 percent prothioconazole-propiconazole OD is prepared by the processing and preparation method of the dispersible oil suspending agent.
Example 5: preparation of 33% prothioconazole-propiconazole OD
The dispersible oil suspending agent comprises the following components in percentage by mass: 30% of prothioconazole, 3% of propiconazole, 3% of polyoxyethylene ether (emulsifier), 3% of polyvinyl alcohol (emulsifier), 6% of sodium dodecyl benzene sulfonate (emulsifier), 5% of sodium alkyl naphthalene sulfonate (dispersant), 6% of fumed silica (thickener), 3% of xanthan gum (thickener), 2% of 1, 2-butanediol (stabilizer), 2% of isopropyl phosphate (stabilizer), 0.6% of propylene glycol (anti-freezing agent), 0.9% of organic silicon (defoaming agent), and 100% of oil-based solvent supplement with the mass ratio of soybean oil to methyl oleate of 1: 6.
The preparation method comprises the following steps: preparing materials according to the mixture ratio, and preparing 33% prothioconazole-propiconazole OD by the processing and preparation method of the dispersible oil suspending agent.
Example 6: preparation of 36% prothioconazole-propiconazole OD
The dispersible oil suspending agent comprises the following components in percentage by mass: 6% of prothioconazole, 30% of propiconazole, 2% of polyoxyethylene ether (emulsifier), 2% of polyvinyl alcohol (emulsifier), 4% of sodium dodecyl benzene sulfonate (emulsifier), 7% of sodium alkyl naphthalene sulfonate (dispersant), 4% of fumed silica (thickener), 2% of xanthan gum (thickener), 1% of 1, 2-butanediol (stabilizer), 4% of butyl epoxystearate (stabilizer), 1.2% of propylene glycol (anti-freezing agent), 0.6% of organic silicon (defoaming agent), and 100% of oil-based solvent supplement with the mass ratio of soybean oil to methyl oleate of 1: 4.
The preparation method comprises the following steps: preparing materials according to the proportion and preparing the 36 percent prothioconazole-propiconazole OD by the processing and preparation method of the dispersible oil suspending agent.
Example 7: preparation of 40% prothioconazole-propiconazole OD
The dispersible oil suspending agent comprises the following components in percentage by mass: 20% of prothioconazole, 20% of propiconazole, 4% of polyoxyethylene ether (emulsifier), 3% of polyvinyl alcohol (emulsifier), 3% of sodium dodecyl benzene sulfonate (emulsifier), 5% of sodium alkyl naphthalene sulfonate (dispersant), 5% of fumed silica (thickener), 2.5% of xanthan gum (thickener), 2% of isopropyl phosphate (stabilizer), 3% of butyl epoxystearate (stabilizer), 1% of ethylene glycol (anti-freezing agent), 1% of organic silicon (defoaming agent), and 100% of an oil-based solvent with the mass ratio of soybean oil to methyl oleate of 1: 6.
The preparation method comprises the following steps: preparing materials according to the proportion and preparing the 40 percent prothioconazole-propiconazole OD by the processing and preparation method of the dispersible oil suspending agent.
Example 8: preparation of 45% prothioconazole-propiconazole OD
The dispersible oil suspending agent comprises the following components in percentage by mass: 15% of prothioconazole, 30% of propiconazole, 2% of polyoxyethylene ether (emulsifier), 6% of polyvinyl alcohol (emulsifier), 2% of sodium dodecyl benzene sulfonate (emulsifier), 8% of sodium alkyl naphthalene sulfonate (dispersant), 3% of fumed silica (thickener), 1.5% of xanthan gum (thickener), 5% of epoxidized soybean oil (stabilizer), 0.9% of ethylene glycol (anti-freezing agent), 0.8% of organic silicon (defoaming agent), and 100% of an oil-based solvent with the mass ratio of soybean oil to methyl oleate of 1: 4.
The preparation method comprises the following steps: the materials are prepared according to the proportion, and the 45 percent prothioconazole-propiconazole OD is prepared by the processing and preparation method of the dispersible oil suspending agent.
Example 9: preparation of 30% prothioconazole-propiconazole OD
The dispersible oil suspending agent comprises the following components in percentage by mass: 20% of prothioconazole, 10% of propiconazole, 8% of polyoxyethylene ether (emulsifier), 2% of polyvinyl alcohol (emulsifier), 2% of sodium dodecyl benzene sulfonate (emulsifier), 6% of sodium alkyl naphthalene sulfonate (dispersant), 4% of fumed silica (thickener), 2% of xanthan gum (thickener), 6% of epoxy linseed oil (stabilizer), 0.5% of glycol (antifreeze), 0.6% of organic silicon (defoamer), and 100% of an oil-based solvent with the mass ratio of soybean oil to methyl oleate of 1: 5.
The preparation method comprises the following steps: the materials are prepared according to the proportion, and 30 percent of prothioconazole-propiconazole OD is prepared by the processing and preparation method of the dispersible oil suspending agent.
Example 10: preparation of 40% prothioconazole-propiconazole OD
Substantially the same as example 7 except that 2% validamycin a (0.05 times of the total mass of prothioconazole and propiconazole) was added during the preparation process.
Example 11: preparation of 40% prothioconazole-propiconazole OD
Substantially the same as example 7 except that 4% of validamycin a (0.1 times of the total mass of prothioconazole and propiconazole) was added during the preparation process.
Example 12: preparation of 30% prothioconazole-propiconazole OD
Substantially the same as in example 9, except that 6% of validamycin a (0.2 times the total mass of prothioconazole and propiconazole) was added during the preparation process.
Preparation example 13: preparation of 40% prothioconazole propiconazole Wettable Powder (WP):
the wettable powder comprises the following components in percentage by mass: 20% of prothioconazole, 20% of propiconazole, 5% of sodium carboxymethylcellulose (dispersing agent), 4% of nekal (wetting agent), 2% of penetrating agent T (penetrating agent), 1% of calcium carbonate (stabilizing agent) and kaolin (filler) for the balance.
The preparation method comprises the following steps: the materials are prepared according to the proportion and the 40 percent prothioconazole-propiconazole WP is prepared by a conventional wettable powder processing and preparation method.
Preparation example 14: preparation of 40% prothioconazole-propiconazole Suspension Concentrate (SC):
the suspending agent comprises the following components in percentage by mass: 20% of prothioconazole, 20% of propiconazole, 5% of sodium lignosulfonate (dispersant), 5% of alkyl naphthalene sulfonate (wetting agent), 0.1% of polyvinyl alcohol (thickener), 0.1% of ethylene glycol (antifreeze), 0.01% of organic silicon (defoamer), and the balance of water.
The preparation method comprises the following steps: preparing materials according to the mixture ratio and preparing 40 percent prothioconazole-propiconazole SC by a conventional suspending agent processing and preparing method.
Preparation example 15: preparation of 40% prothioconazole-propiconazole water dispersible granule (WG).
The weight percentage of each component is as follows: 20% of prothioconazole, 20% of propiconazole, 3% of sodium dodecyl benzene sulfonate (wetting agent), 4% of dispersant NNO (dispersant), 2.5% of polyvinylpyrrolidone (disintegrant), 5% of xanthan gum (binder) and diatomite (filler) to make up the balance.
The preparation method comprises the following steps: preparing materials according to the proportion and preparing the 40 percent prothioconazole-propiconazole WG by a conventional water dispersible granule processing and preparing method.
Third, field drug effect test
Field efficacy example 1: the dispersible oil suspending agent containing prothioconazole and propiconazole is used for field control experiments on wheat scab, powdery mildew, rust disease and wheat grain DON toxin.
The dispersible oil suspension containing prothioconazole and propiconazole in preparation examples 1 to 9 respectively takes prothioconazole OD (Anhui Jiuyi agriculture GmbH), 250g/L propiconazole Emulsifiable Concentrate (EC) (Michengda Switzerland crop protection GmbH) and 50% carbendazim WP (Jiangsu Lanfeng Biochemical industry GmbH) as control agents to develop field efficacy tests for preventing and treating wheat scab, powdery mildew, rust disease and wheat grain DON toxin.
The test treatment method comprises the following steps: from 10 months to 6 months in 2021 in 2020, Zhenjiang in Jiangsu hilly areaThe agricultural science and research institute agricultural science and technology innovation center test field (119.304 DEG E, 31.964 DEG N, altitude 21m) carries out the field prevention and control test of 12 medicaments on wheat scab, powdery mildew, rust disease and wheat grain DON toxin. The test field soil is Sichuan horse liver soil, the organic matter content is medium, and the tested wheat variety is Zhenmai No. 12'. In recent years, scab, powdery mildew and rust of wheat in test fields occur to different degrees, and fertilizer water and worm grass are managed according to the convention in the growth period of wheat. The experiment was performed with 13 treatments, which were: preparation examples 1 to 9, the treatment dose of the medicament was set to 180g/hm for the effective administration dose of prothioconazole and propiconazole2(the total effective application dose of the field of the sterilization main effective components of the prothioconazole and the propiconazole is 180g/hm2Calculated), the treatment doses of 30% prothioconazole OD and 250g/L propiconazole EC are both provided with an effective administration dose of 180g/hm2The treatment dosage of 50 percent carbendazim WP is also set as the effective application dosage of 750g/hm2(recommended product dosage) and spraying equal amount of clear water as control, each treatment is repeated for 3 times, and the total number of the treatment is 39 cells, and the area of each cell is 30m2The cells are provided with protection rows and are randomly arranged in blocks. The application is carried out for 2 times at intervals of 7d, when wheat is about 10% raised (4 months and 15 days 2021), the WBD-16 type electric sprayer manufactured by Zhengzhou Ludi agricultural machinery Co., Ltd is used for the 1 st uniform spraying application. The liquid spraying amount is 600L/hm2And spraying equal amount of clear water in the control treatment area, and not spraying any other medicament after the application until the test is finished.
The method for investigating and calculating the pesticide effect of wheat scab comprises the following steps: after the occurrence of head blight stabilized (5 months and 14 days 2021), the onset of head blight was investigated, and 500 ears were investigated for each treatment by sampling five diagonal lines. The grading standard of the severity of the ear of disease is as follows: the disease grade 1 spikelets account for less than 25% of the total spike, the disease grade 2 spikelets account for 25% -50% of the total spike, the disease grade 3 spikelets account for 50% -75% of the total spike, and the disease grade 4 spikelets account for more than 75% of the total spike. The disease index and the prevention and treatment effect are respectively calculated by the following formulas: disease index [ Σ (number of ears at each stage × corresponding disease-level numerical value)/total number of ears investigated × highest-level representative value ] × 100; the control effect is [ (control disease index-treatment disease index)/control disease index ] × 100%.
The method for investigating and calculating the drug effect of wheat powdery mildew comprises the following steps: sampling is carried out at five points on the diagonal line of each cell, all plants in 1 square ruler are investigated at each point, and flag leaves and the first leaves below the flag leaves are investigated by each plant. The number and severity of the diseased leaves were investigated and documented. Severity was graded as 7: the area of the 1-grade scab accounts for less than 1% of the whole leaf, the area of the 2-grade scab accounts for 2% -5% of the whole leaf, the area of the 3-grade scab accounts for 6% -l 0% of the whole leaf, the area of the 4-grade scab accounts for l 1% -30% of the whole leaf, the area of the 5-grade scab accounts for 3% -60% of the whole leaf, the area of the 6-grade scab accounts for 61% -80% of the whole leaf, and the area of the 7-grade scab accounts for more than 81% of the whole leaf. The disease index and the prevention and treatment effect are respectively calculated by the following formulas: disease index [ Σ (number of diseased leaves at each level × corresponding disease level value)/total number of investigated leaves × highest representative value ] × 100; the prevention and treatment effect is [ (control disease index-treatment disease index)/control disease index ] × 100%.
The wheat rust disease drug effect investigation and calculation method comprises the following steps: sampling is carried out at five points on the diagonal line of each cell, all plants in 1 square ruler are investigated at each point, and flag leaves and the first leaves below the flag leaves are investigated by each plant. The number and severity of the diseased leaves were investigated and documented. Severity was graded as 6: the area of the grade 1 lesion spots is less than 5% of the whole leaf, the area of the grade 2 lesion spots is less than 10% of the whole leaf, the area of the grade 3 lesion spots is less than 25% of the whole leaf, the area of the grade 4 lesion spots is less than 40% of the whole leaf, the area of the grade 5 lesion spots is less than 65% of the whole leaf, and the area of the grade 6 lesion spots is more than 65% of the whole leaf. The disease index and the prevention and treatment effect are respectively calculated by the following formulas: disease index [ Σ (number of diseased leaves at each level × corresponding disease level value)/total number of investigated leaves × highest representative value ] × 100; the control effect is [ (control disease index-treatment disease index)/control disease index ] × 100%.
The field control effect investigation and calculation method of the wheat grain DON toxin comprises the following steps: after wheat maturity (6 months and 1 day 2021), all treated diagonal five-point samples were taken from each cell, 0.25m per point2After all wheat ears are manually threshed, dried in the sun and uniformly mixed, crushing each processed grain sample by using a high-speed crusher, sieving the crushed grain sample by using a 20-mesh sieve, strictly cleaning the crushed grain sample to avoid mutual pollution, and collecting each processed sample powder to perform DON toxin detection. Slightly improving liquid chromatography-tandem mass spectrometry (LC-MS) to detect DON toxin in sample powder, weighing 5g of sample powder, placing in a 50mL centrifuge tube, adding 25mL 84% acetonitrile solution (extractive solution), placing on a shaker at 140r/min, shaking for 30min, 300 r/minCentrifuging at 0r/min for 5min, collecting supernatant, filtering with graphitized carbon column, drying the collected solution with nitrogen, redissolving with 1mL 10% methanol, filtering with 0.22 μm microporous membrane, and detecting. The LC-MS detection conditions are as follows: agilent model 1290 UPLC system, column: agilent C18 column (column length 100mm, column inner diameter 2.1mm, packing particle diameter 1.7 μm), column temperature: 40 ℃; sample introduction amount: 2 mu L of the solution; flow rate: 0.2 mL/min; mobile phase: a (5mmol/L ammonium acetate aqueous solution), B (10% methanol); gradient elution: 90% of A-10% of B (0-1 min), 10% of A-90% of B (4-5 min), 10% of A-90% of B (6min), and 90% of A-10% of B (6-10 min). AB Sciex 4500 mass spectrum, ionization mode: electrospray ionization mode (ESI); mass spectrum scanning mode: multiple reaction monitoring mode (MRM); ion source temperature: 500 ℃; residence time: 100 ms; atomizing: 50 psi; auxiliary gas: 50 psi; air curtain air: 35 psi; spraying voltage: 5500V (ESI +); collision cell emission voltage: 6V (ESI +); DON, 3-ADON and 15-ADON parent ions are 297.2, 339 and 339Da respectively, and DON, 3-ADON and 15-ADON quanta ions are 249, 231 and 137Da respectively.
The content of the DON toxin is expressed by the total amount of the DON toxin/dry weight of the sample powder (mu g/dry weight of the powder), and the control effect of different bactericides on the DON toxin of the wheat grains is calculated. Control DON toxin control effect (control DON toxin content-treated DON toxin content)/control DON toxin content × 100%.
The test results show that the effective dose (180 g/hm) is applied in the same way2) In the following examples 1-9, the field control effect of the dispersible oil suspension containing prothioconazole and propiconazole on wheat scab, powdery mildew, rust disease and wheat grain DON toxin is higher than that of a control medicament, namely 30% prothioconazole OD and 250g/L propiconazole EC, and the difference is obvious; and is significantly better than the control agent 50% carbendazim WP at the recommended dose (table 2).
The results show that the dispersible oil suspension containing prothioconazole and propiconazole has excellent field control effect on wheat scab, powdery mildew, rust disease and seed DON toxin, can exert multiple effects of applying one medicament to efficiently control wheat scab, powdery mildew, rust disease and seed DON toxin, and has obvious synergistic effect compared with a single agent after the sterilization effect is compounded according to a preferable proportion. Therefore, the dispersible oil suspending agent containing prothioconazole and propiconazole has the advantages of reducing drug efficacy, delaying the generation of disease drug resistance, and has important significance for the comprehensive control of wheat scab, powdery mildew, rust disease and seed DON toxin.
TABLE 2 field control of wheat scab, powdery mildew, rust and grain DON toxin by the agents prepared in the examples of the present invention
Note that the treatment doses of preparation examples 1-9 were given as effective doses of prothioconazole and propiconazole and were 180g/hm2(ii) a The data in the same column is marked with different lower case letters to indicate that the difference is significant (P)<0.05)。
Field efficacy example 2: the difference from the field efficacy example 1 is that the dispersible oil suspension containing prothioconazole and propiconazole of the invention is the agents obtained in examples 7, 10 and 11, the differences of field control effect on wheat scab, powdery mildew, rust disease and seed DON toxin after the auxiliary material validamycin A is added are examined, and the results are as follows:
the test result shows that 40 percent of prothioconazole-propiconazole OD300g/hm2The field control effect on wheat scab, powdery mildew, rust disease and seed DON toxin is 82.76%, 83.06%, 84.93% and 80.18% respectively; after 2% validamycin A (0.05 times of the total mass of the prothioconazole and the propiconazole) is added, 40% prothioconazole-propiconazole OD300g/hm2The field control effects on wheat scab, powdery mildew, rust disease and seed DON toxin are 86.06%, 84.70%, 85.96% and 84.39% respectively, and the control effect difference is obvious before and after 2% validamycin A is added; after 4 percent of validamycin A (0.1 time of the total mass of the prothioconazole and the propiconazole) is added, 40 percent of prothioconazole-propiconazole OD300g/hm2The field control effect on wheat scab, powdery mildew, rust disease and seed DON toxin is 86.93 percent, 86.61 percent respectively,86.79 percent and 89.12 percent, and the difference of the control effect is obvious before and after adding 4 percent validamycin A. 40% Prothioconazole-propiconazole OD600g/hm2The field control effect on wheat scab, powdery mildew, rust disease and seed DON toxin is respectively 94.11%, 91.26%, 90.92% and 87.89%; after 2% validamycin A (0.05 times of the total mass of the prothioconazole and the propiconazole) is added, 40% prothioconazole-propiconazole OD600g/hm2The field control effects on wheat scab, powdery mildew, rust and grain DON toxin are respectively 95.83%, 92.35%, 91.85% and 95.79%, and the control effect difference is obvious before and after 2% validamycin A is added; after 4 percent of validamycin A (0.1 time of the total mass of the prothioconazole and the propiconazole) is added, 40 percent of prothioconazole-propiconazole OD600g/hm2The field control effects on wheat scab, powdery mildew, rust disease and seed DON toxin are 96.84%, 93.99%, 92.57% and 97.19% respectively, and the control effect difference is obvious before and after 4% validamycin A is added (Table 3).
The result shows that the test agent combination has obvious synergistic effect on the field control effect of wheat scab, powdery mildew, rust disease and grain DON toxin, especially on the field control effect of the wheat grain DON toxin after the auxiliary material validamycin A is added into the dispersible oil suspending agent containing prothioconazole and propiconazole.
TABLE 340% field control of prothioconazole propiconazole OD on wheat scab, powdery mildew, rust and grain DON toxin (comparison of efficacy after addition of Validamycin A)
Note: the data in the same column followed by different lower case letters indicated significant differences (P < 0.05).
Field efficacy example 3: the same field efficacy example 1, except that the dispersible oil suspension containing prothioconazole and propiconazole of the present invention is used as the preparation example 7, and 40% prothioconazole-propiconazole WP, 40% prothioconazole-propiconazole SC and 40% prothioconazole-propiconazole WG prepared in the preparation examples 13-15, and the differences of different formulation formulations of prothioconazole and propiconazole on wheat scab, powdery mildew, rust disease and grain DON toxin in field are examined, and the results are as follows:
the test result shows that 40 percent of prothioconazole-propiconazole OD300g/hm2The field control effect on wheat scab, powdery mildew, rust disease and seed DON toxin is 81.27%, 82.42%, 83.13% and 77.13% respectively; 40% prothioconazole-propiconazole WP 300g/hm2The field control effects on wheat scab, powdery mildew, rust and DON toxin of grains are 76.15%, 74.64%, 79.11% and 74.43% respectively; 40% prothioconazole-propiconazole SC 300g/hm2The field control effect on wheat scab, powdery mildew, rust disease and seed DON toxin is 79.15%, 76.08%, 79.98% and 74.64% respectively; 40% prothioconazole-propiconazole WG 300g/hm2The field control effect on wheat scab, powdery mildew, rust disease and seed DON toxin is 78.45%, 76.37%, 80.09% and 74.84% respectively (Table 4).
The results show that after the prothioconazole and the propiconazole are compounded, the dispersible oil suspending agent prepared when the effective components and the contents thereof are the same has better control effect on wheat scab, powdery mildew, rust disease and seed DON toxin than wettable powder, suspending agent and water dispersible granules. The reason for this is probably that the prothioconazole is off-white powder which is not dissolved in water and oil phase, and the propiconazole is faint yellow viscous liquid (liquid crude oil), so that the dispersible oil suspending agent is prepared by compounding, the compound formulation is more matched, and the drug effect can be better exerted.
TABLE 4 field control of different combinations of prothioconazole and propiconazole on scab, powdery mildew, rust disease and DON toxin in grains of wheat
Note: the data in the same column are marked with different lower case letters indicating significant differences (P < 0.05).
Field efficacy example 4: the dispersible oil suspending agent containing prothioconazole and propiconazole is used for field control experiments on rice blast and false smut.
The dispersible oil suspensions containing prothioconazole and propiconazole of preparation examples 1 to 9 were subjected to field efficacy tests for controlling rice blast and false smut using 30% prothioconazole OD (amhui-yi agriculture division ltd) and 250g/L propiconazole EC (swozhou zihengda crop protection ltd) as control agents, respectively.
The test treatment method comprises the following steps: in the period from 5 months to 11 months in 2021, 11 kinds of field prevention and control tests of the pesticide on rice blast and false smut are carried out in experimental fields (119.304 degrees E, 31.964 degrees N, altitude 21m) of agricultural science and technology innovation center of Zhenjiang agricultural science research institute in Jiangsu hilly area. The test field soil is Sichuan horse liver soil, the organic matter content is medium, and the tested rice variety is Zhendao No. 18. In recent years, the rice blast and false smut of test fields occur in different degrees, and the rich water and the worm grass damage are managed according to the routine in the rice growth period. The experiment was performed with 12 treatments, which were: preparation examples 1 to 9, the treatment doses of the agents were set to be 150g/hm for the effective administration of prothioconazole and propiconazole2(the total effective application dose of the field of the sterilization main effective components of the prothioconazole and the propiconazole is 150g/hm2Calculated), the treatment doses of 30% prothioconazole OD and 250g/L propiconazole EC are also respectively provided with an effective administration dose of 150g/hm2Spraying equal amount of clear water as control, repeating each treatment for 3 times, and obtaining 36 cells with area of 30m2The cells are provided with protection rows and are randomly arranged in blocks. The WBD-16 electric sprayer produced by Zhengzhou Ludi agricultural machinery Co., Ltd is used for uniformly spraying for the first time 2 times at intervals of 7d and 5-7 d before the opening of the rice (8 months and 26 days in 2021). The liquid spraying amount is 600L/hm2And spraying equal amount of clear water in the control treatment area, and not spraying any other medicament after the application until the test is finished.
The rice blast pesticide effect investigation and calculation method comprises the following steps: at 30d (10 months and 2 days in 2021), the incidence of the rice panicle plague is investigated by a parallel skip sampling method, 20 holes are investigated in each cell, and the disease index and the prevention and treatment effect are calculated. The grading standard of the severity of the rice blast is as follows: grade 1, the disease is caused by individual branches and stalks, and the loss of each ear is less than 5%; grade 2, 1/3 branches and stalks are attacked, and the loss of each ear is about 20%; grade 3, the neck or main axis of the ear is attacked, the grains are half full, and the loss of each ear is about 50 percent; grade 4, the neck of the spike is attacked, the number of grains is too small, and the loss of each spike is about 70%; grade 5, the neck of the ear develops into white ear, and the loss of each ear is about 90%. The disease index and the prevention and treatment effect are respectively calculated by the following formulas: disease index [ Σ (number of ears at each stage × corresponding disease-level numerical value)/total number of ears investigated × highest-level representative value ] × 100; the prevention and treatment effect is [ (control disease index-treatment disease index)/control disease index ] × 100%.
The rice false smut drug effect investigation and calculation method comprises the following steps: in the rice wax ripeness stage (10 months and 18 days in 2021), the incidence of the rice panicle plague is investigated by a parallel skip sampling method, 20 holes are investigated in each cell, and the disease index and the prevention and treatment effect are calculated. The severity grading standard of false smut is as follows: 1 grade, each ear has 1 diseased grain; 2-grade, each ear has 2-4 diseased grains; 5-7 diseased grains are arranged on each ear of 3 grades; 4-grade, each ear has 8-10 diseased grains; grade 5, more than 10 diseased grains are in each ear. The disease index and the prevention and treatment effect are respectively calculated by the following formulas: disease index [ Σ (number of ears at each stage × corresponding disease-level numerical value)/total number of ears investigated × highest-level representative value ] × 100; the prevention and treatment effect is [ (control disease index-treatment disease index)/control disease index ] × 100%.
The test results show that the effective dose (150 g/hm) is applied in the same way2) In the following, examples 1 to 9, the dispersible oil suspension containing prothioconazole and propiconazole exhibited field control effects on rice blast and false smut that were both higher than those of the control agents, namely 30% prothioconazole OD and 250g/L propiconazole EC, and were significantly different (table 5).
The dispersible oil suspending agent containing prothioconazole and propiconazole has excellent field control effect on rice blast and false smut, can exert multiple effects of efficiently preventing and controlling the rice blast and the false smut by applying one medicament, and has obvious synergistic effect compared with a single agent after being compounded in an optimal proportion. Therefore, the dispersible oil suspending agent containing prothioconazole and propiconazole has the advantages of reducing pesticide and improving efficiency and has important significance for comprehensive prevention and control of rice diseases.
TABLE 5 field control of rice blast and false smut with the agents prepared in the examples of the present invention
Note that the treatment doses of preparation examples 1-9 were in the range of 150g/hm of the sum of the effective doses of prothioconazole and propiconazole for administration2(ii) a The data in the same column is marked with different lower case letters to indicate that the difference is significant (P)<0.05)。
Field efficacy example 5: the difference from the field efficacy example 4 is that the dispersible oil suspension containing prothioconazole and propiconazole of the invention is the agents obtained in examples 7, 10 and 11, the difference of field control effect on rice blast and false smut after the addition of the auxiliary material validamycin A is examined, and the results are as follows:
the test result shows that 40 percent of prothioconazole-propiconazole OD 225g/hm2The field control effect on rice blast and false smut is 83.00 percent and 81.59 percent respectively; after 2% validamycin A (0.05 times of the total mass of the prothioconazole and the propiconazole) is added, 40% prothioconazole-propiconazole OD 225g/hm2The field control effect on rice blast and false smut is 85.68 percent and 85.40 percent respectively, and the control effect difference is obvious before and after 2 percent validamycin A is added; after 4 percent of validamycin A (0.1 time of the total mass of the prothioconazole and the propiconazole) is added, 40 percent of prothioconazole-propiconazole OD 225g/hm2The field control effect on rice blast and false smut is 88.03% and 87.62% respectively, and the control effect difference is obvious before and after 4% validamycin A is added. 40% Prothioconazole-propiconazole OD300g/hm2The field control effect on rice blast and false smut is 86.91 percent and 85.08 percent respectively; after 2% validamycin A (0.05 times of the total mass of prothioconazole and propiconazole) is added, 40% prothioconazole-propiconazole OD300g/hm2The field control effect on rice blast and false smut is 89.71 percent respectively88.25%, and the difference of the control effect is obvious before and after the 2% validamycin A is added; after 4 percent of validamycin A (0.1 time of the total mass of the prothioconazole and the propiconazole) is added, 40 percent of prothioconazole-propiconazole OD300g/hm2The field control effect on rice blast and false smut is 91.28% and 90.16% respectively, and the control effect difference is obvious before and after 4% validamycin A is added (Table 6).
The result shows that the test agent combination has obvious synergistic effect on the field control effect of rice blast and false smut after the auxiliary material validamycin A is added into the dispersible oil suspending agent containing prothioconazole and propiconazole.
TABLE 640% field control of prothioconazole propiconazole OD against Rice blast and false smut (comparison of efficacy after addition of Validamycin A)
Note: the data in the same column are marked with different lower case letters indicating significant differences (P < 0.05).
Field efficacy example 6: the same field efficacy example 4, except that the dispersible oil suspension containing prothioconazole and propiconazole of the present invention was used as the preparation example 7, and 40% prothioconazole-propiconazole WP, 40% prothioconazole-propiconazole SC and 40% prothioconazole-propiconazole WG prepared in the preparation examples 13 to 15, and the differences in field control effects of different formulation formulations of prothioconazole and propiconazole on rice blast and false smut were examined, the results were as follows:
the test result shows that 40 percent of prothioconazole-propiconazole OD300g/hm2The field control effect on rice blast and false smut is 87.28 percent and 86.67 percent respectively; 40% prothioconazole-propiconazole WP 300g/hm2The field control effect on rice blast and false smut is 83.88 percent and 82.11 percent respectively; 40% prothioconazole-propiconazole SC 300g/hm2The field control effect on rice blast and false smut is 85.26 percent and 84.21 percent respectively; 40% ProthiobacillusOxazole-propiconazole WG 300g/hm2The field control effect on rice blast and false smut was 84.76% and 84.56%, respectively (table 7).
This shows that after prothioconazole and propiconazole are compounded, the prevention effect of the dispersible oil suspending agent prepared by the formulation when the effective components and the contents thereof are the same is better than the prevention effect of the wettable powder, the suspending agent and the water dispersible granule. The probably is that the compound formulation of the prothioconazole and the propiconazole is dispersible oil suspending agent, the formulation is extremely matched, and the drug effect is more favorably exerted and the prevention effect of the drug is improved.
TABLE 7 field control of different combinations of prothioconazole and propiconazole against rice blast and false smut
Note: the data in the same column followed by different lower case letters indicated significant differences (P < 0.05).
Field efficacy example 7: the field control test of the dispersible oil suspending agent containing prothioconazole and propiconazole on grape anthracnose.
The dispersible oil suspension containing prothioconazole and propiconazole of preparation examples 1 to 9 were subjected to field efficacy tests for controlling grape anthracnose using 30% prothioconazole OD (amhui agricultural products limited) and 250g/L propiconazole EC (mr. chengda, switzerland crop protection limited) as control agents, respectively.
The test treatment method comprises the following steps: the test is carried out in rural farmlands of farmers in rural villages of white rabbits, towns and rabbits, provinces of Jiangsu province, the periphery of the test field is a grape planting area, the soil texture is loam, and the organic matter content is medium. The test summer black is open-air trellis cultivation, the plant spacing is about 4m, and the row spacing is 3 m. The seedlings are transplanted in 2015 years and are 6 years old, and the growth vigor is good. The test area has good drainage, irrigation, fertilization and management. The experiment was performed with 12 treatments, which were: the preparation of the examples 1-9,the treatment dosage of the medicament is set as the effective administration dosage of the prothioconazole and the propiconazole to be 150g/hm2(the total effective application dose of the field of the sterilization main effective components of the prothioconazole and the propiconazole is 150g/hm2Calculated), the treatment doses of 30% prothioconazole OD and 250g/L propiconazole EC are also respectively provided with an effective administration dose of 150g/hm2Spraying equal amount of clear water as control, repeating each treatment for 3 times, and obtaining 36 cells with area of 30m2The cells are provided with protection rows and are arranged randomly in blocks. The WBD-16 electric sprayer manufactured by Ongzhou Ludi agricultural machinery Co., Ltd was used for uniform spray application 3 times at intervals of 10d before flowering of grapes (5.6.2021), 1 st time. The amount of the sprayed liquid is 750L/hm2And spraying equal amount of clear water in the control treatment area, and not spraying any other medicament after the application until the test is finished.
The investigation and calculation method of the drug effect of grape anthracnose comprises the following steps: after the bagged grapes are ripe, randomly sampling and investigating 30-spike grapes in each cell, and counting the morbidity and disease indexes. Disease grading criteria were as follows, grade 0: the whole spike is disease-free; level 1: 1/4 the onset of fruit clusters; and 2, stage: 1/4-1/2 of fruit clusters; and 3, level: 1/2-3/4 of fruit clusters; 4, level: 3/4 above ear. Disease index ═ Σ [ damage level × number of diseased ears at that level ]/[ total number of investigated ears × 4] × 100; the prevention and treatment effect is (contrast disease index-treatment disease index)/contrast disease index x 100%.
The test results show that the effective dose (150 g/hm) is applied in the same way2) In the following, the dispersible oil suspension containing prothioconazole and propiconazole of examples 1 to 9 have field control effects on grape anthracnose which are both higher than those of the control agents 30% prothioconazole OD and 250g/L propiconazole EC and have significant differences (Table 8).
The result shows that the dispersible oil suspending agent containing prothioconazole and propiconazole has excellent field control effect on grape anthracnose, and the sterilization effect after the compound with the optimal proportion is obvious in synergy compared with that of a single agent. Therefore, the dispersible oil suspending agent containing prothioconazole and propiconazole has the advantages of reducing drug consumption, improving the effect and having important significance for comprehensively preventing and treating grape diseases.
TABLE 8 field control of grape anthracnose with agents prepared according to the examples of the invention
| Reagent for testing | Effective dose/(g/hm)2) | Index of disease condition | Prevention effect/%) |
| Example 1 | 150 | 1.13d | 87.66b |
| Example 2 | 150 | 1.10de | 87.99ab |
| Example 3 | 150 | 1.12de | 87.77b |
| Example 4 | 150 | 1.02de | 88.86ab |
| Example 5 | 150 | 1.09de | 88.10ab |
| Example 6 | 150 | 1.06de | 88.43ab |
| Example 7 | 150 | 0.99e | 89.19a |
| Example 8 | 150 | 1.06de | 88.43ab |
| Example 9 | 150 | 1.02de | 88.86ab |
| 30% Prothioconazole OD | 150 | 1.64c | 82.10c |
| 250g/L propiconazole EC | 150 | 2.38b | 74.02d |
| CK | / | 9.16a | / |
Note that the treatment doses of preparation examples 1-9 were in the range of 150g/hm of the sum of the effective doses of prothioconazole and propiconazole for administration2(ii) a The data in the same column is marked with different lower case letters to indicate that the difference is significant (P)<0.05)。
Field efficacy example 8: the difference from the field efficacy example 7 lies in that the dispersible oil suspension containing prothioconazole and propiconazole of the invention is the agents obtained in examples 7, 10 and 11, the difference of field control effect on grape anthracnose after the auxiliary material validamycin A is added is examined, and the results are as follows:
the test result shows that 40 percent of prothioconazole-propiconazole OD 225g/hm2The field control effect on grape anthracnose is 80.91 percent; after 2% validamycin A (0.05 times of the total mass of the prothioconazole and the propiconazole) is added, 40% prothioconazole-propiconazole OD 225g/hm2The field control effect on grape anthracnose is 84.60%, and the control effect difference is obvious before and after 2% validamycin A is added; after 4 percent of validamycin A (0.1 time of the total mass of the prothioconazole and the propiconazole) is added, 40 percent of prothioconazole-propiconazole OD 225g/hm2The field control effect on grape anthracnose is 89.24%, and the control effect difference is obvious before and after 4% validamycin A is added. 40% Prothioconazole-propiconazole OD300g/hm2The field control effect on grape anthracnose is 87.34%; after 2% validamycin A (0.05 times of the total mass of the prothioconazole and the propiconazole) is added, 40% prothioconazole-propiconazole OD300g/hm2The field control effect on grape anthracnose is 89.98%, and the control effect difference is obvious before and after 2% validamycin A is added; after 4 percent of validamycin A (0.1 time of the total mass of the prothioconazole and the propiconazole) is added, 40 percent of prothioconazole-propiconazole OD300g/hm2The field control effect on grape anthracnose is 92.83%, and the control effect difference is obvious before and after 4% validamycin A is added (Table 9).
The result shows that the test agent combination has obvious synergistic effect on the field control effect of the grape anthracnose after the auxiliary material validamycin A is added into the dispersible oil suspending agent containing prothioconazole and propiconazole.
TABLE 940% field control of prothioconazole propiconazole OD against grape anthracnose
(comparison of drug Effect after addition of Validamycin A)
Note: the data in the same column followed by different lower case letters indicated significant differences (P < 0.05).
Field efficacy example 9: the field control test of the tea tree anthracnose by using the dispersible oil suspending agent containing prothioconazole and propiconazole.
The dispersible oil suspension containing prothioconazole and propiconazole prepared in preparation examples 1 to 9 respectively takes 30% prothioconazole OD (Anhui Jiuyi agricultural products Co., Ltd.) and 250g/L propiconazole emulsion EC (Switzerland Xiongdada crop protection Co., Ltd.) as control medicaments to carry out field efficacy tests for controlling anthracnose of tea trees.
The test treatment method comprises the following steps: the test is carried out in a tea garden No. 118 (Longshan tea field) of Xiangxiang Zhenlongcun in sentence-capacity city of Jiangsu province, the periphery of the test field is a tea tree planting area, the soil texture is loam, and the organic matter content is medium. The tested tea tree variety is a double-row strip-planting tea garden in a low-lying area of Longjing 43, the height of the tree is about 75cm, the width of a canopy is about 1.0 m, the row spacing is about 1.5 m, and the tea tree is transplanted in 2013 years and has good growth vigor. The test area has good drainage, irrigation, fertilization and management. The experiment was performed with 12 treatments, which were: preparation examples 1 to 9, the treatment dose of the medicament was set to 150g/hm for the effective administration dose of prothioconazole and propiconazole2(the total effective application dose of the field of the sterilization main effective components of the prothioconazole and the propiconazole is 150g/hm2Calculated), the treatment doses of 30% prothioconazole OD and 250g/L propiconazole EC are also respectively provided with an effective administration dose of 150g/hm2Spraying equal amount of clear water as control, repeating each treatment for 3 times, and obtaining 36 cells with area of 30m2The cells are provided with protection rows and are randomly arranged in blocks. The application is carried out for 2 times at intervals of 10d, and the WBD-16 electric sprayer manufactured by Zhengzhou Ludi agricultural machinery Co., Ltd is used for the 1 st uniform spraying application at the summer tip growth period of the tea trees (6 months and 16 days 2021). The amount of the sprayed liquid is 750L/hm2And spraying equal amount of clear water in the control treatment area, and not spraying any other medicament after the application until the test is finished.
The method for investigating and calculating the anthracnose drug effect of the tea trees comprises the following steps: and (4) after 2 times of medicine taking, randomly sampling and investigating 3 points in each cell, investigating the grown leaves and the old leaves of the upper branch and the middle branch at each point, investigating 100 leaves at each point, and counting the disease condition and the disease index of the leaves. Disease grading criteria were as follows, grade 0: no disease spots; level 1: the area of the lesion spots accounts for less than 5% of the area of the whole leaf; and 3, level: the area of the lesion spots accounts for 6 to 25 percent of the area of the whole leaf; and 5, stage: the area of the lesion spots accounts for 26 to 50 percent of the area of the whole leaf; and 7, stage: the area of the lesion spots accounts for 51 to 75 percent of the area of the whole leaf; and 9, stage: the area of the lesion spots accounts for more than 76% of the area of the whole leaf. Disease index ═ Σ [ victimization level × number of diseased leaves at that level ]/[ total number of investigated leaves × 4] × 100; the prevention and treatment effect is (contrast disease index-treatment disease index)/contrast disease index x 100%.
The test results show that the effective dose (150 g/hm) is applied in the same way2) In the following, the dispersible oil suspension containing prothioconazole and propiconazole of examples 1 to 9 have field control effects on anthracnose of tea trees which are both higher than those of control agents such as 30% prothioconazole OD and 250g/L propiconazole EC and have significant differences (Table 10).
The result shows that the dispersible oil suspending agent containing prothioconazole and propiconazole has excellent field control effect on anthracnose of tea trees, and the sterilization effect is obvious in synergism compared with that of a single agent after the dispersible oil suspending agent is compounded in a preferred proportion. Therefore, the dispersible oil suspending agent containing prothioconazole and propiconazole has the advantages of reducing drug consumption, improving effect and having important significance for comprehensive prevention and control of anthracnose of tea trees.
TABLE 10 field control of anthracnose of tea plants with agents prepared according to the examples of the invention
Note that the treatment doses of preparation examples 1-9 were in the range of 150g/hm of the sum of the effective doses of prothioconazole and propiconazole for administration2(ii) a The data in the same column is marked with different lower case letters to indicate that the difference is significant (P)<0.05)。
Field efficacy example 10: the difference from the field effect example 9 lies in the test agent, the cell design and the application method. The test agents were the dispersible oil-based suspension containing prothioconazole and propiconazole of the present invention, preparation example 7, and 40% prothioconazole-propiconazole WP, 40% prothioconazole-propiconazole SC, and 40% prothioconazole-propiconazole WG prepared in preparation examples 13 to 15; the cell area is 667m2Repeatedly investigating the disease according to 3 in a cell without repetition; the pesticide application method comprises applying pesticide by using a Dajiang T30 type plant protection unmanned aerial vehicle, wherein the liquid spraying amount is 30L/hm2. The difference of different compound formulations of prothioconazole and propiconazole in field control effect on anthracnose of tea trees under the flying prevention and pesticide application conditions is investigated, and the results are as follows:
the test result shows that under the condition of flying prevention and pesticide application of a plant protection unmanned aerial vehicle, 40 percent of prothioconazole-propiconazole OD, 40 percent of prothioconazole-propiconazole WP, 40 percent of prothioconazole-propiconazole SC and 40 percent of prothioconazole-propiconazole WG 300g/hm2The field control of tea tree anthracnose at the dose was 86.57%, 80.29%, 82.94% and 82.31% respectively (table 11).
This shows that, after the prothioconazole and the propiconazole are compounded, the prevention effect of the dispersible oil suspending agent prepared by the preparation formulation when the effective components and the contents thereof are the same and the plant protection unmanned aerial vehicle flies and prevents the drug application is better than the prevention effect of the wettable powder, the suspending agent and the water dispersible granule. This probably is because prothioconazole and propiconazole compound formulation are dispersible oil suspending agent, and the formulation extremely matches, more is favorable to plant protection unmanned aerial vehicle to fly to prevent applying medicine and better performance drug effect and has promoted the medicament and prevent the effect.
TABLE 11 field control of anthracnose of tea plants with different combinations of prothioconazole and propiconazole (flying control application)
Note: the data in the same column are marked with different lower case letters indicating significant differences (P < 0.05).
Field efficacy example 11: the field control test of the dispersible oil suspending agent containing prothioconazole and propiconazole on tomato leaf mold is carried out.
The dispersible oil suspension containing prothioconazole and propiconazole of preparation examples 1 to 9 were subjected to field efficacy tests for controlling tomato leaf mold using 30% prothioconazole OD (amjeldahl ltd) and 250g/L propiconazole EC (swozhou zihengda crop protection ltd) as control agents, respectively.
The test treatment method comprises the following steps: the test is carried out in a tomato planting greenhouse of white rabbit township, Xijing village farmers in sentence-appearance city, Jiangsu province, the test field is a vegetable continuous cropping greenhouse, the soil texture is clay soil, and the organic matter content is medium. The tomato to be tested is Suhong 2003, and the tomato leaf mold in the test greenhouse is damaged to different degrees every year. The experiment was performed with 12 treatments, which were: preparation examples 1 to 9, the treatment dose of the medicament was set to 150g/hm for the effective administration dose of prothioconazole and propiconazole2(the total effective application dose of the field of the sterilization main effective components of the prothioconazole and the propiconazole is 150g/hm2Calculated), the treatment doses of 30% prothioconazole OD and 250g/L propiconazole EC are also both provided with an effective administration dose of 150g/hm2Spraying equal amount of clear water as control, repeating each treatment for 3 times, and obtaining 36 cells with area of 30m2The cells are provided with protection rows and are randomly arranged in blocks. The pesticide is applied for 2 times at intervals of 10d, and the WBD-16 electric sprayer produced by Zhengzhou Ludi agricultural machinery Co., Ltd is used for uniformly spraying and applying the pesticide to stems and leaves of plants such as the front and back of leaves for the 1 st time at the initial stage of tomato flowering (6 months and 16 days in 2021). The amount of the sprayed liquid is 750L/hm2And spraying equal amount of clear water in the control treatment area, and not spraying any other medicament after the application until the test is finished.
The method for investigating and calculating the pesticide effect of the tomato leaf mold comprises the following steps: at 14d (7 months and 10 days 2021) after 2 times of drug administration, 3 spots per cell were sampled, and 5 plants per spot. Taking a representative compound leaf from the upper part, the middle part and the lower part of each plant respectively, and classifying by the lesion area of each lobule on the compound leaf accounting for the area percentage of the whole lobule, wherein the classification standard is as follows, and the classification is 0 grade: no disease spots; level 1: the lesion area accounts for less than 5% of the whole leaf area; and 3, stage: the lesion area accounts for 6 to 10 percent of the whole leaf area; and 5, stage: the lesion area accounts for 11 to 20 percent of the whole leaf area; and 7, stage: the lesion area accounts for 21 to 50 percent of the whole leaf area; and 9, stage: the lesion area accounts for more than 50% of the whole leaf area. The disease index is [ Σ (number of diseased leaves at each level × corresponding disease level value)/total investigated leaf number × highest level representative value ] × 100; the prevention and treatment effect is [ (control disease index-treatment disease index)/control disease index ] × 100%.
The test results show that the effective dose (150 g/hm) is applied in the same way2) In the following, the dispersible oil suspension containing prothioconazole and propiconazole of examples 1 to 9 have higher field control effect on tomato leaf mold than the control medicaments of 30% prothioconazole OD and 250g/L propiconazole EC and have obvious difference (Table 12).
The results show that the dispersible oil suspending agent containing prothioconazole and propiconazole has excellent field control effect on tomato leaf mold, and the sterilization effect after the compound with the optimal proportion is obvious in synergy compared with that of a single agent. Therefore, the dispersible oil suspending agent containing prothioconazole and propiconazole has the advantages of reducing pesticide dosage, improving efficacy and having important significance for comprehensively preventing and treating tomato leaf mold.
TABLE 12 field control of tomato leaf mold by agents prepared in accordance with the present examples
| Reagent for testing | Effective dose/(g/hm)2) | Index of disease condition | Prevention effect/%) |
| Example 1 | 150 | 2.51 d | 91.07a |
| Example 2 | 150 | 2.65d | 90.58a |
| Example 3 | 150 | 2.53d | 91.00a |
| Example 4 | 150 | 2.47d | 91.22a |
| Example 5 | 150 | 2.53d | 91.00a |
| Example 6 | 150 | 2.55d | 90.93a |
| Example 7 | 150 | 2.52d | 91.04a |
| Example 8 | 150 | 2.47d | 91.22a |
| Example 9 | 150 | 2.55d | 90.93a |
| 30% Prothioconazole OD | 150 | 3.72c | 86.77b |
| 250g/L propiconazole EC | 150 | 6.10b | 78.31c |
| CK | / | 28.12a | / |
Note that the treatment doses of preparation examples 1-9 were in the range of 150g/hm of the sum of the effective doses of prothioconazole and propiconazole for administration2(ii) a The data in the same column is marked with different lower case letters to indicate that the difference is significant (P)<0.05)。
Field efficacy example 12: the same field efficacy example 11, except that the dispersible oil suspension containing prothioconazole and propiconazole of the present invention was used as the preparation example 7, and the 40% prothioconazole-propiconazole WP, 40% prothioconazole-propiconazole SC and 40% prothioconazole-propiconazole WG prepared in the preparation examples 13 to 15, the differences in field control effect of different formulation formulations of prothioconazole and propiconazole on tomato leaf mold were examined, and the results were as follows:
the test results showed 40% prothioconazole-propiconazole OD, 40% prothioconazole-propiconazole WP, 40% prothioconazole-propiconazole SC and 40% prothioconazole-propiconazoleCycloxazole WG 300g/hm2The field control effect on tomato leaf mold at the dose was 91.06%, 87.78%, 88.36% and 88.09%, respectively (table 13).
This shows that after the prothioconazole and the propiconazole are compounded, the prevention effect of the dispersible oil suspending agent on the tomato leaf mold is better than the prevention effect of the wettable powder, the suspending agent and the water dispersible granule when the effective components and the contents thereof are the same. The reason for this is probably that the dispersible oil suspending agent is prepared by compounding prothioconazole and propiconazole, so that the compound formulation is more matched and the drug effect can be better exerted.
TABLE 13 field control of tomato leaf mold by different combinations of prothioconazole and propiconazole
| Treatment of | Finger for disease | Prevention effect/%) |
| 40% Prothioconazole-propiconazole OD300g/hm2 | 2.31b | 91.06a |
| 40% prothioconazole-propiconazole WP 300g/hm2 | 3.16b | 87.78c |
| 40% prothioconazole-propiconazole SC 300g/hm2 | 3.01b | 88.36b |
| 40% prothioconazole-propiconazole WG 300g/hm2 | 3.08b | 88.09bc |
| CK | 25.85a | / |
Note: the data in the same column are marked with different lower case letters indicating significant differences (P < 0.05).
Field efficacy example 13: the field control test of the dispersible oil suspending agent containing prothioconazole and propiconazole on mulberry sclerotinia rot is carried out.
The field efficacy tests for controlling morula sclerotiorum were conducted using the dispersible oil suspensions containing prothioconazole and propiconazole of preparation examples 1 to 9, respectively, and 30% prothioconazole OD (amjiu yi agriculture ltd) and 250g/L propiconazole EC (mr. switzerland chengda crop protection ltd) as control agents.
The test treatment method comprises the following steps: the test is carried out in the Maoshan Zhentongxia village farmer fruit mulberry field in the sentence capacity city of Jiangsu province, the test field is the open-air cultivation field of fruit mulberry, the soil texture is clay loam, and the organic matter content is medium. The mulberry fruit to be tested is 10, and the mulberry sclerotinia sclerotiorum in the test field has different damage degrees every year. The experiment was performed with 12 treatments, which were: preparation examples 1 to 9, the treatment dose of the medicament was set to 150g/hm for the effective administration dose of prothioconazole and propiconazole2(the total effective application dose of the field of the sterilization main effective components of the prothioconazole and the propiconazole is 150g/hm2Calculated), the treatment doses of 30% prothioconazole OD and 250g/L propiconazole EC are also respectively provided with an effective administration dose of 150g/hm2Spraying equal amount of clear water as control, repeating each treatment for 3 times, totally 33 cells with area of about 48m2The total number of the mulberry trees is 4, and the protection rows are arranged in the subdistrict and are randomly arranged in blocks. The application is carried out for 2 times at intervals of 10d, and the stem and leaf of mulberry plants are uniformly sprayed and applied for the 1 st time by using a WBD-16 electric sprayer produced by Zhengzhou Ludi agricultural machinery Co., Ltd at the beginning of the flowering period of mulberry (3 months and 5 days 2021). Amount of liquid sprayedIs 600L/hm2And spraying equal amount of clear water in the control treatment area, and not spraying any other medicament after the application until the test is finished.
The mulberry sclerotinia sclerotiorum drug effect investigation and calculation method comprises the following steps: 21d (4 months and 5 days in 2021) after 2 times of medicine application, the number of morula sclerotinia sclerotiorum disease fruits and the total number of fruits in each cell (4 mulberry trees) are investigated, and the disease fruit rate is counted. The control effect is [ (control fruit disease rate-treatment fruit disease rate)/control fruit disease rate ] × 100%.
The test results show that the effective dose (150 g/hm) is applied in the same way2) In the following, the dispersible oil suspensions of examples 1-9 containing prothioconazole and propiconazole all had higher field control effect on morula sclerotinia sclerotiorum than the control agents 30% prothioconazole OD and 250g/L propiconazole EC and the difference was significant (table 14).
The result shows that the dispersible oil suspending agent containing prothioconazole and propiconazole has excellent field control effect on the morula sclerotinia rot, and the sterilization effect after the compound with the optimal proportion is obvious in synergy compared with that of a single agent. Therefore, the dispersible oil suspending agent containing prothioconazole and propiconazole has the advantages of reducing drug consumption, improving the effect and having important significance for comprehensively preventing and treating mulberry sclerotinia rot.
TABLE 14 field control of morula alba sclerotinia by the agents prepared in the examples of the present invention
| Reagent for testing | Effective dose/(g/hm)2) | Index of disease condition | Prevention effect/%) |
| Example 1 | 150 | 3.07d | 91.56a |
| Example 2 | 150 | 3.15d | 91.34a |
| Example 3 | 150 | 3.17d | 91.28a |
| Example 4 | 150 | 3.21d | 91.17a |
| Example 5 | 150 | 3.17d | 91.28a |
| Example 6 | 150 | 3.13d | 91.39a |
| Example 7 | 150 | 3.16d | 91.31a |
| Example 8 | 150 | 3.07d | 91.56a |
| Example 9 | 150 | 3.04d | 91.64a |
| 30% Prothioconazole OD | 150 | 4.56c | 87.46b |
| 250g/L propiconazole EC | 150 | 8.45b | 76.76c |
| CK | / | 36.36a | / |
Note that the treatment doses of preparation examples 1-9 were in the range of 150g/hm of the sum of the effective doses of prothioconazole and propiconazole for administration2(ii) a The data in the same column is marked with different lower case letters to indicate that the difference is significant (P)<0.05)。
Field efficacy example 14: the difference from the field efficacy example 13 lies in the reagent to be tested, the cell design and the application method. The test agents were the dispersible oil-based suspension containing prothioconazole and propiconazole of the present invention, preparation example 7, and 40% prothioconazole-propiconazole WP, 40% prothioconazole-propiconazole SC, and 40% prothioconazole-propiconazole WG prepared in preparation examples 13 to 15; the cell area is 667m2Repeatedly investigating the disease according to 3 in a cell without repetition; the pesticide application method comprises applying pesticide by using a Dajiang T30 type plant protection unmanned aerial vehicle, wherein the liquid spraying amount is 30L/hm2. Investigating the field control effect of different compound formulations of prothioconazole and propiconazole on morula sclerotiorum under the condition of flying control applicationThe difference, results are as follows:
the test result shows that under the condition of flying prevention and pesticide application of a plant protection unmanned aerial vehicle, 40 percent of prothioconazole-propiconazole OD, 40 percent of prothioconazole-propiconazole WP, 40 percent of prothioconazole-propiconazole SC and 40 percent of prothioconazole-propiconazole WG 300g/hm2The field control effect on morula alba sclerotiniose at the dose was 90.64%, 86.46%, 88.21 and 88.13%, respectively (table 15).
This indicates that, after prothioconazole and propiconazole are compounded, the control effect of the dispersible oil suspending agent prepared in the form of the plant protection unmanned aerial vehicle flying prevention application with the same effective components and content is better than the control effect of the wettable powder, the suspending agent and the water dispersible granule. This probably is because prothioconazole and propiconazole compound formulation are dispersible oil suspending agent, and the formulation extremely matches, more is favorable to plant protection unmanned aerial vehicle to fly to prevent applying medicine and better exert the drug effect and promoted the medicament and prevent the effect.
TABLE 15 field control of Mulberry sclerotinia with different combinations of prothioconazole and propiconazole (flying control application)
| Treatment of | Finger for disease | Prevention effect/%) |
| 40% Prothioconazole-propiconazole OD300g/hm2 | 3.36c | 90.64a |
| 40% prothioconazole propiconazole WP 300g/hm2 | 4.86b | 86.46c |
| 40% prothioconazole-propiconazole SC 300g/hm2 | 4.23bc | 88.21b |
| 40% prothioconazole-propiconazole WG 300g/hm2 | 4.26bc | 88.13b |
| CK | 35.89a | / |
Note: the data in the same column followed by different lower case letters indicated significant differences (P < 0.05).
Claims (10)
1. A dispersible oil suspending agent containing prothioconazole and propiconazole is characterized by comprising 1-40% of prothioconazole, 1-40% of propiconazole, 3-12% of emulsifier, 2-8% of dispersant, 0.5-10% of thickener, 0.5-7% of stabilizer, 0.2-2% of antifreeze, 0.2-1% of defoamer and the balance of oil-based solvent; the emulsifier is a mixture of polyoxyethylene ether, polyvinyl alcohol and sodium dodecyl benzene sulfonate; the dispersant is alkyl naphthalene sulfonate; the thickening agent is a mixture of fumed silica and xanthan gum; the oil-based solvent is a mixture consisting of soybean oil and methyl oleate; the antifreezing agent is ethylene glycol or propylene glycol; the defoaming agent is organic silicon.
2. The dispersible oil suspension containing prothioconazole and propiconazole according to claim 1, wherein the mass ratio of the mixture of polyoxyethylene ether, polyvinyl alcohol and sodium dodecyl benzene sulfonate is 1-8: 2-6: 1-4.
3. The dispersible oil suspension concentrate containing prothioconazole and propiconazole according to claim 1, wherein the stabilizer is any one or more of epoxidized soybean oil, epoxidized linseed oil, 1, 2-butanediol, isopropyl phosphate and butyl epoxystearate.
4. The dispersible oil suspension concentrate containing prothioconazole and propiconazole according to claim 1, wherein the percentage content of prothioconazole and propiconazole in the dispersible oil suspension concentrate is 10% -50%.
5. The dispersible oil suspension concentrate containing prothioconazole and propiconazole according to claim 1, wherein the oil-based solvent is a mixture of soybean oil and methyl oleate in a mass ratio of 1: 4-8.
6. The dispersible oil suspension containing prothioconazole and propiconazole according to claim 1, further comprising an auxiliary material validamycin A, wherein the dosage of the auxiliary material validamycin A is 0.05-0.2 times of the total mass of the prothioconazole and the propiconazole.
7. The dispersible oil suspension concentrate containing prothioconazole and propiconazole according to claim 1, wherein the mass ratio of the mixture of the fumed silica and the xanthan gum is 2: 1.
8. The dispersible oil suspension containing prothioconazole and propiconazole according to claim 1, wherein the mass ratio of prothioconazole to propiconazole is 1-15: 1-15.
9. A process for preparing the dispersible oil suspension concentrate containing prothioconazole and propiconazole according to claim 1, which comprises the steps of:
step (1): adding an emulsifier and a dispersant into an oil-based solvent in sequence, and mixing and dispersing uniformly;
step (2): stirring and adding prothioconazole and propiconazole crude oil under high-speed shearing;
and (3): adding a thickening agent and a defoaming agent, and stirring and mixing;
and (4): grinding under zirconium bead medium until the particle size is less than 4 μm;
and (5): and adding a stabilizer and an antifreezing agent, and discharging after the product is detected to be qualified to obtain a finished product.
10. The use of the dispersible oil suspension concentrate containing prothioconazole and propiconazole according to any one of claims 1 to 9 for controlling wheat scab, wheat powdery mildew, wheat rust, wheat kernel deoxynivalenol toxin, rice blast, false smut, grape anthracnose, tea tree anthracnose, tomato leaf mold and mulberry sclerotinia.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102273461A (en) * | 2011-08-25 | 2011-12-14 | 陕西美邦农药有限公司 | Synergistic pesticide composition containing prothioconazole and triazoles |
| CN102578103A (en) * | 2012-01-20 | 2012-07-18 | 联保作物科技有限公司 | Sterilizing composition and preparation thereof |
| US20130324403A1 (en) * | 2011-03-03 | 2013-12-05 | Dsm Ip Assets B.V. | New antifungal compositions |
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|---|---|---|---|---|
| US20130324403A1 (en) * | 2011-03-03 | 2013-12-05 | Dsm Ip Assets B.V. | New antifungal compositions |
| CN102273461A (en) * | 2011-08-25 | 2011-12-14 | 陕西美邦农药有限公司 | Synergistic pesticide composition containing prothioconazole and triazoles |
| CN102578103A (en) * | 2012-01-20 | 2012-07-18 | 联保作物科技有限公司 | Sterilizing composition and preparation thereof |
| CN106857532A (en) * | 2017-04-28 | 2017-06-20 | 陕西上格之路生物科学有限公司 | Application of the bactericidal composition containing Boscalid on rot is prevented and treated |
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