CN116725019A - Methanesulfonyl bacteria azole suspending agent and preparation method thereof - Google Patents
Methanesulfonyl bacteria azole suspending agent and preparation method thereof Download PDFInfo
- Publication number
- CN116725019A CN116725019A CN202310693798.1A CN202310693798A CN116725019A CN 116725019 A CN116725019 A CN 116725019A CN 202310693798 A CN202310693798 A CN 202310693798A CN 116725019 A CN116725019 A CN 116725019A
- Authority
- CN
- China
- Prior art keywords
- methanesulfonyl
- bacteria
- suspending agent
- azole
- 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.)
- Pending
Links
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 title claims abstract description 152
- 241000894006 Bacteria Species 0.000 title claims abstract description 143
- 125000004170 methylsulfonyl group Chemical group [H]C([H])([H])S(*)(=O)=O 0.000 title claims abstract description 138
- 239000000375 suspending agent Substances 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 230000001580 bacterial effect Effects 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
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- 235000006040 Prunus persica var persica Nutrition 0.000 claims abstract description 8
- FJJCIZWZNKZHII-UHFFFAOYSA-N [4,6-bis(cyanoamino)-1,3,5-triazin-2-yl]cyanamide Chemical compound N#CNC1=NC(NC#N)=NC(NC#N)=N1 FJJCIZWZNKZHII-UHFFFAOYSA-N 0.000 claims abstract description 8
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- 150000001875 compounds Chemical class 0.000 claims description 13
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- 241000607479 Yersinia pestis Species 0.000 claims description 10
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 9
- 239000011734 sodium Substances 0.000 claims description 9
- 229910052708 sodium Inorganic materials 0.000 claims description 9
- KVCGISUBCHHTDD-UHFFFAOYSA-M sodium;4-methylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1 KVCGISUBCHHTDD-UHFFFAOYSA-M 0.000 claims description 9
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- ZCQWOFVYLHDMMC-UHFFFAOYSA-N Oxazole Chemical compound C1=COC=N1 ZCQWOFVYLHDMMC-UHFFFAOYSA-N 0.000 claims description 3
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- 239000005868 Metconazole Substances 0.000 description 4
- VMFXMTJCTSYHCF-HHQUSWFZSA-N [(2r,3r,4s,5r)-5-(hexylamino)-4-hydroxy-2-(hydroxymethyl)-6-[(7-hydroxy-4-oxo-1,3a,5,6,7,7a-hexahydroimidazo[4,5-c]pyridin-2-yl)amino]oxan-3-yl] carbamate Chemical compound CCCCCCN[C@@H]1[C@H](O)[C@@H](OC(N)=O)[C@@H](CO)OC1\N=C\1NC(C(=O)NCC2O)C2N/1 VMFXMTJCTSYHCF-HHQUSWFZSA-N 0.000 description 4
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- XWPZUHJBOLQNMN-UHFFFAOYSA-N metconazole Chemical compound C1=NC=NN1CC1(O)C(C)(C)CCC1CC1=CC=C(Cl)C=C1 XWPZUHJBOLQNMN-UHFFFAOYSA-N 0.000 description 4
- 229920000417 polynaphthalene Polymers 0.000 description 4
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- MJUNZSNOBFDUNV-UHFFFAOYSA-N 1-methylsulfonylbutan-1-ol Chemical compound CCCC(O)S(C)(=O)=O MJUNZSNOBFDUNV-UHFFFAOYSA-N 0.000 description 3
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- FKASFBLJDCHBNZ-UHFFFAOYSA-N 1,3,4-oxadiazole Chemical compound C1=NN=CO1 FKASFBLJDCHBNZ-UHFFFAOYSA-N 0.000 description 1
- SWWQQSDRUYSMAR-UHFFFAOYSA-N 1-[(4-hydroxyphenyl)methyl]-1,2,3,4-tetrahydroisoquinoline-6,7-diol;hydrochloride Chemical group Cl.C1=CC(O)=CC=C1CC1C2=CC(O)=C(O)C=C2CCN1 SWWQQSDRUYSMAR-UHFFFAOYSA-N 0.000 description 1
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- FKKAGFLIPSSCHT-UHFFFAOYSA-N 1-dodecoxydodecane;sulfuric acid Chemical compound OS(O)(=O)=O.CCCCCCCCCCCCOCCCCCCCCCCCC FKKAGFLIPSSCHT-UHFFFAOYSA-N 0.000 description 1
- KLSJWNVTNUYHDU-UHFFFAOYSA-N Amitrole Chemical group NC1=NC=NN1 KLSJWNVTNUYHDU-UHFFFAOYSA-N 0.000 description 1
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- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 1
- 241001272684 Xanthomonas campestris pv. oryzae Species 0.000 description 1
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- PSZYNBSKGUBXEH-UHFFFAOYSA-N naphthalene-1-sulfonic acid Chemical class C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/82—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with three ring hetero atoms
-
- 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
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Abstract
The application relates to a methylsulfonyl bacteria azole suspending agent and a preparation method thereof. The methanesulfonyl bacteria azole suspending agent comprises: 20wt% of methanesulfonyl bacteria azole and 3-12 wt% of surfactant; 0.5 to 2.5 weight percent of thickener; 2-6wt% of antifreezing agent; 0.3 to 0.5 weight percent of organosilicon defoamer and the balance of deionized water. The raw materials are subjected to wet sanding to obtain the methanesulfonyl bacteria azole suspending agent. It can be used for preventing and treating bacterial diseases such as bacterial leaf blight (Xoo), bacterial leaf spot (Xoc), citrus canker (Xac), cabbage black rot, peach perforation, cabbage soft rot, melon fine corner, tobacco bacterial wilt, watermelon fruit rot, tomato bacterial wilt, etc.
Description
Technical Field
The application belongs to the field of pesticides, and particularly relates to a 20% methylsulfonyl azole water suspension and a preparation method thereof.
Background
The plant bacterial disease is a second plant disease next to fungi, and has the characteristics of quick disease occurrence, wide distribution, difficult control and the like. In recent years, with the change of crop cultivation system and environmental climate in China, bacterial diseases of crops such as rice bacterial leaf blight (Xoo), bacterial leaf streak disease (Xoc), citrus canker (Xac), cabbage black rot, peach perforation, chinese cabbage soft rot, melon fine angle disease, tobacco bacterial wilt, watermelon fruit rot and tomato bacterial wilt show a tendency of serious occurrence in China. The prevention and treatment means aiming at plant bacterial diseases mainly take chemical pesticides as main materials, and copper preparations are used at the maximum amount, but the copper preparations have the problems of poor safety, easiness in occurrence of copper poisoning and the like. At present, high-efficiency and safe chemical agents are seriously lacked for prevention and treatment, and great losses are caused for agricultural production.
The methanesulfonyl bacteria azole is a novel bactericide independently created by Guizhou university, has the characteristics of high efficiency, low toxicity, low risk and the like, has good control effect on bacterial diseases such as bacterial leaf blight of rice, bacterial wilt of tomato, bacterial leaf spot of rice, canker of fruit trees and the like under the condition that the dosage is 75-150 g/hectare, and is used for pesticide production registration by biochemical companies assigned to Guangxi rural areas. However, the methylsulfonyl bacteria azole has active chemical properties, and under the condition of selecting an unsuitable auxiliary agent, the methylsulfonyl bacteria azole suspending agent can have high decomposition rate of the original medicine in the long-term storage process, so that the problems of difficult registration of pesticides and difficult actual production and application are caused.
Physical and chemical properties of methanesulfonyl bacteria oxazole: molecular weight 242.02. The raw material is needle crystal with melting point of 102-104 ℃. Is insoluble in water and easily soluble in common organic solvents. The original drug is stable to light and heat and is easy to decompose under alkaline conditions (ph=10). The 1,3, 4-oxadiazole in the methanesulfonyl bacteria azole structure is an electron-deficient heterocycle, is influenced by a methanesulfonyl group which is a strong electron-withdrawing group on a 2-position, can be attacked by a nucleophilic reagent containing polar functional groups such as hydroxyl, sulfhydryl or amino, and the like, and has addition elimination reaction and demethyl removal. Therefore, according to the decomposition principle of the methanesulfonyl bacteria, the application develops a favorable technical formula for stabilizing the methanesulfonyl bacteria suspending agent by screening proper auxiliary agents so as to solve the problem of unstable raw materials in the 2-year storage process.
Disclosure of Invention
In order to solve the problems in the prior art, the application provides a preparation formula of a 20% methylsulfonyl bacteria azole water suspension which is beneficial to the stability of raw materials, comprising active ingredients methylsulfonyl bacteria azole, a wetting dispersant, a thickener, an antifreezing agent, an antifoaming agent and water, wherein the weight ratio of the components is 20wt%, 3-12 wt%, 0.5-2.5 wt%, 2-6 wt% and 0.3-0.5 wt% respectively, and the water is complemented to 100%;
the surfactant screened by the application comprises a dispersing agent or a wetting agent, is a compound of ionic or nonionic auxiliary agents, and comprises macromolecular amphiphilic anionic nonionic surfactant compounds, phosphate esters, lignin sulfonate, salts of phenolsulfonic acid or naphthalene sulfonic acid, salts of polyacrylic acid, sulfosuccinate, alkyl sulfonate, alkylaryl sulfonate, alkyl sulfate, lauryl ether sulfate, fatty alcohol sulfate, sulfonate formaldehyde condensate, sulfated hexadecyl-, heptadecyl-and stearyl alcohols and sulfated fatty alcohol glycol ether;
the defoaming agent is polydimethylsiloxane in the organic silicon defoaming agent with the weight percent of 0.3-0.5;
the antifreezing agent is inorganic salt;
the thickener is one or two of magnesium aluminum silicate SF-40 and xanthan gum.
Preferably, the dispersing agent and the wetting agent are composed of a macromolecular amphiphilic anionic non-ionic surfactant compound SC29, sodium dibenzosulfonate HAS024, naphthalene sulfonic acid sodium salt formaldehyde condensate NNO and any one of sodium paratoluenesulfonate, sodium methane sulfinate or polynaphthalene formaldehyde sodium sulfonate according to the weight ratio of 2:2:2:1.5; more preferably, the wetting dispersant consists of a macromolecular amphiphilic anionic non-ionic surfactant compound SC29, sodium dibenzosulfonate HAS024, naphthalene sulfonate sodium formaldehyde condensate NNO and sodium paratoluenesulfonate according to the weight ratio of 2:2:2:1.5.
Preferably, the thickener is 2% magnesium aluminum silicate SF-40 or 1% magnesium aluminum silicate and 0.05% xanthan gum.
The 20% methylsulfonyl bacteria suspension agent for preventing and treating plant bacterial diseases is prepared by taking a dispersing agent, a wetting agent, an antifreezing agent and water according to the weight percentage, stirring and dissolving, adding methylsulfonyl bacteria and a thickening agent according to the weight percentage, uniformly mixing under the action of a shearing machine, pumping the mixed slurry into a sanding machine for grinding, adding an organosilicon antifoaming agent according to the weight percentage, carrying out particle size test every 1h, stopping stirring after D90 is equal to 6.0 mu m, and filtering to obtain the 20% methylsulfonyl bacteria suspension agent.
The main significance of the developed formulation is that the problem of degradation of the drug in the methylsulfonyl fungus suspending agent in the long-term storage process can be effectively relieved by widely screening the wetting dispersant. Compared with the prior patent (CN 104365589A), the methanesulfonyl bacteria azole suspending agent prepared by the application has the characteristics of good water-in dispersibility, contribution to the stability of the original medicine after being stored within 2 years, and the like.
1. Screening of wetting dispersants
The 20% methylsulfonyl bacteria azole suspending agent is prepared by compounding a macromolecular amphiphilic anionic non-ionic surfactant compound with different types of surfactants, and the water dispersibility of the raw medicine and the decomposition rate of the raw medicine after thermal storage are measured after thermal storage, and the specific results are shown in table 1.
Table 1 selection of wetting dispersants
As shown in the results of table 1, the addition of sulfonate adjuvant was found to be beneficial to the stability of the drug substance by screening for different types of adjuvant. The methylsulfonyl bacteria azole suspending agent compounded by the macromolecular amphiphilic anionic non-ionic surfactant compound SC29, sodium dibenzoyl sulfonate HAS024, naphthalene sulfonic acid sodium salt formaldehyde condensate NNO and sodium paratoluenesulfonate or sodium methane sulfinate or sodium polynaphthalene formaldehyde sulfonate HAS good dispersibility, and the decomposition rate of the original medicine after heat storage is controlled within 5 percent.
For screening the optimal amounts of the auxiliary agents such as sodium p-toluenesulfonate, sodium polynaphthalene formaldehyde sulfonate and sodium methane sulfinate, three contents of 0.5%, 1.5% and 3.0% were respectively set for screening, and specific results are shown in Table 2.
TABLE 2 selection of adjuvant dosage
As shown in the results of Table 2, the decomposition rate of the methanesulfonyl myclobutanil after heat storage was lower than 5% at three different contents. Sodium methane sulfinate is relatively expensive and generally water dispersible. The suspension agent turns yellow after the sodium polynaphthalene formaldehyde sulfonate is added, and the appearance is affected. The stability of the original medicine is good, the price is relatively low, and the appearance of the suspending agent is relatively better after the sodium paratoluenesulfonate is added, so that the preferable wetting dispersant formula is SC29 in comprehensive consideration of cost and properties: HOS040: NNO: sodium p-toluenesulfonate=2: 2:2:1.5.
2. Screening of thickeners
Aqueous suspending agents often suffer from storage physical stability problems such as particle agglomeration, sedimentation, water evolution, and thickening and caking. The formula is easy to generate sedimentation and water separation under long-time storage, and can improve sedimentation stability by increasing viscosity. The viscosity is too large, the product is not easy to pour, the wall hanging is serious, and the processing production and the use are difficult. Suitable viscosities provide good stability and high suspension rates for the formulation. According to the related theory and combining the characteristic of unstable chemical property of the methylsulfonyl bacteria, the experiment changes the viscosity by a method of screening the dosage of magnesium aluminum silicate and xanthan gum without changing the types of auxiliary agents needed by the prescreened formulation, but the increase of the viscosity possibly reduces the automatic dispersibility of the water suspending agent, so the water-in dispersibility is improved by increasing the dosage of NNO of the dispersing agent. The specific results are shown in Table 3 and FIG. 1.
TABLE 3 selection of thickeners
As shown in Table 3, too much addition of xanthan gum resulted in some effect on the flowability and water dispersibility of the formulation system. Therefore, 2% of magnesium aluminum silicate is selected as a thickener or 1% of magnesium aluminum silicate is compounded with 0.05% of xanthan gum under the condition of not affecting the water-in dispersibility, so that the sedimentation stability of the suspending agent is improved, and meanwhile, the water-in dispersibility of the preparation is improved by improving the NNO content.
3. Selection of the amount of defoamer
The wetting and dispersing agent is mostly sulfonate, and a large number of bubbles can appear in the processing process to influence the grinding effect. Therefore, some organic silicon defoamer is usually added into the suspending agent, but the proper amount of defoamer is added, and the excessive addition can reduce the surface tension of the system, so that the layering phenomenon becomes more obvious. Too little addition and insignificant defoaming effect. In this test, a general purpose silicone defoamer was selected for testing, and the specific results are shown in table 4.
TABLE 4 selection of defoamer usage
As shown in Table 4, the amount of the antifoaming agent used was small, and a large amount of bubbles generated during the grinding process could not be effectively solved. When the dosage is controlled to be 0.3-0.5%, fewer bubbles are generated in the preparation process, and the grinding is facilitated.
4. Selection of antifreeze
The pesticide suspending agent using water as a dispersion medium can keep stability under the severe cold low temperature condition in the storage process, and a certain amount of proper antifreezing agent is usually required to be added. When glycerol is used as an antifreezing agent, the viscosity of the system increases and the fluidity is poor. When ethylene glycol is used as an antifreezing agent, the stability and fluidity of the preparation are good, but after thermal storage, the decomposition rate of the raw medicine is high. When sodium chloride is used as the antifreezing agent, the bottom of the antifreezing agent can be precipitated very little after cold storage, but the decomposition degree of the raw medicine can not be increased. Thus, sodium chloride was chosen as the best antifreeze.
5. Influence of particle size on the stability of the drug substance after thermal storage
After the auxiliary agent is determined, the methylsulfonyl bacteria azole water suspending agents (with the number of 1-6) with different particle sizes are prepared, after the hot storage, the content of the raw pesticide is measured by adopting a pesticide thermal stability measuring method GB/T19136-2003, and then the decomposition rate of the raw pesticide after the hot storage is analyzed, and the specific results are shown in Table 5 and figures 2-6.
TABLE 5 influence of particle size on the stability of crude drugs
As shown in Table 5 and FIGS. 2 to 4, when the particle size of the 20% aqueous suspension of methanesulfonyl bacteria prepared by using the above-mentioned auxiliary agent is larger than 10. Mu.m, the decomposition rate of the crude drug after heat storage (54.+ -. 2) is large and is 20% or more. When the particle size of the suspending agent raw material is 5-8 mu m, the decomposition rate is about 5-10%, and the stability requirement is met. This shows that the formula and the particle size have important influence on the chemical stability of the original drug of the methylsulfonyl bacteria water suspension agent, and the smaller the particle size is, the better the chemical stability of the original drug is, but the smaller the particle size is, so that the industrial production is not easy.
6. Determination of preferred formulations and methods of preparation
And finally determining a preferred formula and the weight ratio thereof through the test screening: methanesulfonyl bacteria azole, macromolecular amphiphilic anionic non-ionic surfactant complex SC29, sodium dibenzosulfonate HAS024, naphthalene sulfonate sodium salt formaldehyde condensate NNO, sodium paratoluenesulfonate: magnesium aluminum silicate, organosilicon defoamer, sodium chloride=20%:2:2:1.5:2:0.4:4, with deionized water to 100%. Under the formulation, the ground suspending agent is favorable for the heat storage stability of the preparation.
Table 6 determination of preferred formulations
7.20% Methanesulfonyl myclobutanil suspension Specification
The main properties of the suspension were tested according to the national standard requirements for pesticide suspensions (GB/T19136-2003), and are shown in Table 7. The result shows that under the formula, the methylsulfonyl bacteria azole water suspending agent is in a milky uniform dispersion system, the dispersibility and the suspension rate are good, and the decomposition rate of the original medicine after heat storage is lower than 10%.
Table 720% physical and chemical Properties of Sulfamoxazole aqueous suspension
Drawings
FIG. 1 is a graph of sedimentation water separation test results; wherein, the number 1 represents that the suspending agent without magnesium aluminum silicate is seriously dissolved out; number 2 represents that the suspending agent added with 2% magnesium aluminum silicate is not obvious in water evolution degree; the suspending agent added with 1% magnesium aluminum silicate and 0.05% xanthan gum is not apparent in water evolution degree as represented by number 3.
FIG. 2 is a liquid chromatogram of the methanesulfonyl myclobutanil prior to thermal storage.
FIG. 3 is a liquid chromatogram of the hot storage of the methanesulfonyl bacteria azole crude drug.
FIG. 4 is a liquid chromatogram of 20% methanesulfonyl bacteria azole suspension, with a particle size D90 of 6.0. Mu.m, after grinding.
FIG. 5 is a graph showing the therapeutic activity of 20% of the suspension of methanesulfonyl bacteria, 95% of the original methanesulfonyl bacteria, and 20% of the wettable powder of methanesulfonyl bacteria on a potted plant of Rhizoctonia solani.
FIG. 6 is a graph showing the potted plant protection activity test of the 20% methylsulfonyl butoxide suspension, 95% methylsulfonyl butoxide technical, and 20% methylsulfonyl butoxide wettable powder in the present application against bacterial leaf blight of rice.
Examples
The application is further illustrated by the following examples. It should be understood that the methods described in the examples of the present application are only for illustrating the present application, and not for limiting the present application, and that simple modifications to the preparation methods of the present application under the concept of the present application are within the scope of the present application as claimed. All the starting materials and solvents used in the examples were commercially available products of the corresponding purity.
Example 1: preparation of 20% methanesulfonyl bacteria azole suspending agent
6.0g of sodium dibenzoyl sulfonate HAS024, 6.0g of naphthalene sulfonic acid sodium salt formaldehyde condensate NNO, 4.5g of sodium paratoluenesulfonate, 12.0g of sodium chloride and 6.0g of macromolecular amphiphilic anionic nonionic surfactant compound SC29 are weighed into a beaker containing 198.3g of secondary water, after stirring and dissolving, 60.0g of methanesulfonyl myclobutanil and 6.0g of magnesium aluminum silicate are added, after shearing and homogenizing, the mixture is poured into a sand mill containing zirconium beads with the volume-mass ratio of 1:1 with a suspending agent, 1.2g of organosilicon defoamer is added, sand milling is started under ice water bath, particle size testing is carried out every 1h, after about 4h, the particle size is tested by a laser particle size analyzer, when D90 is about equal to 6 mu m, stirring is stopped, and 20% methanesulfonyl myclobutanil suspending agent is obtained after filtering.
Example 2: chromatographic conditions for measuring content of crude drug
Chromatographic column: XDB-C18; mobile phase: methanol-water (volume ratio 60:40); flow rate: 1.0mL/min; column temperature: 25 ℃; detection wavelength: 264nm; sample injection amount: 10. Mu.L; methanesulfonyl myclobutanil retention time: 8min.
Fig. 2-3 show that the content of the raw materials in the preferred formula is measured by using a high performance liquid chromatography instrument, and the result shows that decomposed substances appear at a peak time of about 5.60 after heat storage, and the decomposition rate is more than 70% calculated by an internal standard method. FIG. 4 is a liquid chromatogram of 20% methanesulfonyl bacteria oxazole suspension with a particle size D90 of 6.0 μm after milling. The decomposition rate is less than 10% by calculation of an internal standard method.
Example 3: main Performance test of Methanesulfonyl myclobutanil aqueous suspension
According to national or industry standards of related pesticides in China (GB/T14825-2006 pesticide suspension rate measuring method, GB/T19136-2003 pesticide heat storage stability measuring method, GB/T19137-2003 pesticide low temperature stability measuring method, HG/T2467.5-2003 pesticide suspending agent product standard writing specification), main technical indexes of the methanesulfonyl bacteria azole suspending agent are measured.
As shown in Table 5 and FIGS. 2 to 4, when the particle size of the 20% aqueous suspension of methanesulfonyl bacteria prepared by using the above-mentioned auxiliary agent is larger than 10. Mu.m, the decomposition rate of the crude drug after heat storage (54.+ -. 2) is large and is 20% or more. When the particle size of the suspending agent raw material is 5-8 mu m, the decomposition rate is about 5-10%, and the stability requirement is met. This shows that the formulation and the particle size have an important effect on the chemical stability of the original drug of the methylsulfonyl azole aqueous suspension, and the smaller the particle size is, the better the chemical stability of the original drug is.
The main properties of the suspension were tested according to the national standard requirements for pesticide suspensions (GB/T19136-2003), and are shown in Table 7. The result shows that under the formula, the methylsulfonyl bacteria azole water suspending agent is in a milky uniform dispersion system, the dispersibility and the suspension rate are good, and the decomposition rate of the original medicine after heat storage is lower than 10%.
Example 4: pesticide efficacy in vitro test
The turbidity method is adopted to test the bacterial leaf blight (Xoo), bacterial leaf streak (Xoc), citrus canker (Xac) and cabbage black rot of riceAntibacterial EC of ten bacteria of peach perforation disease, cabbage soft rot, melon fine angle disease, tobacco bacterial wilt, watermelon fruit rot and tomato bacterial wilt 50 Value test:
1. test materials: gun head (5 mL,1mL, 200. Mu.L), 15mL centrifuge tube, secondary water, 2mL EP tube, NB medium all required sterilization.
2. NB medium: beef peptone 3g, peptone 5g, yeast powder 1g, glucose 10g, and secondary water 1L. Subpackaging into test tubes (4 mL/branch), pH=7.0-7.2
3. The operation steps are as follows:
(1) An amount of the compound to be tested was weighed and then dissolved with a corresponding volume (200 μl) of DMSO. A 5% solution system was prepared and diluted to the desired concentration in proportion and the volume was fixed to 4mL with 0.1% tween solution.
(2) 1mL of the mixed solution of the medicinal liquid and warm water was sucked up by a pipette, and the mixed solution was added to a test tube containing 4mL of the culture solution.
(3) 200. Mu.L of the mixed solution (culture medium) was aspirated with a pipette, and the OD was measured with a 96-well plate and recorded.
(4) 50 mu L of bacterial leaf blight (Xoo), bacterial leaf streak (Xoc) of rice, citrus canker (Xac), black rot of cabbage, perforation disease of peach tree, soft rot of Chinese cabbage, melon fine angle disease, tobacco bacterial wilt, watermelon fruit rot and bacterial wilt of tomato are respectively added into each test tube.
(5) Put into a shaker set at 28℃and 180rpm.
(6) After 24h-36h (OD of CK 0.6-0.8), the OD was measured and recorded, and then the inhibition was calculated.
Corrected OD = sterile medium OD
Inhibition ratio = (corrected control medium bacterial liquid OD value-corrected bacteria-containing medium OD value)/corrected control medium bacterial liquid OD value 100
4. Activity data:
20% of the methanesulfonyl bacteria azole suspending agent has excellent antibacterial activity on ten bacterial diseases such as bacterial blight bacteria (Xoo) of rice, and EC thereof 50 Thiazole zinc suspending agent with value being 20% better than that of control medicine20% of thiabendazole suspending agent, 95% of methylsulfonyl bacteria azole original drug and 20% of methylsulfonyl bacteria azole wettable powder.
Table 8 EC of 20% Methanesulfonyl myclobutanil suspension and the like on Xoo 50 Value of
From Table 8, it can be seen that the application has EC of 20% of the methylsulfonyl fungus suspending agent, 95% of the methylsulfonyl fungus original drug and 20% of the methylsulfonyl fungus wettable powder on rice bacterial blight bacteria 50 The values were 3.72. Mu.g/mL, 6.19. Mu.g/mL and 4.38. Mu.g/mL, respectively. Wherein, the application 20 percent of the methanesulfonyl bacteria azole suspending agent EC 50 The value activity is superior to that of a control medicine, namely 20 percent of thiazole zinc suspending agent (12.78 mug/mL), 20 percent of thiabendazole copper suspending agent (71.28 mug/mL) and 95 percent of methanesulfonyl bacteria azole crude drug (6.19 mug/mL) and 20 percent of methanesulfonyl bacteria azole wettable powder (4.38 mug/mL).
Table 9 EC of 20% Methanesulfonyl myclobutanil suspension and the like against Xoc 50 Value of
From Table 9, it can be seen that the application has EC of 20% of the methanesulfonyl bacteria suspension, 95% of the methanesulfonyl bacteria original drug and 20% of the methanesulfonyl bacteria wettable powder on rice bacterial leaf spot bacteria 50 The values were 3.95. Mu.g/mL, 11.21. Mu.g/mL and 6.33. Mu.g/mL, respectively. Wherein, the application 20 percent of the methanesulfonyl bacteria azole suspending agent EC 50 The value activity is superior to that of a control medicine, namely 20 percent thiazole zinc suspending agent (29.11 mug/mL), 20 percent thiabendazole suspending agent (81.28 mug/mL) and 95 percent methanesulfonyl bacteria azole crude drug (11.21 mug/mL) and 20 percent methanesulfonyl bacteria azole wettable powder (6.33 mug/mL).
EC of 20% Methanesulfonyl myclobutanil suspension and the like on Xac 50 Value of
As can be seen from Table 10, the application has the EC of 20% of the methylsulfonyl bacteria suspension, 95% of the methylsulfonyl bacteria original drug and 20% of the methylsulfonyl bacteria wettable powder on citrus canker bacteria 50 The values were 6.35. Mu.g/mL, 12.07. Mu.g/mL and 25.52. Mu.g/mL, respectively. Wherein, the application 20 percent of the methanesulfonyl bacteria azole suspending agent EC 50 The value activity is superior to that of a control medicine, namely 20 percent thiazole zinc suspending agent (43.82 mu g/mL), 20 percent thiabendazole suspending agent (124.52 mu g/mL) and 95 percent methanesulfonyl bacteria azole crude drug (12.07 mu g/mL) and 20 percent methanesulfonyl bacteria azole wettable powder (25.52 mu g/mL).
EC of 20% methanesulfonyl bacteria suspension and the like of Table 11 against Pythium gracile 50 Value of
From Table 11, it can be seen that the application has EC of 20% of the methanesulfonyl bacteria suspension, 95% of the methanesulfonyl bacteria active pharmaceutical ingredient and 20% of the methanesulfonyl bacteria wettable powder on the black rot of cabbage 50 The values were 9.37. Mu.g/mL, 14.17. Mu.g/mL and 11.71. Mu.g/mL, respectively. Wherein, the application 20 percent of the methanesulfonyl bacteria azole suspending agent EC 50 The value activity is superior to that of a control medicine, namely 20 percent thiazole zinc suspending agent (42.17 mug/mL), 20 percent thiabendazole suspending agent (117.43 mug/mL) and 95 percent methanesulfonyl bacteria azole crude drug (14.17 mug/mL) and 20 percent methanesulfonyl bacteria azole wettable powder (11.71 mug/mL).
EC of 20% methanesulfonyl bacteria suspension of Table 12 compound to peach tree canker 50 Value of
As can be seen from Table 12, the application has EC of 20% of the methanesulfonyl bacteria suspension, 95% of the methanesulfonyl bacteria active pharmaceutical ingredient and 20% of the methanesulfonyl bacteria wettable powder on the peach perforated bacteria 50 The values were 12.79. Mu.g/mL, 23.56. Mu.g/mL and 17.60. Mu.g/mL, respectively. Wherein, the application 20 percent of the methanesulfonyl bacteria azole suspending agent EC 50 The value activity is superior to that of a control medicine, namely 20 percent thiazole zinc suspending agent (74.99 mug/mL), 20 percent thiabendazole copper suspending agent (367.66 mug/mL) and 95 percent methanesulfonyl bacteria azole crude drug (23.56 mug/mL) and 20 percent methanesulfonyl bacteria azole wettable powder (17.60 mug/mL).
EC of 20% methanesulfonyl bacteria suspension of Table 13 compound to cabbage soft rot disease 50 Value of
From Table 13, it can be seen that the application uses 20% of the methanesulfonyl bacteria suspension, 95% of the methanesulfonyl bacteria active pharmaceutical ingredient and 20% of the methanesulfonyl bacteria wettable powder to prepare EC of Chinese cabbage soft rot fungi 50 The values were 12.72. Mu.g/mL, 16.10. Mu.g/mL and 13.79. Mu.g/mL, respectively. Wherein, the application 20 percent of the methanesulfonyl bacteria azole suspending agent EC 50 The value activity is superior to that of a control medicine, namely 20 percent of thiazole zinc suspending agent (27.34 mug/mL), 20 percent of thiabendazole copper suspending agent (144.46 mug/mL) and 95 percent of methanesulfonyl bacteria azole crude drug (16.10 mug/mL) and 20 percent of methanesulfonyl bacteria azole wettable powder (13.79 mug/mL).
EC of 20% methanesulfonyl bacteria suspension of Table 14 against melon keratosis 50 Value of
As can be seen from Table 14, the 20% of the methanesulfonyl bacteria suspension, 95% of the methanesulfonyl bacteria original drug and 20% of the methanesulfonyl bacteria wettable powder of the application are used for treating melon leptosphaeriaEC 50 The values were 21.43. Mu.g/mL, 50.43. Mu.g/mL and 64.32. Mu.g/mL, respectively. Wherein, the application 20 percent of the methanesulfonyl bacteria azole suspending agent EC 50 The value activity is superior to that of a control medicine, namely 20 percent thiazole zinc suspending agent (64.31 mug/mL), 20 percent thiabendazole copper suspending agent (100.00 mug/mL) and 95 percent methanesulfonyl bacteria azole crude drug (50.43 mug/mL) and 20 percent methanesulfonyl bacteria azole wettable powder (64.32 mug/mL).
EC of 20% methanesulfonyl bacteria azole suspending agent and the like of Table 15 compound against ralstonia solanacearum 50 Value of
From Table 15, it can be seen that the application has EC of 20% of the methanesulfonyl bacteria suspension, 95% of the methanesulfonyl bacteria active pharmaceutical ingredient and 20% of the methanesulfonyl bacteria wettable powder on tobacco bacterial wilt 50 The values were 18.20. Mu.g/mL, 19.04. Mu.g/mL and 51.35. Mu.g/mL, respectively. Wherein, the application relates to the methanesulfonyl bacteria azole suspending agent EC 50 The value activity is superior to that of a control medicine, namely 20 percent of thiazole zinc suspending agent (44.11 mug/mL), 20 percent of thiabendazole copper suspending agent (106.49 mug/mL) and 95 percent of methanesulfonyl bacteria azole crude drug (19.04 mug/mL) and 20 percent of methanesulfonyl bacteria azole wettable powder (51.35 mug/mL).
EC of 20% methanesulfonyl bacteria azole suspending agent and the like of Table 16 compound against watermelon fruit rot pathogen 50 Value of
As can be seen from Table 16, the application has EC of 20% of the methanesulfonyl bacteria suspension, 95% of the methanesulfonyl bacteria active pharmaceutical ingredient and 20% of the methanesulfonyl bacteria wettable powder on the watermelon fruit rot bacteria 50 The values were 33.40. Mu.g/mL, 40.47. Mu.g/mL and 49.38. Mu.g/mL, respectively. Wherein, the application relates to the methanesulfonyl bacteria azole suspending agent EC 50 The value activity is superior to that of a control medicine, namely 20 percent of thiazole zinc suspending agent (54.36 mug/mL), 20 percent of thiabendazole copper suspending agent (180.89 mug/mL) and 20 percent of methanesulfonyl bacteria azole crude drug (40.47 mug/mL) and 20 percent of methanesulfonyl bacteria azole wettable powder (49.38 mug/mL).
Table 17 Compound 20%EC of methanesulfonyl bacteria azole suspending agent and the like on bacterial wilt of tomato 50 Value of
From Table 17, it can be seen that the application has EC of 20% of the methanesulfonyl bacteria suspension, 95% of the methanesulfonyl bacteria active pharmaceutical ingredient and 20% of the methanesulfonyl bacteria wettable powder on the bacterial wilt of tomato 50 The values were 22.62. Mu.g/mL, 43.29. Mu.g/mL and 68.70. Mu.g/mL, respectively. Wherein, the application 20 percent of the methanesulfonyl bacteria azole suspending agent EC 50 The value activity is superior to that of a control medicine, namely 20 percent thiazole zinc suspending agent (88.13 mug/mL), 20 percent thiabendazole copper suspending agent (141.25 mug/mL) and 95 percent methanesulfonyl bacteria azole crude drug (43.29 mug/mL) and 20 percent methanesulfonyl bacteria azole wettable powder (68.70 mug/mL).
Example 5: living potted plant test for pesticide effect
The living body pot protection and treatment effect test of the 20% methylsulfonyl bacteria suspension agent of the application on rice bacterial leaf blight at the concentration of 200 mug/mL is tested by adopting a leaf cutting method.
Therapeutic activity:
the scissors dipped with bacterial liquid of rice bacterial leaf blight are used for cutting off 1/3cm part of the leaf tip of the rice leaf, after 24 hours, the 20% methylsulfonyl bacteria suspending agent, 95% methylsulfonyl bacteria original drug and 20% methylsulfonyl bacteria wettable powder are selected, DMSO is respectively added for dissolution, then 0.1% Tween-80 solution is used for preparing a medicament with the concentration of 200 mug/mL, and the medicament is uniformly sprayed on the rice leaf until the liquid drops, and meanwhile, clear water contrast without the medicament is arranged. 10-15 leaves are treated for each rice plant. The disease spot length of the rice leaves is measured after 14 days of application, and the control effect is calculated according to the disease spot length.
Protective activity:
the application selects 20% of methylsulfonyl bacteria suspending agent, 95% of methylsulfonyl bacteria original drug and 20% of methylsulfonyl bacteria wettable powder, 200 mu L of DMSO is respectively added for dissolution, 0.1% of Tween-80 solution is respectively used for preparing medicaments with the concentration of 200 mu g/mL, the medicaments are uniformly sprayed on rice leaves until the water drops, after 24 hours, scissors containing rice bacterial blight bacteria are used for cutting and inoculating, bacterial solution is at the position of 1/3 of the tips of the rice leaves, and clear water control without medicaments is arranged. 10-15 leaves per treatment, 3 replicates. The disease spot length of the rice leaves is measured after 14 days of application, and the control effect is calculated according to the disease spot length.
TABLE 18 in vivo therapeutic Activity of 20% Methanesulfonyl myclobutanil suspension of the application on bacterial leaf blight of Rice
As can be seen from Table 18, the therapeutic activities of the 20% methylsulfonylmeconazole suspending agent, the 20% methylsulfonylmeconazole powder and the 95% methylsulfonylmeconazole prodrug of the present application were 40.8%, 35.4% and 35.9%, respectively, at a concentration of 200. Mu.g/mL. The 20% methylsulfonyl bacteria azole suspending agent (40.8%) of the application has activity superior to that of 95% methylsulfonyl bacteria azole original drug (35.9%), and 20% methylsulfonyl bacteria wettable powder (35.4%), which is equivalent to that of 3% Zhongshengmycin wettable powder (39.0%).
TABLE 19 in vivo protective Activity of 20% Methanesulfonyl myclobutanil suspension of the application against bacterial leaf blight of Rice
As can be seen from Table 19, the therapeutic activities of the 20% methylsulfonylmeconazole suspending agent, 95% methylsulfonylmeconazole technical and 20% methylsulfonylmeconazole wettable powders according to the present application were 41.5%, 30.6% and 36.2%, respectively, at a concentration of 200. Mu.g/mL. Wherein, the activity of the 20 percent of the methylsulfonyl myclobutanil suspending agent (41.5 percent) is better than that of the 95 percent of the methylsulfonyl myclobutanil original drug (30.6 percent) and the 20 percent of the methylsulfonyl myclobutanil wettable powder (36.2 percent).
Example 6: field efficacy control test of methylsulfonyl myclobutanil suspending agent developed by plant protection institute of agricultural academy of sciences of Guangdong province
Selection of test subjects, crops and varieties: bacterial leaf blight (Bacterial leafblight caused by Xanthomonas oryzae); rice (variety: yuenongsi silk seedling).
Test agent: 20% methanesulfonyl myclobutanil suspending agent (Guizhou university fine chemical research and development center)
Control agent: 3% of Zhenshengmycin wettable powder (Shenzhen Nop Xin nong Chemie Co., ltd.) and 20% of metconazole wettable powder (Shenzhen Nop Xin nong Chemie Co., ltd.).
TABLE 20 design for test agent
Cell arrangement: six treatments were set up for the test, four replicates, 24 cells total, cells arranged in random granules.
Table 21 cell random arrangement
Cell area or plant number: 20 square meters, about 500-530 plants, repeat times: 4 times.
The using method comprises the following steps: and (5) adding water and spraying.
Applicator instrument: s16 type electric compression sprayer.
The volume of the used materials is as follows: the liquid medicine amount per mu is 45 liters.
Drug data for controlling other pests: no other bactericides are applied during the test, and a polyhedrin suspending agent and 10% imidacloprid WP are added during the application to prevent and control cnaphalocrocis medinalis and rice planthoppers.
Soil data: the soil of the test land is clay loam, has moderate fertility, has 2.84 percent of organic matter content and 5.7 pH value, and has good irrigation and fertilization conditions.
The investigation method comprises the following steps: five diagonal lines of each cell are sampled, 50 plants are investigated at each point, the top leaf and two leaves below the top leaf are investigated for each plant, the total plant number, the disease number and the disease progression are recorded, and the disease index and the control effect are calculated.
Disease grading standard: level 0: no disease; stage 1: the area of the lesion is less than 10% of the area of the leaf; 3 stages: the area of the lesion is 11% -25% of the area of the leaf; 5 stages: the area of the lesion is 26% -45% of the area of the leaf: the 7-level disease spot area is 46% -65% of the leaf area: the area of the disease spots is more than 66% of the leaf area.
Drug effect calculation method
Disease index = (Σ (number of individual disease plants×relative number))/(total number of investigation×9) ×100
Control (%) = (1- (pre-control zone index of disease x post-administration zone index of disease)/(post-control zone index of disease x pre-administration zone index of disease)) ×100
Direct impact on crops: no phytotoxicity phenomenon of the test agent on the rice (Yuenongsi seedlings) to be tested is found in the test period.
Yield and quality of the product: yield and quality were not investigated.
Effects on other pests: no effect of the test agent on other pests was found.
Effects on beneficial organisms: no influence of the test agent on the beneficial organisms was found.
Results and analysis:
table 22 test results of 20% methylsulfonylmeconazole suspending agent for preventing and treating bacterial leaf blight of rice
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The prevention and treatment effects of each treatment on bacterial leaf blight of rice are shown in table 22, the average disease of three tested concentration treatments of 75 g/hectare (25 ml/mu), 120 g/hectare (40 ml/mu) and 150 g/hectare (50 ml/mu) are respectively 3.66, 2.54 and 2.03, the average disease is reduced with the increase of the applied concentration, the average disease difference between the treatments reaches a significant level, compared with the control medicament, the average disease of 120 g/hectare (40 ml/mu) treated with 20% of the methanesulfonyl bacteria suspending agent is not significant compared with the treatment difference of 300 g/hectare (100 g/mu) (2.59) treated with 20% of the penconazole wettable powder of the control medicament, and the average disease of 150 g/hectare (50 ml/mu) treated with 20% of the methanesulfonyl bacteria suspending agent is significantly lower than that of the treatment of the two control medicaments.
The average prevention effect of the treatment of three tested concentrations of 75 g/hectare (25 ml/mu), 120 g/hectare (40 ml/mu) and 150 g/hectare (50 ml/mu) on rice bacterial blight is 67.99%, 76.96% and 83.00%, respectively, the average prevention effect is improved along with the increase of the applied concentration, the average prevention effect difference among the treatments reaches a significant level, compared with the control medicament, the average prevention effect of the treatment of 120 g/hectare (40 ml/mu) of the 20% methylsulfonylmenazole suspending agent is equivalent to the prevention effect of the treatment of 300 g/hectare (100 g/mu) (77.71%) of the 20% methylsulfonylmenazole wettable powder of the control medicament, and the average prevention effect of the treatment of 150 g/hectare (50 ml/mu) of the 20% methylsulfonylmenazole suspending agent is significantly higher than that of the treatment of two control medicaments. The trend of the results of the 19 days after the second application and the 15 days after the third application were substantially similar.
The treatment of three tested concentrations of the 20% methanesulfonyl bacteria suspension agent has good control effect on rice bacterial leaf blight, and is worth further experimental demonstration. In the test process, three tested concentration treatments of the 20% methylsulfonyl bacteria suspension agent have no phytotoxicity phenomenon on rice (Yuenongsi seedlings), the rice leaves grow normally, no lodging phenomenon is seen, and the agent is safe for rice.
Example 7: field efficacy control test of methylsulfonyl myclobutanil suspending agent in Guangxi Zhuang autonomous region pesticide verification
Test object: bacterial leaf blight
Test crop: rice plant
Variety: extra-excellent 524
Crop cultivation and environmental conditions: the test is carried out in a paddy field which is used in a manchurian and late paddy field in a county of Shangzheng and a town of Shangzheng in ShangxiLin county, the mother material of the test field is a tidal mud field formed by developing river alluvium, the organic matter content is 1.7 percent, the pH value is 5.8, the topography is low, the water and fertilizer management is medium, and the nitrogenous fertilizer is applied in a partial manner. The previous crop is rice, the rice growth period is a poking period when the first pesticide is applied, and the field cultivation management of each test plot is basically consistent.
Test agent: 20% of methanesulfonyl bacteria azole suspending agent, which is provided by the research and development center of fine chemical engineering at Guizhou university.
Control agent: 3% of a wettable powder of Zhongshengmycin (commercially available from Redbefon biotechnology Co., dongguan, guangdong); 20% of wettable powder of the leaf-dried azole, jiangxi He Yi chemical Co.
TABLE 23 test design of reagents for test
Table 24 cell random arrangement
Cell area (or number of plants): 25 square meters
Number of repetitions: 4
Pesticide application method
The using method comprises the following steps: spray method
Applicator instrument: the applied medicine applying apparatus is knapsack hand sprayer (Shandong guard brand WS-16), conical single nozzle, and has working pressure of 0.2-0.3MPa and 0.35-0.5L/Min.
The use capacity is as follows: the amount of the applied liquid was 900 liters/hectare for each of the 3 applications.
Drug data for controlling other pests: no bactericide was used during the test, and the used insecticides were: 25% pymetrozine WP and 2% bacteriocin EC.
Soil data: the test field is a tidal mud field formed by developing river alluvium, the organic matter content of the soil is 1.8%, and the pH value is 5.8.
Investigation time and number: disease cardinality was investigated the first time before administration and control effect was investigated 10 days after the 3 rd administration.
The investigation method comprises the following steps: five diagonal points of each cell are sampled, 50 plants are investigated at each point, each plant surveys flag leaves and two leaves below the flag leaves, and the total leaf number and the grading method of the leaf numbers of each stage of diseases are recorded as follows:
level 0: the whole plant is free from diseases; stage 1: the area of the lesion is less than 10% of the area of the leaf; 3 stages: the area of the lesion is about 11-25% of the area of the leaf; 5 stages: the area of the disease spots is about 26 to 45 percent of the area of the leaves; 7 stages: the area of the disease spots is about 46 to 65 percent of the area of the leaves; stage 9: the area of the lesion is more than 65% of the area of the leaf.
The drug effect calculation method comprises the following steps:
disease index = (Σ (number of individual disease plants×relative number))/(total number of investigation×9) ×100
Control (%) = (1- (pre-control zone index of disease x post-administration zone index of disease)/(post-control zone index of disease x pre-administration zone index of disease)) ×100
Direct impact on crops: the experimental process is observed that no other adverse effect of the medicament on the growth of rice is found. Results and analysis:
table 25 test results of 20% Methanesulfonyl myclobutanil suspension for controlling bacterial leaf blight of Rice
15 times after three times of application, the prevention and treatment effects of each treatment on rice bacterial leaf blight are shown in Table 24: the 20% methylsulfonyl bacteria azole suspending agent has the advantages that the prevention effect is improved along with the increase of the using dosage, and the prevention effect among three treatments is obviously different. Compared to the control agent: the control effect of 75 g/hectare of 20% of the methanesulfonyl bacteria azole suspending agent is less than 45 g/hectare of the 3% of the Zhongshengmycin wettable powder and the control effect of 375 g/hectare of 20% of the metconazole wettable powder are obviously different, and the control effect of 120 g/hectare is not obviously different from that of two control agents; the prevention effect of the wettable powder of the Zhongshengmycin with the concentration of 150 g/hectare higher than 3 percent is obviously different from that of the wettable powder of the metconazole with the concentration of 20 percent.
The 20% methylsulfonyl bacteria azole suspending agent has a good control effect on rice bacterial leaf blight, and has no adverse effect on rice growth under test dose. The comprehensive test results suggest that the effective component amount is 120-150 g/hectare, and the application and prevention are started in the early occurrence period of the bacterial blight of rice, and the application is further performed at intervals of about 10 according to the disease condition.
Experimental results of Guangdong province and Guangxi Zhuang nationality show that the control effect of the obtained 20% "methylsulfonylmezole" suspending agent is basically equivalent to that of the traditional medicament, namely, the metconazole, at the dosage of 120 g/hectare, and no obvious difference exists. The consumption per mu is reduced by 60 percent compared with the traditional bactericide.
Claims (10)
1. A methanesulfonyl bacteria azole suspension agent, comprising: 20wt% of methanesulfonyl bacteria oxazole; 3-12 wt% of surfactant; 0.5 to 2.5 weight percent of thickener; 2-6wt% of antifreezing agent; 0.3 to 0.5 weight percent of organic silicon defoamer; the balance of deionized water; the raw materials are subjected to wet sanding to obtain the 20% methanesulfonyl bacteria azole suspending agent.
2. The methanesulfonyl bacteria azole suspension according to claim 1, characterized in that: the suspending agent has a suspended particle size of 5-8 μm.
3. The methanesulfonyl bacteria azole suspension according to claim 1, characterized in that: the surfactant is selected from ionic or nonionic dispersing agents or wetting agents; preferably, the weight percentage of dispersant or wetting agent is 7.5%.
4. A methanesulfonyl bacteria azole suspension according to claim 3, characterized in that: the dispersing agent and the wetting agent consist of a macromolecular amphiphilic anionic non-ionic surfactant compound SC29, sodium dibenzosulfonate HAS024, naphthalene sulfonate sodium salt formaldehyde condensate NNO and sodium paratoluenesulfonate according to the weight ratio of 2:2:2:1.5.
5. The methanesulfonyl bacteria azole suspension according to claim 1, characterized in that: the thickener is selected from one or two of magnesium aluminum silicate SF-40 or xanthan gum.
6. The methanesulfonyl bacteria azole suspension according to claim 1, characterized in that the antifreeze is selected from sodium chloride.
7. The anti-methanesulfonyl bacteria azole suspension according to claim 1, characterized in that: the defoamer is selected from polydimethyl siloxane.
8. The method for preparing the methanesulfonyl bacteria azole suspending agent according to claim 1, characterized in that: and (3) taking the surfactant, the antifreezing agent and the water according to the weight percentage, stirring and dissolving, adding the methanesulfonyl bacteria azole and the thickening agent according to the weight percentage, uniformly mixing under the action of a shearing machine, then pumping the mixed slurry into a sanding machine for grinding, adding the organic silicon defoamer according to the weight percentage, carrying out particle size test every 1 hour, stopping stirring after D90 is smaller than 8 mu m, and filtering to obtain the 20% methanesulfonyl bacteria azole suspending agent.
9. A method for controlling agricultural plant diseases and insect pests, which is characterized by comprising the following steps: allowing the suspension concentrate according to any one of claims 1 to 7 to act on a pest or its living environment, wherein the pest is rice bacterial leaf blight (Xoo), rice bacterial streak (Xoc), citrus canker (Xoc), cabbage black rot, peach perforation, chinese cabbage soft rot, melon fine angle, tobacco bacterial wilt, watermelon fruit rot and tomato bacterial wilt.
10. A method for protecting plants from agricultural pests comprising the step of contacting a pest with the suspension of any one of claims 1-7, said pest being rice bacterial blight (Xoo), bacterial leaf streak (Xoc), citrus canker (Xac), cabbage black rot, peach perforation, cabbage soft rot, melon fine angle, tobacco bacterial wilt, watermelon fruit rot and tomato bacterial wilt.
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