CN104521989A - Compound composition containing 2-(p-fluorophenyl)-5-methanesulfonyl-1,3,4-oxadiazole and amide bactericides and preparation - Google Patents
Compound composition containing 2-(p-fluorophenyl)-5-methanesulfonyl-1,3,4-oxadiazole and amide bactericides and preparation Download PDFInfo
- Publication number
- CN104521989A CN104521989A CN201410788182.3A CN201410788182A CN104521989A CN 104521989 A CN104521989 A CN 104521989A CN 201410788182 A CN201410788182 A CN 201410788182A CN 104521989 A CN104521989 A CN 104521989A
- Authority
- CN
- China
- Prior art keywords
- bacterium azoles
- methylsulfonyl bacterium
- acid amide
- azoles
- amide fungicides
- 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
Abstract
The invention provides a compound composition containing 2-(p-fluorophenyl)-5-methanesulfonyl-1,3,4-oxadiazole and amide bactericides. The compound composition comprises active components A and B, wherein the active component A is 2-(p-fluorophenyl)-5-methanesulfonyl-1,3,4-oxadiazole; the component B is a bactericidal activity compound selected from the amide bactericides; the weight ratio of the component A to the component B is 50:1 to 1:50; and the total weight of the active components is 0.1-90%. After a prompter or filler is added, the compound bactericidal composition can be processed into dosage foams such as wettable powder, water dispersible granules, a suspending agent, a microemulsion, an emulsion in water, granules and emulsifying oil. After the active components A and B are compounded, a remarkable synergistic effect is achieved, various bacterial diseases and most of diseases caused by higher fungi can be effectively prevented and treated, and the effects of increasing efficiency, simultaneously treating diseases, delaying the pesticide resistance, reducing the dosage and the cost, saving hours and labor and the like are achieved.
Description
Technical field
The present invention relates to technical field of pesticide, especially relate to complex composition and the preparation thereof of methylsulfonyl bacterium azoles and acid amide fungicides mixture.
Background technology
Chemical agent is the important means of control bacterial disease and fungal disease, at present still based on chemical control.Some medicaments have good prevention and therapy effect to bacterial disease, but of less types for the chemical agent preventing and treating bacterial disease, and alternative leeway is less.For many years, on the market for preventing and treating medicament mainly copper agent class and the antibiotics of bacterial disease, product category is few, updates slow, and plantation family continuous several times uses similar medicament in a large number, causes the pesticide resistance that pathogenetic bacteria is powerful to these medicaments.Gradually, how effectively prevention and control bacterial disease and fungal disease causing harm to crop, and improve control efficiency, prevent the drug-fast reinforcement of pathogen, become the great difficult problem in plantation family and urgent demand.Therefore, the efficient bactericide of development of new, has great meaning to agricultural production.
For this reason, Guizhou University's independent research also has the new type bactericide " one class preventing and control crop bacteriosis oxadiazole sulfone compound (patent No. is ZL201110314246.2) " of independent intellectual property rights, and its structural formula is:
The step of preparation process of this compound and condition:
(1) the different preparation replacing sour methyl ester intermediate: with different organic acids and absolute methanol for raw material, back flow reaction 6-10 hour under sulphuric acid catalysis, decompression separating methanol, after saturated sodium bicarbonate aqueous solution adjusts ph=7, separatory obtains different methyl formates;
(2) preparation of the different formylhydrazine intermediate replaced: be dissolved in methyl alcohol with different methyl formates, then slowly add 40%-80% hydrazine hydrate, till back flow reaction is complete, separates out the formylhydrazine of different replacement after cooling;
(3) 2-sulfydryl-5-replaces the preparation of-1,3,4-oxadiazole intermediate: with the formylhydrazine of above-mentioned preparation and KOH, carbon disulphide for raw material, ethanol is solvent, and back flow reaction is complete, de-ethanol, adjusts PH=5 to obtain 2-sulfydryl-5-and replaces-1,3,4-oxadiazole;
(4) 2-thioether-5-replaces-1,3, the preparation of 4-oxadiazole intermediate: replace-1 with above-mentioned 2-sulfydryl-5-, 3,4-oxadiazole is raw material, after the water-soluble solution of hydro-oxidation sodium, be obtained by reacting corresponding sulfide compound with 1-2 by the dimethyl sulfate of mole (second) ester or halogenated hydrocarbons etc.;
(5) 2-methyl (ethyl) sulfonyl-5-replaces the preparation of-1,3,4-oxadiazole.
With corresponding thioether for raw material, be dissolved in glacial acetic acid, 2%-7% potassium permanganate solution or 30% hydrogen peroxide oxidation obtain corresponding sulfone compound.
Summary of the invention
Dui Yu oxadiazole sulfone compound, applicant researches and develops further, is selected from the fluorine in halogen atom, R as Rn
2select the methyl of C1-C5 alkyl and get the structural formula of oxadiazole sulfone compound:
Its chemical name is 2-(to fluorophenyl)-5-mesyl-1,3,4-oxadiazole, is called for short methylsulfonyl bacterium azoles.
The concrete syntheti c route of compound methylsulfonyl bacterium azoles is as follows:
(1) to the synthesis of fluorobenzoyl hydrazine
(2) 2-sulfydryl-5-is to the synthesis of fluorophenyl-1,3,4-oxadiazole
(3) 2-Dimethyl sulfide-5-is to the synthesis of fluorophenyl-1,3,4-oxadiazole
(4) 2-(to fluorophenyl)-5-mesyl-1,3,4-oxadiazole target compound is prepared
Applicant studies discovery further, and methylsulfonyl bacterium azoles is the control bacterial disease medicament of novel structure, by suppressing the synthesis of pathogene energy, the growth of anti-bacteria and breeding.Methylsulfonyl bacterium azoles has the feature of interior suction, conduction, and after infiltration blade epidermis, energy transporting is to other positions of same blade.A large amount of isolated tests shows, methylsulfonyl bacterium azoles has good inhibitory action to causing the various pathogenetic bacterias of phytobacterial disease, and namely directly anti-bacteria is bred.Through repeatedly pot experiment and field control effectiveness test checking, show that methylsulfonyl bacterium azoles all has good control efficiency to crop bacterial disease, especially good control effect is all had to bacterial blight of rice, slice disease, tobacco bacterial wilt, bacterial wilt of tomato, citrus bacterial canker disease etc., and plant growth can be stimulated to a certain extent healthy and strong, improve the resistance of crop.This compound has efficiently, the feature of wide spectrum, use safety, is a bactericide having much exploitation potential quality.
Acid amide fungicides is the organic compound containing amide structure in a class chemical constitution, and amides compound has had the history of decades as bactericide, so far existing more than 30 kind commercialization.Acid amide fungicides still occupies considerable status in bactericide market, the world, but this series bactericidal agent action site is more single, current pathogen has also produced certain pesticide resistance to this series bactericidal agent, therefore, resists the effective way with delaying drug resistance development by composite channel by being.Acid amide fungicides is mainly fluorine azoles bacterium acid amides, fluorine pyrrole bacterium acid amides, Boscalid, metalaxyl, flutolanil, mandipropamid, flusulfamide, Silthiopham, fluopicolide, zoxamide, fenfuram, fenoxanil, fenhexamid, Guardian at present.
Fluorine azoles bacterium acid amides (fluxapyroxad): CAS 907204-31-3, chemical name is 3-(difluoromethyl)-1-methyl-N-(3,4,5-trifluoro [1, the two benzene of 1-]-2-base))-1H-pyrazole-4-carboxamide, succinate dehydrogenase inhibitors, is developed by BASF Aktiengesellschaft.
Fluorine pyrrole bacterium acid amides (fluopyram): CAS 658066-35-4, chemical name is N-{2-[the chloro-5-of 3-(trifluoromethyl)-2-pyridine radicals] ethyl-α, α, the fluoro-O-toluamide of α-three, a kind of new benzamides series bactericidal agent of Bayer Bitterfeld GmbH crop science company exploitation, is mainly used in broad leaf crop being prevented and treated the microbial disease of ascus.
Boscalid (boscalid): CAS 188425-85-6, chemical name is the chloro-N-of 2-(4 '-chlorodiphenyl-2-base) vitamin PP, Boscalid is the Novel tobacco acid amide fungicides developed by BASF Aktiengesellschaft, is mainly used in preventing and treating powdery mildew, gray mold, various rot, brown rot and root rot etc.
Metalaxyl (metalaxyl): CAS 57837-19-1, chemical name is D, L-N-(2,6-3,5-dimethylphenyl)-N-(2-methoxyl group acetyl) methyl lactamine, interior absorption special efficacy bactericide, has protection and therapeutic action.
Flutolanil (flutolanil): CAS 66332-96-5, chemical name is 37 1 isopropoxy-2-(trifluoromethyl) benzanilides, the systemic fungicide of Amada Co., Ltd.'s exploitation, be used for preventing and treating the fungus-caused disease of some Basidiomycetes, and the rice banded sclerotial blight that rhizoctonia causes.
Mandipropamid (mandipropamid): CAS 374726-62-2, chemical name is 2-(the chloro-phenyl of 4-)-N-[2-(3-methoxyl group-4-(2-propargyl alcoholate)-phenyl-ethane base]-2-(2-propargyl alcoholate)-acetamide, all has good preventive effect to large absolutely number by ovum microbial leaf portion and fruit disease.
Flusulfamide (flusulfamide): CAS 106917-52-6, chemical name is toluol sulfonanilide between 2 ', 4-bis-chloro-α, α, α-three fluoro-4 '-nitro, is a kind of bactericide being mainly used in soil treatment.
Silthiopham (silthiopham): CAS 175217-20-6, chemical name is N-pi-allyl 4,5-dimethyl-2-trimethyl silicane thiophene-3-carboxylic acid amides, and have good prolection, the longevity of residure is long.Main as seed treatment.
Fluopicolide (fluopicolide): CAS 239110-15-7; chemical name is 2; the chloro-N-of 6-bis-[(the chloro-5-trifluoromethyl of 3--2-pyridine radicals) methyl] benzamide; this medicine protectiveness is good, permeability is strong; there is higher biologically active to Oomycete fungal disease, there is good control efficiency.
Zoxamide (zoxamide): CAS 156052-68-5; chemical name is 3; the chloro-N-of 5-bis-(the chloro-1-ethyl of 3--1-methyl-2-oxopropyl)-4-methyl; be that one has efficient protective fungicide, there is long lasting period and good resistance of rainwater washing against performance.
Fenfuram (fenfuram): CAS 24691-80-3, chemical name is 2-methylfuran-3-carboxylic acyl, is a kind of seed dressing with the new replacement mercurial of systemic action, has excellent activity to the most germs of Basidiomycetes.
Fenoxanil (fenoxanil): CAS 115852-48-7, chemical name is N-(1-itrile group-1,2-dimethyl propyl)-2-(2,4-dichlorophenoxy) propionamide is a kind of acid amide fungicides of current China recommendation on paddy rice.
Fenhexamid (fenhexamid): CAS 126833-17-8, chemical formula C14H17Cl2NO2, a kind of acid amide fungicides, seed treatment, seedling growing box inorganic agent, belongs to interior suction, protective fungicide.
Guardian (ethaboxam): CAS 162650-77-3, chemical name is (RS)-N-(alpha-cyano-2-thenyl)-4-ethyl-2-(ethylamino-) thiazole-5-formamide, it is the thiazole amide bactericide of L G Life Sciences of Korea S exploitation, registration is obtained, main control oomycetes disease in Korea S.
In view of this, for the deficiency that prior art exists, the object of the invention is to provide a kind of complex composition containing methylsulfonyl bacterium azoles and acid amide fungicides, this complex composition has obvious synergistic function relative to single dose, improve bactericidal activity, reduce dosage, reduce costs, expanding prevention is composed, and also delays the pesticide resistance of pathogen.
In order to actual arrival object of the present invention, the technical scheme taked is:
The invention provides a kind of complex composition containing methylsulfonyl bacterium azoles and acid amide fungicides, described complex composition is made up of active components A and B; Described active components A is methylsulfonyl bacterium azoles, and its chemical name is 2-(to fluorophenyl)-5-mesyl-1,3,4-oxadiazole; Active component B is selected from the one in following acid amide fungicides: fluorine azoles bacterium acid amides, fluorine pyrrole bacterium acid amides, Boscalid, metalaxyl, flutolanil, mandipropamid, flusulfamide, Silthiopham, fluopicolide, zoxamide, fenfuram, fenoxanil, fenhexamid, Guardian.
The complex composition of above-described methylsulfonyl bacterium azoles and acid amide fungicides, in order to ensure that bactericidal composition has better synergistic effect and control efficiency, the weight ratio of methylsulfonyl bacterium azoles and acid amide fungicides is 50:1 to 1:50.
The complex composition of above-described methylsulfonyl bacterium azoles and acid amide fungicides, in order to ensure that bactericidal composition has better synergistic effect and control efficiency, the preferred 10:1 to 1:20 of weight ratio of methylsulfonyl bacterium azoles and acid amide fungicides.
The complex composition of above-described methylsulfonyl bacterium azoles and acid amide fungicides, preferably, described acid amide fungicides is selected from the one in fluorine azoles bacterium acid amides, fluorine pyrrole bacterium acid amides, Boscalid, metalaxyl.
The present invention also provides the preparation containing methylsulfonyl bacterium azoles and acid amide fungicides, and described preparation is by weight containing the bactericidal composition according to claim 1 of 0.1-90%, and all the other are agriculturally acceptable carrier and auxiliary agent, are then prepared into disinfectant use in agriculture.
The above-described preparation containing methylsulfonyl bacterium azoles and acid amide fungicides, preferably, the according to claim 1 bactericidal composition of described disinfectant use in agriculture by weight containing 1-80%.
Above-described bactericide also comprises in pesticidal preparations the functional aid and thinner that meet agricultural use.That is, described bactericide can add functional aid, thinner and other auxiliary material, can be mixed with the preparation of wetting powder, suspending agent, microemulsion, aqueous emulsion, water dispersible granules, granule, seed coat agent, soluble powder, soluble liquid, suspension emulsion, dry suspending agent, ultra low volume liquids or other formulation.
In embodiments more provided by the invention, the formulation that bactericide can be prepared is preferably wetting powder, water dispersible granules, suspending agent, aqueous emulsion, microemulsion, granule, missible oil.
Carrier comprises solid carrier and liquid-carrier.
Solid carrier comprises white carbon, kaolin, water, potter's clay, bentonite, diatomite, earth powder, precipitated calcium carbonate, montmorillonite, urea, borax.
Liquid-carrier comprises dimethylbenzene, methyl oleate, solvent naphtha, ethanol, cyclohexanone, ethyl acetate, 1-METHYLPYRROLIDONE, dimethyl sulfoxide (DMSO), methyl naphthalene, water.
As preferably, solvent of the present invention is one or more in ethanol, solvent naphtha 200#, solvent naphtha 150#, methyl naphthalene, N methyl pyrrolidone.
In embodiments more provided by the invention, described auxiliary agent comprises emulsifier, wetting dispersing agent, also can add other conventional functionality auxiliary agents such as antifreezing agent, thickener, defoamer, disintegrant, film forming agent if desired.
Emulsifier comprises nonionic emulsifier and anionic emulsifier.The preferred polyoxyethylene nonylphenol ether of nonionic emulsifier, dibenzyl xenyl APEO, fatty alcohol-polyoxyethylene ether, styryl phenyl APEO, alkylphenol polyoxyethylene sulfosuccinates, phenethyl phenyl polyoxyethylene poly-oxygen propylene aether, AMS phenol formaldehyde resin APEO, alkyl phenol formaldehyde resin polyoxyethylene ether, terminal hydroxy group polyoxyethylene poly-oxygen propylene aether, alkyl phenol polyoxyethylene polyoxypropylene ether, styrylphenol formaldehyde resin polyoxyethylene poly-oxygen propylene aether, castor oil polyoxyethylene ether, styrylphenol formaldehyde resin PULLRONIC F68 block type polyethers.Anionic emulsifier mainly comprises calcium dodecyl benzene sulfonate, triphen ethyl phenol polyoxy ether phosphate amine salt, thermally coupled distillation columns amine salt, castor oil polyoxyethylene ether phosphate amine salt.
Wetting agent is selected from fatty alcohol-polyoxyethylene ether, naphthalene sulfonate, lauryl sodium sulfate, one or more combinations in alkyl phenol resin polyoxyethylene ether sulfate, fatty acid amide N-metilsulfate, alkylbenzenesulfonate, lauryl alcohol polyethylene glycol oxide base ether, tallow ethyoxyl amine salt, Negel, sldium lauryl sulfate, neopelex, sodium butylnaphthalenesulfonate.
Dispersant is selected from acrylate homopolymer sodium salt, maleic acid disodium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, rosin segmented APEO polyoxypropylene ether sulfonate, terminal hydroxy group polyoxyethylene poly-oxygen propylene aether block copolymer, triphen ethyl phenol polyoxyethylene ether phosphate, fatty alcohol-polyoxyethylene ether phosphoric acid, to hydroxyphenyl lignin sulfonic acid sodium salt, di-2-ethylhexylphosphine oxide methyl naphthalene sulfonic acid, alkylaryl APEO, fatty acid glyceride APEO, aryl phenol polyoxyethylene succinate sulfonate, octylphenol polyethylene oxyethylene group ether sulfate, the phonetic formaldehyde condensation products sodium sulfate salt of alkylphenol-polyethenoxy, polyoxyethylene carboxylate, one or more in diisobutyl naphthalene sulfonic acids.
Thickener be selected from xanthans, aluminium-magnesium silicate, gum Arabic, pectin any one or a few.
Antifreezing agent be selected from glycerine, propane diols, ethylene glycol, isopropyl alcohol, urea any one or a few.
Disintegrant is selected from: any one or a few in potassium chloride, sodium chloride, ammonium chloride, sodium phosphate, potassium phosphate, ammonium phosphate, potassium sulfate, ammonium sulfate, sodium sulphate, potash, ammonium carbonate, sodium carbonate, diammonium phosphate, calcium chloride, urea, bentonite.
Above-mentioned bactericidal composition can be used for control crop bacterial disease and fungal disease.
Bactericide of the present invention can be used by commonsense method, as spraying cauline leaf process, also can soil treatment, and such as solid root spreads fertilizer over the fields or liquid fills with root, can also dress seed, to soak seed or seed pelleting uses.
Bactericidal composition of the present invention and bactericide have following beneficial effect relative to prior art:
(1) bactericidal composition of the present invention, in certain ratio range, mixture shows excellent synergistic effect, and the co-toxicity coefficient preventing and treating crop pest is greater than 120, and the bactericidal effect of the composition of mixture is significantly improved compared with its single dose.
(2) reduce using dosage, reduce peasant's drug cost.
(3) utilize two kinds of active components to carry out reasonably mixture to the different mode of action of pathogen, the different mechanism of action, both extended the Pesticide use life-span, delayed again the drug-fast generation of pathogen.
Embodiment
Below by embodiment, the invention will be further described.It should be noted that, the embodiment of the present invention is only used for the present invention is described, instead of limitation of the present invention.The former medicine of methylsulfonyl bacterium azoles used in the present invention is provided by Guizhou University, and other former medicines used and preparation are commercial.In the application if no special instructions, percentage is all weight percentage.
One, the preparation of wetting powder
Methylsulfonyl bacterium azoles, acid amide fungicides, wetting agent, dispersant, white carbon, filler are mixed, after airslide disintegrating mill is pulverized, stirs 30min, obtain the wetting powder of bactericide of the present invention.
Two, the preparation of water dispersible granules
Methylsulfonyl bacterium azoles, acid amide fungicides, wetting agent, dispersant, white carbon, filler are mixed, after airslide disintegrating mill is pulverized, stir 30min, mediate with water, after add in fluidized-bed granulation dryer and carry out granulation, drying, obtain the water dispersible granules of bactericide of the present invention.
Three, the preparation of microemulsion
Methylsulfonyl bacterium azoles and acid amide fungicides are added in liquid-carrier, after stirring, obtains transparent mixed liquor; In above-mentioned mixed liquor, add emulsifier, be stirred to emulsifier and dissolve completely; Under the mixing speed of 50r/min, deionized water is joined and is above-mentionedly dissolved with in the mixed liquor of emulsifier, at ambient temperature, stir 30min, obtain the micro emulsion of homogeneous transparent; In above-mentioned micro emulsion, add antifreezing agent, stir, obtain the microemulsion of bactericide of the present invention.Formula composition:
Four, the preparation of suspending agent
By emulsifier, antifreezing agent, thickener, deionized water mixing, mix through high speed shear, add methylsulfonyl bacterium azoles, acid amide fungicides successively, abrading-ball 2 ~ 3 hours in ball crusher, the suspending agent of obtained bactericide of the present invention.
Five, the preparation of missible oil
Active ingredient methylsulfonyl bacterium azoles and acid amide fungicides are added liquid-carrier and emulsifier, after stirring, obtains transparent mixed liquor, be i.e. the missible oil of obtained bactericide of the present invention.
Six, the preparation of aqueous emulsion
By Methanesulfomide azoles, acid amide fungicides, emulsifier, liquid-carrier, be dissolved into uniform oil phase; Part water, antifreezing agent are mixed uniformly aqueous phase; While high-speed stirred, oil phase is added aqueous phase in a kettle., open clipper and carry out high speed shear, and add remaining water and supply, shear about half an hour, form aqueous emulsion.The i.e. aqueous emulsion of obtained bactericide of the present invention.
Seven, the preparation of granule
Methylsulfonyl bacterium azoles, acid amide fungicides, auxiliary agent, solid carrier are mixed in airtight compounding kettle, adopts the granulation of coating method, after screening, drying, inspection, namely obtain the granule of bactericide of the present invention.
BIOLOGICAL ACTIVITY EXAMPLES
In order to clear and definite methylsulfonyl bacterium azoles mixed with acid amide fungicides time control efficiency to several bacterial disease and fungal disease, and to compare with single dose, find composite meaning, We conducted Toxicity Determination and field control effectiveness test.
Toxicity Determination:
Following indoor biometrics test adopts the abundant method of Sun Yun to calculate co-toxicity coefficient (CTC) and evaluates mixed effect.
Toxicity index TI (B)=(EC of standard agent A
50the EC of ÷ B agent
50) × 100
Actual toxicity index ATI (AB)=(EC of A
50the EC of ÷ AB
50) × 100
Theoretical toxicity index TTI (AB)=TI (the A) × A percentage+TI (B) in the mixture × percentage of B in mixture
Actual measurement toxicity index (ATI)=(standard agent EC
50÷ reagent agent EC
50) × 100
In theoretical toxicity index (TTI)=A medicament toxicity index × mixture A percentage composition+B medicament toxicity index × mixture in the percentage composition of B
Co-toxicity coefficient (CTC)=[the theoretical toxicity index (TTI) of mixture actual measurement toxicity index (ATI) ÷ mixture] × 100
Evaluation criterion: (CTC) >=120 show as synergistic effect; CTC≤80 show as antagonism; 80 < CTC < 120 show as summation action.
Toxicity Determination embodiment one:
Below that methylsulfonyl bacterium azoles is tested with fluorine azoles bacterium acid amides, fluorine pyrrole bacterium acid amides, flutolanil, mandipropamid, flusulfamide, the composite Toxicity Determination to bacterial leaf streak of rice of Silthiopham respectively.
Adopt in vitro nephelometry to carry out Toxicity Determination, select bacterial leaf streak of rice to be target target, repeat 4 times, latter 24 hours check results of investigating.Be independent variable x with drug concentration (mg/l) logarithm value, with the probit value of the corrected mortality of its correspondence for dependent variable y, set up virulence regression equation respectively, obtain the co-toxicity coefficient of two single dose different ratio, the results are shown in Table 17.Experimental technique adopts the abundant method of Sun Yun to calculate co-toxicity coefficient (CTC) and evaluates mixed effect.
Concrete grammar: adopt in vitro Nephelometric Determination, design concentration on the basis of preliminary experiment, each medicament is joined respectively in NA liquid nutrient medium, gradient dilution makes pastille medium, Inoculated Rice Xanthomonas campestris PV.oryzicola is placed on 28 DEG C of about shaken cultivation 24h, its turbidity (turbidity and bacterium amount be changing into positive correlation) is measured with transmissometer, the inhibiting rate that each chemicals treatment breeds bacterial growth is calculated according to the turbidity of blank and the turbidity of process, by the linear regression analysis between the probit value of inhibiting rate and the logarithm value of serial drug concentration, obtain the EC50 value of each medicament, CTC value.The results are shown in Table 1 ~ table 4.
The joint toxicity measuring result of table 1 methylsulfonyl bacterium azoles and the composite control bacterial leaf streak of rice of fluorine azoles bacterium acid amides
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 10.65 | 100.00 | / | / |
| Fluorine azoles bacterium acid amides (B) | 173.26 | 6.15 | / | / |
| A:B＝50:1 | 8.73 | 121.99 | 98.16 | 124.28 |
| A:B＝40:1 | 8.12 | 131.16 | 97.71 | 134.23 |
| A:B＝30:1 | 7.56 | 140.87 | 96.97 | 145.27 |
| A:B＝20:1 | 7.10 | 150.00 | 95.53 | 157.02 |
| A:B＝10:1 | 7.05 | 151.06 | 91.47 | 165.16 |
| A:B＝5:1 | 7.19 | 148.12 | 84.36 | 175.59 |
| A:B＝2.5:1 | 7.58 | 140.50 | 73.18 | 191.98 |
| A:B＝1:1 | 9.38 | 113.54 | 53.07 | 213.93 |
| A:B＝1:2.5 | 17.05 | 62.46 | 32.96 | 189.50 |
| A:B＝1:5 | 27.29 | 39.03 | 21.79 | 179.11 |
| A:B＝1:10 | 42.18 | 25.25 | 14.68 | 172.01 |
| A:B＝1:20 | 62.18 | 17.13 | 10.62 | 161.34 |
| A:B＝1:30 | 76.46 | 13.93 | 9.17 | 151.82 |
| A:B＝1:40 | 89.44 | 11.91 | 8.44 | 141.15 |
| A:B＝1:50 | 106.12 | 10.04 | 7.99 | 125.65 |
| A:B＝1:60 | 118.81 | 8.96 | 7.69 | 116.64 |
From table 1, methylsulfonyl bacterium azoles and the composite control bacterial leaf streak of rice of fluorine azoles bacterium acid amides are (50 ~ 1) by weight: time between (1 ~ 50), and the CTC value of each process is all greater than 120, and composite both showing have synergistic effect.Especially, be (10 ~ 1) by weight: time between (1 ~ 20), the CTC of each process is all greater than 161, and synergy is particularly remarkable.
The joint toxicity measuring result of table 2 methylsulfonyl bacterium azoles and the composite control bacterial leaf streak of rice of fluorine pyrrole bacterium acid amides
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 11.03 | 100.00 | / | / |
| Fluorine pyrrole bacterium acid amides (C) | 194.39 | 5.67 | / | / |
| A:C＝50:1 | 8.93 | 123.52 | 98.15 | 125.84 |
| A:C＝40:1 | 8.67 | 127.22 | 97.70 | 130.22 |
| A:C＝30:1 | 7.79 | 141.59 | 96.96 | 146.04 |
| A:C＝20:1 | 7.48 | 147.46 | 95.51 | 154.39 |
| A:C＝10:1 | 7.39 | 149.26 | 91.42 | 163.25 |
| A:C＝5:1 | 7.59 | 145.32 | 84.28 | 172.43 |
| A:C＝2.5:1 | 8.25 | 133.70 | 73.05 | 183.02 |
| A:C＝1:1 | 9.60 | 114.90 | 52.84 | 217.45 |
| A:C＝1:2.5 | 17.54 | 62.88 | 32.62 | 192.75 |
| A:C＝1:5 | 27.73 | 39.78 | 21.40 | 185.91 |
| A:C＝1:10 | 42.81 | 25.77 | 14.25 | 180.82 |
| A:C＝1:20 | 66.92 | 16.48 | 10.17 | 162.13 |
| A:C＝1:30 | 79.34 | 13.90 | 8.72 | 159.48 |
| A:C＝1:40 | 92.78 | 11.89 | 7.97 | 149.07 |
| A:C＝1:50 | 116.28 | 9.49 | 7.52 | 126.08 |
| A:C＝1:60 | 129.67 | 8.51 | 7.22 | 117.81 |
From table 2, it is active that methylsulfonyl bacterium azoles and fluorine pyrrole bacterium acid amides composite control bacterial leaf streak of rice have good indoor virulence, be (50 ~ 1) by weight: time between (1 ~ 50), the CTC value of each process is all greater than 120, and composite both showing have synergistic effect.Especially, when weight ratio is (10 ~ 1): time between (1 ~ 20), the CTC of each process is all greater than 162, and synergy is particularly remarkable.
Table 3 methylsulfonyl bacterium azoles respectively with the joint toxicity measuring result of flutolanil, the composite control bacterial leaf streak of rice of mandipropamid
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 10.13 | 100.00 | / | / |
| Flutolanil (F) | 175.18 | 5.78 | / | / |
| Mandipropamid (G) | 177.41 | 5.71 | / | / |
| A:F＝50:1 | 8.16 | 124.14 | 98.15 | 126.48 |
| A:F＝35:1 | 7.59 | 133.47 | 97.38 | 137.05 |
| A:F＝20:1 | 7.10 | 142.68 | 95.51 | 149.38 |
| A:F＝10:1 | 6.85 | 147.88 | 91.43 | 161.74 |
| A:F＝5:1 | 6.94 | 145.97 | 84.30 | 173.16 |
| A:F＝2.5:1 | 7.13 | 142.08 | 73.08 | 194.41 |
| A:F＝1:1 | 8.42 | 120.31 | 52.89 | 227.46 |
| A:F＝1:2.5 | 16.24 | 62.38 | 32.70 | 190.74 |
| A:F＝1:5 | 25.57 | 39.62 | 21.49 | 184.39 |
| A:F＝1:10 | 40.57 | 24.97 | 14.35 | 174.03 |
| A:F＝1:20 | 61.07 | 16.59 | 10.27 | 161.53 |
| A:F＝1:35 | 85.16 | 11.90 | 8.40 | 141.61 |
| A:F＝1:50 | 105.83 | 9.57 | 7.63 | 125.45 |
| A:G＝50:1 | 8.56 | 118.34 | 98.15 | 120.57 |
| A:G＝35:1 | 7.81 | 129.71 | 97.38 | 133.19 |
| A:G＝20:1 | 7.28 | 139.15 | 95.51 | 145.69 |
| A:G＝10:1 | 6.92 | 146.39 | 91.43 | 160.11 |
| A:G＝5:1 | 6.80 | 148.97 | 84.28 | 176.75 |
| A:G＝2.5:1 | 7.13 | 142.08 | 73.06 | 194.46 |
| A:G＝1:1 | 8.40 | 120.60 | 52.85 | 228.16 |
| A:G＝1:2.5 | 15.70 | 64.52 | 32.65 | 197.62 |
| A:G＝1:5 | 26.19 | 38.68 | 21.42 | 180.53 |
| A:G＝1:10 | 41.11 | 24.64 | 14.28 | 172.54 |
| A:G＝1:20 | 60.48 | 16.75 | 10.20 | 164.21 |
| A:G＝1:35 | 86.17 | 11.76 | 8.33 | 141.14 |
| A:G＝1:50 | 109.13 | 9.28 | 7.56 | 122.80 |
From table 3, methylsulfonyl bacterium azoles all has good indoor virulence respectively with flutolanil, mandipropamid composite control bacterial leaf streak of rice active, be (50 ~ 1) by weight: time between (1 ~ 50), the CTC value of each process is all greater than 120, shows that methylsulfonyl bacterium azoles is composite with flutolanil, mandipropamid respectively and all shows obvious synergistic effect afterwards.Especially, when weight ratio is (10 ~ 1): time between (1 ~ 20), the CTC of each process is all greater than 160, and synergy is particularly remarkable.
Table 4 methylsulfonyl bacterium azoles respectively with the joint toxicity measuring result of flusulfamide, the composite control bacterial leaf streak of rice of Silthiopham
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 10.47 | 100.00 | / | / |
| Flusulfamide (B1) | 136.07 | 7.69 | / | / |
| Silthiopham (B2) | 157.19 | 6.66 | / | / |
| A:H＝50:1 | 8.58 | 122.03 | 98.19 | 124.28 |
| A:H＝35:1 | 7.88 | 132.87 | 97.44 | 136.36 |
| A:H＝20:1 | 7.50 | 139.60 | 95.60 | 146.02 |
| A:H＝10:1 | 7.03 | 148.93 | 91.61 | 162.58 |
| A:H＝5:1 | 7.17 | 146.03 | 84.62 | 172.57 |
| A:H＝2.5:1 | 7.39 | 141.68 | 73.63 | 192.43 |
| A:H＝1:1 | 9.14 | 114.55 | 53.85 | 212.73 |
| A:H＝1:2.5 | 15.48 | 67.64 | 34.07 | 198.53 |
| A:H＝1:5 | 25.74 | 40.68 | 23.08 | 176.25 |
| A:H＝1:10 | 38.56 | 27.15 | 16.09 | 168.80 |
| A:H＝1:20 | 53.63 | 19.52 | 12.09 | 161.48 |
| A:H＝1:35 | 78.33 | 13.37 | 10.26 | 130.30 |
| A:H＝1:50 | 87.99 | 11.90 | 9.50 | 125.19 |
| A:I＝50:1 | 8.54 | 122.60 | 98.17 | 124.89 |
| A:I＝35:1 | 7.37 | 142.06 | 97.41 | 145.84 |
| A:I＝20:1 | 7.00 | 149.57 | 95.56 | 156.53 |
| A:I＝10:1 | 6.87 | 152.40 | 91.51 | 166.53 |
| A:I＝5:1 | 6.94 | 150.86 | 84.44 | 178.66 |
| A:I＝2.5:1 | 7.64 | 137.04 | 73.33 | 186.88 |
| A:I＝1:1 | 8.15 | 128.47 | 53.33 | 240.89 |
| A:I＝1:2.5 | 15.98 | 65.52 | 33.33 | 196.58 |
| A:I＝1:5 | 25.21 | 41.53 | 22.22 | 186.93 |
| A:I＝1:10 | 38.79 | 26.99 | 15.15 | 178.21 |
| A:I＝1:20 | 56.88 | 18.41 | 11.11 | 165.75 |
| A:I＝1:35 | 83.32 | 12.57 | 9.25 | 135.80 |
| A:I＝1:50 | 101.03 | 10.36 | 8.49 | 122.05 |
From table 4, methylsulfonyl bacterium azoles all has good indoor virulence respectively with flusulfamide, Silthiopham composite control bacterial leaf streak of rice active, be (50 ~ 1) by weight: time between (1 ~ 50), CTC value is all greater than 120, shows that methylsulfonyl bacterium azoles is composite with flusulfamide, Silthiopham respectively and all shows obvious synergistic effect afterwards.Especially, when by weight be (10 ~ 1): time between (1 ~ 20), the CTC respectively processed all is greater than 160, and synergy is particularly remarkable.
Toxicity Determination embodiment two:
Below that methylsulfonyl bacterium azoles is tested with Boscalid, metalaxyl, fluopicolide, zoxamide, fenfuram, fenoxanil, fenhexamid, the composite Toxicity Determination to bacterial wilt of peanut of Guardian respectively.
After being activated on NA medium by bacterial wilt of peanut pathogen, be made into bacterium stoste with sterile water, the clump count grown after bacterium stoste is diluted to coated plate 100ul is the bacteria suspension of about 100, for subsequent use.
Get 400ul bacteria suspension and equivalent agricultural chemicals single dose mixes, 100ul is got with liquid-transfering gun, be placed on ready-made NA flat board, with sterilized " L " shape glass bar by even for bacteria suspension coating, cultivate 48h for 28 DEG C, counting clump count, and press formulae discovery bacteriostasis rate, bacterium colony inhibiting rate (%)=(contrast clump count-process clump count)/contrast clump count × 100, often process repetition 4 times, replace pesticide-treated for contrast with sterile water, the result of gained adopts Excel software analysis, calculate the EC50 of each medicament, and calculate co-toxicity coefficient according to the abundant method of Sun Yun.The results are shown in Table 5 ~ table 9.
The Toxicity Determination result of table 5 methylsulfonyl bacterium azoles and the composite control bacterial wilt of peanut of Boscalid
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 13.48 | 100.00 | / | / |
| Boscalid (D) | 103.62 | 13.01 | / | / |
| A:D＝50:1 | 11.10 | 121.44 | 98.29 | 123.55 |
| A:D＝40:1 | 10.26 | 131.38 | 97.88 | 134.23 |
| A:D＝30:1 | 9.16 | 147.16 | 97.19 | 151.41 |
| A:D＝20:1 | 8.94 | 150.78 | 95.86 | 157.30 |
| A:D＝10:1 | 8.83 | 152.66 | 92.09 | 165.77 |
| A:D＝5:1 | 9.17 | 147.00 | 85.50 | 171.93 |
| A:D＝2.5:1 | 9.57 | 140.86 | 75.15 | 187.45 |
| A:D＝1:1 | 10.84 | 124.35 | 56.50 | 220.08 |
| A:D＝1:2.5 | 19.06 | 70.72 | 37.86 | 186.79 |
| A:D＝1:5 | 28.78 | 46.84 | 27.51 | 170.27 |
| A:D＝1:10 | 37.96 | 35.51 | 20.92 | 169.77 |
| A:D＝1:20 | 47.49 | 28.38 | 17.15 | 165.50 |
| A:D＝1:30 | 59.54 | 22.64 | 15.82 | 143.15 |
| A:D＝1:40 | 64.20 | 21.00 | 15.13 | 138.77 |
| A:D＝1:50 | 75.59 | 17.83 | 14.71 | 121.19 |
| A:D＝1:60 | 79.96 | 16.86 | 14.44 | 116.79 |
From table 5, it is active that methylsulfonyl bacterium azoles and Boscalid composite control bacterial wilt of peanut have higher indoor virulence, be (50 ~ 1) by weight: between (1 ~ 50), the CTC value of each process is all greater than 120, both explanations are composite has obvious synergistic effect, and weight ratio its synergy degree different is also different, when weight ratio is (20 ~ 1): time between (1 ~ 10), CTC is all greater than 165, and synergy highly significant is described.
Table 6 methylsulfonyl bacterium azoles and the composite Toxicity Determination result to bacterial wilt of peanut of metalaxyl
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 14.51 | 100.00 | / | / |
| Metalaxyl (E) | 51.67 | 28.08 | / | / |
| A:E＝50:1 | 11.71 | 123.91 | 98.59 | 125.68 |
| A:E＝40:1 | 10.46 | 138.72 | 98.25 | 141.20 |
| A:E＝30:1 | 9.59 | 151.30 | 97.68 | 154.90 |
| A:E＝20:1 | 9.47 | 153.22 | 96.58 | 158.65 |
| A:E＝10:1 | 9.41 | 154.20 | 93.46 | 164.98 |
| A:E＝5:1 | 9.65 | 150.36 | 88.01 | 170.84 |
| A:E＝2.5:1 | 9.78 | 148.36 | 79.45 | 186.73 |
| A:E＝1:1 | 10.56 | 137.41 | 64.04 | 214.56 |
| A:E＝1:2.5 | 15.04 | 96.48 | 48.63 | 198.39 |
| A:E＝1:5 | 19.54 | 74.26 | 40.07 | 185.33 |
| A:E＝1:10 | 24.26 | 59.81 | 34.62 | 172.76 |
| A:E＝1:20 | 27.58 | 52.61 | 31.51 | 166.98 |
| A:E＝1:30 | 30.82 | 47.08 | 30.40 | 154.86 |
| A:E＝1:40 | 34.38 | 42.20 | 29.84 | 141.46 |
| A:E＝1:50 | 39.80 | 36.46 | 29.49 | 123.62 |
| A:E＝1:60 | 42.46 | 34.17 | 29.26 | 116.79 |
From table 6, it is active that methylsulfonyl bacterium azoles and metalaxyl composite control bacterial wilt of peanut have higher indoor virulence, be (50 ~ 1) by weight: between (1 ~ 50), the CTC value of each process is all greater than 120, both explanations are composite has obvious synergistic effect, and weight ratio its synergy degree different is also different, when weight ratio is (20 ~ 1): time between (1 ~ 10), the CTC of each process is all greater than 164, and synergy highly significant is described.
Table 7 methylsulfonyl bacterium azoles respectively with fluopicolide, the composite Toxicity Determination result to bacterial wilt of peanut of zoxamide
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 10.47 | 100.00 | / | / |
| Fluopicolide (J) | 65.21 | 16.06 | / | / |
| Zoxamide (K) | 74.38 | 14.08 | / | / |
| A:J＝50:1 | 8.58 | 122.03 | 98.35 | 124.07 |
| A:J＝35:1 | 7.90 | 132.53 | 97.67 | 135.70 |
| A:J＝20:1 | 7.21 | 145.21 | 96.00 | 151.26 |
| A:J＝10:1 | 6.84 | 153.07 | 92.37 | 165.72 |
| A:J＝5:1 | 7.25 | 144.41 | 86.01 | 167.90 |
| A:J＝2.5:1 | 7.55 | 138.68 | 76.02 | 182.43 |
| A:J＝1:1 | 8.96 | 116.85 | 58.03 | 201.37 |
| A:J＝1:2.5 | 13.12 | 79.80 | 40.04 | 199.31 |
| A:J＝1:5 | 19.08 | 54.87 | 30.05 | 182.63 |
| A:J＝1:10 | 25.14 | 41.65 | 23.69 | 175.82 |
| A:J＝1:20 | 31.79 | 32.93 | 20.05 | 164.24 |
| A:J＝1:35 | 39.04 | 26.82 | 18.39 | 145.85 |
| A:J＝1:50 | 48.37 | 21.65 | 17.70 | 122.28 |
| A:K＝50:1 | 8.49 | 123.32 | 98.32 | 125.43 |
| A:K＝35:1 | 7.42 | 141.11 | 97.61 | 144.56 |
| A:K＝20:1 | 7.06 | 148.30 | 95.91 | 154.63 |
| A:K＝10:1 | 6.89 | 151.96 | 92.19 | 164.84 |
| A:K＝5:1 | 7.01 | 149.36 | 85.68 | 174.32 |
| A:K＝2.5:1 | 7.59 | 137.94 | 75.45 | 182.83 |
| A:K＝1:1 | 8.49 | 123.32 | 57.04 | 216.21 |
| A:K＝1:2.5 | 13.71 | 76.37 | 38.63 | 197.71 |
| A:K＝1:5 | 20.26 | 51.68 | 28.40 | 181.98 |
| A:K＝1:10 | 28.84 | 36.30 | 21.89 | 165.86 |
| A:K＝1:20 | 35.28 | 29.68 | 18.17 | 163.35 |
| A:K＝1:35 | 42.66 | 24.54 | 16.46 | 149.08 |
| A:K＝1:50 | 54.37 | 19.26 | 15.76 | 122.18 |
From table 7, methylsulfonyl bacterium azoles all has higher indoor virulence respectively with fluopicolide, zoxamide composite control bacterial wilt of peanut active, be (50 ~ 1) by weight: composite between (1 ~ 50), the CTC value of each process is all greater than 120, illustrate methylsulfonyl bacterium azoles respectively with fluopicolide, zoxamide is composite has obvious synergistic effect, and weight ratio its synergy degree different is also different, when weight ratio is (20 ~ 1): time between (1 ~ 10), CTC is all greater than 163, and synergy highly significant is described.
Table 8 methylsulfonyl bacterium azoles respectively with fenfuram, the composite Toxicity Determination result to bacterial wilt of peanut of fenoxanil
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 12.49 | 100.00 | / | / |
| Fenfuram (L) | 86.43 | 14.45 | / | / |
| Fenoxanil (M) | 107.24 | 11.65 | / | / |
| A:L＝50:1 | 10.14 | 123.18 | 98.32 | 125.28 |
| A:L＝35:1 | 9.03 | 138.32 | 97.62 | 141.68 |
| A:L＝20:1 | 8.63 | 144.73 | 95.93 | 150.87 |
| A:L＝10:1 | 8.29 | 150.66 | 92.22 | 163.37 |
| A:L＝5:1 | 8.76 | 142.58 | 85.74 | 166.29 |
| A:L＝2.5:1 | 9.11 | 137.10 | 75.56 | 181.45 |
| A:L＝1:1 | 11.21 | 111.42 | 57.23 | 194.70 |
| A:L＝1:2.5 | 15.48 | 80.68 | 38.89 | 207.45 |
| A:L＝1:5 | 23.56 | 53.01 | 28.71 | 184.66 |
| A:L＝1:10 | 33.47 | 37.32 | 22.23 | 167.88 |
| A:L＝1:20 | 41.08 | 30.40 | 18.52 | 164.13 |
| A:L＝1:35 | 49.51 | 25.23 | 16.83 | 149.92 |
| A:L＝1:50 | 61.94 | 20.16 | 16.13 | 125.03 |
| A:M＝50:1 | 10.26 | 121.73 | 98.27 | 123.88 |
| A:M＝35:1 | 9.57 | 130.51 | 97.55 | 133.80 |
| A:M＝20:1 | 8.82 | 141.61 | 95.79 | 147.83 |
| A:M＝10:1 | 8.24 | 151.58 | 91.97 | 164.82 |
| A:M＝5:1 | 8.56 | 145.91 | 85.27 | 171.11 |
| A:M＝2.5:1 | 8.91 | 140.18 | 74.76 | 187.52 |
| A:M＝1:1 | 9.98 | 125.15 | 55.82 | 224.19 |
| A:M＝1:2.5 | 17.46 | 71.53 | 36.89 | 193.91 |
| A:M＝1:5 | 25.05 | 49.86 | 26.37 | 189.06 |
| A:M＝1:10 | 36.83 | 33.91 | 19.68 | 172.33 |
| A:M＝1:20 | 48.12 | 25.96 | 15.85 | 163.72 |
| A:M＝1:35 | 62.73 | 19.91 | 14.10 | 141.20 |
| A:M＝1:50 | 75.08 | 16.64 | 13.38 | 124.34 |
From table 8, methylsulfonyl bacterium azoles all has higher indoor virulence respectively with fenfuram, fenoxanil composite control bacterial wilt of peanut active, be (50 ~ 1) by weight: between (1 ~ 50), the CTC value of each process is all greater than 120, illustrate methylsulfonyl bacterium azoles respectively with fenfuram, fenoxanil is composite has obvious synergistic effect, and weight ratio its synergy degree different is also different, when weight ratio is in (20 ~ 1): time between (1 ~ 10), the CTC of each process is all greater than 163, and synergy highly significant is described.
Table 9 methylsulfonyl bacterium azoles respectively with fenhexamid, the composite Toxicity Determination result to bacterial wilt of peanut of Silthiopham
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 13.29 | 100.00 | / | / |
| Fenhexamid (N) | 105.44 | 12.60 | / | / |
| Guardian (O) | 106.71 | 12.45 | / | / |
| A:N＝50:1 | 11.14 | 119.30 | 98.29 | 121.38 |
| A:N＝35:1 | 10.76 | 123.51 | 97.57 | 126.59 |
| A:N＝20:1 | 9.33 | 142.44 | 95.84 | 148.63 |
| A:N＝10:1 | 8.64 | 153.82 | 92.05 | 167.10 |
| A:N＝5:1 | 8.85 | 150.17 | 85.43 | 175.77 |
| A:N＝2.5:1 | 9.78 | 135.89 | 75.03 | 181.11 |
| A:N＝1:1 | 10.85 | 122.49 | 56.30 | 217.56 |
| A:N＝1:2.5 | 17.78 | 74.75 | 37.57 | 198.93 |
| A:N＝1:5 | 26.13 | 50.86 | 27.17 | 187.19 |
| A:N＝1:10 | 36.86 | 36.06 | 20.55 | 175.46 |
| A:N＝1:20 | 48.54 | 27.38 | 16.77 | 163.30 |
| A:N＝1:35 | 65.71 | 20.23 | 15.03 | 134.55 |
| A:N＝1:50 | 73.94 | 17.97 | 14.32 | 125.53 |
| A:O＝50:1 | 11.17 | 118.98 | 98.28 | 121.06 |
| A:O＝35:1 | 9.81 | 135.47 | 97.57 | 138.85 |
| A:O＝20:1 | 9.26 | 143.52 | 95.83 | 149.76 |
| A:O＝10:1 | 8.88 | 149.66 | 92.04 | 162.60 |
| A:O＝5:1 | 9.03 | 147.18 | 85.41 | 172.32 |
| A:O＝2.5:1 | 9.77 | 136.03 | 74.99 | 181.40 |
| A:O＝1:1 | 12.47 | 106.58 | 56.23 | 189.55 |
| A:O＝1:2.5 | 17.42 | 76.29 | 37.47 | 203.62 |
| A:O＝1:5 | 25.73 | 51.65 | 27.05 | 190.98 |
| A:O＝1:10 | 37.19 | 35.74 | 20.41 | 175.06 |
| A:O＝1:20 | 48.68 | 27.30 | 16.62 | 164.23 |
| A:O＝1:35 | 62.44 | 21.28 | 14.89 | 142.98 |
| A:O＝1:50 | 75.58 | 17.58 | 14.17 | 124.09 |
From table 9, methylsulfonyl bacterium azoles all has higher indoor virulence respectively with fenhexamid, Silthiopham composite control bacterial wilt of peanut active, be (50 ~ 1) by weight: between (1 ~ 50), the CTC value of each process is all greater than 120, illustrate methylsulfonyl bacterium azoles respectively with fenhexamid, Silthiopham is composite has obvious synergistic effect, and weight ratio its synergy degree different is also different, when weight ratio is (20 ~ 1): time between (1 ~ 10), the CTC of each process is all greater than 162, and synergy highly significant is described.
Toxicity Determination embodiment three:
Below that methylsulfonyl bacterium azoles is tested with fluorine azoles bacterium acid amides, fluorine pyrrole bacterium acid amides, flutolanil, mandipropamid, flusulfamide, the composite Toxicity Determination to rice sheath blight disease of Silthiopham respectively.
Under aseptic technique, the sterilising medium 36ml melted in advance by pipette, extract is in aseptic conical flask, add the liquid 4ml with 0.1% Tween 80 aqueous solution dilution again, fully shake up, then equivalent pours 4 diameters into is in the culture dish of 9cm, make pastille flat board, if the process not containing medicament is blank.By cultured pathogen, aseptically beat with the sterilizing card punch of diameter 5mm and get bacterium cake, with transfer needle, pure culture biscuits involvng inoculation is dull and stereotyped central in pastille, mycelia faces down, and covers ware lid, is placed in 26 DEG C of insulating box moisturizings and cultivates.When the colony diameter of blank accounts for ware footpath over half, use kind of calliper colony diameter, each bacterium colony right-angled intersection method vertical survey diameter is each once, average, calculate mycelial growth inhibition rate, mycelial growth inhibition rate probability value according to each drug concentration logarithm value and correspondence does regression analysis, calculates the EC50 of each medicament, and calculates the co-toxicity coefficient of mixture according to the abundant method of Sun Yun.The results are shown in Table 10 ~ table 13.
The Toxicity Determination result of table 10 methylsulfonyl bacterium azoles and the composite water prevention rice sheath blight of fluorine azoles bacterium acid amides
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 34.22 | 100.00 | / | / |
| Fluorine azoles bacterium acid amides (B) | 0.31 | 11038.71 | / | / |
| A:B＝50:1 | 8.75 | 391.09 | 314.48 | 124.36 |
| A:B＝40:1 | 6.84 | 500.29 | 366.80 | 136.39 |
| A:B＝30:1 | 5.24 | 653.05 | 452.86 | 144.21 |
| A:B＝20:1 | 3.57 | 958.54 | 620.89 | 154.38 |
| A:B＝10:1 | 1.93 | 1773.06 | 1094.43 | 162.01 |
| A:B＝5:1 | 0.98 | 3491.84 | 1923.12 | 181.57 |
| A:B＝2.5:1 | 0.57 | 6003.51 | 3225.35 | 186.14 |
| A:B＝1:1 | 0.31 | 11038.71 | 5569.35 | 198.20 |
| A:B＝1:2.5 | 0.24 | 14258.33 | 7913.36 | 180.18 |
| A:B＝1:5 | 0.21 | 16295.24 | 9215.59 | 176.82 |
| A:B＝1:10 | 0.20 | 17110.00 | 10044.28 | 170.35 |
| A:B＝1:14 | 0.19 | 18010.53 | 10309.46 | 174.70 |
| A:B＝1:20 | 0.20 | 17110.00 | 10517.82 | 162.68 |
| A:B＝1:30 | 0.23 | 14878.26 | 10685.85 | 139.23 |
| A:B＝1:40 | 0.25 | 13688.00 | 10771.91 | 127.07 |
| A:B＝1:50 | 0.26 | 13161.54 | 10824.23 | 121.59 |
| A:B＝1:60 | 0.29 | 11800.00 | 10859.39 | 108.66 |
From table 10, it is active that methylsulfonyl bacterium azoles and the fluorine azoles bacterium acid amides composite water prevention rice sheath blight all have higher indoor virulence, be (50 ~ 1) by weight: between (1 ~ 50), the CTC value of each process is all greater than 120, methylsulfonyl bacterium azoles is described and fluorine azoles bacterium acid amides is composite has obvious synergistic effect, and weight ratio its synergy degree different is also different, when weight ratio is (20 ~ 1): time between (1 ~ 10), the CTC of each process is all greater than 162, and synergy highly significant is described.
The Toxicity Determination result of table 11 methylsulfonyl bacterium azoles and the composite water prevention rice sheath blight of fluorine pyrrole bacterium acid amides
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 31.30 | 100.00 | / | / |
| Fluorine pyrrole bacterium acid amides (C) | 0.94 | 3329.79 | / | / |
| A:C＝50:1 | 15.18 | 206.19 | 163.33 | 126.24 |
| A:C＝40:1 | 13.20 | 237.12 | 178.78 | 132.64 |
| A:C＝30:1 | 10.72 | 291.98 | 204.19 | 143.00 |
| A:C＝20:1 | 8.19 | 382.17 | 253.80 | 150.58 |
| A:C＝10:1 | 4.87 | 642.71 | 393.62 | 163.28 |
| A:C＝5:1 | 2.66 | 1176.69 | 638.30 | 184.35 |
| A:C＝2.5:1 | 1.59 | 1968.55 | 1022.80 | 192.47 |
| A:C＝1:1 | 0.87 | 3597.70 | 1714.89 | 209.79 |
| A:C＝1:2.5 | 0.67 | 4671.64 | 2406.99 | 194.09 |
| A:C＝1:5 | 0.63 | 4968.25 | 2791.49 | 177.98 |
| A:C＝1:10 | 0.62 | 5048.39 | 3036.17 | 166.27 |
| A:C＝1:20 | 0.60 | 5216.67 | 3175.99 | 164.25 |
| A:C＝1:30 | 0.69 | 4536.23 | 3225.60 | 140.63 |
| A:C＝1:40 | 0.74 | 4229.73 | 3251.01 | 130.11 |
| A:C＝1:50 | 0.79 | 3962.03 | 3266.46 | 121.29 |
| A:C＝1:60 | 0.85 | 3682.35 | 3276.84 | 112.38 |
From table 11, it is active that methylsulfonyl bacterium azoles and the fluorine pyrrole bacterium acid amides composite water prevention rice sheath blight all have higher indoor virulence, be (50 ~ 1) by weight: between (1 ~ 50), the CTC value of each process is all greater than 120, methylsulfonyl bacterium azoles is described and fluorine pyrrole bacterium acid amides is composite has obvious synergistic effect, and weight ratio its synergy degree different is also different, when weight ratio is (20 ~ 1): time between (1 ~ 10), the CTC of each process is all greater than 163, and synergy highly significant is described.
Table 12 methylsulfonyl bacterium azoles respectively with flutolanil, the composite Toxicity Determination result to rice sheath blight disease of mandipropamid
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 31.68 | 100.00 | / | / |
| Flutolanil (F) | 0.27 | 11733.33 | / | / |
| Two alkynyl amide (G) | 0.81 | 3911.11 | / | / |
| A:F＝50:1 | 7.83 | 404.60 | 328.10 | 123.31 |
| A:F＝35:1 | 5.18 | 611.58 | 423.15 | 144.53 |
| A:F＝20:1 | 3.07 | 1031.92 | 653.97 | 157.79 |
| A:F＝10:1 | 1.61 | 1967.70 | 1157.58 | 169.98 |
| A:F＝5:1 | 0.87 | 3641.38 | 2038.89 | 178.60 |
| A:F＝2.5:1 | 0.48 | 6600.00 | 3423.81 | 192.77 |
| A:F＝1:1 | 0.24 | 13200.00 | 5916.67 | 223.10 |
| A:F＝1:2.5 | 0.19 | 16673.68 | 8409.52 | 198.27 |
| A:F＝1:5 | 0.18 | 17600.00 | 9794.44 | 179.69 |
| A:F＝1:10 | 0.17 | 18635.29 | 10675.76 | 174.56 |
| A:F＝1:20 | 0.17 | 18635.29 | 11179.37 | 166.69 |
| A:F＝1:35 | 0.19 | 16673.68 | 11410.19 | 146.13 |
| A:F＝1:50 | 0.22 | 14400.00 | 11505.23 | 125.16 |
| A:G＝50:1 | 14.68 | 215.80 | 174.73 | 123.51 |
| A:G＝35:1 | 11.85 | 267.34 | 205.86 | 129.86 |
| A:G＝20:1 | 7.35 | 431.02 | 281.48 | 153.13 |
| A:G＝10:1 | 4.21 | 752.49 | 446.46 | 168.55 |
| A:G＝5:1 | 2.47 | 1282.59 | 735.19 | 174.46 |
| A:G＝2.5:1 | 1.48 | 2140.54 | 1188.89 | 180.05 |
| A:G＝1:1 | 0.84 | 3771.43 | 2005.56 | 188.05 |
| A:G＝1:2.5 | 0.59 | 5369.49 | 2822.22 | 190.26 |
| A:G＝1:5 | 0.56 | 5657.14 | 3275.93 | 172.69 |
| A:G＝1:10 | 0.53 | 5977.36 | 3564.65 | 167.68 |
| A:G＝1:20 | 0.51 | 6211.76 | 3729.63 | 166.55 |
| A:G＝1:35 | 0.62 | 5109.68 | 3805.25 | 134.28 |
| A:G＝1:50 | 0.68 | 4658.82 | 3836.38 | 121.44 |
From table 12, it is active that methylsulfonyl bacterium azoles and flutolanil, the mandipropamid composite water prevention rice sheath blight all have higher indoor virulence, be (50 ~ 1) by weight: between (1 ~ 50), the CTC value of each process is all greater than 120, methylsulfonyl bacterium azoles and flutolanil are described, mandipropamid is composite has obvious synergistic effect, and weight ratio its synergy degree different is also different, when weight ratio is (20 ~ 1): time between (1 ~ 10), the CTC of each process is all greater than 166, and synergy highly significant is described.
Table 13 methylsulfonyl bacterium azoles respectively with the Toxicity Determination result of flusulfamide, the composite water prevention rice sheath blight of Silthiopham
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 32.75 | 100.00 | / | / |
| Flusulfamide (H) | 4.75 | 689.47 | / | / |
| Silthiopham (I) | 0.71 | 4612.68 | / | / |
| A:H＝50:1 | 24.26 | 135.00 | 111.56 | 121.01 |
| A:H＝35:1 | 22.24 | 147.26 | 116.37 | 126.54 |
| A:H＝20:1 | 17.33 | 188.98 | 128.07 | 147.56 |
| A:H＝10:1 | 12.58 | 260.33 | 153.59 | 169.50 |
| A:H＝5:1 | 9.43 | 347.30 | 198.25 | 175.18 |
| A:H＝2.5:1 | 6.45 | 507.75 | 268.42 | 189.16 |
| A:H＝1:1 | 3.20 | 1023.44 | 394.74 | 259.27 |
| A:H＝1:2.5 | 3.13 | 1046.33 | 521.05 | 200.81 |
| A:H＝1:5 | 3.10 | 1056.45 | 591.23 | 178.69 |
| A:H＝1:10 | 3.01 | 1088.04 | 635.89 | 171.11 |
| A:H＝1:20 | 2.97 | 1102.69 | 661.40 | 166.72 |
| A:H＝1:35 | 3.52 | 930.40 | 673.10 | 138.23 |
| A:H＝1:50 | 3.97 | 824.94 | 677.92 | 121.69 |
| A:I＝50:1 | 14.29 | 229.18 | 188.48 | 121.59 |
| A:I＝35:1 | 11.53 | 284.04 | 225.35 | 126.04 |
| A:I＝20:1 | 7.41 | 441.97 | 314.89 | 140.36 |
| A:I＝10:1 | 3.89 | 841.90 | 510.24 | 165.00 |
| A:I＝5:1 | 2.31 | 1417.75 | 852.11 | 166.38 |
| A:I＝2.5:1 | 1.25 | 2620.00 | 1389.34 | 188.58 |
| A:I＝1:1 | 0.62 | 5282.26 | 2356.34 | 224.17 |
| A:I＝1:2.5 | 0.57 | 5745.61 | 3323.34 | 172.89 |
| A:I＝1:5 | 0.50 | 6550.00 | 3860.56 | 169.66 |
| A:I＝1:10 | 0.47 | 6968.09 | 4202.43 | 165.81 |
| A:I＝1:20 | 0.45 | 7277.78 | 4397.79 | 165.49 |
| A:I＝1:35 | 0.54 | 6064.81 | 4487.32 | 135.15 |
| A:I＝1:50 | 0.58 | 5646.55 | 4524.19 | 124.81 |
From table 13, it is active that methylsulfonyl bacterium azoles and flusulfamide, the Silthiopham composite water prevention rice sheath blight all have higher indoor virulence, be (50 ~ 1) by weight: between (1 ~ 50), the CTC value of each process is all greater than 120, methylsulfonyl bacterium azoles and flusulfamide are described, Silthiopham is composite has obvious synergistic effect, and weight ratio its synergy degree different is also different, when weight ratio is (20 ~ 1): time between (1 ~ 10), the CTC of each process is all greater than 165, and synergy highly significant is described.
Toxicity Determination embodiment four:
Below that methylsulfonyl bacterium azoles is tested with the Toxicity Determination of Boscalid, metalaxyl, fluopicolide, zoxamide, fenfuram, fenoxanil, fenhexamid, the composite control cucumber downy mildew of Guardian respectively.
Prepare pathogeny blade, with 4 DEG C of distillation washing lower blade back side Pseudoperonospora cubensis sporangiums, be made into suspension (concentration is every milliliter of 1 × 105 ~ 1 × 107 sporangiums).The medicament mother liquor 0.05% Tween 80 aqueous solution is diluted to corresponding concentration, the plant leaf two sides evenly sprayed in cultivation in advance to 4 ~ 6 leaf periods soaks to whole, often process and repeat for 4 times, if be blank with the process of fresh water spraying, after dispenser 24h, Fresh spores capsule suspension spray is inoculated in vacuum side of blade, at every d continuous illumination/dark each 12h alternately, temperature is 17 DEG C ~ 22 DEG C, and relative moisture is cultivate under the condition of more than 90%.When the blank incidence of disease reaches more than 50% time stage investigation incidence, calculate disease index and preventive effect, preventive effect probability value according to each drug concentration logarithm value and correspondence does regression analysis, calculates the EC50 of lattice medicament, and calculates the co-toxicity coefficient of mixture according to the abundant method of Sun Yun.The results are shown in Table 14 ~ table 18.
The Toxicity Determination result of table 14 methylsulfonyl bacterium azoles and the composite control cucumber downy mildew of Boscalid
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 22.36 | 100.00 | / | / |
| Boscalid (D) | 14.67 | 152.42 | / | / |
| A:D＝50:1 | 18.18 | 122.99 | 101.03 | 121.74 |
| A:D＝40:1 | 16.20 | 138.02 | 101.28 | 136.28 |
| A:D＝30:1 | 14.72 | 151.90 | 101.69 | 149.38 |
| A:D＝20:1 | 14.19 | 157.58 | 102.50 | 153.74 |
| A:D＝10:1 | 13.27 | 168.50 | 104.77 | 160.84 |
| A:D＝5:1 | 11.68 | 191.44 | 108.74 | 176.06 |
| A:D＝2.5:1 | 10.24 | 218.36 | 114.98 | 189.92 |
| A:D＝1:1 | 9.31 | 240.17 | 126.21 | 190.30 |
| A:D＝1:2.5 | 9.21 | 242.78 | 137.44 | 176.64 |
| A:D＝1:5 | 9.13 | 244.91 | 143.68 | 170.45 |
| A:D＝1:10 | 9.05 | 247.07 | 147.65 | 167.33 |
| A:D＝1:20 | 9.02 | 247.89 | 149.92 | 165.35 |
| A:D＝1:30 | 9.32 | 239.91 | 150.73 | 159.17 |
| A:D＝1:40 | 10.65 | 209.95 | 151.14 | 138.91 |
| A:D＝1:50 | 11.47 | 194.94 | 151.39 | 128.77 |
| A:D＝1:60 | 14.39 | 155.39 | 151.56 | 102.52 |
The Toxicity Determination result of table 15 methylsulfonyl bacterium azoles and the composite control cucumber downy mildew of metalaxyl
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 23.68 | 100.00 | / | / |
| Metalaxyl (E) | 0.68 | 3482.35 | / | / |
| A:E＝50:1 | 11.20 | 211.43 | 166.32 | 127.12 |
| A:E＝40:1 | 9.45 | 250.58 | 182.50 | 137.31 |
| A:E＝30:1 | 7.86 | 301.27 | 209.11 | 144.07 |
| A:E＝20:1 | 5.74 | 412.54 | 261.06 | 158.02 |
| A:E＝10:1 | 3.47 | 682.42 | 407.49 | 167.47 |
| A:E＝5:1 | 2.04 | 1160.78 | 663.73 | 174.89 |
| A:E＝2.5:1 | 1.21 | 1957.02 | 1066.39 | 183.52 |
| A:E＝1:1 | 0.58 | 4082.76 | 1791.18 | 227.94 |
| A:E＝1:2.5 | 0.51 | 4643.14 | 2515.97 | 184.55 |
| A:E＝1:5 | 0.49 | 4832.65 | 2918.63 | 165.58 |
| A:E＝1:10 | 0.46 | 5147.83 | 3174.87 | 162.14 |
| A:E＝1:20 | 0.44 | 5381.82 | 3321.29 | 162.04 |
| A:E＝1:30 | 0.49 | 4832.65 | 3373.24 | 143.26 |
| A:E＝1:40 | 0.51 | 4643.14 | 3399.86 | 136.57 |
| A:E＝1:50 | 0.57 | 4154.39 | 3416.03 | 121.61 |
| A:E＝1:60 | 0.63 | 3758.73 | 3426.90 | 109.68 |
Table 16 methylsulfonyl bacterium azoles respectively with the Toxicity Determination result of fluopicolide, the composite control cucumber downy mildew of zoxamide
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 22.47 | 100.00 | / | / |
| Fluopicolide (J) | 3.14 | 715.61 | / | / |
| Zoxamide (K) | 4.21 | 533.73 | / | / |
| A:J＝50:1 | 16.47 | 136.43 | 112.07 | 121.74 |
| A:J＝35:1 | 13.24 | 169.71 | 117.10 | 144.93 |
| A:J＝20:1 | 11.34 | 198.15 | 129.31 | 153.23 |
| A:J＝10:1 | 8.69 | 258.57 | 155.96 | 165.79 |
| A:J＝5:1 | 6.14 | 365.96 | 202.60 | 180.63 |
| A:J＝2.5:1 | 4.12 | 545.39 | 275.89 | 197.69 |
| A:J＝1:1 | 2.15 | 1045.12 | 407.80 | 256.28 |
| A:J＝1:2.5 | 2.12 | 1059.91 | 539.72 | 196.38 |
| A:J＝1:5 | 2.10 | 1070.00 | 613.00 | 174.55 |
| A:J＝1:10 | 2.06 | 1090.78 | 659.64 | 165.36 |
| A:J＝1:20 | 2.03 | 1106.90 | 686.29 | 161.29 |
| A:J＝1:35 | 2.23 | 1007.62 | 698.50 | 144.25 |
| A:J＝1:50 | 2.52 | 891.67 | 703.53 | 126.74 |
| A:K＝50:1 | 16.67 | 134.79 | 108.50 | 124.23 |
| A:K＝35:1 | 13.49 | 166.57 | 112.05 | 148.66 |
| A:K＝20:1 | 11.67 | 192.54 | 120.65 | 159.58 |
| A:K＝10:1 | 9.57 | 234.80 | 139.43 | 168.40 |
| A:K＝5:1 | 7.48 | 300.40 | 172.29 | 174.36 |
| A:K＝2.5:1 | 5.24 | 428.82 | 223.92 | 191.50 |
| A:K＝1:1 | 3.56 | 631.18 | 316.86 | 199.20 |
| A:K＝1:2.5 | 3.21 | 700.00 | 409.81 | 170.81 |
| A:K＝1:5 | 2.87 | 782.93 | 461.44 | 169.67 |
| A:K＝1:10 | 2.75 | 817.09 | 494.30 | 165.30 |
| A:K＝1:20 | 2.68 | 838.43 | 513.08 | 163.41 |
| A:K＝1:35 | 3.16 | 711.08 | 521.68 | 136.30 |
| A:K＝1:50 | 3.54 | 634.75 | 525.22 | 120.85 |
Table 17 methylsulfonyl bacterium azoles respectively with the Toxicity Determination result of fenfuram, the composite control cucumber downy mildew of fenoxanil
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 23.31 | 100.00 | / | / |
| Fenfuram (L) | 3.35 | 695.82 | / | / |
| Fenoxanil (M) | 7.61 | 306.31 | / | / |
| A:L＝50:1 | 17.39 | 134.04 | 111.68 | 120.02 |
| A:L＝35:1 | 13.85 | 168.30 | 116.55 | 144.40 |
| A:L＝20:1 | 11.67 | 199.74 | 128.37 | 155.60 |
| A:L＝10:1 | 9.28 | 251.19 | 154.17 | 162.93 |
| A:L＝5:1 | 7.05 | 330.64 | 199.30 | 165.90 |
| A:L＝2.5:1 | 4.53 | 514.57 | 270.23 | 190.42 |
| A:L＝1:1 | 2.92 | 798.29 | 397.91 | 200.62 |
| A:L＝1:2.5 | 2.26 | 1031.42 | 525.59 | 196.24 |
| A:L＝1:5 | 2.23 | 1045.29 | 596.52 | 175.23 |
| A:L＝1:10 | 2.21 | 1054.75 | 641.66 | 164.38 |
| A:L＝1:20 | 2.13 | 1094.37 | 667.45 | 163.96 |
| A:L＝1:35 | 2.34 | 996.15 | 679.27 | 146.65 |
| A:L＝1:50 | 2.69 | 866.54 | 684.14 | 126.66 |
| A:M＝50:1 | 17.60 | 132.44 | 104.05 | 127.29 |
| A:M＝35:1 | 15.11 | 154.27 | 105.73 | 145.91 |
| A:M＝20:1 | 13.58 | 171.65 | 109.82 | 156.29 |
| A:M＝10:1 | 11.87 | 196.38 | 118.76 | 165.36 |
| A:M＝5:1 | 9.81 | 237.61 | 134.38 | 176.82 |
| A:M＝2.5:1 | 8.17 | 285.31 | 158.94 | 179.50 |
| A:M＝1:1 | 5.86 | 397.78 | 203.15 | 195.80 |
| A:M＝1:2.5 | 5.31 | 438.98 | 247.36 | 177.47 |
| A:M＝1:5 | 5.12 | 455.27 | 271.92 | 167.43 |
| A:M＝1:10 | 4.97 | 469.01 | 287.55 | 163.11 |
| A:M＝1:20 | 4.87 | 478.64 | 296.48 | 161.44 |
| A:M＝1:35 | 5.36 | 434.89 | 300.58 | 144.68 |
| A:M＝1:50 | 6.25 | 372.96 | 302.26 | 123.39 |
Table 18 methylsulfonyl bacterium azoles respectively with the Toxicity Determination result of fenhexamid, the composite control cucumber downy mildew of Silthiopham
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 23.31 | 100.00 | / | / |
| Fenhexamid (N) | 4.81 | 484.62 | / | / |
| Guardian (O) | 3.62 | 643.92 | / | / |
| A:N＝50:1 | 17.17 | 135.76 | 107.54 | 126.24 |
| A:N＝35:1 | 15.33 | 152.05 | 110.68 | 137.38 |
| A:N＝20:1 | 13.70 | 170.15 | 118.32 | 143.81 |
| A:N＝10:1 | 10.55 | 220.95 | 134.97 | 163.71 |
| A:N＝5:1 | 8.34 | 279.50 | 164.10 | 170.32 |
| A:N＝2.5:1 | 6.12 | 380.88 | 209.89 | 181.47 |
| A:N＝1:1 | 4.26 | 547.18 | 292.31 | 187.19 |
| A:N＝1:2.5 | 3.21 | 726.17 | 374.73 | 193.79 |
| A:N＝1:5 | 3.15 | 740.00 | 420.51 | 175.98 |
| A:N＝1:10 | 3.12 | 747.12 | 449.65 | 166.15 |
| A:N＝1:20 | 3.06 | 761.76 | 466.30 | 163.36 |
| A:N＝1:35 | 3.54 | 658.47 | 473.93 | 138.94 |
| A:N＝1:50 | 3.87 | 602.33 | 477.07 | 126.25 |
| A:O＝50:1 | 17.34 | 134.43 | 110.67 | 121.47 |
| A:O＝35:1 | 13.97 | 166.86 | 115.11 | 144.96 |
| A:O＝20:1 | 12.16 | 191.69 | 125.90 | 152.26 |
| A:O＝10:1 | 9.58 | 243.32 | 149.45 | 162.81 |
| A:O＝5:1 | 7.24 | 321.96 | 190.65 | 168.87 |
| A:O＝2.5:1 | 5.15 | 452.62 | 255.41 | 177.22 |
| A:O＝1:1 | 3.48 | 669.83 | 371.96 | 180.08 |
| A:O＝1:2.5 | 2.59 | 900.00 | 488.52 | 184.23 |
| A:O＝1:5 | 2.41 | 967.22 | 553.27 | 174.82 |
| A:O＝1:10 | 2.36 | 987.71 | 594.48 | 166.15 |
| A:O＝1:20 | 2.31 | 1009.09 | 618.02 | 163.28 |
| A:O＝1:35 | 2.69 | 866.54 | 628.81 | 137.81 |
| A:O＝1:50 | 2.87 | 812.20 | 633.26 | 128.26 |
From table 14-table 18, methylsulfonyl bacterium azoles is respectively with all have higher indoor virulence respectively with Boscalid, metalaxyl, fluopicolide, zoxamide, fenfuram, fenoxanil, fenhexamid, Guardian composite control cucumber downy mildew active, be (50 ~ 1) by weight: CTC value composite in the scope of (1 ~ 50) is all greater than 120, methylsulfonyl bacterium azoles is described and acid amide fungicides is composite has obvious synergistic effect, and weight ratio its synergy degree different is also different; When weight ratio is (20 ~ 1): time between (1 ~ 10), the CTC of each process is all greater than 162, illustrates that synergy is particularly remarkable.
Land for growing field crops test examples
In order to clear and definite methylsulfonyl bacterium azoles and acid amide fungicides alone with time mixed to the control efficiency of each crop pest and insect pest, and can the result of clear and definite Toxicity Determination (i.e. synergistic effect) be confirmed in field, present invention applicant at home different regions has carried out a large amount of field trials.
Contrast medicament is:
CK1:30% methylsulfonyl bacterium azoles wetting powder, self-control;
Ck2:30% fluorine azoles bacterium acid amides wetting powder, self-control;
CK3:41.7% fluorine pyrrole bacterium amide suspending agents, registration card number PD20121664F130024, Bayer Cropscience (China) Co., Ltd, commercial;
CK4:50% Boscalid water dispersible granules, registration card number PD20081106F130004, Shanghai Lvze Bio-technology Co., Ltd., commercial;
CK5:25% metalaxyl wetting powder, registration card number PD20110517, Zhejiang Heben Science & Technology Co., Ltd., commercial;
Field efficacy embodiment one: the field control effectiveness test of control bacterial wilt of peanut
Test method: with reference to " pesticide field efficacy medicine test criterion (NY/T1464.32-2010) " regulation application method, first time sprays dispenser when beginning to see diseased plant, and after 10d, second time sprays dispenser.Dispenser twice altogether, each process plot area is 40m2, number of repetition 4 times.The incidence of each community of 10d, 20d sampling survey after second time dispenser, records total strain number and diseased plant number, calculates disease index and preventive effect.The results are shown in Table 19:
The field control effectiveness test result of bacterial wilt of peanut prevented and treated by table 19
Known according to field control effectiveness test result table 19, methylsulfonyl bacterium azoles respectively with when fluorine azoles bacterium acid amides, fluorine pyrrole bacterium acid amides, Boscalid, metalaxyl composite control bacterial wilt of peanut under the prerequisite of a small amount of single dose consumption of consumption, its preventive effect apparently higher than contrast single dose show obvious synergistic effect.Complex preparation 20d after second time medicine can also keep good drug effect (all more than 70%), and the lasting period is long.
Field efficacy embodiment two: the field control effectiveness test of the water prevention rice sheath blight
Test method and computational methods reference " GB/T17980.20-2000 pesticide field efficacy medicine test criterion () the 20th part: bactericidal agent for preventing and treating rice sheath blight disease ", every plot area 20m
2, often process and repeat for 4 times, if clear water is treated to blank, carry out spray pesticide in their early stage, the dispenser of interval 7d second time.Respectively at 14d investigation result after 7d, second time medicine before first time medicine, after second time medicine, in units of strain, classification investigation incidence, calculates disease index, preventive effect.The results are shown in Table 20:
The field control effectiveness test result of the table 20 water prevention rice sheath blight
Can find out according to field control effectiveness test result table 20, methylsulfonyl bacterium azoles respectively with fluorine azoles bacterium acid amides, fluorine pyrrole bacterium acid amides, Boscalid, metalaxyl during the composite water prevention rice sheath blight under consumption is less than the prerequisite of single dose consumption, its preventive effect shows obvious synergistic effect apparently higher than contrast single dose.Complex preparation 14d after second time medicine can also keep good drug effect (all more than 70%), and the lasting period is long.
Claims (8)
1. contain a complex composition for methylsulfonyl bacterium azoles and acid amide fungicides, it is characterized in that, described complex composition is made up of active components A and B; Described active components A is methylsulfonyl bacterium azoles, and its chemical name is 2-(to fluorophenyl)-5-mesyl-1,3,4-oxadiazole; Active component B is selected from the one in following acid amide fungicides: fluorine azoles bacterium acid amides, fluorine pyrrole bacterium acid amides, Boscalid, metalaxyl, flutolanil, mandipropamid, flusulfamide, Silthiopham, fluopicolide, zoxamide, fenfuram, fenoxanil, fenhexamid, Guardian.
2. the complex composition containing methylsulfonyl bacterium azoles and acid amide fungicides according to claim 1, it is characterized in that, described methylsulfonyl bacterium azoles and the weight ratio of acid amide fungicides are 50: 1 to 1:50.
3. the complex composition containing methylsulfonyl bacterium azoles and acid amide fungicides according to claim 2, it is characterized in that, described methylsulfonyl bacterium azoles and the weight ratio of acid amide fungicides are 10: 1 to 1:20.
4. one kind contains the preparation of methylsulfonyl bacterium azoles and acid amide fungicides, it is characterized in that, described preparation is by weight containing the arbitrary described complex composition of the claim 1-3 of 0.1-90%, and all the other are agriculturally acceptable carrier and auxiliary agent, are then prepared into disinfectant use in agriculture.
5. the preparation containing methylsulfonyl bacterium azoles and acid amide fungicides according to claim 5, is characterized in that, the arbitrary described complex composition of the claim 1-3 of described disinfectant use in agriculture by weight containing 1-80%.
6. the preparation containing methylsulfonyl bacterium azoles and acid amide fungicides according to claim 5, it is characterized in that, the formulation that described disinfectant use in agriculture can be prepared is wetting powder, water dispersible granules, microemulsion, missible oil, aqueous emulsion, suspending agent or granule.
7. the purposes of the complex composition described in claim 1-3 in control crop bacterial disease.
8. the purposes of the complex composition described in claim 1-3 in control crop fungal disease.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410788182.3A CN104521989B (en) | 2014-12-18 | 2014-12-18 | Containing methylsulfonyl bacterium azoles and the complex composition of acid amide fungicides and preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410788182.3A CN104521989B (en) | 2014-12-18 | 2014-12-18 | Containing methylsulfonyl bacterium azoles and the complex composition of acid amide fungicides and preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104521989A true CN104521989A (en) | 2015-04-22 |
| CN104521989B CN104521989B (en) | 2016-08-17 |
Family
ID=52837771
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410788182.3A Active CN104521989B (en) | 2014-12-18 | 2014-12-18 | Containing methylsulfonyl bacterium azoles and the complex composition of acid amide fungicides and preparation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104521989B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106035381A (en) * | 2016-06-27 | 2016-10-26 | 中国烟草总公司郑州烟草研究院 | Bactericide composition containing benzamide bactericides and biocontrol bacterium, preparation and applications of bactericide composition and preparation |
| CN106359406A (en) * | 2016-11-26 | 2017-02-01 | 佛山市普尔玛农化有限公司 | Fungicidal composition containing 2-methyl sulfone-5-(2,4-dichlorophenyl)-1,2,3-oxadiazole and fluopicolide and application of fungicidal composition |
| CN107006491A (en) * | 2016-01-28 | 2017-08-04 | 响水县智诚知识产权信息服务有限公司 | A kind of azoles of bacterium containing methylsulfonyl and the bactericidal composition of fluorobenzene ether amide |
| CN109717195A (en) * | 2017-10-30 | 2019-05-07 | 佛山市盈辉作物科学有限公司 | A kind of bactericidal composition for disliking bacterium azoles and zoxamide containing dichloro |
| EP3442337A4 (en) * | 2016-04-11 | 2019-12-18 | Basf Se | Pesticidally active mixtures of tioxazafen |
| US10701937B2 (en) | 2015-02-11 | 2020-07-07 | Basf Se | Pesticidal mixture comprising a pyrazole compound, an insecticide and a fungicide |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106689146A (en) * | 2017-01-03 | 2017-05-24 | 佛山市普尔玛农化有限公司 | Sterilization composition containing 2-methylsulfone-5-(2,4-dichlorophenyl)-1,2,3-oxadiazole and benzovindiflupyr |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5166165A (en) * | 1990-10-20 | 1992-11-24 | Bayer Aktiengesellschaft | Fungicidal agents based on heterocyclically substituted sulphones |
| CN102499247A (en) * | 2011-10-17 | 2012-06-20 | 贵州大学 | Oxadiazole sulfone compound for controlling bacterial crop diseases |
-
2014
- 2014-12-18 CN CN201410788182.3A patent/CN104521989B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5166165A (en) * | 1990-10-20 | 1992-11-24 | Bayer Aktiengesellschaft | Fungicidal agents based on heterocyclically substituted sulphones |
| CN102499247A (en) * | 2011-10-17 | 2012-06-20 | 贵州大学 | Oxadiazole sulfone compound for controlling bacterial crop diseases |
Non-Patent Citations (1)
| Title |
|---|
| 杨吉春 等: "酰胺类杀菌剂新品种开发进展", 《农药》, vol. 47, no. 1, 10 January 2008 (2008-01-10), pages 6 - 9 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10701937B2 (en) | 2015-02-11 | 2020-07-07 | Basf Se | Pesticidal mixture comprising a pyrazole compound, an insecticide and a fungicide |
| CN107006491A (en) * | 2016-01-28 | 2017-08-04 | 响水县智诚知识产权信息服务有限公司 | A kind of azoles of bacterium containing methylsulfonyl and the bactericidal composition of fluorobenzene ether amide |
| EP3442337A4 (en) * | 2016-04-11 | 2019-12-18 | Basf Se | Pesticidally active mixtures of tioxazafen |
| CN106035381A (en) * | 2016-06-27 | 2016-10-26 | 中国烟草总公司郑州烟草研究院 | Bactericide composition containing benzamide bactericides and biocontrol bacterium, preparation and applications of bactericide composition and preparation |
| CN106359406A (en) * | 2016-11-26 | 2017-02-01 | 佛山市普尔玛农化有限公司 | Fungicidal composition containing 2-methyl sulfone-5-(2,4-dichlorophenyl)-1,2,3-oxadiazole and fluopicolide and application of fungicidal composition |
| CN109717195A (en) * | 2017-10-30 | 2019-05-07 | 佛山市盈辉作物科学有限公司 | A kind of bactericidal composition for disliking bacterium azoles and zoxamide containing dichloro |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104521989B (en) | 2016-08-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104521989B (en) | Containing methylsulfonyl bacterium azoles and the complex composition of acid amide fungicides and preparation | |
| CN103155936B (en) | Plant disease control composition containing phenazino-1-carboxylic acid | |
| CN109418268B (en) | Bactericidal preparation and application thereof | |
| CN105248424A (en) | Sterilization composition and application thereof | |
| CN107197872A (en) | Composition pesticide and its application comprising folpet and fluorine azoles ring bacterium amine | |
| CN105340911A (en) | Pesticide composition as well as preparation method and application thereof | |
| CN104585184A (en) | Compound composition containing methanesulfonyl azole | |
| CN104542585A (en) | Fungicide composition and application thereof | |
| CN104521988A (en) | Compound composition containing 2-(p-fluorophenyl)-5-methanesulfonyl-1,3,4-oxadiazole and Copper(succinate+glutarate+adipate) and preparation | |
| CN104521991B (en) | A kind of containing methylsulfonyl bacterium azoles and the complex composition of chlorobromide isocyanuric acid and preparation | |
| CN104488900B (en) | A kind of complex composition of the azoles of bacterium containing methylsulfonyl and anabasine insecticide | |
| CN104488896B (en) | Containing methylsulfonyl bacterium azoles and the complex composition of methoxy acrylic bactericide and preparation | |
| CN102228035B (en) | Herbicide composition containing bispyribacsodium and oxaziclomefone | |
| CN104336036A (en) | Fungicidal composition and application thereof | |
| CN104522035A (en) | Compound composition containing 2-(p-fluorophenyl)-5-methanesulfonyl-1,3,4-oxadiazole and leasn and preparation | |
| CN104542611A (en) | Bactericidal composition containing mandipropamid | |
| CN104488926B (en) | A kind of containing methylsulfonyl bacterium azoles and the complex composition of thifluzamide and preparation | |
| CN104488897B (en) | The complex composition and preparation of the azoles of bacterium containing methylsulfonyl and carbamate fungicide | |
| CN104542695B (en) | A kind of containing methylsulfonyl bacterium azoles and the complex composition of toxic fluoride phosphate and preparation | |
| CN107318865A (en) | The composition pesticide of captan and furametpyr compounding | |
| CN104488903A (en) | Compound composition containing methanesulphonyl myclobutanil and saisentong | |
| CN104488930A (en) | Compound composition containing methanesulphonyl myclobutanil and zhongshengmycin and preparation | |
| CN104521990B (en) | A kind of containing methylsulfonyl bacterium azoles and the complex composition of Flutriafol and antibacterial | |
| CN104488909A (en) | Compound composition and preparation containing methylsulfonyl azole and azoxystrobin | |
| CN104488899B (en) | A kind of containing methylsulfonyl bacterium azoles and the complex composition of zinc thiazole and preparation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |