CN104522030A - Compound composition containing 2-(p-fluorophenyl)-5-methanesulfonyl-1,3,4-oxadiazole and imidazole bactericides and preparation - Google Patents
Compound composition containing 2-(p-fluorophenyl)-5-methanesulfonyl-1,3,4-oxadiazole and imidazole bactericides and preparation Download PDFInfo
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Abstract
The invention discloses a compound composition containing 2-(p-fluorophenyl)-5-methanesulfonyl-1,3,4-oxadiazole and imidazole bactericides and a preparation. The compound composition is composed of 2-(p-fluorophenyl)-5-methanesulfonyl-1,3,4-oxadiazole and the imidazole bactericides, wherein the weight ratio of 2-(p-fluorophenyl)-5-methanesulfonyl-1,3,4-oxadiazole to the imidazole bactericides is (30-1):(1-30). The compound composition disclosed by the invention accounts for 0.1-90% of the weight percentage of the agricultural bactericides. Compared with a single preparation, the compound composition disclosed by the invention has a remarkable synergistic effect, is used for preventing and controlling crop diseases and is capable of improving the preventing and controlling effects and reducing the dosage of a pesticide as well as the pesticide application frequency and long in lasting period.
Description
Technical field
The present invention relates to technical field of pesticide, particularly the complex composition of two kinds of fungicide active ingredients and preparation thereof.
Background technology
In production practices, often kind of disease is not often occur separately, such as while bacterial disease occurs, and frequent concomitant infections fungal disease.Fungal disease occurs the most general in plant disease, and account for more than 80% of all disease species, its extent of injury also can not be despised.In recent years, with the adjustment of pattern of farming, what cause various crop pest in recent years presents the trend increased the weight of year by year, and occurring area increases year by year, brings significant damage to agricultural production.The medicament that can be used for simultaneously preventing and treating bacterial disease and fungal disease in the market lacks.For this reason, applicant, through a large amount of experimental studies, finds new medicament methylsulfonyl bacterium azoles and imidazoles is bactericide compounded all has good preventive effect to vegetative bacteria and fungal disease.Through retrieval, the complex composition of the imidazoles bactericide such as the methylsulfonyl bacterium azoles that the present invention relates to and Prochloraz, has no report both at home and abroad.
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.
Imidazoles bactericide therapeutic activity is obvious, strong to the direct killing power of germ.Wherein Prochloraz is still the best medicament of the obstinate germ of the various anthracnose of radical cure.Also better to the effect such as rice blast, take-all.Common imidazoles bactericide mainly contains: Prochloraz, imazalil, cyazofamid, fluorine bacterium azoles, Fenamidone, pefurazoate.Imidazoles bactericide mentioned by the present invention is known and published pesticide species.
Prochloraz (prochloraz), CA registration number is 67747-09-5, chemical name is N-propyl group-N-[α-(2,4,6-Trichlorophenoxy)-1H-imidazoles-1-formamide, imidazoles broad-spectrum germicide, the various crop disease caused for sac fungi and imperfect fungus has special efficacy.
Imazalil (imazalil), CA registration number is 35554-44-0, chemical name is 1-{2-(2,4-dichlorophenyl)-2-(2-propenyloxy group) ethyl }-1H-imidazoles, interior absorption wide-spectrum bactericide, this medicine affects cell permeability of the membrane, physiological function and lipid anabolism, thus destroys the cell membrane of mould.The formation of mould fungus inhibition spore simultaneously.
Cyazofamid (cyazofamid), CA registration number is 120116-88-3, and chemical name is the chloro-2-cyano group of 4--N; N-dimethyl-5-p-methylphenyl imidazoles-1-sulfonamide; a kind of novel low-toxicity bactericide, have good prolection and certain interior suction therapeutic activity, the lasting period is long.
Fenamidone (fenamidone), CA registration number is 161326-34-7, chemical name is the chloro-2-cyano group of 4--N, N-dimethyl-5-p-methylphenyl imidazoles-1-sulfonamide, the imidazoles bactericide developed by BayerCrop Science company, thinking that its mechanism of action is the phosphorylation acting on Intramitochondrial electron transport system, hinder oxidation from ADP to ATP, playing the effect of sterilization by hindering pathogen to produce the necessary energy of breeding.
Pefurazoate (pefurazoate), CA registration number is 101903-30-4, chemical name is penta-4-thiazolinyl-N-furfuryl group-TMSIM N imidazole-1-base carbonyl-DL-high lactamine ester, imidazoles bactericide, its mechanism of action is the biosynthesis of the cell membrane important component part ergosterol destroying and stop germ, affects the breeding of germ and the synthesis of gibberellin.
In view of this, for the deficiency that prior art exists, the invention provides a kind of complex composition and the preparation thereof that contain methylsulfonyl bacterium azoles and imidazoles bactericide.This complex composition and preparation thereof have obvious synergistic function compared with single dose; can effectively prevent and treat crop bacterial disease and fungal disease; reduce the using dosage of agricultural chemicals; save drug cost; reduce spraying times; also delay the pesticide resistance of pathogen, be conducive to the comprehensive regulation of environmental protection and agricultural disease.
In order to reach object of the present invention, the technical scheme taked is:
The invention provides a kind of complex composition containing methylsulfonyl bacterium azoles and imidazoles bactericide, described complex composition is with A and B for active component, and wherein A is methylsulfonyl bacterium azoles, and B is imidazoles bactericide; The chemical name of described methylsulfonyl bacterium azoles is 2-(to fluorophenyl)-5-mesyl-1,3,4-oxadiazole; Described imidazoles bactericide be selected from Prochloraz, imazalil, cyazofamid, fluorine bacterium azoles, Fenamidone, pefurazoate any one.
The above-described complex composition containing methylsulfonyl bacterium azoles and imidazoles bactericide, preferably, described methylsulfonyl bacterium azoles and the weight ratio of imidazoles bactericide are (30:1) ~ (1:30).
The above-described complex composition containing methylsulfonyl bacterium azoles and imidazoles bactericide, more preferably, the weight ratio of above-mentioned methylsulfonyl bacterium azoles and imidazoles bactericide is (10:1) ~ (1:10).
The present invention also provides a kind of preparation containing methylsulfonyl bacterium azoles and imidazoles bactericide, the bactericide of control corps diseases, comprise acceptable auxiliary material on complex composition and agricultural chemicals that more than the present invention provides, be then prepared into the disinfectant use in agriculture of control corps diseases.
The above contains the preparation of methylsulfonyl bacterium azoles and imidazoles bactericide, and as preferred mode, the weight percentage that described complex composition accounts for above-mentioned disinfectant use in agriculture is 0.1% ~ 90%.
The above is containing the preparation of the bactericide of methylsulfonyl bacterium azoles and imidazoles, and being more preferably the weight percentage that described complex composition accounts for above-mentioned disinfectant use in agriculture is 1% ~ 80%.
The above contains the preparation of methylsulfonyl bacterium azoles and imidazoles bactericide, and described disinfectant use in agriculture can be mixed with multiple formulation according to the universal method of this area.
In embodiments more provided by the invention, the formulation of control corps diseases disinfectant use in agriculture is wetting powder, water dispersible granules, aqueous emulsion, suspending agent, granule.
In embodiments more provided by the invention, in Pesticide Science, acceptable auxiliary material is the mixture of a kind of and auxiliary agent in filler, solvent.In the Pesticide Science of those skilled in the art's accreditation, acceptable auxiliary material is all within protection scope of the present invention, and the present invention does not limit at this
Described filler is kaolin, bentonite, talcum powder, precipitated calcium carbonate, diatomite, potter's clay, attapulgite, atlapulgite, gypsum or urea.
Solvent can be toluene, dimethylbenzene, methyl oleate, methyl naphthalene, solvent naphtha, turpentine oil, vegetable oil, carrene, chloroform, methyl alcohol, ethanol, isopropyl alcohol, butanols, isoamyl alcohol, cyclohexanone, isophorone.
During described complex composition obtaining liq formulation, the solvent used is one or more in water and organic solvent, wherein organic solvent preferred alcohol, 1-METHYLPYRROLIDONE, methyl naphthalene, 200# solvent naphtha, 150# solvent naphtha.
In embodiments more provided by the invention, described auxiliary agent comprises surfactant, wetting dispersing agent, also can add other conventional functionality auxiliary agents such as antifreezing agent, thickener, stabilizing agent, defoamer, disintegrant, film forming agent if desired.
Surfactant comprises thermally coupled distillation columns, triphenyl vinyl phenol polyoxyethylene ether phosphate, styrene polyoxyethylene ether ammonium sulfate salt, alkyl biphenyl ether disulfonic acid magnesium salts, benzyl dimethyl phenol polyoxyethyl ether, phenyl phenol APEO, alkylphenol-formaldehyde resin polyoxyethyl ether, phenethyl fluosite polyoxyethyl ether, phenethyl phenol polyoxyethanyl polypropylene-base ether, ethylene oxide-propylene oxide block copolymer, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, alkylaryl polyoxyethylene polyoxypropylene ether, alkylaryl polyoxyethylene poly-oxygen propylene aether, sorbitan monostearate, sorbitan fatty acid ester APEO, one or more in fatty alcohol-polyoxyethylene ether.
Wetting dispersing agent comprises sodium lignin sulfonate, calcium lignosulfonate, Negel, two (alkyl) naphthalenesulfonate formaldehyde condensation compound, sodium methylene bis-naphthalene sulfonate, aryl phenol polyoxyethylene succinate sulfonate, succinate sodium sulfonate, sldium lauryl sulfate, octylphenol polyethylene oxyethylene group ether sulfate, polycarboxylate, alkyl benzene sulfonate calcium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, polyoxyethylene carboxylate, condensation compound of methyl naphthalene sulfonic acid and formaldehyde sulphate, naphthalene sulfonic acid-formaldehyde condensation product, methanonaphthalene sodium sulfonate, dibutyl naphthalenesulfonic acid formaldehyde condensation products, N-Methyl fatty acyl taurines sodium, alkylphenol polyoxyethylene formaldehyde condensation products sulphate, alkylphenol polyoxyethylene phosphate, the withered powder of tea, saponin, lignosulfite, aliphatic alcohol sulfate, dodecyl sodium sulfate, fatty acid amide-N methyl taurine sodium salt, sodium sulfate of polyethenoxy ether of fatty alcohol, pull open powder.
Disintegrant comprises potassium phosphate, potash, potassium sulfate, sodium chloride, sodium sulphate, sodium phosphate, ammonium sulfate.
Antifreezing agent comprises glycerine, propane diols, ethylene glycol, isopropyl alcohol, urea.
Complex composition provided by the invention is applicable to control crop bacterial disease, as bacterial blight of rice and slice disease, solanaceous vegetable bacterial wilt, cucurbit wilt, tobacco bacterial wilt of peanut, cucumber bacterial angular leaf spot, soft rot of cabbage, oranges and tangerines canker of tomato etc.Be not limited only to this, also have agriculturally common all bacterial diseases, all can in its prevention and treatment range.
Described complex composition provided by the invention is applicable to control crop fungal disease, as rice blast, cucurbits fusarium wilt, leaf spot of peanut, anthracnose of tobacco, mango anthracnose, citrus scab etc.
The present composition can be used by commonsense method, as added the process of water spray cauline leaf, also can spread fertilizer over the fields or water by root, can also dress seed or seed pelleting use.Be mainly used in prevention and corntrol bacterial disease and fungal disease, to guarantee crop yield.
The advantage that complex composition of the present invention has compared to existing technology:
1, complex composition of the present invention and preparation thereof, have obvious synergistic function relative to single dose, bactericidal effect is apparently higher than single dose.
2, reduce the using dosage of agricultural chemicals, reduce peasant's drug cost.
3, by two different classes of fungicide compoundings, both have the different modes of action, the different mechanism of action, and expanding prevention is composed, and has both extended the Pesticide use life-span, delays again the generation of pest resistance to insecticide.
Embodiment
The present invention's the following example is described, but does not limit the scope of the invention, and 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, to roll over hundred calculating.Content in embodiment is weight percentage,
Embodiment prepared by preparation:
The preparation of Application Example one wetting powder
By methylsulfonyl bacterium azoles (being called for short first sulphur), the mixing of imidazoles bactericide, dispersant, wetting agent, filler, mix in mixed cylinder, mix again after airslide disintegrating mill is pulverized, namely can be made into the wetting powder of disinfectant use in agriculture of the present invention.Specifically see the following form.
The preparation of Application Example two granule
Methylsulfonyl bacterium azoles (being called for short first sulphur), imidazoles bactericide, wetting dispersing agent, disintegrant, filler are mixed; pulverize, stir after adding water-wet, then use screw extruder pelletizer granulation; sieve after drying, obtain the granule of disinfectant use in agriculture of the present invention.Specifically see the following form:
The preparation of Application Example three, aqueous emulsion
Methylsulfonyl bacterium azoles (being called for short first sulphur), imidazoles bactericide, solvent, surfactant are added together, make to be dissolved into homogeneous oil phase; Water, antifreezing agent are mixed, becomes homogeneous aqueous phase.Under high velocity agitation, aqueous phase is added oil phase, the aqueous emulsion of obtained disinfectant use in agriculture of the present invention.Specifically see the following form:
The preparation of Application Example four suspending agent
By methylsulfonyl bacterium azoles (being called for short first sulphur), the mixing of imidazoles bactericide, antifreezing agent, thickener, surfactant, water, mix through high speed shear, add methylsulfonyl bacterium azoles, imidazoles bactericide successively, abrading-ball 2 ~ 3 hours in ball crusher, the suspending agent of obtained disinfectant use in agriculture of the present invention.Specifically see the following form:
The preparation of Application Example five water dispersible granules
Methylsulfonyl bacterium azoles (be called for short first sulphur), imidazoles bactericide, wetting dispersing agent, disintegrant, filler are obtained together the particle diameter needed through air-flow crushing, obtain semi-product material.Material dosing is sent in fluidized bed granulating dryer through granulating and after drying, obtaining the water dispersible granules of disinfectant use in agriculture of the present invention.Specifically see the following form
BIOLOGICAL ACTIVITY EXAMPLES
In order to verify methylsulfonyl bacterium azoles and the bactericide compounded drug effect to crop bacterial disease and fungal disease of imidazoles, specify built agent to compare single dose and whether have synergistic effect, whether can reach the double object controlled, reduce dosage, We conducted Toxicity Determination and field control effectiveness test.
Toxicity Determination:
Below raw test is tested and is adopted Sun Yun abundant method calculating co-toxicity coefficient (CTC) to evaluate 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: (the water prevention rice bacterial leaf blight)
Bacterium solution preparation: bacterial classification cultured in test tube is extracted test tube tampon near alcolhol burner place, pour 10ml sterile water into, with disinfection inoculation pin, germ on inclined-plane is scraped gently, make spore suspension, being poured into by this spore suspension is equipped with in the sterilizing triangular flask of several glass marbles in advance again, cross bacteriological filtration liquid with sterile gauze after shake 5min, put in another sterilizing triangular flask, namely make required bacterium liquid.
Experimental technique: by beef extract-peptone agar medium melt, to be cooled to 45 DEG C ~ 50 DEG C time, aseptically pour into rapidly in sterilizing culture dish together with 0.2ml bacterial suspension, every ware 15ml medium, shakes up rear cooled and solidified.With card punch (aperture 4mm) punching after sterilizing, 1ml liquid is dripped in circular hole, be placed in after 28 DEG C of insulating boxs cultivate 2d, measure 2 diameters of inhibition zone by right-angled intersection method with slide measure, average, calculate inhibiting rate, obtain virulence curve and EC
50, and press Sun Yun abundant method calculating co-toxicity coefficient.
Measurement result is in table 1 ~ table 3.
The joint toxicity measuring result of table 1 methylsulfonyl bacterium azoles and the composite water prevention rice bacterial leaf blight of Prochloraz
| EC 50(μg/ml) | ATI | TTI | CTC | |
| Methylsulfonyl bacterium azoles (A) | 10.97 | 100.00 | / | / |
| Prochloraz (B) | 37.85 | 28.98 | / | / |
| A:B＝40:1 | 9.58 | 114.51 | 98.27 | 116.53 |
| A:B＝30:1 | 8.94 | 122.71 | 97.71 | 125.58 |
| A:B＝20:1 | 8.26 | 132.81 | 96.62 | 137.46 |
| A:B＝10:1 | 7.63 | 143.77 | 93.54 | 153.70 |
| A:B＝4:1 | 6.8 | 161.32 | 85.80 | 188.03 |
| A:B＝2:1 | 5.93 | 184.99 | 76.33 | 242.37 |
| A:B＝1:1 | 6.94 | 158.07 | 64.49 | 245.10 |
| A:B＝1:2 | 10.88 | 100.83 | 52.66 | 191.49 |
| A:B＝1:4 | 13.67 | 80.25 | 43.19 | 185.82 |
| A:B＝1:10 | 19.73 | 55.60 | 35.44 | 156.89 |
| A:B＝1:20 | 23.71 | 46.27 | 32.36 | 142.96 |
| A:B＝1:30 | 28.72 | 38.20 | 31.27 | 122.14 |
| A:B＝1:40 | 30.72 | 35.71 | 30.71 | 116.26 |
From measurement result table 1, methylsulfonyl bacterium azoles and Prochloraz by weight be (30:1) ~ (1:30) scope in composite, the co-toxicity coefficient of the water prevention rice bacterial leaf blight all reaches more than 120, has obvious synergistic effect.Particularly, when composite in the scope that weight ratio is (10:1) ~ (1:10), the co-toxicity coefficient of each process reaches more than 153, and synergy is particularly remarkable.
The joint toxicity measuring result of table 2 methylsulfonyl bacterium azoles and the composite water prevention rice bacterial leaf blight of fluorine bacterium azoles
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 10.97 | 100.00 | / | / |
| Fluorine bacterium azoles (B) | 77.17 | 14.22 | / | / |
| A:B＝40:1 | 11.77 | 93.20 | 97.91 | 95.19 |
| A:B＝30:1 | 9.08 | 120.81 | 97.23 | 124.25 |
| A:B＝20:1 | 8.43 | 130.13 | 95.92 | 135.67 |
| A:B＝10:1 | 7.74 | 141.73 | 92.20 | 153.72 |
| A:B＝5:1 | 6.82 | 160.85 | 85.70 | 187.68 |
| A:B＝2:1 | 6.14 | 178.66 | 71.41 | 250.21 |
| A:B＝1:1 | 8.73 | 125.66 | 57.11 | 220.04 |
| A:B＝1:2 | 13.67 | 80.25 | 42.81 | 187.45 |
| A:B＝1:5 | 23.48 | 46.72 | 28.51 | 163.86 |
| A:B＝1:10 | 32.47 | 33.79 | 22.01 | 153.47 |
| A:B＝1:20 | 41.96 | 26.14 | 18.30 | 142.86 |
| A:B＝1:30 | 52.19 | 21.02 | 16.98 | 123.77 |
| A:B＝1:40 | 60.72 | 18.07 | 16.31 | 110.79 |
From measurement result table 2, methylsulfonyl bacterium azoles and fluorine bacterium azoles by weight be (30:1) ~ (1:30) scope in composite, the co-toxicity coefficient of the water prevention rice bacterial leaf blight all reaches more than 120, has obvious synergistic effect.Particularly, when composite in the scope that weight ratio is (10:1) ~ (1:10), the co-toxicity coefficient of each process reaches more than 153, synergy highly significant.
The joint toxicity measuring result of table 3 methylsulfonyl bacterium azoles and the composite water prevention rice bacterial leaf blight of pefurazoate
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 10.97 | 100.00 | / | / |
| Pefurazoate (B) | 64.79 | 16.93 | / | / |
| A:B＝40:1 | 11.77 | 93.20 | 97.97 | 95.13 |
| A:B＝30:1 | 9.17 | 119.63 | 97.32 | 122.92 |
| A:B＝20:1 | 8.35 | 131.38 | 96.04 | 136.79 |
| A:B＝10:1 | 7.83 | 140.10 | 92.45 | 151.55 |
| A:B＝5:1 | 6.49 | 169.03 | 86.16 | 196.19 |
| A:B＝2:1 | 5.97 | 183.75 | 72.31 | 254.12 |
| A:B＝1:1 | 8.88 | 123.54 | 58.47 | 211.30 |
| A:B＝1:2 | 12.39 | 88.54 | 44.62 | 198.42 |
| A:B＝1:5 | 18.97 | 57.83 | 30.78 | 187.90 |
| A:B＝1:10 | 29.68 | 36.96 | 24.48 | 150.96 |
| A:B＝1:20 | 35.82 | 30.63 | 20.89 | 146.62 |
| A:B＝1:30 | 44.78 | 24.50 | 19.61 | 124.92 |
| A:B＝1:40 | 52.16 | 21.03 | 18.96 | 110.94 |
From measurement result table 3, methylsulfonyl bacterium azoles and pefurazoate by weight be (30:1) ~ (1:30) scope in composite, the co-toxicity coefficient of the water prevention rice bacterial leaf blight all reaches more than 120, has obvious synergistic effect.Particularly, when composite in the scope that weight ratio is (10:1) ~ (1:10), the co-toxicity coefficient of each process reaches more than 150, synergy highly significant.
Toxicity Determination embodiment two: (control citrus bacterial canker disease)
Test is with reference to " pesticide bioassay technology " (old spring chief editor, publishing house of Beijing Agricultural University publishes) and " farm-chemical indoor determination test rule NY/T1156.2-2006 ".This test adopts inhibition zone method.On aseptic operating platform, poured into by NA medium on NA flat board, after drying, the citrus processing bacteria suspension spreading rod getting 0.1ml is applied on NA flat board equably.After drying, punch in dull and stereotyped central authorities with the card punch of diameter 7mm, then get 100 μ l liquids in aperture.Each concentration 5 repetition.To add the process of sterile water in aperture for blank.Be placed on the insulating box aseptic culture of 28 ± 0.5 DEG C after process, take out after 2d.Adopt right-angled intersection method to measure the antibacterial circle diameter (in units of millimeter) of each process respectively, and calculate mean value, the inhibiting rate of antibacterial circle diameter.Carry out statistical analysis with DPS data processing software, calculate the EC of each medicament
50, then press the abundant method of Sun Yun and calculate co-toxicity coefficient (CTC).
Measurement result is in table 4 ~ table 7.
The joint toxicity measuring result of table 4 methylsulfonyl bacterium azoles and the composite control citrus bacterial canker disease of Prochloraz
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 8.67 | 100.00 | / | / |
| Prochloraz (B) | 46.76 | 18.54 | / | / |
| A:B＝50:1 | 8.19 | 105.86 | 98.40 | 107.58 |
| A:B＝30:1 | 7.27 | 119.26 | 97.37 | 122.48 |
| A:B＝20:1 | 7.03 | 123.33 | 96.12 | 128.31 |
| A:B＝15:1 | 6.67 | 129.99 | 94.91 | 136.96 |
| A:B＝10:1 | 6.18 | 140.29 | 92.59 | 151.51 |
| A:B＝5:1 | 5.37 | 161.45 | 86.42 | 186.82 |
| A:B＝3:1 | 5.74 | 151.05 | 79.64 | 189.67 |
| A:B＝1:1 | 8.49 | 102.12 | 59.27 | 172.29 |
| A:B＝1:3 | 13.35 | 64.94 | 38.91 | 166.92 |
| A:B＝1:5 | 16.29 | 53.22 | 32.12 | 165.71 |
| A:B＝1:10 | 21.78 | 39.81 | 25.95 | 153.42 |
| A:B＝1:15 | 25.87 | 33.51 | 23.63 | 141.81 |
| A:B＝1:20 | 29.46 | 29.43 | 22.42 | 131.26 |
| A:B＝1:30 | 33.27 | 26.06 | 21.17 | 123.10 |
| A:B＝1:50 | 41.27 | 21.01 | 20.14 | 104.32 |
From measurement result table 4, methylsulfonyl bacterium azoles and Prochloraz all reach more than 120 by weight the co-toxicity coefficient of composite control citrus bacterial canker disease in the scope for (30:1) ~ (1:30), and both explanations are composite has obvious synergistic effect to control citrus bacterial canker disease.Particularly, weight ratio is (10:1): composite in (1:10) scope, and the co-toxicity coefficient of each process reaches more than 151, synergy highly significant.
The joint toxicity measuring result of table 5 methylsulfonyl bacterium azoles and the composite control citrus bacterial canker disease of imazalil
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 8.67 | 100.00 | / | / |
| Imazalil (B) | 113.58 | 7.63 | / | / |
| A:B＝50:1 | 9.12 | 95.07 | 98.19 | 96.82 |
| A:B＝30:1 | 7.19 | 120.58 | 97.02 | 124.29 |
| A:B＝20:1 | 6.83 | 126.94 | 95.60 | 132.78 |
| A:B＝15:1 | 6.49 | 133.59 | 94.23 | 141.77 |
| A:B＝10:1 | 6.18 | 140.29 | 91.60 | 153.15 |
| A:B＝5:1 | 5.83 | 148.71 | 84.61 | 175.77 |
| A:B＝2:1 | 5.37 | 161.45 | 69.21 | 233.28 |
| A:B＝1:1 | 6.94 | 124.93 | 53.82 | 232.14 |
| A:B＝1:2 | 10.93 | 79.32 | 38.42 | 206.45 |
| A:B＝1:5 | 21.82 | 39.73 | 23.03 | 172.55 |
| A:B＝1:10 | 35.89 | 24.16 | 16.03 | 150.70 |
| A:B＝1:15 | 46.35 | 18.71 | 13.41 | 139.53 |
| A:B＝1:20 | 55.24 | 15.70 | 12.03 | 130.45 |
| A:B＝1:30 | 67.19 | 12.90 | 10.61 | 121.58 |
| A:B＝1:50 | 78.64 | 11.02 | 9.44 | 116.73 |
From measurement result table 5, methylsulfonyl bacterium azoles and imazalil all reach more than 120 by weight the co-toxicity coefficient of composite control citrus bacterial canker disease in the scope for (30:1) ~ (1:30), and both explanations are composite has obvious synergistic effect to control citrus bacterial canker disease.Particularly, weight ratio is (10:1): composite in (1:10) scope, and the co-toxicity coefficient of each process reaches more than 150, synergy highly significant.
The joint toxicity measuring result of table 6 methylsulfonyl bacterium azoles and the composite control citrus bacterial canker disease of cyazofamid
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 8.67 | 100.00 | / | / |
| Cyazofamid (B) | 124.92 | 6.94 | / | / |
| A:B＝50:1 | 8.72 | 99.43 | 98.18 | 101.27 |
| A:B＝30:1 | 7.24 | 119.75 | 97.00 | 123.46 |
| A:B＝20:1 | 6.97 | 124.39 | 95.57 | 130.16 |
| A:B＝15:1 | 6.44 | 134.63 | 94.18 | 142.94 |
| A:B＝10:1 | 6.17 | 140.52 | 91.54 | 153.51 |
| A:B＝5:1 | 5.76 | 150.52 | 84.49 | 178.15 |
| A:B＝2:1 | 5.29 | 163.89 | 68.98 | 237.60 |
| A:B＝1:1 | 7.31 | 118.60 | 53.47 | 221.81 |
| A:B＝1:2 | 12.18 | 71.18 | 37.96 | 187.52 |
| A:B＝1:5 | 24.67 | 35.14 | 22.45 | 156.54 |
| A:B＝1:10 | 37.27 | 23.26 | 15.40 | 151.05 |
| A:B＝1:15 | 48.18 | 18.00 | 12.76 | 141.06 |
| A:B＝1:20 | 58.27 | 14.88 | 11.37 | 130.84 |
| A:B＝1:30 | 69.29 | 12.51 | 9.94 | 125.85 |
| A:B＝1:50 | 84.56 | 10.25 | 8.77 | 116.98 |
From measurement result table 6, methylsulfonyl bacterium azoles and cyazofamid all reach more than 120 by weight the co-toxicity coefficient of composite control citrus bacterial canker disease in the scope for (30:1) ~ (1:30), and both explanations are composite has obvious synergistic effect to control citrus bacterial canker disease.Particularly, weight ratio is (10:1): composite in (1:10) scope, and the co-toxicity coefficient of each process reaches more than 151, synergy highly significant.
The joint toxicity measuring result of table 7 methylsulfonyl bacterium azoles and the composite control citrus bacterial canker disease of Fenamidone
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 8.67 | 100.00 | / | / |
| Fenamidone (B) | 108.76 | 7.97 | / | / |
| A:B＝50:1 | 7.96 | 108.92 | 98.20 | 110.92 |
| A:B＝30:1 | 7.31 | 118.60 | 97.03 | 122.23 |
| A:B＝20:1 | 7.04 | 123.15 | 95.62 | 128.80 |
| A:B＝15:1 | 6.56 | 132.16 | 94.25 | 140.23 |
| A:B＝10:1 | 6.20 | 139.84 | 91.63 | 152.61 |
| A:B＝5:1 | 5.64 | 153.72 | 84.66 | 181.57 |
| A:B＝3:1 | 6.33 | 136.97 | 76.99 | 177.90 |
| A:B＝1:1 | 6.79 | 127.69 | 53.99 | 236.52 |
| A:B＝1:3 | 14.87 | 58.31 | 30.98 | 188.21 |
| A:B＝1:5 | 22.73 | 38.14 | 23.31 | 163.64 |
| A:B＝1:10 | 34.57 | 25.08 | 16.34 | 153.51 |
| A:B＝1:15 | 44.83 | 19.34 | 13.72 | 140.92 |
| A:B＝1:20 | 53.65 | 16.16 | 12.35 | 130.81 |
| A:B＝1:30 | 63.09 | 13.74 | 10.94 | 125.61 |
| A:B＝1:50 | 74.56 | 11.63 | 9.78 | 118.94 |
From measurement result table 7, methylsulfonyl bacterium azoles and Fenamidone all reach more than 120 by weight the co-toxicity coefficient of composite control citrus bacterial canker disease in the scope for (30:1) ~ (1:30), and both explanations are composite has obvious synergistic effect to control citrus bacterial canker disease.Particularly, weight ratio is (10:1): composite in (1:10) scope, and the co-toxicity coefficient of each process reaches more than 1521, synergy highly significant.
Toxicity Determination embodiment three: (control Muskmelon Fusarium wilt)
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 EC of each medicament
50, and the co-toxicity coefficient of mixture is calculated according to the abundant method of Sun Yun.
Measurement result is in table 8 ~ table 13.
The joint toxicity measuring result of table 8 methylsulfonyl bacterium azoles and the composite control Muskmelon Fusarium wilt of Prochloraz
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 17.42 | 100.00 | / | / |
| Prochloraz (B) | 0.09 | 19355.56 | / | / |
| A:B＝40:1 | 2.740 | 635.77 | 569.65 | 111.61 |
| A:B＝30:1 | 2.011 | 866.24 | 721.15 | 120.12 |
| A:B＝20:1 | 1.274 | 1367.35 | 1016.93 | 134.46 |
| A:B＝10:1 | 0.623 | 2796.15 | 1850.51 | 151.10 |
| A:B＝8:1 | 0.564 | 3088.65 | 2239.51 | 137.92 |
| A:B＝5:1 | 0.328 | 5310.98 | 3309.26 | 160.49 |
| A:B＝2:1 | 0.115 | 15147.83 | 6518.52 | 232.38 |
| A:B＝1:1 | 0.069 | 25246.38 | 9727.78 | 259.53 |
| A:B＝1:2 | 0.069 | 25246.38 | 12937.04 | 195.15 |
| A:B＝1:5 | 0.067 | 26000.00 | 16146.30 | 161.03 |
| A:B＝1:8 | 0.066 | 26393.94 | 17216.05 | 153.31 |
| A:B＝1:10 | 0.065 | 26800.00 | 17605.05 | 152.23 |
| A:B＝1:15 | 0.070 | 24885.71 | 18152.08 | 137.10 |
| A:B＝1:20 | 0.073 | 23863.01 | 18438.62 | 129.42 |
| A:B＝1:30 | 0.076 | 22921.05 | 18734.41 | 122.35 |
From measurement result table 8, methylsulfonyl bacterium azoles and Prochloraz all reach more than 120 by weight the composite co-toxicity coefficient to Muskmelon Fusarium wilt in the scope for (30:1) ~ (1:30), and both explanations composite control Muskmelon Fusarium wilt in this ratio range has obvious synergistic effect.Particularly, when composite in the scope that weight ratio is (10:1) ~ (1:10), the co-toxicity coefficient of each process reaches more than 151, synergy highly significant.
The joint toxicity measuring result of table 9 methylsulfonyl bacterium azoles and the composite control Muskmelon Fusarium wilt of imazalil
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 17.52 | 100.00 | / | / |
| Imazalil (B) | 1.4 | 1251.43 | / | / |
| A:B＝40:1 | 11.72 | 149.49 | 128.08 | 116.71 |
| A:B＝30:1 | 10.23 | 171.26 | 137.14 | 124.88 |
| A:B＝14:1 | 6.92 | 253.18 | 176.76 | 143.23 |
| A:B＝10:1 | 5.58 | 313.98 | 204.68 | 153.40 |
| A:B＝8:1 | 4.72 | 371.19 | 227.94 | 162.85 |
| A:B＝5:1 | 3.18 | 550.94 | 291.90 | 188.74 |
| A:B＝3:1 | 1.72 | 1018.60 | 387.86 | 262.62 |
| A:B＝1:1 | 1.01 | 1734.65 | 675.71 | 256.71 |
| A:B＝1:3 | 1 | 1752.00 | 963.57 | 181.82 |
| A:B＝1:5 | 1 | 1752.00 | 1059.52 | 165.36 |
| A:B＝1:8 | 1 | 1752.00 | 1123.49 | 155.94 |
| A:B＝1:10 | 1.01 | 1734.65 | 1146.75 | 151.27 |
| A:B＝1:14 | 1.09 | 1607.34 | 1174.67 | 136.83 |
| A:B＝1:20 | 1.14 | 1536.84 | 1196.60 | 128.43 |
| A:B＝1:30 | 1.15 | 1523.48 | 1214.29 | 125.46 |
From measurement result table 9, methylsulfonyl bacterium azoles and imazalil all reach more than 120 by weight the composite co-toxicity coefficient to Muskmelon Fusarium wilt in the scope for (30:1) ~ (1:30), and both explanations composite control Muskmelon Fusarium wilt in this ratio range has obvious synergistic effect.Particularly, when composite in the scope that weight ratio is (10:1) ~ (1:10), the co-toxicity coefficient of each process reaches more than 151, synergy highly significant.
The joint toxicity measuring result of table 10 methylsulfonyl bacterium azoles and the composite control Muskmelon Fusarium wilt of cyazofamid
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 16.53 | 100.00 | / | / |
| Cyazofamid (B) | 1.51 | 1094.70 | / | / |
| A:B＝40:1 | 11.37 | 145.38 | 124.26 | 117.00 |
| A:B＝30:1 | 9.86 | 167.65 | 132.09 | 126.92 |
| A:B＝14:1 | 7.71 | 214.40 | 166.31 | 128.91 |
| A:B＝10:1 | 5.54 | 298.38 | 190.43 | 156.69 |
| A:B＝8:1 | 4.68 | 353.21 | 210.52 | 167.78 |
| A:B＝4:1 | 3.19 | 518.18 | 298.94 | 173.34 |
| A:B＝2:1 | 1.76 | 939.20 | 431.57 | 217.63 |
| A:B＝1:1 | 1.06 | 1559.43 | 597.35 | 261.06 |
| A:B＝1:2 | 1.03 | 1604.85 | 763.13 | 210.30 |
| A:B＝1:4 | 1.05 | 1574.29 | 895.76 | 175.75 |
| A:B＝1:8 | 1.07 | 1544.86 | 984.18 | 156.97 |
| A:B＝1:10 | 1.09 | 1516.51 | 1004.27 | 151.01 |
| A:B＝1:14 | 1.14 | 1450.00 | 1028.39 | 141.00 |
| A:B＝1:20 | 1.18 | 1400.85 | 1047.34 | 133.75 |
| A:B＝1:30 | 1.27 | 1301.57 | 1062.61 | 122.49 |
From measurement result table 10, methylsulfonyl bacterium azoles and cyazofamid all reach more than 120 by weight the composite co-toxicity coefficient to Muskmelon Fusarium wilt in the scope for (30:1) ~ (1:30), and both explanations composite control Muskmelon Fusarium wilt in this ratio range has obvious synergistic effect.Particularly, when composite in the scope that weight ratio is (10:1) ~ (1:10), the co-toxicity coefficient of each process reaches more than 151, synergy highly significant.
The joint toxicity measuring result of table 11 methylsulfonyl bacterium azoles and the composite control Muskmelon Fusarium wilt of fluorine bacterium azoles
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 18.37 | 100.00 | / | / |
| Fluorine bacterium azoles (B) | 1.20 | 1530.83 | / | / |
| A:B＝50:1 | 17.29 | 106.25 | 128.06 | 82.97 |
| A:B＝40:1 | 13.68 | 134.28 | 134.90 | 99.54 |
| A:B＝30:1 | 10.24 | 179.39 | 146.16 | 122.74 |
| A:B＝20:1 | 7.44 | 246.91 | 168.13 | 146.85 |
| A:B＝10:1 | 5.27 | 348.58 | 230.08 | 151.51 |
| A:B＝4:1 | 2.93 | 626.96 | 386.17 | 162.36 |
| A:B＝2:1 | 1.59 | 1155.35 | 576.94 | 200.25 |
| A:B＝1:1 | 0.94 | 1954.26 | 815.42 | 239.66 |
| A:B＝1:2 | 0.71 | 2587.32 | 1053.89 | 245.50 |
| A:B＝1:4 | 0.77 | 2385.71 | 1244.67 | 191.67 |
| A:B＝1:10 | 0.85 | 2161.18 | 1400.76 | 154.29 |
| A:B＝1:20 | 0.93 | 1975.27 | 1462.70 | 135.04 |
| A:B＝1:30 | 1.02 | 1800.98 | 1484.68 | 121.30 |
| A:B＝1:40 | 1.22 | 1505.74 | 1495.93 | 100.66 |
| A:B＝1:50 | 1.37 | 1340.88 | 1502.78 | 89.23 |
From measurement result table 11, methylsulfonyl bacterium azoles and fluorine bacterium azoles all reach more than 120 by weight the composite co-toxicity coefficient to Muskmelon Fusarium wilt in the scope for (30:1) ~ (1:30), and both explanations composite control Muskmelon Fusarium wilt in this ratio range has obvious synergistic effect.Particularly, when composite in the scope that weight ratio is (10:1) ~ (1:10), the co-toxicity coefficient of each process reaches more than 151, synergy highly significant.
The joint toxicity measuring result of table 12 methylsulfonyl bacterium azoles and the composite control Muskmelon Fusarium wilt of Fenamidone
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 18.37 | 100.00 | / | / |
| Fenamidone (B) | 1.10 | 1670.00 | / | / |
| A:B＝40:1 | 13.74 | 133.70 | 138.29 | 96.68 |
| A:B＝30:1 | 10.02 | 183.33 | 150.65 | 121.70 |
| A:B＝20:1 | 7.64 | 240.45 | 174.76 | 137.58 |
| A:B＝10:1 | 4.89 | 375.66 | 242.73 | 154.77 |
| A:B＝4:1 | 2.34 | 785.04 | 414.00 | 189.62 |
| A:B＝2:1 | 1.17 | 1570.09 | 623.33 | 251.89 |
| A:B＝1:1 | 0.96 | 1913.54 | 885.00 | 216.22 |
| A:B＝1:2 | 0.91 | 2018.68 | 1146.67 | 176.05 |
| A:B＝1:4 | 0.83 | 2213.25 | 1356.00 | 163.22 |
| A:B＝1:10 | 0.78 | 2355.13 | 1527.27 | 154.20 |
| A:B＝1:20 | 0.83 | 2213.25 | 1595.24 | 138.74 |
| A:B＝1:30 | 0.92 | 1996.74 | 1619.35 | 123.30 |
| A:B＝1:40 | 1.07 | 1716.82 | 1631.71 | 105.22 |
From measurement result table 12, methylsulfonyl bacterium azoles and Fenamidone all reach more than 120 by weight the composite co-toxicity coefficient to Muskmelon Fusarium wilt in the scope for (30:1) ~ (1:30), and both explanations composite control Muskmelon Fusarium wilt in this ratio range has obvious synergistic effect.Particularly, when composite in the scope that weight ratio is (10:1) ~ (1:10), the co-toxicity coefficient of each process reaches more than 154, synergy highly significant.
The joint toxicity measuring result of table 13 methylsulfonyl bacterium azoles and the composite control Muskmelon Fusarium wilt of pefurazoate
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 18.37 | 100.00 | / | / |
| Pefurazoate (B) | 3.86 | 475.91 | / | / |
| A:B＝40:1 | 14.27 | 128.73 | 109.17 | 117.92 |
| A:B＝30:1 | 13.53 | 135.77 | 112.13 | 121.09 |
| A:B＝20:1 | 11.34 | 161.99 | 117.90 | 137.40 |
| A:B＝10:1 | 9.07 | 202.54 | 134.17 | 150.95 |
| A:B＝5:1 | 6.49 | 283.05 | 162.65 | 174.02 |
| A:B＝2:1 | 3.76 | 488.56 | 225.30 | 216.85 |
| A:B＝1:1 | 2.87 | 640.07 | 287.95 | 222.28 |
| A:B＝1:2 | 2.59 | 709.27 | 350.60 | 202.30 |
| A:B＝1:5 | 2.24 | 820.09 | 413.26 | 198.45 |
| A:B＝1:10 | 2.74 | 670.44 | 441.73 | 151.77 |
| A:B＝1:20 | 2.96 | 620.61 | 458.01 | 135.50 |
| A:B＝1:30 | 3.19 | 575.86 | 463.78 | 124.17 |
| A:B＝1:40 | 3.37 | 545.10 | 466.74 | 116.79 |
From measurement result table 12, methylsulfonyl bacterium azoles and pefurazoate are in the scope of (30:1) ~ (1:30) by weight
The composite co-toxicity coefficient to Muskmelon Fusarium wilt all reaches more than 120, and both explanations are composite control muskmelon in this ratio range
Fusarium wilt has obvious synergistic effect.Particularly, when composite in the scope that weight ratio is (10:1) ~ (1:10), respectively
The co-toxicity coefficient of process reaches more than 150, synergy highly significant.
Land for growing field crops test examples
Composite bactericide composition of the present invention, its active component methylsulfonyl bacterium azoles is (in all land for growing field crops test examples, easy in order to state, can with " first sulphur " representative " methylsulfonyl bacterium azoles ") with imidazoles is bactericide compounded, there is obvious synergistic function, indoor synergistic results obtains checking in field, further illustrates below with several field efficacy embodiment.
Contrast medicament:
CK1:20% methylsulfonyl bacterium azoles wetting powder, self-control;
CK2:10% pefurazoate EW, self-control;
CK3:10% Fenamidone EW, self-control;
CK4:25% Prochloraz EC, registration card number PD20080328, Sichuan Lanyue Science & Technology Co., Ltd., commercial;
CK5:20% imazalil EW, registration card number LS20140058, Jiangsu Sword Agrochemical Co., Ltd., commercial;
CK6:100g/L cyazofamid SC, registration card number PD20141025, Shengnong Biological-Chemical Products Co., Ltd., Shanghai, commercial;
CK7:30% fluorine bacterium azoles WP, registration card number PD20121474, Shaanxi Meibang Pesticide Co., Ltd., commercial.
Field efficacy embodiment one: the field control effectiveness test of the water prevention rice bacterial leaf blight
Test method and computational methods are with reference to " GB/T17980.19-2000 pesticide field efficacy medicine test criterion (one) bactericidal agent for preventing and treating paddy rice leaf diseases ", every plot area 20m2, often process and repeat for 4 times, if clear water is treated to blank, spray pesticide is carried out, the dispenser of interval 7d second time in their early stage.Respectively at 14d investigation result after 7d, second time medicine before first time medicine, after second time medicine, classification investigation incidence, calculates disease index, preventive effect.The results are shown in Table 14 and table 15:
The field control effectiveness test result of table 14 methylsulfonyl bacterium azoles and the composite water prevention rice bacterial leaf blight of Prochloraz
Known according to field test results table 14, when methylsulfonyl bacterium azoles and the composite water prevention rice bacterial leaf blight of Prochloraz, when active ingredient dosage is less than single dose, all obtain the control efficiency higher than single dose, after second time medicine, the preventive effect of 15d is higher than single dose more than 18.14%.After second time medicine, 14d can also keep good drug effect (more than 74%), and the lasting period is long, minimizing spraying times that can be suitable in practical application.
Table 15 methylsulfonyl bacterium azoles respectively with the field control effectiveness test result of fluorine bacterium azoles, the composite water prevention rice bacterial leaf blight of pefurazoate
Known according to field test results table 15, methylsulfonyl bacterium azoles is respectively with fluorine bacterium azoles, pefurazoate during composite control of plant bacterial wilt, when active ingredient dosage is less than single dose, all obtain the control efficiency higher than single dose, after second time medicine, the preventive effect of 15d is higher than single dose more than 18.81%.After second time medicine, 14d can also keep good drug effect (more than 78%), and the lasting period is long, minimizing spraying times that can be suitable in practical application.
Field efficacy embodiment two: the field control effectiveness test of control citrus bacterial canker disease
Test method and computational methods are with reference to " GB/T17980.103-2004 pesticide field efficacy medicine test criterion (two) the 103rd part: bactericidal agent for preventing and treating citrus bacterial canker disease ", every community is for becoming fruit tree 3 strain in age, often process and repeat for 4 times, if clear water is treated to blank, spray pesticide is carried out, the dispenser of interval 7d second time in their early stage.Respectively at 14d investigation result after 7d, second time medicine before first time medicine, after second time medicine, in units of blade, classification investigation incidence, calculates disease index, preventive effect.The results are shown in Table 16:
Table 16 methylsulfonyl bacterium azoles respectively with the field control effectiveness test result of imazalil, cyazofamid, the composite control citrus bacterial canker disease of Fenamidone
Known according to field test results table 16, methylsulfonyl bacterium azoles is respectively with imazalil, cyazofamid, Fenamidone during composite control citrus bacterial canker disease, when active ingredient dosage is less than single dose, all obtain the control efficiency higher than single dose, after second time medicine, the preventive effect of 15d is higher than single dose more than 19.76%.After second time medicine, 14d can also keep good drug effect (more than 77%), and the lasting period is long, minimizing spraying times that can be suitable in practical application.
Field efficacy embodiment three: the field control effectiveness test of control Muskmelon Fusarium wilt
Test method and computational methods are with reference to " GB/T17980.113-2004 pesticide field efficacy medicine test criterion (two) the 113rd part: bactericidal agent for preventing and treating cucurbits fusarium wilt ", every plot area 30m2, often process and repeat for 4 times, non-dispenser is treated to blank, carry out the dispenser of filling root in their early stage, interval 10d executes second time medicine.Respectively at 30d investigation result after 15d, medicine after medicine before medicine, after second time medicine, investigate all plant of each community, record total strain number, diseased plant number, calculate diseased plant rate, preventive effect.The results are shown in Table 17, table 18:
The field control effectiveness test result of table 17 methylsulfonyl bacterium azoles and the composite control Muskmelon Fusarium wilt of Prochloraz
Known according to field test results table 17, when methylsulfonyl bacterium azoles and the composite control Muskmelon Fusarium wilt of Prochloraz, when active ingredient dosage is less than single dose, all obtain the control efficiency higher than single dose, after second time medicine, the preventive effect of 15d is higher than single dose more than 21.65%.After second time medicine, 30d can also keep good drug effect (more than 73%), and the lasting period is long, minimizing spraying times that can be suitable in practical application.
Table 18 methylsulfonyl bacterium azoles is the field control effectiveness test result of composite control Muskmelon Fusarium wilt with imazalil, cyazofamid etc. respectively
Known according to field test results table 18, methylsulfonyl bacterium azoles is respectively with imazalil, cyazofamid, fluorine bacterium azoles, Fenamidone, pefurazoate during composite control Muskmelon Fusarium wilt, when active ingredient dosage is less than single dose, all obtain the control efficiency higher than single dose, after second time medicine, the preventive effect of 15d is higher than single dose more than 34.78%.After second time medicine, 30d can also keep good drug effect (more than 75%), and the lasting period is long, minimizing spraying times that can be suitable in practical application.
Claims (8)
1. contain a complex composition for methylsulfonyl bacterium azoles and imidazoles bactericide, it is characterized in that, described complex composition is with A and B for active component, and wherein A is methylsulfonyl bacterium azoles, and B is imidazoles bactericide; The chemical name of described methylsulfonyl bacterium azoles is 2-(to fluorophenyl)-5-mesyl-1,3,4-oxadiazole, described imidazoles bactericide be selected from Prochloraz, imazalil, cyazofamid, fluorine bacterium azoles, Fenamidone, pefurazoate any one.
2. the complex composition containing methylsulfonyl bacterium azoles and imidazoles bactericide according to claim 1, it is characterized in that, described methylsulfonyl bacterium azoles and the weight ratio of imidazoles bactericide are (30:1) ~ (1:30).
3. the complex composition containing methylsulfonyl bacterium azoles and imidazoles bactericide according to claim 2, it is characterized in that, described methylsulfonyl bacterium azoles and the weight ratio of imidazoles bactericide are (10:1) ~ (1:10).
4. containing a preparation for methylsulfonyl bacterium azoles and imidazoles bactericide, it is characterized in that, comprise acceptable auxiliary material on complex composition according to any one of claims 1 to 3 and agricultural chemicals, be then prepared into the disinfectant use in agriculture of control corps diseases.
5. the preparation containing methylsulfonyl bacterium azoles and imidazoles bactericide according to claim 4, it is characterized in that, the weight percentage that described complex composition accounts for described disinfectant use in agriculture is 0.1% ~ 90%.
6. the preparation containing methylsulfonyl bacterium azoles and imidazoles bactericide according to claim 5, it is characterized in that, the weight percentage that described complex composition accounts for described disinfectant use in agriculture is 1% ~ 80%.
7. the preparation containing methylsulfonyl bacterium azoles and imidazoles bactericide according to claim 4, it is characterized in that, the formulation of described disinfectant use in agriculture is wetting powder, water dispersible granules, aqueous emulsion, suspending agent, granule.
8. the purposes of the complex composition as described in any one of claims 1 to 3 in the bacillary or fungal disease of control crops.
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| CN109511664A (en) * | 2017-09-18 | 2019-03-26 | 佛山市盈辉作物科学有限公司 | A kind of bactericidal composition for disliking bacterium azoles and cyazofamid containing dichloro |
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| CN101861871A (en) * | 2010-03-02 | 2010-10-20 | 陕西美邦农资贸易有限公司 | Sterilization compound containing imazalil and prochloraz |
| CN102499247A (en) * | 2011-10-17 | 2012-06-20 | 贵州大学 | Oxadiazole sulfone compound for controlling bacterial crop diseases |
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| US5166165A (en) * | 1990-10-20 | 1992-11-24 | Bayer Aktiengesellschaft | Fungicidal agents based on heterocyclically substituted sulphones |
| CN101861871A (en) * | 2010-03-02 | 2010-10-20 | 陕西美邦农资贸易有限公司 | Sterilization compound containing imazalil and prochloraz |
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| CN109511664A (en) * | 2017-09-18 | 2019-03-26 | 佛山市盈辉作物科学有限公司 | A kind of bactericidal composition for disliking bacterium azoles and cyazofamid containing dichloro |
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