CN104488898A - Compound composition containing methylsulfonylconazole and xinjunan acetate and fungicide - Google Patents
Compound composition containing methylsulfonylconazole and xinjunan acetate and fungicide Download PDFInfo
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- CN104488898A CN104488898A CN201410788043.0A CN201410788043A CN104488898A CN 104488898 A CN104488898 A CN 104488898A CN 201410788043 A CN201410788043 A CN 201410788043A CN 104488898 A CN104488898 A CN 104488898A
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Abstract
The invention discloses a compound composition containing methylsulfonylconazole and xinjunan acetate and a fungicide of the compound composition. The composition consists of methylsulfonylconazole and xinjunan acetate, wherein the chemical name of methylsulfonylconazole is 2-(para-fluorophenyl)-5-methylsulfonyl-1,3,4-oxadiazole; and the weight ratio of methylsulfonylconazole to xinjunan acetate is (40-1):(1-40), and preferentially, (10-1):(1-10). The fungicide disclosed by the invention comprises the compound composition and pesticide acceptable adjuvants, wherein the content of the fungicidal composition is 0.1-90% of the weight of the fungicide. The compound composition and fungicide thereof disclosed by the invention show obvious synergism when used for preventing and controlling diseases, the prevention and control effect is improved, the dosage of active ingredients is reduced, the prevention and control cost is lowered, and the generation of drug resistance of pathogenic bacteria is delayed.
Description
Technical field
The present invention relates to technical field of pesticide, particularly relate to two kinds of bactericide compounded composition pesticides.
Background technology
In recent years, agricultural chemicals " 3R " problem has caused a series of agricultural product security problem, and the agricultural chemicals research and development of high efficiency, low-residual, low resistance have become plant protection people obligation one can't decline of new generation.Along with the successive optimization of cropping pattern and planting technology, crop is bacillary, the generation of fungal disease progressively substitutes and more serious, and bactericide resistance problem progressively highlights.Secondly, plantation family continuous several times or the medicament that use is similar in a large number, the pesticide resistance causing pathogenetic bacteria powerful to these medicaments causes pathogenetic bacteria to produce stronger pesticide resistance to these medicaments, causes preventive effect to reduce.And crops are while bacterial disease occurs, also likely there is fungal disease, now peasant household selects two kinds of medicament collocation to use usually, but the dosage of two kinds of medicament mixtures arbitrarily adds, cause dosage large, the waste of medicament, and two medicament mixtures not only reach not evil to disease does not reach synergistic effect, play antagonism on the contrary.Therefore, the medicament of the microbicide compositions prevention and control bacterial disease of development of new high-efficiency broad spectrum and the thing that forms a complete set of thereof, have 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 studies further, is selected from the fluorine in halogen atom as Rn, and R2 selects the methyl of C1-C5 alkyl and get s 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 a kind of novel bacterial disease pesticide control, can infiltrate plant epidermis, after Uptake and translocation, act on target leaf, is synthesized, the Growth and reproduction of final anti-bacteria by the energy of anti-bacteria.Show that methylsulfonyl bacterium azoles has good control effect to serial diseases such as bacterial blight of rice, cucumber bacterial angular leaf spot, citrus bacterial canker disease, bacterial wilt of peanut, softs rot of cabbage through great many of experiments.Having the feature of high-efficiency low-toxicity, wide spectrum, safety, is a kind ofly have the novel green agricultural chemicals being developed as large tonnage product potential quality.But methylsulfonyl bacterium azoles, as alone for a long time, easily develops immunity to drugs, its bactericidal activity reduces, and drug effect declines.Research finds that itself and pungent bacterium amine acetate have good synergistic effect.
Pungent bacterium amine acetate is a kind of environment-friendly type amino acids high molecular polymer bactericide, is the bactericide of a kind of environment-friendly type, efficient, wide spectrum, low toxicity.Have the advantages that permeability is strong, the cell membrane of pathogenic microorganism can be penetrated, enter in pathogen cell; killing fungus, bacterium and virus, and the position that energy rapid healing is impaired, form diaphragm in the stem of plant, leaf, fruit face after dispenser; organize germ subintrusion again, there is fabulous control efficiency.
Therefore, the object of this invention is to provide a kind of complex composition, this complex composition and bactericide thereof show obvious synergistic function at control bacterial disease and some fungi, Disease relative to single dose.
In order to reach the order of invention, the technical solution used in the present invention is:
The invention provides a kind of complex composition containing methylsulfonyl bacterium azoles and pungent bacterium amine acetate, this complex composition is made up of methylsulfonyl bacterium azoles and pungent bacterium amine acetate; Wherein, the chemical name of methylsulfonyl bacterium azoles is 2-(to fluorophenyl)-5-mesyl-1,3,4-oxadiazole.
The above contains the complex composition of methylsulfonyl bacterium azoles and pungent bacterium amine acetate, in order to ensure that there is better control efficiency and synergistic effect, as preferably, the weight ratio of above-described methylsulfonyl bacterium azoles and pungent bacterium amine acetate is (40:1) ~ (1:40).
The above contains the complex composition of methylsulfonyl bacterium azoles and pungent bacterium amine acetate, and preferred, the weight ratio of above-described methylsulfonyl bacterium azoles and pungent bacterium amine acetate is (10:1) ~ (1:10).
The present invention also provides a kind of bactericide containing methylsulfonyl bacterium azoles and pungent bacterium amine acetate, and this bactericide comprises acceptable adjuvant on the above-described complex composition of the present invention and agricultural chemicals.
Preferably, the above-described bactericide containing methylsulfonyl bacterium azoles and pungent bacterium amine acetate, the weight percentage that described complex composition accounts for described bactericide is 0.1% ~ 90%.
More preferably, the above-described bactericide containing methylsulfonyl bacterium azoles and pungent bacterium amine acetate, the weight percentage that described complex composition accounts for described bactericide is 1% ~ 80%.
On agricultural chemicals of the present invention, acceptable adjuvant is the mixture of a kind of and auxiliary agent in solvent and filler.Usually can be used for any solvent of preparation agricultural chemicals, filler and auxiliary agent all can use, the present invention does not limit at this.
Filler is selected from one or more in white carbon, kaolin, potter's clay, bentonite, diatomite, earth powder, potassium sulfate or urea.
Solvent is selected from one or more in dimethylbenzene, trimethylbenzene, dimethyl formamide, ethanol, methyl alcohol, solvent naphtha, methyl naphthalene or 1-METHYLPYRROLIDONE.
Auxiliary agent of the present invention can comprise one or more in surfactant, defoamer, thickener, disintegrant and antifreezing agent as required, can also comprise other auxiliary agents that the industry is conventional as required.
Surfactant comprises polyoxyethylene sorbitan fatty acid ester series and comprises fatty alcohol-polyoxyethylene ether series and comprise AEO-9, polyoxyethylene nonylphenol ether series is condensation compound of alkyl phenol and epoxy ethane, OP series comprises OP-10, OP-18, polyoxyethylene nonylphenol ether series comprises NP-10, NP-15, , non-ionic surface active agent series comprises 37#, triphen ethyl phenol APEO series comprises 602#, two phenethyl phenol polyethenoxy ether series comprises 606#, calcium dodecyl benzene sulfonate (500#), poly carboxylic acid derivative's (being called for short CF), acrylic acid and propionamide copolymer (being called for short DA), one or more in desugar the sodium lignin sulfonate of classification (being called for short M-9).
Wetting dispersing agent comprises K12, diisobutyl sodium naphthalene sulfonate (abbreviation pulls open powder), di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate (being called for short NNO), acrylic acid and propionamide copolymer (being called for short DA), dispersing agent MF (being called for short MF), Sodium Polyacrylate (being called for short DC), desugar the sodium lignin sulfonate of classification (being called for short M-9), the sodium lignin sulfonate (being called for short M-10) of desugar condensation and modification, lignosulfonates (being called for short M-11), poly carboxylic acid derivative's (being called for short CF), one or more in sodium lignin sulfonate (be called for short M-14).
Thickener comprises xanthans, aluminium-magnesium silicate, gum Arabic, pectin etc.
Disintegrant comprises sodium chloride, ammonium chloride, sodium carbonate, ammonium carbonate, sodium sulphate, potassium sulfate, sodium phosphate.
Antifreezing agent comprises isopropyl alcohol, propane diols, glycerine, ethylene glycol, urea.
Bactericidal composition of the present invention can be mixed with wetting powder, microemulsion, aqueous emulsion, water dispersible granules, suspending agent, missible oil, kind clothing suspending agent or granule according to the method that this area is general.
Bactericidal composition of the present invention is applicable to control crop bacterial disease, or prevent and treat crop bacterial disease and fungoid, Disease, as such as bacterial leaf streak of rice, tobacco bacterial wilt, Cucumber wilt, citrus bacterial canker disease, bacterial wilt of tomato, Muskmelon Fusarium wilt, bacterial blight of rice, cucumber bacterial angular leaf spot, bacterial wilt of peanut, soft rot of Chinese cabbage, tomato late blight, leaf spot of peanut, downy mildew of crucifers, gray mold of cucumber, tomato virus disease, tobacco virus, Virus Diseases of Rice etc. simultaneously.
The present composition can be used by commonsense method, as added the process of water spray cauline leaf, also can execute by root, can also dress seed or seed pelleting use.Be mainly used in the crops such as paddy rice, tobacco, cucumber, tomato, peanut, capsicum, oranges and tangerines, prevention and corntrol bacterial disease and some fungi and Disease, guarantee output.
Complex composition of the present invention has following advantage compared to existing technology:
1, by showing for the indoor virulence of Different Crop disease and field control effectiveness test result, methylsulfonyl bacterium azoles and pungent bacterium amine acetate composite within the scope of certain proportion, have obvious synergistic function, co-toxicity coefficient is greater than 120.Meanwhile, both composite rear active ingredient dosages are fewer than single dose, but control efficiency is far above single dose, has both reduced active ingredient dosage, has reduced cost accounting again.
2, expanding prevention spectrum.Complex composition provided by the invention is mainly used in preventing and treating bacterial disease, can also doublely cure the disease viral disease and fungal disease, and control spectrum is wide.
3, the lasting period of complex composition of the present invention to crop pest is long, delays the pesticide resistance of pathogen simultaneously.Methylsulfonyl bacterium azoles and pungent bacterium amine acetate are broad-spectrum germicide, and the mechanism of action has bigger difference, and both are composite can play complementary synergistic effect, increases the action site to action target each other, thus can guarantee crop yield to the full extent.
Embodiment
The present invention's the following example is described, but does not limit the scope of the 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.Wherein active component (A) for methylsulfonyl bacterium azoles (in following form be called for short (methylsulfonyl); Active component (B) is pungent bacterium amine acetate.
embodiment prepared by preparation:
For unification, below prepare the adjuvant used whole use abbreviation of embodiment or commercial disignation.
One, the preparation of microemulsion
Methylsulfonyl bacterium azoles and pungent bacterium amine acetate are added in solvent, after stirring, obtains transparent mixed liquor; In above-mentioned mixed liquor, add surfactant, be stirred to emulsifier and dissolve completely; Under the mixing speed of 50r/min, the water of surplus is joined and is above-mentionedly dissolved with in the mixed liquor of surfactant, at ambient temperature, stir 30min, obtain the liquid of homogeneous transparent; Finally add antifreezing agent, stir, obtain the microemulsion of bactericide of the present invention.Formula composition:
Two, the preparation of wetting powder
Methylsulfonyl bacterium azoles, pungent bacterium amine acetate, wetting dispersing agent, filler are mixed, after airslide disintegrating mill is pulverized, stirs 30min, obtain the wetting powder of bactericide of the present invention.
Three, the preparation of suspending agent
By antifreezing agent, thickener, auxiliary agent, moisture content mixing, mix through high speed shear, add methylsulfonyl bacterium azoles, pungent bacterium amine acetate successively, abrading-ball 2 ~ 3 hours in ball crusher, the suspending agent of obtained bactericide of the present invention.
Four, the preparation of aqueous emulsion
By methylsulfonyl bacterium azoles, pungent bacterium amine acetate, surfactant and solvent, 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 thickener and remaining water, shear about half an hour, form aqueous emulsion, be i.e. the aqueous emulsion of obtained bactericide of the present invention.
Five, the preparation of water dispersible granules
Methylsulfonyl bacterium azoles, pungent bacterium amine acetate, wetting dispersing agent, white carbon, filler are mixed, after airslide disintegrating mill is pulverized, stir 30min, through mediating, after add in fluidized-bed granulation dryer and carry out granulation, drying, obtain the water dispersible granules of bactericide of the present invention.
Six, the preparation of missible oil
Methylsulfonyl bacterium azoles and pungent bacterium amine acetate are added in solvent, then adds surfactant, after stirring, obtain transparent mixed liquor, be i.e. the missible oil of obtained bactericide of the present invention.
Seven, suspension seed-coating agent
By methylsulfonyl bacterium azoles and pungent bacterium amine acetate through air-flow crushing, adding assistant (comprising surfactant and dispersant), film forming agent, thickener, antifreezing agent and water mix rear completely, drop into sand mill in proportion and grind 2 times, until it is 2-3 μm that the grain fineness of suspension reaches D50, D90 < 8 μm, the i.e. suspension seed-coating agent of obtained bactericide of the present invention.
Eight, granule
Methylsulfonyl bacterium azoles, pungent bacterium amine acetate, wetting dispersing agent, disintegrant, filler are mixed, pulverizes, stir after adding water-wet, then use screw extruder pelletizer granulation, sieve after drying, be i.e. the granule of obtained bactericide of the present invention.
| Embodiment | Methylsulfonyl bacterium azoles | Pungent bacterium amine acetate | Wetting dispersing agent | Disintegrant | Filler |
| 33 | 0.6g | 0.4g | CF is 3g; M-11 is 2g | Ammonium chloride 20g | Clay supplies 100g |
| 34 | 3g | 1g | NNO is 3g, K12 is 1g | Potassium sulfate 5g | 100g supplied by urea |
The present composition, except can being made into above formulation, can also make the multiple formulations such as micro-capsule suspension, injection drying agent, ultra low volume.
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 is: co-toxicity coefficient >=120 show as synergistic effect; Co-toxicity coefficient≤80 show as antagonism; 80< co-toxicity coefficient <120 shows as summation action.
The Toxicity Determination of control bacterial leaf streak of rice:
Test method: adopt in vitro nephelometry to carry out Toxicity Determination, selects bacterial leaf streak of rice to be target target, repeats 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 1.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 EC of each medicament
50value, CTC value.
The Toxicity Determination result of table 1 methylsulfonyl bacterium azoles and the composite control bacterial leaf streak of rice of pungent bacterium amine acetate
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 5.64 | 100.00 | / | / |
| Pungent bacterium amine acetate (B) | 76.42 | 7.38 | / | / |
| A:B＝40:1 | 4.72 | 119.49 | 97.74 | 122.25 |
| A:B＝30:1 | 4.31 | 130.86 | 97.01 | 134.89 |
| A:B＝25:1 | 4.20 | 134.29 | 96.44 | 139.25 |
| A:B＝20:1 | 4.01 | 140.65 | 95.59 | 147.14 |
| A:B＝14:1 | 3.96 | 142.42 | 93.83 | 151.80 |
| A:B＝10:1 | 3.87 | 145.74 | 91.58 | 159.14 |
| A:B＝5:1 | 3.54 | 159.32 | 84.56 | 188.41 |
| A:B＝2:1 | 3.43 | 164.43 | 69.13 | 237.87 |
| A:B＝1:1 | 4.18 | 134.93 | 53.69 | 251.31 |
| A:B＝1:2 | 6.04 | 93.38 | 38.25 | 244.10 |
| A:B＝1:5 | 10.41 | 54.18 | 22.82 | 237.45 |
| A:B＝1:10 | 20.57 | 27.42 | 15.80 | 173.53 |
| A:B＝1:14 | 26.08 | 21.63 | 13.55 | 159.54 |
| A:B＝1:20 | 31.19 | 18.08 | 11.79 | 153.36 |
| A:B＝1:25 | 36.49 | 15.46 | 10.94 | 141.25 |
| A:B＝1:30 | 41.94 | 13.45 | 10.37 | 129.70 |
| A:B＝1:40 | 48.19 | 11.70 | 9.64 | 121.42 |
| A:B＝1:50 | 55.68 | 10.13 | 9.20 | 110.15 |
From table 1, methylsulfonyl bacterium azoles and pungent bacterium amine acetate are all greater than 120 by weight for the co-toxicity coefficient of composite control bacterial leaf streak of rice in (40:1) ~ (1:40) scope, have notable synergistic effect; When weight ratio is in (10:1) ~ (1:10) scope, the co-toxicity coefficient of each process is all greater than 150, and synergy is particularly remarkable.
The Toxicity Determination of control tobacco virus:
Test method indoor pot tobacco susceptible variety plant, to the 4-5 leaf phase, with the isopyknic viral juice frictional inoculation of liquid mixing of different ratio variable concentrations, often processes 3 strains, 3 leaves of often selecting good strains in the field for seed, repeats 4 times, 3-4 days " Invest, Then Investigate " withered spot numbers, calculate inhibiting rate, use EC
50value is pressed the abundant method of Sun Yun and is calculated co-toxicity coefficient, and measurement result is in table 2.
The Toxicity Determination result of table 2 methylsulfonyl bacterium azoles and the composite control tobacco virus of pungent bacterium amine acetate
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 94.62 | 100.00 | / | / |
| Pungent bacterium amine acetate (B) | 66.38 | 142.54 | / | / |
| A:B＝40:1 | 75.26 | 125.72 | 101.04 | 124.43 |
| A:B＝30:1 | 71.43 | 132.47 | 101.37 | 130.67 |
| A:B＝20:1 | 64.39 | 146.95 | 102.03 | 144.03 |
| A:B＝10:1 | 57.73 | 163.90 | 103.87 | 157.80 |
| A:B＝4:1 | 49.86 | 189.77 | 108.51 | 174.89 |
| A:B＝2:1 | 39.85 | 237.44 | 114.18 | 207.95 |
| A:B＝1:1 | 30.53 | 309.92 | 121.27 | 255.56 |
| A:B＝1:2 | 35.87 | 263.79 | 128.36 | 205.50 |
| A:B＝1:4 | 40.42 | 234.09 | 134.03 | 174.65 |
| A:B＝1:10 | 44.86 | 210.92 | 138.68 | 152.10 |
| A:B＝1:20 | 48.39 | 195.54 | 140.52 | 139.15 |
| A:B＝1:30 | 51.67 | 183.12 | 141.17 | 129.72 |
| A:B＝1:40 | 54.92 | 172.29 | 141.51 | 121.75 |
| A:B＝1:50 | 56.64 | 167.06 | 141.71 | 117.89 |
From table 2, methylsulfonyl bacterium azoles and pungent bacterium amine acetate are all greater than 120 by weight for the co-toxicity coefficient of composite control tobacco virus in (40:1) ~ (1:40) scope, have notable synergistic effect; When weight ratio is in (10:1) ~ (1:10) scope, the co-toxicity coefficient of each process is greater than 150, and synergy is particularly remarkable.
The Toxicity Determination of control tomato late blight:
Test method: by cultured tomato late blight disease fungus spore deionized water from wash-out, filtration medium, is prepared into every milliliter containing 1 × 10 ~ 1 × 10
7the spore suspension of individual spore, for subsequent use.Prepare medicament mother liquor, be diluted to corresponding concentration with the 0.1% Tween 80 aqueous solution.With the liquid of liquid-transfering gun draws equal amounts (each 0.5ml) and spore suspension in small test tube, mix.Drawing above-mentioned mixed liquor with micro sample adding appliance drips on concave slide, and then frame is put in the culture dish with shallow seated groundwater, and after adding a cover, in 26 DEG C of insulating boxs, moisturizing is cultivated.Often process and repeat for 4 times, and establish the process not containing medicament not make blank.When blank spore germination rate reaches more than 90%, investigate each process spore germination number, and record investigation sum, calculate spore germination rate and relative inhibition, probability value according to the spore germination relative inhibition of 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.
Table 3 methylsulfonyl bacterium azoles and the composite Toxicity Determination result of preventing and treating leaf spot of peanut of pungent bacterium amine acetate
| Composition | EC 50(μg/ml) | ATI | TTI | CTC |
| Methylsulfonyl bacterium azoles (A) | 27.28 | 100.00 | / | / |
| Pungent bacterium amine acetate (B) | 17.36 | 157.14 | / | / |
| A:B＝50:1 | 22.64 | 120.49 | 101.12 | 119.16 |
| A:B＝40:1 | 21.49 | 126.94 | 101.39 | 125.20 |
| A:B＝30:1 | 20.86 | 130.78 | 101.84 | 128.41 |
| A:B＝20:1 | 19.54 | 139.61 | 102.72 | 135.91 |
| A:B＝10:1 | 17.12 | 159.35 | 105.19 | 151.48 |
| A:B＝5:1 | 14.27 | 191.17 | 109.52 | 174.55 |
| A:B＝3:1 | 11.54 | 236.40 | 119.05 | 198.57 |
| A:B＝1:1 | 8.64 | 315.74 | 128.57 | 245.58 |
| A:B＝1:3 | 7.83 | 348.40 | 138.10 | 252.29 |
| A:B＝1:5 | 9.59 | 284.46 | 147.62 | 192.70 |
| A:B＝1:10 | 11.65 | 234.16 | 151.95 | 154.11 |
| A:B＝1:20 | 12.09 | 225.64 | 154.42 | 146.12 |
| A:B＝1:30 | 13.27 | 205.58 | 155.30 | 132.37 |
| A:B＝1:40 | 14.24 | 191.57 | 155.75 | 123.00 |
From table 3, methylsulfonyl bacterium azoles and pungent bacterium amine acetate are all greater than 120 by weight for the composite co-toxicity coefficient preventing and treating leaf spot of peanut in (40:1) ~ (1:40) scope, have notable synergistic effect; When weight ratio is in (10:1) ~ (1:10) scope, the co-toxicity coefficient of each process is greater than 151, and synergy is particularly remarkable.
The field control effectiveness test of control bacterial leaf streak of rice:
Test method: with reference to G B/T 17980.105-2004 pesticide field efficacy medicine test criterion (two) the 105th part: bactericidal agent for preventing and treating bacterial leaf streak of rice;
Controlling object: bacterial leaf streak of rice
Test site: Nanning doube bridge
Experimental plot: choose 36 community, randomized arrangement, is divided into 9 groups, often organizes 4 repetitions, totally 9 corresponding 9 process.
Test method: adopt directed spraying method, first time dispenser is spaced apart 7 days apart from second time spraying time.
Investigation method: adopt diagonal sampling, get 5 points altogether, 25 clumps often (100 strain), investigate respectively for before medicine, after medicine 7 days and 14 days.
Contrast medicament 2:1.8% pungent bacterium amine acetate aqua, registration card number: PD20101188, Xian District, Shanxi Province Jia Ke agrochemical Co., Ltd, commercial.
The field control effectiveness test result of bacterial leaf streak of rice prevented and treated by table 4
From result of the test table 4, during control bacterial leaf streak of rice, identical (the active ingredient dosage 20g/667m of active ingredient dosage
2) even less when, after methylsulfonyl bacterium azoles+pungent bacterium amine acetate second time medicine, the control efficiency of 7d is respectively higher than single dose, exceeds methylsulfonyl bacterium azoles respectively, the control efficiency of pungent bacterium amine acetate single dose is more than 25.66%, more than 30.46%; And after second time medicine, 14d still can reach the preventive effect of more than 77%, and the lasting period is long.
The field control effectiveness test of control tobacco virus:
Test method and drug effect computational methods: with reference to NY/T1464.8-2007 pesticide field efficacy medicine test criterion: bactericidal agent for preventing and treating tomato virus disease;
Controlling object: tobacco virus;
Test site: Wuming, Nanning.
Experimental plot: 36 communities are chosen in field, are divided into 9 groups, often organizes 4 repetitions, random number;
Test method: adopt directed spraying method with test medicine process different districts respectively, first time dispenser is spaced apart 7 days apart from second time spraying time.
Investigation method: every 5, community sampling, often some investigation 6 strains, investigate total strain number and the diseased plant number of tobacco in each community for before medicine, after medicine 7 days and 14 days respectively.
Contrast medicament 2:1.8% pungent bacterium amine acetate aqua, registration card number: PD20101188, Xian District, Shanxi Province Jia Ke agrochemical Co., Ltd, commercial.
The field control effectiveness test result of tobacco virus prevented and treated by table 5
From result of the test table 5, during control tobacco virus, identical (the active ingredient dosage 15g/667m of active ingredient dosage
2) even less when, after methylsulfonyl bacterium azoles+pungent bacterium amine acetate second time medicine, the control efficiency of 7d is respectively higher than single dose, exceeds methylsulfonyl bacterium azoles respectively, the control efficiency of pungent bacterium amine acetate single dose is more than 29.4%, more than 23.23%; And after second time medicine, 14d still can reach the preventive effect of more than 78%, and the lasting period is long.
The field control effectiveness test of control tomato late blight:
Test method: with reference to GB/T17980.31-2000 field control effectiveness test criterion () the 31st part: bactericidal agent for preventing and treating tomato late blight.
Controlling object: tomato late blight
Test site: Nanning Shi Bu
Experimental plot: choose 36 communities, randomized arrangement, each community 20 ㎡, each process 4 repetition, totally 9 process;
Test method: adopt directed spraying method, first time dispenser is spaced apart 7 days apart from second time spraying time.
Investigation method: every random 5 samplings in community, often click two strains, 10 leaves are investigated in every strain point upper, middle and lower, and the percentage accounting for whole leaf area with the lesion area on every a slice leaf carrys out classification, while investigation blade, investigation sick fruit number comprises fallen fruits, shows control efficiency so that diseased fruit rate is embedding.Before dispenser, investigation once, is investigated once for after dispenser 7 days and 14 days respectively.
Contrast medicament 2:1.8% pungent bacterium amine acetate aqua, registration card number: PD20101188, Xian District, Shanxi Province Jia Ke agrochemical Co., Ltd, commercial.
The field control effectiveness test result of tomato late blight prevented and treated by table 6
From result of the test table 6, during control tomato late blight, identical (the active ingredient dosage 20g/667m of active ingredient dosage
2) even less when, after methylsulfonyl bacterium azoles+pungent bacterium amine acetate second time medicine, the control efficiency of 7d is respectively higher than single dose, exceeds methylsulfonyl bacterium azoles respectively, the control efficiency of pungent bacterium amine acetate single dose is more than 31%, more than 37.12%; And after second time medicine, 14d still can reach the preventive effect of more than 79%, and the lasting period is long.
Claims (10)
1. contain a complex composition for methylsulfonyl bacterium azoles and pungent bacterium amine acetate, it is characterized in that: described complex composition is made up of methylsulfonyl bacterium azoles and pungent bacterium amine acetate; Wherein, the chemical name of methylsulfonyl bacterium azoles is 2-(to fluorophenyl)-5-mesyl-1,3,4-oxadiazole.
2. a kind of complex composition containing methylsulfonyl bacterium azoles and pungent bacterium amine acetate according to claim 1, is characterized in that: the weight ratio of described methylsulfonyl bacterium azoles and pungent bacterium amine acetate is (40:1) ~ (1:40).
3. a kind of complex composition containing methylsulfonyl bacterium azoles and pungent bacterium amine acetate according to claim 1 and 2, it is characterized in that, the weight ratio of described methylsulfonyl bacterium azoles and pungent bacterium amine acetate is (10:1) ~ (1:10).
4. contain a bactericide for methylsulfonyl bacterium azoles and pungent bacterium amine acetate, it is characterized in that, comprise acceptable adjuvant on the arbitrary described complex composition of claim 1-3 and agricultural chemicals, be then prepared into agriculture bactericide.
5. contain the bactericide of methylsulfonyl bacterium azoles and pungent bacterium amine acetate according to claim 4, it is characterized in that, the weight percentage that described complex composition accounts for described bactericide is 0.1% ~ 90%.
6. contain the bactericide of methylsulfonyl bacterium azoles and pungent bacterium amine acetate according to claim 5, it is characterized in that, the weight percentage that described complex composition accounts for described bactericide is 1% ~ 80%.
7. according to the arbitrary described bactericide containing methylsulfonyl bacterium azoles and pungent bacterium amine acetate of claim 4-6, it is characterized in that, described bactericide is mixed with wetting powder, microemulsion, aqueous emulsion, water dispersible granules, suspending agent, missible oil, kind clothing suspending agent or granule.
8. according to claim 4 containing the bactericide of methylsulfonyl bacterium azoles and pungent bacterium amine acetate, it is characterized in that: on described agricultural chemicals, acceptable adjuvant is the mixture of a kind of and auxiliary agent in solvent and filler.
9. the application of the complex composition as described in as arbitrary in claim 1-3 in control crop bacterial disease.
10. the application of the complex composition as described in as arbitrary in claim 1-3 in control crop fungal disease and Disease.
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| CN107897190A (en) * | 2017-11-28 | 2018-04-13 | 谭贵友 | The complex composition and fungicide of a kind of lactams of ketoxime containing isolonglifolene and Xinjunan acetate |
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| CN102499247A (en) * | 2011-10-17 | 2012-06-20 | 贵州大学 | Oxadiazole sulfone compound for controlling bacterial crop diseases |
| CN103053559A (en) * | 2012-12-29 | 2013-04-24 | 广东中迅农科股份有限公司 | Xinjunan acetate-propamocarb hydrochloride sterilization composition |
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| CN102499247A (en) * | 2011-10-17 | 2012-06-20 | 贵州大学 | Oxadiazole sulfone compound for controlling bacterial crop diseases |
| CN103053559A (en) * | 2012-12-29 | 2013-04-24 | 广东中迅农科股份有限公司 | Xinjunan acetate-propamocarb hydrochloride sterilization composition |
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| CN107897190A (en) * | 2017-11-28 | 2018-04-13 | 谭贵友 | The complex composition and fungicide of a kind of lactams of ketoxime containing isolonglifolene and Xinjunan acetate |
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