CN101983565A - Sterilization composite containing fluopyram - Google Patents
Sterilization composite containing fluopyram Download PDFInfo
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- CN101983565A CN101983565A CN201010584567XA CN201010584567A CN101983565A CN 101983565 A CN101983565 A CN 101983565A CN 201010584567X A CN201010584567X A CN 201010584567XA CN 201010584567 A CN201010584567 A CN 201010584567A CN 101983565 A CN101983565 A CN 101983565A
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Abstract
The invention relates to a sterilization composite in the field of pesticide compounding, which is formed by compounding the active ingredient of the fluopyram and the sterilization active ingredient selected from any one of the propineb, the azoxystrobin and the methyl as the active ingredient. The weight percentage of the two active ingredients is 70-1:10-90, and the preferred weight percentage is 40-1:25-60. The weight percentage of the active ingredients of the sterilization composite is 1 to 90%, the preferred weight percentage is 15 to 70%, and the balance of the allowed and acceptable auxiliary ingredients in pesticide. The sterilization composite can be prepared into the emulsion, the micro emulsion, the emulsifiable concentrate, the suspending agent, the wettable powder and the water dispersible granule according to the existing methods. The sterilization composite of the invention is mainly used in the prevention and the cure of the diseases of the powdery mildew, the downy mildew, the rust disease, the leaf fungal diseases, the cladosporium cucumerinum, the rot and the like of the vegetables, the grains such as the wheat and the like, and the fruit trees caused by the germs.
Description
Technical field
The present invention relates to a kind of Synergistic sterilizing composition pesticide, be specifically related to a kind of fluorine pyrrole bacterium acid amides and composite Synergistic bactericidal composition of arbitrary fungicide active ingredient that is selected from Propineb, Fluoxastrobin, the kresoxim-methyl of comprising.
Background technology
Fluorine pyrrole bacterium acid amides, English common name fluopyram, chemical name is N-{2-[3-chloro-5-(trifluoromethyl)-2-pyridine radicals] ethyl-α, α, α-three fluoro-O-toluamide }, be a kind of new benzamides series bactericidal agent, shift by the electronics that hinders succinate dehydrogenase in the respiratory chain and suppress mitochondrial respiratory.Be mainly used in the microbial disease of control capsule on the broad leaf crop.To the downy mildew on the vegetables such as cucumber, custard squash, powdery mildew, the downy mildew of fruit tree etc. causes that by germ multiple diseases has favorable effect.Its chemical structural formula is:
Propineb (propineb), molecular formula are (C
5H
8N
2S
4Zn)
x, chemical name: acrylic bisdithiocarbamic zinc.Propineb belongs to the benzene thiocarbamates; it is a kind of protective fungicide of quick-acting, long residual, wide spectrum; downy mildew of crops such as vegetables, grape, tobacco and morning, the late blight of tomato and potato all there are good protective effect, and the disease of powdery mildew, rust and Botrytis is also had fixed inhibitory action.As alternaria leaf spot of apple, Chinese cabbage downy mildew, cucumber downy mildew, downy mildew of garpe, early blight of tomato and late blight, target and late blight, mango anthracnose, Alternaria alternate.
Fluoxastrobin, common name amistar, molecular formula C
22H
17N
3O
5, Chinese is: (E)-[2-[6-(2-cyano-benzene oxygen) pyrimidine-4-base oxygen] phenyl]-the 3-methoxy-methyl acrylate.Be methoxy acrylic bactericide, efficiently, wide spectrum, nearly all mycota (Ascomycotina, Basidiomycotina, Mastigomycotina and Deuteromycotina) disease such as powdery mildew, rust, glume blight, net blotch, downy mildew, rice blast etc. are all had good activity.Can be used for cauline leaf spraying, seed treatment, also can carry out soil treatment, be mainly used in cereal, paddy rice, peanut, grape, potato, fruit tree, vegetables, coffee, lawn etc.
Kresoxim-methyl (kresoxim-methyl) is the methoxy acrylic new type bactericide of BASF Aktiengesellschaft, molecular formula: C
18H
19NO
4, chemical name: methyl (E)-2-methoxyimino-2-[2-(O-toloxyl) phenyl] and acetate.Kresoxim-methyl belongs to the cell mitochondrial respiration inhibitor, by at cytochrome b and C
1Between electronics shift and suppress mitochondrial respiratory, the supply of interference cell energy makes the pathogen cell death.Tool is protected, treats, is rooted out, infiltration, systemic activity, and fungicidal spectrum is wide, and the plurality of plant diseases that sac fungi, flagellum mattress and imperfect fungus are caused has the better prevention effect.
Use separately because above bactericide is long-term, preventive effect begins to fall, and has produced pesticide resistance to a certain degree, and simultaneously, above bactericide has in various degree inhibitory action to the growth of crop when high dose uses slightly, cause poisoning easily.The inventor discovers by a series of, the fluorine pyrrole bacterium acid amides Synergistic bactericidal composition composite with being selected from arbitrary fungicide active ingredient in Propineb, Fluoxastrobin, the kresoxim-methyl has extremely strong synergistic effect to the target bacterium, improve bactericidal activity greatly, thereby finished the present invention.And about fluorine pyrrole bacterium acid amides and be selected from the composite of arbitrary fungicide active ingredient in Propineb, Fluoxastrobin, the kresoxim-methyl, do not see relevant report at present at home and abroad as yet.
Summary of the invention
Based on above situation, the object of the present invention is to provide the low bactericidal composition of a kind of efficient, low toxicity, use cost to satisfy the needs of agricultural production.Two kinds of active component combination backs produce synergistic effect, can also avoid the drug-fast generation of germ and delay the drug-fast generation speed of germ when improving preventive effect.
The objective of the invention is to realize by following measure:
A kind of bactericidal composition based on fluorine pyrrole bacterium acid amides, it is characterized in that with active ingredient (A) fluorine pyrrole bacterium acid amides and (B) being selected from arbitrary fungicide active ingredient in Propineb, Fluoxastrobin, the kresoxim-methyl and carry out compositely, the percentage by weight of effective constituents A and B is 70～1: 10～90.
Above-mentioned four kinds of active ingredients all are bactericide well known in the art, can obtain by various commercial channel, and as a kind of improvement of the present invention, the percentage by weight of effective constituents A and B preferred 40～1: 25～60.
Describedly carry out composite bactericidal composition with active ingredient fluorine pyrrole bacterium acid amides and arbitrary fungicide active ingredient of being selected from Propineb, Fluoxastrobin, the kresoxim-methyl, the gross mass content of two kinds of active components of A, B in preparation is 1%-90%, preferred 15%-70%; All the other are usual auxiliaries in the agricultural chemicals.
It is one of key character of the present invention that two kinds of active components of A, B are re-dubbed new compositions according to a certain percentage, and another feature is that the formulation that the bactericidal composition of the described A of containing, two kinds of active components of B can be made into is aqueous emulsion, microemulsion, missible oil, suspending agent, wetting powder, water dispersible granules.
One of technical scheme of the present invention, described bactericidal composition are aqueous emulsion, and the percentage by weight of component is:
Effective constituents A 1～70%
Active ingredient B 10～90%
Emulsifier 3～30%
Solvent 5～15%
Cosolvent 5～20%
Antimicrobial 0.1～1%
Stabilizing agent 2～15%
Antifreezing agent 2～5%
Defoamer 0.1～8%
Thickener 0.2～2%
Water surplus
The concrete production stage of this aqueous emulsion is: at first former medicine A is added with B, solvent and emulsifier, cosolvent and be in the same place, make and be dissolved into uniform oil phase; With part water, antifreeze, other insecticides adjuvant such as antimicrobial mixes into uniform water; When the reactor high speed stirs, oil phase is added water, slowly add water, open clipper and carry out high speed shear, and add remaining water, shear half an hour approximately, form the aqueous emulsion of oil-in-water type until reaching the phase inversion point.Promptly make the aqueous emulsion of the bactericidal composition that contains A and two kinds of active components of B.
Solvent can be alkyl phthalate class (as phthalic acid ester dimethyl ester, diethylester, dibutyl ester, phthalic acid ester butyl ester benzyl ester etc.), (cation can be glyoxaline cation, pyridylium, alkyl ammonium cation, alkyl ammonium cation, alkyl phosphorus cation etc. to the ionic liquid kind solvent, and anion commonly used has Cl
-, Br
-, AlCl
4 -, [BF
4]
-, [PF
4]
-, [CF
3SO
3]
-[(CF
3SO
3)
2N]
-Deng), N-alkyl pyrrolidine ketone (as N-n-octyl pyrrolidones, N-dodecyl pyrrolidones etc.), high boiling point aromatic hydrocarbon solvent (as Solvesso100,150,200 etc.), available one of them or its combination.
Emulsifier is non-ionic surface active agents such as phosphoric acid ester anion surfactant or EO/PO block copolymer, macromolecule graft copolymers, polystyrene-based polyoxyethylene groups ethers, agricultural newborn 1601*, castor oil polyoxyethylene ether class, polyoxyethylene nonylphenol ether class, fatty alcohol polyethenoxy ether class, available one of them or its combination.
Thickener is xanthans, gelatin, modified starch, CMC, hydroxymethyl ethyl cellulose, hydroxyethylcellulose, hydroxypropyl cellulose, polyvinylpyrrolidone, polyvinyl alcohol etc., available one of them or its combination.
Stabilizing agent can be one or more the mixture in urea, methyl alcohol, soluble starch, sodium sorbate, pyrogallic acid, aminobenzoic acid, cresyl glycidyl ether, the phenyl glycidyl ether.
Antifreezing agent is ethylene glycol, propane diols, propane diols, diethylene glycol etc., available one of them or its combination.
Antimicrobial is Sodium Benzoate, benzisothiazole ketone, sorbic acid, 2-bromo-2-nitro-propyl group-1,3-glycol, formaldehyde etc., available one of them or its combination.
The pH regulator agent is phosphoric acid, glacial acetic acid, citric acid, maleic acid etc., available one of them or its combination.
Defoamer is silicone defoaming agent, mineral oil, alcohols etc., available one of them or its combination.
Two of technical scheme of the present invention, when described bactericidal composition is microemulsion, but used additives has:
Effective constituents A 1～70%
Active ingredient B 10～90%
Emulsifier 10～30%
Antifreezing agent 1～8%
Stabilizing agent 0.5～10%
Conventional solvent cosolvent 20～50%
Solvent and cosolvent have one or more the mixture in methyl alcohol, ethanol, butanols, ethylene glycol, propane diols, glycerine, polyethylene glycol, acetone, cyclohexanone, pyrrolidones, toluene, dimethylbenzene, ethyl acetate, dimethyl formamide (DMF), the dimethyl sulfoxide (DMSO) (DMSO).
Emulsifier is alkylbenzene naphthalene sulfonate, alkylphenol polyoxyethylene phosphate, diphenyl phenol polyethenoxy polyethenoxy ether, styrenated phenol APEO, alkylphenol polyoxyethylene formaldehyde condensation products, diphenyl phenol polyethenoxy polyformaldehyde condensation product, castor oil ethylene oxide adduct and derivative thereof, for example farming breast 300, farming breast 500, farming breast 600, Nongru-700, agricultural newborn SorplKS, OX2511, NNO, NP series etc., emulsifier can be one or more mixture.
Antifreezing agent has one or more the mixture in ethylene glycol, propane diols, glycerine, polyethylene glycol, the sorbierite.
Stabilizing agent can be one or more the mixture in urea, methyl alcohol, soluble starch, sodium sorbate, pyrogallic acid, aminobenzoic acid, cresyl glycidyl ether, the phenyl glycidyl ether.
Three of technical scheme of the present invention, described bactericidal composition are cream preparation, and the percentage by weight of component is:
Effective constituents A 1～70%
Active ingredient B 10～90%
Conventional emulsifier 10～30%
Conventional solvent 20～50%
Conventional synergist 1～5%
The concrete production stage of this cream preparation adds emulsifier, the synergist back that stirs after the dissolving fully again and becomes the oily liquids of transparent and homogeneous for earlier effective constituents A, B being added in the solvent, and can promptly makes the cream preparation of described bactericidal composition of the present invention.
Four of technical scheme of the present invention, described bactericidal composition are suspending agent, and the percentage by weight of component is:
Effective constituents A 1～70%
Active ingredient B 10～90%
Dispersant 5～20%
Antifreezing agent 1～5%
Thickener 0.1～2%
Defoamer 0.1～0.8%
Water surplus
The concrete production stage of this suspending agent is earlier other auxiliary agents to be mixed, mix through high speed shear, add effective constituents A, B, abrading-ball is 2～3 hours in ball crusher, make a diameter all below 5mm, make the suspending agent preparation of described bactericidal composition of the present invention.
Wetting dispersing agent is one or more the mixture in lignosulfonates, alkylsulfonate, aliphatic alcohol sulfate, alkylaryl sulfonates, polyaryl phenol polyoxy ethyl ether phosphate alkylamine salt, polyoxyethylene fatty acid ester, alkylphenol polyoxyethylene phosphate, Fluhyzon formaldehyde condensation products, polyoxyethylene polyoxypropylene block copolymer, alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether, CMC (CMC), the polyvinyl alcohol (PVA).
Thickener is one or more the mixture in CMC, polyvinyl alcohol, xanthans, gum Arabic, sodium alginate, polyvinylpyrrolidone, bentonite, aluminium-magnesium silicate, the gypsum.
Penetrating agent is one or both the mixture among Laurocapram, the JFC.
Defoamer can be one or more the mixture in organic silicone oil, methyl alcohol, ethanol, the epoxidized soybean oil.
Antifreezing agent is one or more the mixture in ethylene glycol, propane diols, glycerine, polyethylene glycol, the sorbierite.
PH value conditioning agent is one or more the mixture in sodium hydroxide, potassium hydroxide, ammoniacal liquor, hydrochloric acid, acetic acid, phosphoric acid or the citric acid.
Solvent and cosolvent have one or more the mixture in water, methyl alcohol, ethanol, butanols, ethylene glycol, propane diols, glycerine, polyethylene glycol, acetone, cyclohexanone, pyrrolidones, toluene, dimethylbenzene, ethyl acetate, dimethyl formamide (DMF), the dimethyl sulfoxide (DMSO) (DMSO).
Five of technical scheme of the present invention, described bactericidal composition is a wetting powder, the percentage by weight of component is:
Effective constituents A 1～70%
Active ingredient B 10～90%
Dispersant 3～10%
Wetting agent 1～5%
The filler surplus.
The concrete production stage of this wetting powder is: by above-mentioned prescription effective constituents A, B and dispersant, wetting agent and filler are mixed, in stirred tank, evenly stir, behind airslide disintegrating mill, mixing, promptly can be made into the wetting powder of the present composition.
Dispersant has one or several the mixture in lignosulfonates, fatty acid amide N methyl taurine sodium salt, alkylphenol polyoxyethylene sulphate, lignosulfite, fatty acid ester sulphate, polyoxyethylene polyoxypropylene block copolymer, alkylphenol polyoxyethylene, the fatty alcohol-polyoxyethylene ether.
Wetting agent is dodecyl benzene sulfonate, farming newborn 2000 series, SOPA230, SOPA270, SOPA235, the withered powder of tea, spaonin powder, draws back one or several the mixture among powder, the wetting and penetrating agent F.
Carrier has one or more the mixture in kaolin, diatomite, atlapulgite, white carbon black, clay, precipitated calcium carbonate, the talcum powder.
Six of technical scheme of the present invention, described bactericidal composition are water dispersible granules, and the percentage by weight of component is:
Effective constituents A 1～70%
Active ingredient B 10～90%
Dispersant 3～10%
Wetting agent 1～10%
Disintegrant 1～5%
The filler surplus
The concrete production stage of this water dispersible granules is: by above-mentioned prescription effective constituents A, B and dispersant, wetting agent, disintegrant and filler are mixed, pulverize with micro jet, through mediating, add then and carry out granulation, drying, screening in the fluidized bed prilling dryer after sample analysis, make the water dispersible granules of described bactericidal composition of the present invention.
Wetting agent is one or several the mixture in fatty acid amide N methyl taurine sodium salt, lignosulfonates, alkylphenol polyoxyethylene sulphate, petroleum sodium sulfonate, alkylnaphthalene sulfonate, fatty acid ester sulphate, alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether, lignosulfite, the withered powder of tea, the spaonin powder.
Dispersant is one or several the mixture in ethoxylated dodecyl alcohol, naphthalenesulfonic acid-formaldehyde condensate, dioctyl sodium sulphosuccinate, the acrylate homopolymer sodium salt.
Disintegrant can be one or more the mixture in urea, magnesium chloride, aluminium chloride, sodium chloride, ammonium sulfate, the bentonite.
Carrier is one or more the mixture in kaolin, diatomite, atlapulgite, white carbon black, clay, precipitated calcium carbonate, talcum powder, the montmorillonite.
Bactericidal composition of the present invention can be used for preventing and treating diseases caused by the bacteria such as powdery mildew on cereal such as various vegetables, wheat and the fruit tree, downy mildew, rust, tikka class disease, scab, rot.Compared with prior art, beneficial effect of the present invention is: 1. composite have an obvious role in synergism, improved control efficiency, enlarged fungicidal spectrum; 2. compare with using the one-component bactericide, the risk that produces poisoning reduces; 3. composition is made up of two kinds of different active ingredients of the mechanism of action, helps avoiding drug-fast generation and delays the drug-fast generation speed of germ; 4. medicament is mixed and has reduced dosage, thereby has reduced cost and the pollution that has alleviated environment.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, the present invention describes with following specific embodiment, but the present invention only limits to these examples absolutely not.The method that the present invention adopts indoor bioassay and field trial to combine.If no special instructions, the ratio of below mentioning (comprising percentage) all is a mass ratio.Should be pointed out that all any modifications of being made within the spirit and principles in the present invention, be equal to replacement and improvement etc., all should be included within protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Indoor biological toxicity test:
(1) experimental subjects:
The powdery mildew of cucumber bacterium, the cucumber cultivation ground collection of not executing fluorine pyrrole bacterium amine and Propineb, kresoxim-methyl, Fluoxastrobin and similar medicament from Shouguang, Shandong separates.Cucumber variety is a Chang Chun Mi Ci.
In pot for growing seedlings, place the greenhouse to cultivate susceptible cucumber variety Chang Chun Mi Ci cultivation, plant grows to three to four leaf after dates, gathers the blade of identical leaf age, is used for cultivation and the mensuration of powdery mildew of cucumber bacterium.
The powdery mildew of cucumber bacterium adopts live body plant method to cultivate under 20 ℃, the condition of 12h alternation of light and darkness, and every 30d changes to be commissioned to train and supports 1 time.With the conidium on the sterile water wash-out incidence of leaf, being mixed with spore concentration is 1 * 10 during inoculation
6The suspension of individual/mL.
(2) experimental pharmacy:
The former medicine of 96% fluorine pyrrole bacterium acid amides is produced by Jiangsu Heyi Chemical Industry Co., Ltd.; The former medicine of 89% Propineb is produced by Limin Chemical Co., Ltd.; The former medicine of 95% kresoxim-methyl, the green agricultural Science and Technology Ltd. in Beijing produces; The former medicine of 95% Fluoxastrobin, the green agricultural Science and Technology Ltd. in Beijing produces.
(3) test method:
The strains tested sensitivity testing:
Adopt the leaf dish method of preserving moisture to carry out toxicity test.Earlier the blade of gathering is prepared into the leaf dish that diameter is 1.5cm, mixing at random, place the series concentration soup that configures to soak 1h respectively, 50 leaf dishes of each concentration, test is with the blank that is treated to of adding medicine not, after soaking end, leaf faces up and puts on the wetting blotting paper of identical liquor strength, soup on the leaf dish is blotted, the spore suspension 10L for preparing is inoculated in leaf dish central authorities, after room temperature is placed 5min, places under 20 ℃, the condition of 12h alternation of light and darkness and cultivate, measure the onset area on the leaf dish behind the 10d, calculate EC
50
On the basis of preliminary experiment, respectively single agent fluorine pyrrole bacterium acid amides and Propineb, kresoxim-methyl, Fluoxastrobin are carried out toxicity test, four EC in order to last method
50Value is respectively 1.5mg/l, 9.8mg/l, 6.9mg/l, 6.1mg/l.
The percentage that accounts for the leaf disc area according to lesion area is divided sick level:
0 grade: scab
1 grade: lesion area accounts for 1%～20% of leaf disc area
2 grades: lesion area accounts for 21%～50% of leaf disc area
3 grades: lesion area accounts for more than 50% of leaf disc area
The mixture toxicity test:
Carry out the toxicity test of mixture according to mixed ratio with single agent toxicity test method.
EC that each that will measure according to the abundant method of Sun Yun handled
50Value is converted into the actual toxicity index (ATI) of using with; According to the proportioning of mixture, obtain theory and use toxicity index (TTI) with, calculate the co-toxicity coefficient (CTC) of mixture by following formula.
Single agent toxicity index=(standard medicament EC
50/ reagent agent EC
50) * 100
ATI=(standard medicament EC
50/ reagent agent (using with) EC
50) * 100
The content (%) of toxicity index X B in using with of content (the %)+B of the toxicity index x A of TII=A in using with
CTC＝(ATI/TTI)×100
If co-toxicity coefficient is big by 120, showing has synergistic effect; If be starkly lower than 100 (below 80), be indicated as antagonism; Between 100～120, be indicated as summation action.
Toxicity Determination example 1: the composite Toxicity Determination of fluorine pyrrole bacterium acid amides and Propineb to the powdery mildew of cucumber bacterium.
The former medicinal DMF dissolving of Propineb, the former medicinal acetone solution of fluorine pyrrole bacterium acid amides is made into 10000 μ g/ml mother liquors, and is in 4 ℃ of preservations, stand-by.
60% fluorine pyrrole bacterium acid amides Propineb mass ratio is respectively 5%+55%, 6%+54%, 10%+50%, 15%+45% and 30%+30% totally 5 combinations that are mixed.
Virulence experiment result and analysis:
The different proportioning fluorine of table 1 pyrrole bacterium acid amides and Propineb mixture are to the virulence of powdery mildew of cucumber bacterium
| The pharmacy quality ratio | Virulence regression equation | The correlation coefficient r value | EC 50(mg/L) |
| Fluorine pyrrole bacterium acid amides (A) | Y＝1.9483X+4.6570 | 0.9948 | 1.5 |
| Propineb (B) | Y＝0.1188X+4.8822 | 0.9895 | 9.8 |
| 1∶11 | Y＝1.0264X+3.9758 | 0.9660 | 9.95 |
| 1∶9 | Y＝1.1451X+3.9797 | 0.9583 | 7.78 |
| 1∶5 | Y＝1.1595X+3.9728 | 0.9690 | 7.69 |
| 1∶3 | Y＝0.5849X+4.5337 | 0.9816 | 6.27 |
| 1∶1 | Y＝1.5653X+3.9959 | 0.9685 | 4.38 |
The composite co-toxicity of table 2 fluorine pyrrole bacterium acid amides and Propineb to the powdery mildew of cucumber bacterium
| Test medicine | Mass ratio | The actual measurement poison refers to | Theoretical poison refers to | Co-toxicity coefficient | Conclusion |
| Fluorine pyrrole bacterium acid amides (A) | 1∶0 | 100.00 | 100.00 | / | / |
| Propineb (B) | 0∶1 | 15.31 | 15.31 | / | / |
| A+B | 1∶11 | 15.07 | 13.42 | 112.3 | Addition |
| A+B | 1∶9 | 19.27 | 14.27 | 135.1 | Synergy |
| A+B | 1∶5 | 19.51 | 17.65 | 110.5 | Addition |
| A+B | 1∶3 | 23.92 | 21.89 | 109.3 | Addition |
| A+B | 1∶1 | 34.21 | 34.59 | 98.9 | Addition |
According to bactericide joint toxicity measuring result, fluorine pyrrole bacterium acid amides Propineb mass ratio is that 1: 9 o'clock co-toxicity coefficient is 135.1, greater than 120, shows as synergistic effect, and other show as summation action, so think that 1: 9 o'clock synergistic effect is best.Suggestion is carried out further field control effectiveness test to the mixture preparation of 1: 9 left and right sides scope of suitable proportion, to estimate its field practical application effect.
Toxicity Determination example 2: the composite Toxicity Determination of fluorine pyrrole bacterium acid amides and kresoxim-methyl to the powdery mildew of cucumber bacterium.
With fluorine pyrrole bacterium acid amides and the former medicinal acetone of kresoxim-methyl is dissolution with solvents, is made into 10000 μ g/ml mother liquors, in 4 ℃ of preservations, stand-by.
56% fluorine pyrrole bacterium acid amides kresoxim-methyl mass ratio is respectively 4.7%+51.3%, 5.6%+50.4%, 9.3%+46.7%, 14%+42% and 28%+28% totally 5 combinations that are mixed.
Virulence experiment result and analysis:
The different proportioning fluorine of table 3 pyrrole bacterium acid amides and kresoxim-methyl mixture are to virulence and the synergistic effect of powdery mildew of cucumber bacterium
| The pharmacy quality ratio | Virulence regression equation | The correlation coefficient r value | EC 50(mg/L) |
| Fluorine pyrrole bacterium acid amides (A) | Y＝1.8938X+4.3898 | 0.9616 | 2.1 |
| Kresoxim-methyl (B) | Y＝1.9386X+3.3738 | 0.9782 | 6.9 |
| 1∶11 | Y＝1.0584X+3.9302 | 0.9471 | 10.25 |
| 1∶9 | Y＝1.2128X+3.8734 | 0.9583 | 8.49 |
| 1∶5 | Y＝0.9353X+4.2563 | 0.9736 | 6.24 |
| 1∶3 | Y＝0.7873X+4.3441 | 0.9693 | 6.81 |
| 1∶1 | Y＝0.6344X+4.5359 | 0.9872 | 5.39 |
The composite co-toxicity of table 4 fluorine pyrrole bacterium acid amides and kresoxim-methyl to the powdery mildew of cucumber bacterium
| Test medicine | Mass ratio | The actual measurement poison refers to | Theoretical poison refers to | Co-toxicity coefficient | Conclusion |
| Fluorine pyrrole bacterium acid amides (A) | 1∶0 | 100.00 | 100.00 | / | / |
| Kresoxim-methyl (B) | 0∶1 | 30.43 | 30.43 | / | / |
| A+B | 1∶11 | 20.50 | 20.31 | 100.9 | Addition |
| A+B | 1∶9 | 24.73 | 20.94 | 118.1 | Addition |
| A+B | 1∶5 | 33.65 | 23.51 | 143.1 | Synergy |
| A+B | 1∶3 | 30.85 | 26.78 | 115.2 | Addition |
| A+B | 1∶1 | 38.93 | 36.52 | 106.6 | Addition |
According to bactericide joint toxicity measuring result, fluorine pyrrole bacterium acid amides kresoxim-methyl mass ratio is that 1: 5 o'clock co-toxicity coefficient is 143.1, greater than 120, shows as synergistic effect, and other show as summation action greater than 100, think that 1: 5 o'clock synergistic effect is best.Suggestion is carried out further field control effectiveness test to the mixture preparation of 1: 5 left and right sides scope of suitable proportion, to estimate its field practical application effect.
Toxicity Determination example 2: fluorine pyrrole bacterium acid amides and azoxystrobin compound are to the Toxicity Determination of powdery mildew of cucumber bacterium.
With fluorine pyrrole bacterium acid amides and the former medicinal acetone of Fluoxastrobin is dissolution with solvents, is made into 10000 μ g/ml mother liquors, in 4 ℃ of preservations, stand-by.
56% fluorine pyrrole bacterium acid amides Fluoxastrobin mass ratio is respectively 4.7%+51.3%, 5.6%+50.4%, 9.3%+46.7%, 14%+42% and 28%+28% totally 5 combinations that are mixed.
Virulence experiment result and analysis:
The different proportioning fluorine of table 5 pyrrole bacterium acid amides and Fluoxastrobin mixture are to virulence and the synergistic effect of powdery mildew of cucumber bacterium
| The pharmacy quality ratio | Virulence regression equation | The correlation coefficient r value | EC 50(mg/L) |
| Fluorine pyrrole bacterium acid amides (A) | Y＝2.0929X+5.0958 | 0.9533 | 0.9 |
| Fluoxastrobin (B) | Y＝1.6504X+3.7039 | 0.9644 | 6.1 |
| 1∶11 | Y＝1.4601X+3.7421 | 0.9645 | 7.27 |
| 1∶9 | Y＝1.3346X+3.9304 | 0.9492 | 6.33 |
| 1∶5 | Y＝1.9809X+3.7820 | 0.9603 | 4.12 |
| 1∶3 | Y＝1.9319X+3.8646 | 0.9617 | 3.87 |
| 1∶1 | Y＝2.0263X+4.1660 | 0.9666 | 2.58 |
Table 6 fluorine pyrrole bacterium acid amides and azoxystrobin compound are to the co-toxicity of powdery mildew of cucumber bacterium
| Test medicine | Mass ratio | The actual measurement poison refers to | Theoretical poison refers to | Co-toxicity coefficient | Conclusion |
| Fluorine pyrrole bacterium acid amides (A) | 1∶0 | 100.00 | 100.00 | / | / |
| Fluoxastrobin (B) | 0∶1 | 14.75 | 14.75 | / | / |
| A+B | 1∶11 | 12.38 | 12.27 | 100.9 | Addition |
| A+B | 1∶9 | 14.22 | 13.04 | 109.1 | Addition |
| A+B | 1∶5 | 21.82 | 16.19 | 134.8 | Synergy |
| A+B | 1∶3 | 23.27 | 20.20 | 115.2 | Addition |
| A+B | 1∶1 | 34.89 | 32.13 | 108.6 | Addition |
According to bactericide joint toxicity measuring result, fluorine pyrrole bacterium acid amides Fluoxastrobin mass ratio is that 1: 5 o'clock co-toxicity coefficient is 134.8, greater than 120, shows as synergistic effect, and other show as summation action greater than 100, think that 1: 5 o'clock synergistic effect is best.Suggestion is carried out further field control effectiveness test to the mixture preparation of 1: 5 left and right sides scope of suitable proportion, to estimate its field practical application effect.
Field trial:
Test example 1: field trial measure fluorine pyrrole bacterium acid amides respectively with Propineb, kresoxim-methyl, the single composite control efficiency of Fluoxastrobin to powdery mildew of cucumber
(1) investigation method
The cucumber ground of test, 4 points are investigated in every sub-district, and every some investigation 2 strains are write down occurring degree with staging, and grade scale is as follows: 0 grade: no scab;
1 grade: lesion area accounts for whole below 5% of leaf area;
3 grades: lesion area accounts for whole leaf area 6%～10%;
5 grades: lesion area accounts for 11%～25% of whole leaf area;
7 grades: lesion area accounts for 26%～50% of whole leaf area;
9 grades: lesion area accounts for whole more than 50% of leaf area.
(2) control time and number of times
Test is investigated 4 times altogether, i.e. disease index investigation before the medicine, preventive effect investigation in 7 days behind the 1st medicine, 7 days and preventive effect investigation in 15 days behind 2 medicines.
(3) drug effect computational methods
Sick leaf rate (the %)=sick number of sheets/investigate total number of sheets * 100
Disease index=∑ (the sick numbers of sheets at different levels * relative level numerical value)/(investigating total number of sheets * 9) * 100
Control efficiency (%)=(1-(disease index behind disease index before the blank district medicine * treatment region medicine)/(disease index before disease index behind the blank district medicine * treatment region medicine)) * 100
(4) poisoning investigation method
Whether continuous 7d range estimation medicament has poisoning to crop after the dispenser.
(5) result of the test and analysis
1. fluorine pyrrole bacterium acid amides and Propineb are composite
Experimental field: the cucumber ground in Yangling District Li Tai township, Shaanxi Province.
Result and analysis:
Each handles the effect of preventing and treating powdery mildew of cucumber table 7
As shown in Table 7, fluorine pyrrole bacterium acid amides and the Propineb effect for powdery mildew of cucumber under 1: 9 proportioning is remarkable; Behind its 1 time, 2 times medicines behind 7 days and 2 medicines 15 days preventive effect significantly be better than two kinds of single agent, illustrate that complex preparation has significant synergistic effect, not only quick-acting is better for germ for it, and lasting effect is also very remarkable; In addition, through field trial checking, the agent of fluorine pyrrole bacterium acid amides list is better than the agent of Propineb list for the preventive effect of powdery mildew of cucumber, and complex preparation and two kinds of single agent all in the using dosage scope to crop safety, have no adverse effects.
2. fluorine pyrrole bacterium acid amides and kresoxim-methyl are composite
Experimental field: the cucumber ground of city, precipice, Sanya, Hainan Province hillside fields.
Result and analysis:
Each handles the effect of preventing and treating powdery mildew of cucumber table 8
As can be seen from Table 8, to prevent and treat the effect of powdery mildew of cucumber remarkable in the combination that is mixed of 56% fluorine pyrrole bacterium acid amides kresoxim-methyl 1: 5.Under the consumption of same every mu 10 gram, the effect of complex preparation significantly is better than two kinds of single agent, and its quick-acting and lasting effect are all relatively good, and be the most outstanding with lasting effect especially.Complex preparation significantly is better than effect under the low concentration consumption in control efficiency under the consumption of high concentration.15 days lasting effect is more remarkable after 7 days control efficiency behind the 1st, 2 medicine reaches 73.23% and 81.89%, the 2 medicine respectively, reaches 85.45%.Result of the test proves that the single agent effect of 41.7% fluorine pyrrole bacterium acid amides SC obviously is better than the single agent of 50% kresoxim-methyl SC.Behind the 2nd medicine 15 days, the highest preventive effect of the single agent of 41.7% fluorine pyrrole bacterium acid amides SC was that the highest preventive effect of the single agent of 79.86%, 50% kresoxim-methyl SC is 78.17%.According to field range estimation, in the test dose scope, plant growth is normal, and each is handled medicament and poisoning phenomenon to cucumber all do not occur, illustrates that it is safe to cucumber.Prevent desirable even more ideal control efficiency at the initial stage of a disease or in advance.
3. fluorine pyrrole bacterium acid amides and azoxystrobin compound
Experimental field: the cucumber ground in cities and towns, precipice, Sanya, Hainan Province.
Result and analysis:
Each handles the effect of preventing and treating powdery mildew of cucumber table 9
As can be seen from Table 9, to prevent and treat the effect of powdery mildew of cucumber remarkable in the combination that is mixed of 56% fluorine pyrrole bacterium acid amides Fluoxastrobin 1: 5.Under the consumption of same every mu 10 gram, the effect of complex preparation significantly is better than two kinds of single agent, and its quick-acting and lasting effect are all relatively good, and be the most outstanding with lasting effect especially.Complex preparation significantly is better than effect under the low concentration consumption in control efficiency under the consumption of high concentration.15 days lasting effect is more remarkable after 7 days control efficiency behind the 1st, 2 medicine reaches 74.27% and 77.16%, the 2 medicine respectively, reaches 84.59%.Result of the test proves that the single agent effect of 41.7% fluorine pyrrole bacterium acid amides SC obviously is better than the single agent of 25% Fluoxastrobin SC.Behind the 2nd medicine 15 days, the highest preventive effect of the single agent of 41.7% fluorine pyrrole bacterium acid amides SC was that the highest preventive effect of the single agent of 80.60%, 25% Fluoxastrobin SC is 78.81%.According to field range estimation, in the test dose scope, plant growth is normal, and each is handled medicament and poisoning phenomenon to cucumber all do not occur, illustrates that it is safe to cucumber.Prevent desirable even more ideal control efficiency at the initial stage of a disease or in advance.
Test example 2: field trial measure fluorine pyrrole bacterium acid amides respectively with Propineb, kresoxim-methyl, the single composite control efficiency of Fluoxastrobin to the custard squash powdery mildew
(1) investigation method
In the custard squash booth experimental field, 4 points are investigated in every sub-district, and every some investigation 2 strains are put down in writing occurring degree with staging, and grade scale is as follows:
0 grade: no scab;
1 grade: lesion area accounts for whole below 5% of leaf area;
3 grades: lesion area accounts for whole leaf area 6%～10%;
5 grades: lesion area accounts for 11%～25% of whole leaf area;
7 grades: lesion area accounts for 26%～50% of whole leaf area;
9 grades: lesion area accounts for whole more than 50% of leaf area.
(2) control time and number of times
Test is investigated 4 times altogether, i.e. disease index investigation before the medicine, preventive effect investigation in 7 days behind the 1st medicine, 7 days and preventive effect investigation in 15 days behind 2 medicines.
(3) drug effect computational methods
Diseased plant leaf (the %)=sick number of sheets/investigate total number of sheets * 100
Disease index=∑ (the sick numbers of sheets at different levels * relative level numerical value)/(investigating total number of sheets * 9) * 100
Control efficiency (%)=(1-(disease index behind disease index before the blank district medicine * treatment region medicine)/(disease index before disease index behind the blank district medicine * treatment region medicine)) * 100
(4) poisoning investigation method
Whether continuous 7d range estimation medicament has poisoning to crop after the dispenser.
(5) result of the test and analysis
1. fluorine pyrrole bacterium acid amides and Propineb are composite
Experimental field: in the custard squash booth in Yangling District Li Tai township, Shaanxi.
Result and analysis:
Each handles the effect of control custard squash powdery mildew table 10
As shown in Table 10, the effect of 1: 9 the combination control custard squash powdery mildew that is mixed of fluorine pyrrole bacterium acid amides Propineb is remarkable.Under the consumption of same every mu 10 gram, the effect of complex preparation significantly is better than two kinds of single agent, and its quick-acting and lasting effect are all relatively good, and be the most outstanding with lasting effect especially.Complex preparation significantly is better than effect under the low concentration consumption in control efficiency under the consumption of high concentration.15 days lasting effect is more remarkable after 7 days control efficiency behind the 1st, 2 medicine reaches 67,60% and 77,43%, the 2 medicine respectively, reaches 83.38%.Result of the test proves that 41.7% fluorine pyrrole bacterium acid amides list agent effect obviously is better than the single agent of 70% Propineb WP.According to field range estimation, in the test dose scope, plant growth is normal, and each is handled medicament and poisoning phenomenon to custard squash all do not occur, illustrates that it is safe to custard squash.
2. fluorine pyrrole bacterium acid amides and kresoxim-methyl are composite
Experimental field: hillside fields custard squash ground, cities and towns, precipice, Sanya, Hainan Province
Result and analysis:
Each handles the effect of control custard squash powdery mildew table 11
As can be seen from Table 11, the effect of 1: 5 the combination control custard squash powdery mildew that is mixed of 56% fluorine pyrrole bacterium acid amides kresoxim-methyl SC is remarkable.Under the consumption of same every mu 10 gram, the effect of complex preparation significantly is better than two kinds of single agent, and its quick-acting and lasting effect are all relatively good, and be the most outstanding with lasting effect especially.Complex preparation significantly is better than effect under the low concentration consumption in control efficiency under the consumption of high concentration.15 days lasting effect is more remarkable after 7 days control efficiency behind the 1st, 2 medicine reaches 72.09% and 79.38%, the 2 medicine respectively, reaches 83.90%.Result of the test proves that the single agent effect of 41.7% fluorine pyrrole bacterium acid amides SC obviously is better than the single agent of 50% kresoxim-methyl SC.Behind the 2nd medicine 15 days, the highest preventive effect of the single agent of 41.7% fluorine pyrrole bacterium acid amides SC was that the highest preventive effect of the single agent of 81.59%, 50% kresoxim-methyl SC is 77.38%.According to field range estimation, in the test dose scope, plant growth is normal, and each is handled medicament and poisoning phenomenon to custard squash all do not occur, illustrates that it is safe to custard squash.Prevent desirable even more ideal control efficiency at the initial stage of a disease or in advance.
3. fluorine pyrrole bacterium acid amides and azoxystrobin compound
Experimental field: in the custard squash booth in cities and towns, precipice, Sanya, Hainan Province.
Result and analysis:
Each handles the effect of control custard squash powdery mildew table 12
As can be seen from Table 12, the effect of 1: 5 the combination control custard squash powdery mildew that is mixed of 56% fluorine pyrrole bacterium acid amides Fluoxastrobin SC is remarkable.Under the consumption of same every mu 10 gram, the effect of complex preparation significantly is better than two kinds of single agent, and its quick-acting and lasting effect are all relatively good, and be the most outstanding with lasting effect especially.Complex preparation significantly is better than effect under the low concentration consumption in control efficiency under the consumption of high concentration.15 days lasting effect is more remarkable after 7 days control efficiency behind the 1st, 2 medicine reaches 72.50% and 77.23%, the 2 medicine respectively, reaches 81.04%.Result of the test proves that the single agent effect of 41.7% fluorine pyrrole bacterium acid amides SC obviously is better than the single agent of 25% Fluoxastrobin SC.Behind the 2nd medicine 15 days, the highest preventive effect of the single agent of 41.7% fluorine pyrrole bacterium acid amides SC was that the highest preventive effect of the single agent of 78.78%, 25% Fluoxastrobin SC is 75.25%.According to field range estimation, in the test dose scope, plant growth is normal, and each is handled medicament and poisoning phenomenon to custard squash all do not occur, illustrates that it is safe to custard squash.Prevent desirable even more ideal control efficiency at the initial stage of a disease or in advance.
In sum, fluorine pyrrole bacterium acid amides Propineb, fluorine pyrrole bacterium acid amides kresoxim-methyl, fluorine pyrrole bacterium acid amides Fluoxastrobin have remarkable prevention effect for Curcurbitaceae white powder germ under reasonable proportioning, and giving prominence to its instant effect, lasting effect is advantage.By composite, not only significantly improved drug effect, enlarged fungicidal spectrum simultaneously, delayed the drug-fast generation of germ.So the popularization of above-mentioned complex preparation has crucial meaning to agricultural production.
Claims (7)
1. pesticide sterilizing composite is characterized in that: is that active ingredient is carried out composite with (A) fluorine pyrrole bacterium acid amides with the arbitrary fungicide active ingredient that (B) is selected from Propineb, Fluoxastrobin, the kresoxim-methyl.
2. bactericidal composition according to claim 1 is characterized in that: the percentage by weight of active components A and B is 70～1:10～90.
3. bactericidal composition according to claim 1 is characterized in that: the percentage by weight of active components A and B is 40～1:25～60.
4. bactericidal composition according to claim 1 is characterized in that: effective constituents A and the B gross weight percentage composition in preparation is 1%-90%.
5. bactericidal composition according to claim 1 is characterized in that: effective constituents A and the B gross weight percentage composition in preparation is preferably 15%-70%.
6. bactericidal composition according to claim 1 is characterized in that: the formulation that bactericidal composition of the present invention can be prepared according to the known method of those skilled in the art of the present technique is aqueous emulsion, microemulsion, missible oil, suspending agent, wetting powder, water dispersible granules.
7. bactericidal composition according to claim 1 is characterized in that: be mainly used in diseases caused by the bacteria such as powdery mildew on cereal such as control vegetables, wheat and the fruit tree, downy mildew, rust, tikka class disease, scab, rot.
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| CN102204537A (en) * | 2011-05-05 | 2011-10-05 | 青岛海利尔药业有限公司 | Antibacterial composition containing fluopicolide and ethofenprox |
| CN102228032A (en) * | 2011-05-09 | 2011-11-02 | 青岛海利尔药业有限公司 | Bactericidal composition containing fluopyram and famoxadone |
| CN102258011A (en) * | 2011-06-03 | 2011-11-30 | 中国农业大学 | Bactericidal pesticide preparation by taking ionic liquid as cosolvent and preparation method thereof |
| CN102428953A (en) * | 2012-01-14 | 2012-05-02 | 陕西美邦农药有限公司 | Bactericidal composition containing silthiopham and methoxy acrylate compound |
| CN103385244A (en) * | 2012-05-08 | 2013-11-13 | 陕西韦尔奇作物保护有限公司 | Bactericidal composition comprising fluxapyroxad and thiocarbamate |
| CN104738050A (en) * | 2015-02-13 | 2015-07-01 | 广西壮族自治区农业科学院农产品质量安全与检测技术研究所 | Ultralow-volume liquid formulation containing benzovindiflupyr and strobilurin bactericide composition |
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| CN106665598A (en) * | 2017-02-18 | 2017-05-17 | 佛山市瑞生通科技有限公司 | Pesticide composition containing benzothiostrobin and fluopyram and application of pesticide composition |
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| CN102204537A (en) * | 2011-05-05 | 2011-10-05 | 青岛海利尔药业有限公司 | Antibacterial composition containing fluopicolide and ethofenprox |
| CN102228032A (en) * | 2011-05-09 | 2011-11-02 | 青岛海利尔药业有限公司 | Bactericidal composition containing fluopyram and famoxadone |
| CN102258011A (en) * | 2011-06-03 | 2011-11-30 | 中国农业大学 | Bactericidal pesticide preparation by taking ionic liquid as cosolvent and preparation method thereof |
| CN102258011B (en) * | 2011-06-03 | 2013-10-23 | 中国农业大学 | Bactericidal pesticide preparation by taking ionic liquid as cosolvent and preparation method thereof |
| CN102428953A (en) * | 2012-01-14 | 2012-05-02 | 陕西美邦农药有限公司 | Bactericidal composition containing silthiopham and methoxy acrylate compound |
| CN103385244A (en) * | 2012-05-08 | 2013-11-13 | 陕西韦尔奇作物保护有限公司 | Bactericidal composition comprising fluxapyroxad and thiocarbamate |
| CN104738050A (en) * | 2015-02-13 | 2015-07-01 | 广西壮族自治区农业科学院农产品质量安全与检测技术研究所 | Ultralow-volume liquid formulation containing benzovindiflupyr and strobilurin bactericide composition |
| CN105475334A (en) * | 2015-11-20 | 2016-04-13 | 广东中迅农科股份有限公司 | Flowable seed coating agent containing fluopyram, azoxystrobin and thiamethoxam |
| CN106719774A (en) * | 2016-11-26 | 2017-05-31 | 佛山市盈辉作物科学有限公司 | A kind of composition pesticide comprising fluopyram |
| CN106665598A (en) * | 2017-02-18 | 2017-05-17 | 佛山市瑞生通科技有限公司 | Pesticide composition containing benzothiostrobin and fluopyram and application of pesticide composition |
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