CN101715771B - Sterilizing composition containing imibenconazole - Google Patents
Sterilizing composition containing imibenconazole Download PDFInfo
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- CN101715771B CN101715771B CN 200910112889 CN200910112889A CN101715771B CN 101715771 B CN101715771 B CN 101715771B CN 200910112889 CN200910112889 CN 200910112889 CN 200910112889 A CN200910112889 A CN 200910112889A CN 101715771 B CN101715771 B CN 101715771B
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Abstract
The invention discloses a sterilizing composition containing two active components. The active component A is selected from 4-chlorobenzyl-N-(2,4-dichlorophenyl)-2(1H-1, 2, 4-triazole-1-yl) ethyl thiooxamate (imibenconazole), and the active component B is selected from any one of the following bactericides: azoxystrobin, ethirimol, propineb, chlorothalonil, polyoxin and zhongshengmycin. The ratio of the two components is 20:1 to 1:40 in parts by weight. The composition can be prepared into missible oil, microemulsion, emulsion in water, suspending agent, aqueous solution agent, wetting powder and water dispersible granules and the like. The sterilizing composition has obvious function of synergism and is applied to preventing and treating plant diseases caused by sac fuagi, Fungi imperfecti and basidiomycetes.
Description
Technical field
The invention belongs to the disinfectant use in agriculture field.
Background technology
Glyoxalin (imibenconazole), 4-chlorobenzyl N-(2,4-dichlorophenyl)-2 (1H-1,2,4-triazol-1-yl) thioacetamide ester, broad spectrum activity triazole bactericidal agent.Mainly be the biosynthesis that destroys and stop the cell membrane important component part ergosterol of germ, thereby destroyed the formation of cell membrane, cause germ dead.
Fluoxastrobin (azoxystrobin); (E)-and 2-{2-[6 (2-cyano-benzene oxygen) pyrimidine-4-yl oxygen] phenyl }-the 3-methoxy acrylate; belong to the wide spectrum methoxy acrylic bactericide; the mitochondrial respiratory inhibitor; namely by shifting to the electronics of cromoci at cytochrome B cl; thereby suppress mitochondrial breathing, have protection, root out, infiltration, systemic activity, suppress spore germination and mycelial growth and produce spore always.
The phonetic phenol of second (ethirimol), 5-butyl-2-ethylamino-4-hydroxyl-6-methylpyrimidine, belong to the miazines bactericide, adenosine deaminase inhibitors, after pathogen contacts, mycelium, conidium, trichogyne there is very strong killing effect, the powerful formation that suppresses spore, systemic fungicide has protection and therapeutic action; Can be absorbed rapidly by plant roots, stem, leaf, and in plant corpus, run to each position, be mainly used in preventing and treating the powdery mildew of crop.
Propineb (propineb), acrylic bisdithiocarbamic zinc belongs to dithiocarbamates, act on the synthetic of fungal cell wall and protein, can suppress infecting and sprouting of spore, can suppress mycelial growth simultaneously, cause its distortion, death.And this medicine contains and is easy to zinc element absorbed by crops, the quality that is conducive to promote plant growth and improves fruit.
Tpn (chlorothalonil); daconil M (2; 4; 5; 6-tetrachloro-1, the 3-benzene dicarbonitrile), belong to organochlorine class protective fungicide; can with the fungal cell in glyceraldehyde 3-phosphate dehydro-genase in the combined with protein of cysteine, destroy the metabolism of cell and loss of life power.Its Main Function is the prevention fungal infection, does not have interior suction conduction, but at plant surface good adhesivity is arranged, and is not subject to rain drop erosion, and the long drug effect phase is arranged.
Polyoxin (polyoxin), the broad-spectrum antibiotics class has the preferably interior conduction of inhaling, and its mechanism of action is to disturb the chitinous biosynthesis of bacterial cell wall, germ tube is with after mycelium contacts medicament, expand the part, breaks, and overflows cell inclusion, and can not normal development cause death, suppress in addition germ and produce spore and scab expansion effect, this medicine does not have toxicity to animal, and plant is not had poisoning.Be used for the multiple fungal diseases such as control paddy rice, wheat, vegetables fruit tree.
Zhongshengmycin (zhongshengmycin) belongs to N-glucosides class alkaline water soluble substance, the protective fungicide that fungicidal spectrum is wider, have tag, osmosis.Its effect: be suppress bacterium protein synthetic to bacterium, cause thalline dead; Be to make the mold fungi deformation of filament to fungi, suppress spore germination and direct killing spores.Bacterial disease and part fungal disease to crops have very high activity, have simultaneously certain production-increasing function.
Summary of the invention
The object of the present invention is to provide a kind of mixed ratio reasonable, control efficiency is good, the synergetic pesticide composition that drug cost is low.
Another object of the present invention is to provide by formulations such as the formulated missible oil of this composition pesticide, microemulsion, aqueous emulsion, suspending agent, wetting powder, water dispersible granules, granules.
Another object of the present invention is to provide the purposes that composition pesticide is used for powdery mildew that control sac fungi, imperfect fungus cause, ring rot of apple, alternaria leaf spot of apple, pear scab, anthracnose of grape.
The resistance that a further object of the present invention is to avoid to use the glyoxalin single dose to bring occurs, degradation problem under the drug effect, the present invention proposes a kind of new bactericidal composition, preparation and the application of composition.
Said composition contains two kinds of active components, and active component A is selected from, 4-chlorobenzyl N-(2,4-dichlorophenyl)-2 (1H-1,2,4-triazol-1-yl) thioacetamide ester, common name: glyoxalin (imibenconazole)
Active component B is selected from following any one bactericide:
(E)-and 2-{2-[6 (2-cyano-benzene oxygen) pyrimidine-4-yl oxygen] phenyl }-the 3-methoxy acrylate, common name: Fluoxastrobin (azoxystrobin)
5-butyl-2-ethylamino-4-hydroxyl-6-methylpyrimidine, common name: the phonetic phenol of second (ethirimol)
Acrylic bisdithiocarbamic zinc, common name: Propineb (propineb)
Polyoxin (polyoxin)
Zhongshengmycin (zhongshengmycin)
Have now found that the bactericidal composition that the present invention proposes has very significantly synergistic effect, have the utmost point to significantly improve to the control efficiency of corps diseases, delay the drug-fast generation of pathogen.Adopt composite bactericidal composition can obviously improve control and result for the treatment of, reduced the usage amount of agricultural chemicals, reduced cost, thereby reached main purpose of the present invention.
The amount of application of compound also depended on the ratio of a kind of compound and another kind of compound and the degree of synergistic effect when the amount that the product of the present composition contains active component depended on independent the use.Wherein the weight ratio of glyoxalin and Fluoxastrobin is 20: 1～1: 40, is preferably 3: 1～1: 10; The weight ratio of glyoxalin and the phonetic phenol of second is 20: 1～1: 40, is preferably 3: 1～1: 10; The weight ratio of glyoxalin and Propineb is 20: 1～1: 40, is preferably 3: 1～1: 20; The weight ratio of glyoxalin and tpn is 20: 1～1: 40, is preferably 3: 1～1: 30; The weight ratio of glyoxalin and polyoxin is 20: 1～1: 40, is preferably 10: 1～1: 3; The weight ratio of glyoxalin and Zhongshengmycin is 20: 1～1: 40, is preferably 7: 1～1: 3.
Active component is 0.5% to 95% of gross weight in the composition of the present invention.
Except the fungicidal activity composition, also can comprise functional aid in the bactericidal composition of the present invention.That is to say that the present composition can add other components such as functional aid, be mixed with the preparation of missible oil, aqueous emulsion, microemulsion, suspending agent, aqua, wetting powder, water dispersible granules or other formulations.
In these preparations, except active component, all contain surfactant, and also can contain the thinners such as organic solvent or cosolvent, carrier (filler) or water according to different dosage form, add in case of necessity other functional aids such as antifreeze, thickener, stabilizing agent, defoamer, disintegrant.Surfactant can be emulsifier, dispersant, wetting agent or bleeding agent.Surfactant can be nonionic with ionic, also can be two or more compound uses.
Described emulsifier is alkylphenol-polyethenoxy (polyoxypropylene) ether, Ben-zylphenol Polyoxyethyl Ether, phenethyl phenol polyethenoxy ether, fatty alcohol-polyoxyethylene ether, polyoxyethylene carboxylate, phenethyl phenol polyethenoxy polyethenoxy ether, castor oil ethylene oxide adduct, alkylphenol polyoxyethylene formaldehyde condensation products, and the phosphate of these compounds, alkyl benzene sulphonate (calcium salt or sodium salt) or directly use commercially available emulsifier monomer and composite product.Concrete example is such as farming breast 500
#Series, 600
#Series, 1600
#Series, NP is serial, OP is serial, AEO is serial, 700
#, 400
#Serial and composite kind 2201,0203B, 2021B, 4103 etc., these all are emulsifier productions well known in the art, market is on sale.
Described dispersant; wetting agent; bleeding agent is lignosulfonates (sodium salt or calcium salts); Negel; condensation compound of methyl naphthalene sulfonic acid and formaldehyde sulphate; naphthalene sulfonic acid-formaldehyde condensation product; methanonaphthalene sodium sulfonate dibutyl naphthalene sulfonic acid-formaldehyde condensation product; N-methyl fatty acyl group sodium taurocholate; alkylphenol polyoxyethylene formaldehyde condensation products sulphate; polymerization of carboxylic acid sodium; the alkylphenol polyoxyethylene phosphate; the withered powder of tea; saponin; lignosulfite; aliphatic alcohol sulfate; dodecyl sodium sulfate; alkylbenzenesulfonate; penetrant t; bleeding agent OT; fatty acid amide-N methyl taurine sodium salt; sodium sulfate of polyethenoxy ether of fatty alcohol; pull open powder; JFC; can use separately, but also compound use.Above-mentioned surfactant all is materials well known in the art, can obtain by various commercial channel.
Described solvent, cosolvent are toluene, dimethylbenzene, chlorobenzene, solvent naphtha, alpha-methyl-naphthalene, turpentine oil, carrene, chloroform, methyl alcohol, ethanol, isopropyl alcohol, butanols, isoamyl alcohol, cyclohexanone, isophorone, acetophenone, ethyl acetate, butyl acetate, N.N-dimethyl formamide, dimethyl sulfoxide (DMSO), methyl cellosolve, ethyl cellosolve, Gao Jinsai ketone, organic amine etc.
Described antifreeze is ethylene glycol, glycerine, propane diols, urea, glycerine, ether diglycol, polyethylene glycol, isopropyl alcohol etc.
Described carrier, filler are white carbon, precipitated calcium carbonate, potter's clay, attapulgite, kaolin, diatomite, bentonite, sepiolite, zeolite, quartz sand, talcum powder, can use separately, also can two kinds or above mixing use.
Described disintegrant has sodium alginate, sodium carboxymethyl starch, sulfuric acid amine, bentonite, urea, calcium chloride.
Described defoamer has bubble enemy, silicone, C
8-10Fatty alcohol, C
10-20Saturated fat acids (such as capric acid, stearic acid etc.) and amide-type.
Described binding agent is starch, dextrin, gum Arabic, soybean protein, gelatine, sodium sulphate, gypsum, polyvinyl alcohol, polyethylene glycol, rosin, paraffin, CMC, sodium silicate.Can use separately, also can two or morely use with.
Can contain toner in the preparation, inorganic pigment iron oxide for example, titanium oxide or Prussian blue; Organic dyestuff is such as A Lizhalin, azo dyes, metal phthalocyanine or kiton colors.In water-base preparation, for preventing moldy metamorphism, need to add a certain amount of preservative, described preservative has Sodium Benzoate, polyformaldehyde, sorbitol, formalin, citric acid, to the yl benzoic acid methyl esters, face phenyl phenol sodium, 1,2-benzisothiazole-3-ketone (code name BIT) etc.
The product that the present invention describes can be the finished product preparation form to be provided, and namely each material mixes in the composition, but the composition of composition also can provide with independent preparation directly mixing in bucket (tank) before using.Concentrate of the present invention usually and water be mixed to get the concentration of required active substance.
Composition of the present invention can be used for various plants, such as Chinese cabbage, wild cabbage, cauliflower, wax gourd, cucumber, tomato, apple, pear tree, lichee, grape, wheat, rape, potato, tobacco and flowers etc.The place of using of the product that composition of the present invention and carrier are made is farmland, orchard or warehouse etc.
Composition of the present invention also can with other compound with weeding, desinsection or bactericidal property particularly the protective fungicide agent composition use, also can use with nematocide, protective agent, growth regulator, nutrient for plants or soil conditioner mixture.Composition of the present invention can be used by common method, such as cast, injection, spraying.Amount of application of the present invention is with weather condition or crop state variation, and time of application can be before or after crop be susceptible.The duration of protective effect is usually relevant with the content of individualized compound in the composition, also relevant with extraneous factor, weather for example, but by using suitable formulation can slow down climatic influences.
The remarkable advantage of composition of the present invention: the one, composition shows extremely strong synergistic effect in certain ratio range, the bactericidal effect of mixed composition is significantly improved than its single dose, thereby reduced using dosage, when reducing peasant's drug cost, reduced influence degree.The 2nd, interracial structure differs larger, and the resistance that the application of said composition can delay single dose occurs and development.
Embodiment:
The present invention is elaborated with following specific embodiment, so that advantage of the present invention is more obvious, but the present invention is limited to absolutely not these examples.Percentage all is weight percentage in the prescription of all preparations, and the processing of biologically-active moiety is effective content.
Formulation examples:
1, the preparation of missible oil
By the prescription requirement, add respectively solvent, former medicine, emulsifier, mix, use in case of necessity the hot bath heating for dissolving, namely obtain transparence missible oil.Such as example 1～3 prescription.
Example 1 (10% missible oil)
Glyoxalin 5%, the phonetic phenol 5% of second, farming breast 500
#7.5%, agricultural newborn 600-2
#4.5%, methyl alcohol 8%, dimethylbenzene complements to 100%.
Example 2 (25% missible oil)
Glyoxalin 5%, Propineb 20%, farming breast 507
#10%, agricultural newborn OX-6533%, methyl alcohol 10%, dimethylbenzene complements to 100%.
Example 3 (30% missible oil)
Glyoxalin 3%, tpn 27%, farming breast 500
#10%, agricultural newborn OX-6355%, methyl alcohol 10%, dimethylbenzene complements to 100%.
2, the preparation of wetting powder
By the prescription requirement, former medicine, various auxiliary agent and filler etc. are fully mixed, behind ultra-fine pulverizer disintegrating, namely obtain converted products.Such as example 4～9 prescriptions.
Example 4 (30% wetting powder)
Glyoxalin 6%, Fluoxastrobin 24%, lauryl sodium sulfate 1.5%, carboxymethyl cellulose 1%, sodium lignin sulfonate 10%, precipitated calcium carbonate complements to 100%.
Example 5 (29% wetting powder)
Glyoxalin 6%, the phonetic phenol 19% of second, lauryl sodium sulfate 1.5%, carboxymethyl cellulose 1%, sodium lignin sulfonate 10%, precipitated calcium carbonate complements to 100%.
Example 6 (50% wetting powder)
Glyoxalin 8%, Propineb 42%, neopelex 1%, white carbon 10%, sodium lignin sulfonate 10%, precipitated calcium carbonate complements to 100%.
Example 7 (50% wetting powder)
Glyoxalin 8%, tpn 42%, neopelex 1%, white carbon 10%, sodium lignin sulfonate 10%, precipitated calcium carbonate complements to 100%.
Example 8 (12% wetting powder)
Glyoxalin 10%, polyoxin 2%, alkyl amide taurate 2%, Fluhyzon formaldehyde condensation 5%, alkylphenol-polyethenoxy phosphate 5%, precipitated calcium carbonate complements to 100%.
Example 9 (10% wetting powder)
Glyoxalin 8%, Zhongshengmycin 2%, neopelex 1%, white carbon 10%, naphtholsulfonic acid formaldehyde condensation products sodium salt 10%, precipitated calcium carbonate complements to 100%.
3, the preparation of aqueous emulsion
Former medicine, solvent, emulsifier and co-emulsifier are added together, make dissolving be even oil phase.Water, antifreeze etc. is mixed, becomes the homogeneous water.Under high-speed stirred, water is joined oil phase or oil phase is joined water, form the aqueous emulsion of favorable dispersibility.Such as example 10～12 prescriptions.
Example 10 (15% aqueous emulsion)
Glyoxalin 3%, the phonetic phenol 12% of second, polyvinyl alcohol 0.8%, in triphenylethylene phenol+oxirane, phosphorylation, the triethanolamine and 8.5%, alkyl-diethylene glycol ether-sodium sulfonate 2.5%, farming breast 2,201 13%, dimethyl formamide 8%, ethylene glycol 5%, water complements to 100%.
Example 11 (35% aqueous emulsion)
Glyoxalin 4%, Propineb 31%, polyvinyl alcohol 0.9%, alkylaryl polyoxyethylene propylene ether 8.5%, farming breast 2,201 15%, dimethyl formamide 12%, ethylene glycol 5%, water complements to 100%.
Example 12 (25% aqueous emulsion)
Glyoxalin 4%, tpn 21%, polyvinyl alcohol 1.5%, alkylaryl polyoxyethylene propylene ether 10%, farming breast 2,201 15%, dimethyl formamide 15%, ethylene glycol 5%, water complements to 100%.
4, the preparation of water-dispersible granules
Former medicine and powder carrier, wet spreading agent and binding agent etc. are carried out co-grinding, after adding again water and mediating, add in the comminutor that the certain specification screen cloth is housed and carry out granulation.And then drying, screening (by the screen cloth scope) namely gets granular product.Such as example 13～14 prescriptions.
Example 13 (40% water-dispersible granules)
Glyoxalin 8%, Fluoxastrobin 32%, methyl naphthalene sulfonate formaldehyde condensate 12%, epoxidized polyether 5%, soluble starch 15%, gypsum complements to 100%.
Example 14 (55% water-dispersible granules)
Glyoxalin 6%, Propineb 49%, methanonaphthalene sodium sulfonate 5%, epoxidized polyether 5%, sodium sulphate, gypsum complements to 100%.
5, the preparation of suspending agent
By the prescription requirement, take water as medium, former medicine, dispersant, suspending agent and antifreezing agent etc. are added in the sand milling still, carry out porphyrize, make suspending agent.Such as example 15～17 prescriptions.
Example 15 (40% suspending agent)
Glyoxalin 8%, the phonetic phenol 32% of second, methyl naphthalene sulfonate formaldehyde condensate 5.5%, white carbon 0.2%, aluminium-magnesium silicate 0.18%, ethylene glycol 4%, silicone a little, water complements to 100%.
Example 16 (50% suspending agent)
Glyoxalin 8%, Propineb 42%, calcium lignosulfonate 5%, white carbon 0.3%, ethylene glycol 4%, silicone a little, water complements to 100%.
Example 17 (40% suspending agent)
Glyoxalin 5%, tpn 35%, methyl naphthalene sulfonic acid naphthaldehyde condensation compound 2.5%, bentonite 1.0%, farming breast 16013%, glycerine 4%, silicone a little, water complements to 100%.
6, the preparation of microemulsion
Former medicine, solvent, emulsifier and co-emulsifier are added together, make dissolving be even oil phase.Water, antifreeze etc. is mixed, becomes the homogeneous water.Under high-speed stirred, water is joined oil phase or oil phase is joined water, form the microemulsion of favorable dispersibility.Such as example 18～20 prescriptions.
Example 18 (20% microemulsion)
Glyoxalin 4%, the phonetic phenol 16% of second, propyl alcohol 7%, phenethyl phenol polyethenoxy ether 10%, carrene 10%, glycerine 5%, water complements to 100%.
Example 19 (30% microemulsion)
Glyoxalin 5%, Propineb 25%, dimethylbenzene 12%, phenyl xenol polyvinylether 15%, ring ethanol 8%, ethylene glycol 8%, water complements to 100%.
Example 20 (25% microemulsion)
Glyoxalin 4%, tpn 21%, ethanol 6%, sodium alkyl benzene sulfonate 8%, the third hexanone 8%, propane diols 6%, water complements to 100%.
7, the preparation of aqua
By the prescription requirement, required solvent is injected reaction pot, then add all pesticide original medicines, stir and make its dissolving, add successively again auxiliary agent, emulsifier, last first alcohol and water is made aqua.Such as example 21～22 prescriptions.
Example 21 (10% aqua)
Glyoxalin 8%, polyoxin 2%, dimethyl formamide 10%, Gao Jinsai ketone 1.5～6%, fatty alcohol-polyoxyethylene ether 5%, alkylphenol polyoxyethylene 5%, fatty diglycollic amide 5%, sulfonic acid 2%, alcohol or water are mended to 100%.
Example 22 (8% aqua)
Glyoxalin 6%, Zhongshengmycin 2%, dimethyl formamide 10%, organic amine 1.5～6%, fatty alcohol-polyoxyethylene ether 5%, alkylphenol polyoxyethylene 5%, fatty diglycollic amide 5%, sulfonic acid 2%, alcohol or water are mended to 100%.
8, the present invention illustrates the synergistic effect that the present invention makes up with following biologically active embodiment.
The joint toxicity measuring of test example 1 glyoxalin and Fluoxastrobin
For the examination bacterium
Pear scab (Venturia pirina Anderh)
The experimental concentration design
Glyoxalin single dose concentration for the treatment of is 4,2,1,0.5,0.25 μ g/ml, Fluoxastrobin single dose concentration for the treatment of is 12,6,3,1.5,0.75 μ g/ml, five concentration gradients are also established in the test of combination medicament, and other establishes the blank of not dosing, and each is processed 4 times and repeats.
Test method
With deionized water wash-out, filtration on medium or the diseased tissues, centrifugal (1000r/min) 5min removes supernatant, adds deionized water, and is centrifugal again with cultured disease fungus spore.At last with deionization with the spore resuspension to every milliliter 1 * 10
5Individual～1 * 10
7Individual spore, and add 0.5% glucose solution., from the low concentration to the high concentration, draw successively liquid 0.5mL and add respectively in the small test tube with pipette or pipettor, then draw the spore suspension 0.5mL for preparing, make liquid and spore suspension mixed in equal amounts even.Draw above-mentioned mixed liquor with micro sample adding appliance and drip on the concave slide, then frame is put in the culture dish with shallow seated groundwater, adds a cover moisturizing and is incubated in the incubator of preference temperature.
Investigation and method of counting
By medicine inspecting institute of the Ministry of Agriculture " farm-chemical indoor determination test rule " method, when the blank spore germination rate reaches 90% when above, the spore germination situation is respectively processed in inspection.Every processing repeats 3 above visuals field of random observation, many 200 of investigation spore sum, and number and spore sum sprouted in record respectively.Spore germ tube length is considered as sprouting greater than the short radius of spore.According to survey data, calculate the spore germination relative inhibition that each is processed.Probability value according to each drug concentration logarithm value and corresponding spore germination relative inhibition is done regression analysis, calculates the EC of each medicament
50, according to Wadley fungicide in mixture synergy evaluation assessment, calculate interactional ratio behind two single dose mixtures (be that SR＜0.5 is antagonism, 0.5≤SR≤1.5 are summation action, and SR＞1.5 are synergistic effect).
Result of the test sees the following form 1.
The joint toxicity measuring result of table 1. glyoxalin and Fluoxastrobin
Result of the test shows: the weight ratio of glyoxalin and Fluoxastrobin is 1: 4 o'clock, and its interaction ratio is respectively 1.94, and the bactericide interaction theory according to GiSi (1985) proposes has the notable synergistic effect.
The joint toxicity measuring of test example 2 glyoxalins and the phonetic phenol of second
For the examination bacterium
Powdery mildew of cucumber (Sphaerotheca Fuligenea (Schlecht) Poll.)
For the examination cucumber variety
" the close thorn in Shandong ", cucumber is potted plant to be cultured to two open and flat phases of few leaf in the greenhouse.
The experimental concentration design
Glyoxalin single dose concentration for the treatment of is 4,2,1,0.5,0.25 μ g/ml, and the phonetic phenol single dose of second concentration for the treatment of is 32,16,8,4,2 μ g/ml, and five concentration gradients are also established in the test of combination medicament, and other establishes the blank of not dosing, and each is processed 4 times and repeats.
Test method
With the pure water that is added with a small amount of surfactant (such as Tween-80 etc.), wash and get the fresh spore that covers with on the Powdery Mildew plant leaf blade, filter with double gauze, making spore concentration is 1 * 10
5The suspension of individual spore/mL, for subsequent use.Liquid is evenly sprayed in the blade face to all wetting, for subsequent use behind the liquid natural air drying.Use the spore suspension spray inoculation.24h inoculation before chemicals treatment.Then postvaccinal examination material natural air drying moves to thermostatic chamber, cultivates 7d～10d under the condition of 20 ℃～24 ℃ of temperature.
Investigation and method of counting
By medicine inspecting institute of the Ministry of Agriculture " farm-chemical indoor determination test rule " method, treat that the sick leaf rate of blank reaches 80% when above, classification investigation is managed incidence everywhere, and 30 leaves are investigated in every processing at least, and grade scale is: 0 grade: anosis;
1 grade: lesion area accounts for below 5% of one-piece blade area;
3 grades: lesion area accounts for 5%～15% of one-piece blade area;
5 grades: lesion area accounts for 15%～25% of one-piece blade area;
7 grades: lesion area accounts for 25%～50% of one-piece blade area;
9 grades: lesion area accounts for 50%～75% of one-piece blade area;
11 grades: lesion area accounts for more than 75% of one-piece blade area.According to survey data, calculate disease index and control efficiency that each is processed.Do regression analysis according to each drug concentration logarithm value and preventive effect probability value, calculate the EC of each medicament
50, according to Wadley fungicide in mixture synergy evaluation assessment, calculate interactional ratio behind two single dose mixtures (be that SR＜0.5 is antagonism, 0.5≤SR≤1.5 are summation action, and SR＞1.5 are synergistic effect).
Result of the test sees the following form 2.
The joint toxicity measuring result of table 2. glyoxalin and the phonetic phenol of second
Result of the test shows: the weight ratio of glyoxalin and the phonetic phenol of second is 1: 3 o'clock, and its interaction ratio is respectively 1.91, and the bactericide interaction theory according to GiSi (1985) proposes has the notable synergistic effect.
The joint toxicity measuring of test example 3 glyoxalins and Propineb
For the examination bacterium
Alternaria leaf spot of apple (Alternaria mali Roberts)
The experimental concentration design
The experimental concentration of thifluzamide single dose is five concentration of 0.8,0.4,0.2,0.1,0.05 μ g/ml, phonetic mould amine concentration for the treatment of is 1.6,0.8,0.4,0.2,0.1 μ g/ml, five concentration gradients are also established in the test of combination medicament, and other establishes the blank of not dosing, and each is processed 4 times and repeats.
Test method
With deionized water wash-out, filtration on medium or the diseased tissues, centrifugal (1000r/min) 5min removes supernatant, adds deionized water, and is centrifugal again with cultured disease fungus spore.At last with deionization with the spore resuspension to every milliliter 1 * 10
5Individual～1 * 10
7Individual spore, and add 0.5% glucose solution., from the low concentration to the high concentration, draw successively liquid 0.5mL and add respectively in the small test tube with pipette or pipettor, then draw the spore suspension 0.5mL for preparing, make liquid and spore suspension mixed in equal amounts even.Draw above-mentioned mixed liquor with micro sample adding appliance and drip on the concave slide, then frame is put in the culture dish with shallow seated groundwater, adds a cover moisturizing and is incubated in the incubator of preference temperature.
Investigation and method of counting
By medicine inspecting institute of the Ministry of Agriculture " farm-chemical indoor determination test rule " method, when the blank spore germination rate reaches 90% when above, the spore germination situation is respectively processed in inspection.Every processing repeats 3 above visuals field of random observation, many 200 of investigation spore sum, and number and spore sum sprouted in record respectively.Spore germ tube length is considered as sprouting greater than the short radius of spore.According to survey data, calculate the spore germination relative inhibition that each is processed.Probability value according to each drug concentration logarithm value and corresponding spore germination relative inhibition is done regression analysis, calculates the EC of each medicament
50, according to Wadley fungicide in mixture synergy evaluation assessment, calculate interactional ratio behind two single dose mixtures (be that SR＜0.5 is antagonism, 0.5≤SR≤1.5 are summation action, and SR＞1.5 are synergistic effect).
Result of the test sees the following form 3.
The joint toxicity measuring result of table 3. glyoxalin and Propineb
Result of the test shows: the weight ratio of glyoxalin and Propineb is 1: 12 o'clock, and its interaction ratio is respectively 2.07, and the bactericide interaction theory according to GiSi (1985) proposes has the notable synergistic effect.
The joint toxicity measuring of test example 4 glyoxalins and tpn
For the examination bacterium
Anthracnose of grape (Sphaceloma ampelinum)
The experimental concentration design
Glyoxalin single dose concentration for the treatment of is 2.4,1.2,0.6,0.3,0.15 μ g/ml, tpn single dose concentration for the treatment of is 24,12,6,3,1.5 μ g/ml, five concentration gradients are also established in the test of combination medicament, and other establishes the blank of not dosing, and each is processed 4 times and repeats.
Test method
Under aseptic technique, process the sterilising medium that will melt in advance according to test and quantitatively add in the aseptic conical flask, from the low concentration to the high concentration, quantitatively draw successively liquid, add respectively in the above-mentioned conical flask, fully shake up.Then to pour 3 above diameters into be in the culture dish of 9cm to equivalent, and the pastille of making respective concentration is dull and stereotyped.With cultured pathogen, under aseptic condition, with the sterilization card punch of diameter 5mm, cut the bacterium cake from colony edge, with inoculator with pure culture biscuits involvng inoculation in the dull and stereotyped central authorities of pastille, mycelia faces up, and covers the ware lid, puts in the incubator of preference temperature and cultivates.
Investigation and method of counting
By medicine inspecting institute of the Ministry of Agriculture " pesticide bioassay test standard " method, according to the growing state investigation cause of disease mycelia growing state of the bacterium in the blank culture dish.Use the kind of calliper colony diameter.Each bacterium colony with right-angled intersection method vertical survey diameter is respectively once got its mean value.Calculate each concentration for the treatment of to the mycelial growth inhibition rate of germ according to investigation result.Probability value according to each drug concentration logarithm value and corresponding spore germination relative inhibition is done regression analysis, calculates the EC of each medicament
50, according to Wadley fungicide in mixture synergy evaluation assessment, calculate interactional ratio behind two single dose mixtures (be that SR＜0.5 is antagonism, 0.5≤SR≤1.5 are summation action, and SR＞1.5 are synergistic effect).
Result of the test sees the following form 4.
The joint toxicity measuring result of table 4. glyoxalin and tpn
Result of the test shows: the weight ratio of glyoxalin and tpn is 1: 15 o'clock, and its interaction ratio is respectively 2.03, and the bactericide interaction theory according to GiSi (1985) proposes has the notable synergistic effect.
The joint toxicity measuring of test example 5 glyoxalins and polyoxin
For the examination bacterium
Alternaria leaf spot of apple (Alternaria mali Roberts)
The experimental concentration design
The experimental concentration of polyoxin single dose is five concentration of 1.6,0.8,0.4,0.2,0.1 μ g/ml, glyoxalin single dose concentration for the treatment of is 3.2,1.6,0.8,0.4,0.2 μ g/ml, five concentration gradients are also established in the test of combination medicament, other establishes the blank of not dosing, and each is processed 4 times and repeats.
Test method
With deionized water wash-out, filtration on medium or the diseased tissues, centrifugal (1000r/min) 5min removes supernatant, adds deionized water, and is centrifugal again with cultured disease fungus spore.At last with deionization with the spore resuspension to every milliliter 1 * 10
5Individual～1 * 10
7Individual spore, and add 0.5% glucose solution., from the low concentration to the high concentration, draw successively liquid 0.5mL and add respectively in the small test tube with pipette or pipettor, then draw the spore suspension 0.5mL for preparing, make liquid and spore suspension mixed in equal amounts even.Draw above-mentioned mixed liquor with micro sample adding appliance and drip on the concave slide, then frame is put in the culture dish with shallow seated groundwater, adds a cover moisturizing and is incubated in the incubator of preference temperature.
Investigation and method of counting
By medicine inspecting institute of the Ministry of Agriculture " farm-chemical indoor determination test rule " method, when the blank spore germination rate reaches 90% when above, the spore germination situation is respectively processed in inspection.Every processing repeats 3 above visuals field of random observation, many 200 of investigation spore sum, and number and spore sum sprouted in record respectively.Spore germ tube length is considered as sprouting greater than the short radius of spore.According to survey data, calculate the spore germination relative inhibition that each is processed.Probability value according to each drug concentration logarithm value and corresponding spore germination relative inhibition is done regression analysis, calculates the EC of each medicament
50, according to Wadley fungicide in mixture synergy evaluation assessment, calculate interactional ratio behind two single dose mixtures (be that SR＜0.5 is antagonism, 0.5≤SR≤1.5 are summation action, and SR＞1.5 are synergistic effect).
Result of the test sees the following form 5.
The joint toxicity measuring result of table 5. glyoxalin and polyoxin
Result of the test shows: the weight ratio of glyoxalin and polyoxin is 5: 1 o'clock, and its interaction ratio is respectively 2.10, and the bactericide interaction theory according to GiSi (1985) proposes has the notable synergistic effect.
The joint toxicity measuring of test example 6 glyoxalins and Zhongshengmycin
Ring rot of apple (Physalospora piricola Nose)
The experimental concentration design
Glyoxalin single dose concentration for the treatment of is 2.4,1.2,0.6,0.3,0.15 μ g/ml, Zhongshengmycin single dose concentration for the treatment of is 12,6,3,1.5,0.75 μ g/ml, five concentration gradients are also established in the test of combination medicament, and other establishes the blank of not dosing, and each is processed 4 times and repeats.
Test method
With deionized water wash-out, filtration on medium or the diseased tissues, centrifugal (1000r/min) 5min removes supernatant, adds deionized water, and is centrifugal again with cultured disease fungus spore.At last with deionization with the spore resuspension to every milliliter 1 * 10
5Individual～1 * 10
7Individual spore, and add 0.5% glucose solution., from the low concentration to the high concentration, draw successively liquid 0.5mL and add respectively in the small test tube with pipette or pipettor, then draw the spore suspension 0.5mL for preparing, make liquid and spore suspension mixed in equal amounts even.Draw above-mentioned mixed liquor with micro sample adding appliance and drip on the concave slide, then frame is put in the culture dish with shallow seated groundwater, adds a cover moisturizing and is incubated in the incubator of preference temperature.
Investigation and method of counting
By medicine inspecting institute of the Ministry of Agriculture " farm-chemical indoor determination test rule " method, when the blank spore germination rate reaches 90% when above, the spore germination situation is respectively processed in inspection.Every processing repeats 3 above visuals field of random observation, many 200 of investigation spore sum, and number and spore sum sprouted in record respectively.Spore germ tube length is considered as sprouting greater than the short radius of spore.According to survey data, calculate the spore germination relative inhibition that each is processed.Probability value according to each drug concentration logarithm value and corresponding spore germination relative inhibition is done regression analysis, calculates the EC of each medicament
50, according to Wadley fungicide in mixture synergy evaluation assessment, calculate interactional ratio behind two single dose mixtures (be that SR＜0.5 is antagonism, 0.5≤SR≤1.5 are summation action, and SR＞1.5 are synergistic effect).
Result of the test sees the following form 6.
The joint toxicity measuring result of table 6. glyoxalin and Zhongshengmycin
Result of the test shows: the weight ratio of glyoxalin and Zhongshengmycin is 3: 1 o'clock, and its interaction ratio is respectively 1.91, and the bactericide interaction theory according to GiSi (1985) proposes has the notable synergistic effect.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (3)
1. a microbicide compositions contains two kinds of active components, it is characterized in that:
Active component A is selected from 4-chlorobenzyl N-(2,4-dichlorophenyl)-2 (1H-1,2,4-triazol-1-yl) thioacetamide ester (glyoxalin), and active component B is selected from Fluoxastrobin; Glyoxalin in the composition and the weight ratio of Fluoxastrobin are 3: 1 ~ 1: 10.
2. according to claim 1 described microbicide compositions is mixed with missible oil, microemulsion, aqueous emulsion, suspending agent, aqua, wetting powder, water dispersible granules or granule.
3. according to claim 1 described microbicide compositions is used for the purposes of powdery mildew that control sac fungi, imperfect fungus cause, ring rot of apple, alternaria leaf spot of apple, pear scab, anthracnose of grape.
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| CN103392719B (en) * | 2011-01-12 | 2014-11-12 | 陕西美邦农药有限公司 | Bactericidal composition containing iminazoles and methoxy acrylates |
| BR102013027977A2 (en) * | 2013-10-30 | 2015-09-15 | Rotam Agrochem Int Co Ltd | method of increasing yield by treatment with fungicidal compositions |
| CN103947649B (en) * | 2014-04-04 | 2016-01-13 | 江门市植保有限公司 | A kind of composition pesticide containing glyoxalin and kasugarnycin |
| EP3826983A1 (en) | 2018-07-23 | 2021-06-02 | Basf Se | Use of substituted 2-thiazolines as nitrification inhibitors |
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| CN101106903A (en) * | 2005-02-04 | 2008-01-16 | 三井化学株式会社 | Plant pathogen control composition and method |
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| CN1976583A (en) * | 2004-06-18 | 2007-06-06 | 拜尔农作物科学股份公司 | Soy seed dressing |
| CN101106903A (en) * | 2005-02-04 | 2008-01-16 | 三井化学株式会社 | Plant pathogen control composition and method |
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| Title |
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| 时春喜等.嘧菌酯与不同杀菌剂混配对苹果斑点落叶病菌的增效作用.《植物保护学报》.2006,第33卷(第4期),447-448. * |
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