CN103070174A - Bactericidal composition containing fluopicolide and cyflufenamid - Google Patents
Bactericidal composition containing fluopicolide and cyflufenamid Download PDFInfo
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- CN103070174A CN103070174A CN2013100227966A CN201310022796A CN103070174A CN 103070174 A CN103070174 A CN 103070174A CN 2013100227966 A CN2013100227966 A CN 2013100227966A CN 201310022796 A CN201310022796 A CN 201310022796A CN 103070174 A CN103070174 A CN 103070174A
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Abstract
The invention relates to a bactericidal composition containing fluopicolide and cyflufenamid. The bactericidal composition is a binary composition of effective components of fluopicolide and cyflufenamid, wherein the mass ratio of the fluopicolide to the cyflufenamid is (6-42): (42-6); and the bactericidal composition comprises 1-80% of the fluopicolide and the cyflufenamid in percentage by mass and the balance of pesticidally usable and acceptable auxiliary components. The bactericidal composition containing fluopicolide and cyflufenamid has dosage forms of emulsifiable oil, a suspension, wettable powder, water dispersible granules, a water emulsion and a microemulsion and is mainly used for controlling grape downy mildew, late blight, and powdery mildew of various crops.
Description
Technical field
The present invention relates to the agriculture chemical compounding technical field, particularly relate to a kind of bactericidal composition that contains fluopicolide and cyflufenamid.
Background technology
Fluopicolide is a kind of novel amide-type systemic fungicide of Beyer Co., Ltd's exploitation; Be mainly used in preventing and treating the microbial disease of Oomycete cause of disease as downy mildew of garpe and late blight etc.Fluopicolide not only has unique mode of action, with other series bactericidal agent, without cross resistance, and has good lasting effect.The chemistry of fluopicolide is called the chloro-5-of the chloro-N-{[3-of 2,6-bis-(trifluoromethyl)-2-pyridine] methyl } benzamide, its chemical structural formula is
.
Cyflufenamid is the exploitation of Japanese Cao Da company, for preventing and treating the acid amide fungicides of various crop powdery mildews, can effectively prevention and control powdery mildew.Powdery mildew to crops such as wheat class, cucumber, strawberry, rose, apple, grapes presents remarkable effect.In addition, the powdery mildew of cucumber bacterium that cyflufenamid has resistance to benzimidazole, triazole type and methoxy acrylic acid class etc. has good effect, the chemical name of cyflufenamid is (Z)-N-[α-(encircling the third methoxyimino)-2, the fluoro-6-of 3-bis-(trifluoromethyl) benzyl]-the 2-phenyl acetamide, its chemical structural formula is
.
Using chemical agent is the most effectively means of controlling plant diseases.But long-term use single chemical bactericide continuously high dose, easily cause the problems such as residual, the environmental pollution of medicament and anti-pesticide resistance fungi development.Reasonably chemical bactericide is composite or be mixed and have the expansion fungicidal spectrum, improve control efficiency, extend the optimum period for applying fertilizer, reduce dosage, reduce poisoning, reduce residual, delay Antifungal resistance and the positive characteristics such as drug-fast generation and development, bactericide compounded is one of the effective method the most addressed the above problem.Exploitation new product bactericide price is constantly soaring, and by contrast, exploitation is efficient with research, low toxicity, low-residual composite be mixed there is small investment, the lead time is short and be subject to domestic and international attention, the numerous and confused dynamics that develops that strengthens.We filter out fluopicolide and cyflufenamid and carry out compositely on the basis of lab screening and field trial, have obvious synergistic effect.And there is no at present the people about the composite bactericidal composition of Boscalid and kresoxim-methyl and application reported.
Summary of the invention
Based on above situation, the object of the invention is to provide a kind of new and effective pesticide sterilizing composite.Be mainly used in preventing and treating downy mildew of garpe, late blight and various crop powdery mildew.
Technical scheme of the present invention realizes by following measures:
A kind of bactericidal composition that contains fluopicolide and cyflufenamid, two yuan of the active ingredient fluopicolide of this bactericidal composition and cyflufenamids are composite, and all the other are auxiliary element.In wherein said Pesticidal combination, the mass ratio of active ingredient fluopicolide and cyflufenamid is 6～42: 42～6, described bactericidal composition of the present invention is through the toxicity test experimental verification, the mass ratio of fluopicolide and cyflufenamid is 6～42: 42～6 o'clock, and synergistic effect is better.
The formulations of pesticide that described bactericidal composition of the present invention can be prepared are missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion.Wherein active ingredient fluopicolide and the cyflufenamid gross mass in preparation accounts for 1%～80% of the whole quality of the pharmaceutical preparations, while wherein accounting for 15%-55%, and toxicity and the residual balance preferably that reaches, cost is also lower.
The specific embodiments of the formulations of pesticide that bactericidal composition of the present invention is mixed with is as follows:
Described bactericidal composition is cream preparation, and the mass fraction of component is: 1～40 part of fluopicolide; 1～40 part of cyflufenamid; 10～30 parts of conventional emulsifiers; 20～50 parts of conventional solvents; 1～5 part of conventional synergist.The concrete production stage of this cream preparation adds emulsifier, the synergist rear oily liquids that becomes transparent and homogeneous that stirs again for first active ingredient fluopicolide and cyflufenamid being added in solvent after dissolving fully, filling, can be made into the cream preparation of the present composition.
Described bactericidal composition is suspending agent, and the mass fraction of component is: 1～40 part of fluopicolide; 1～40 part of cyflufenamid; 5～20 parts of dispersants; 1～5 part of antifreezing agent; 0.1～2 part of thickener; 0.1～0.8 part of defoamer; 0～10 part of penetrating agent; 0.1～5 part of pH value conditioning agent; Water, surplus.The concrete production stage of this suspending agent is for first mixing other auxiliary agents, mix through high speed shear, add active ingredient fluopicolide and cyflufenamid, in ball crusher, abrading-ball is 2～3 hours, make a diameter all below 5mm, can be made into the suspending agent preparation of the present composition.
Described bactericidal composition is wetting powder, and the mass fraction of component is: 1～40 part of fluopicolide; 1～40 part of cyflufenamid; 3～10 parts of dispersants; 1～5 part of wetting agent; Filler, surplus.The concrete production stage of this wetting powder is: by above-mentioned formula, the active ingredient fluopicolide is mixed with cyflufenamid and dispersant, wetting agent and filler, uniform stirring in stirred tank, mixing after airslide disintegrating mill, can be made into the wetting powder of the present composition.
Described bactericidal composition is water dispersible granules, and the mass fraction of component is: 1～40 part of fluopicolide; 1～40 part of cyflufenamid; 3～10 parts of dispersants; 1～10 part of wetting agent; 1～5 part of disintegrant; Filler, surplus.The concrete production stage of this water dispersible granules is: by above-mentioned formula, the active ingredient fluopicolide is mixed with cyflufenamid and dispersant, wetting agent, disintegrant and filler, with micro jet, pulverize, through mediating, then add in the fluidized bed prilling dryer and carry out granulation, drying, screening by sample analysis, can be made into the water dispersible granules of the present composition.
Described bactericidal composition is aqueous emulsion, and the mass fraction of component is: 1～40 part of fluopicolide; 1～40 part of cyflufenamid; 3～30 parts of emulsifier; 5～15 parts of solvents; 2～15 parts of stabilizing agents; 1～5 part of antifreezing agent; 0.1～8 part of defoamer; 0.2～2 part of thickener; Water, surplus.The concrete production stage of this aqueous emulsion is: at first fluopicolide and cyflufenamid, solvent and emulsifier, cosolvent are added together, make to be dissolved into uniform oil phase; By part water, antifreeze, other the insecticides adjuvant such as antimicrobial mixes into uniform water; When the reactor high speed stirs, oil phase is added to water, slowly add water until reach the phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear about half an hour, form the aqueous emulsion of oil-in-water type, can be made into the aqueous emulsion of the present composition.
Described bactericidal composition is microemulsion, and the mass fraction of component is: 1～40 part of fluopicolide, 1～40 part of cyflufenamid, 10～30 parts of emulsifier, 1～8 part of antifreezing agent, 0.5～10 part of stabilizing agent, 20～50 parts of conventional solvent cosolvents.Fluopicolide and cyflufenamid are dissolved fully with cosolvent, then add other compositions such as emulsifier, antifreezing agent stabilizing agent, evenly mix, finally add water, after fully stirring, can be made into microemulsion.
Wherein above-described emulsifier is selected from calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, the alkylphenol polyoxyethylene sulfosuccinate, styrylphenol polyoxyethylene ether, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base ester, any or more than one any mixtures than forming in polyoxyethylene aliphatic alcohol ether.
Described solvent is dimethylbenzene or biodiesel, toluene, and diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, turpentine oil, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), one or more in the water equal solvent are arbitrarily than the mixture formed.
Described dispersant is selected from polycarboxylate, lignosulfonates, alkylphenol polyoxyethylene methyl ether condensate sulfate, the alkylsulfonate calcium salt, the naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol polyoxyethylene, polyoxyethylene carboxylate, aliphatic amine polyoxyethylene ether, one or more in the fatty acid glyceride APEO.
Described wetting agent is selected from lauryl sodium sulfate, calcium dodecyl benzene sulfonate, and Nekal BX, moistening bleeding agent F, alkylbenzenesulfonate polyoxyethylene triphen is phosphenylic acid salt dimly, spaonin powder, silkworm excrement, one or more in the soapberry powder.
Described disintegrant is selected from bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, one or more in sodium bicarbonate.
Described thickener is selected from xanthans, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose, Magnesiumaluminumsilicate, in polyvinyl alcohol one or more.
Described stabilizing agent is selected from sodium citrate, a kind of in resorcinol.
Described antifreezing agent is selected from ethylene glycol, propane diols, one or more in glycerine.
Described defoamer is selected from silicone oil, silicone compound, C
10-20the saturated fat acid compounds, C
8-10one or more of fatty alcohol.
Described filler is selected from kaolin, diatomite, bentonite, attapulgite, white carbon, starch, one or more in precipitated calcium carbonate.
The present invention be take the composite bactericide that fluopicolide and cyflufenamid be active ingredient and is had obvious synergistic effect, delays the drug-fast generation in key, and has reduced to become to produce cost and use cost, can be used for the improvement of resistance disease.Be mainly used in preventing and treating downy mildew of garpe, late blight and various crop powdery mildew.
Embodiment
For making technical scheme of the present invention, purpose and advantage are clearer, and the present invention describes with following specific embodiment, but the present invention is not limited to these examples.The mode that effect experiment of the present invention adopts indoor biometrics and field trial to combine, if no special instructions, the ratio of below mentioning is all ratio of quality and the number of copies.
Embodiment: fluopicolide proportioning co-toxicity experiments different from cyflufenamid.
1.1 reagent agent
The former medicine of 96 % fluopicolide, the former medicine of 95% cyflufenamid, above-mentioned former medicine provides by research and development department of extra large rel medicine company limited company.
1.2 test target
Never executed fluopicolide and cyflufenamid from Shouguang, Shandong and cucumber of the same type gathers and separates potted plantly, for the examination cucumber variety: Chang Chun Mi Ci.
1.3 test method
1.3.1 medicament preparation
First use the former medicine of acetone solution, according to the result of preliminary experiment, two appropriate former medicines are made into to 7 different proportionings, with acetone, each processing is diluted to respectively to 7 concentration gradients more stand-by, the ratio of 7 fluopicolide proportioning active ingredients different from cyflufenamid is respectively 6:42; 12:36; 18:30; 24:24; 30:18; 36:12; 42:6.
Susceptible cucumber variety Chang Chun Mi Ci cultivation, in pot for growing seedlings, is placed in to greenhouse and cultivates, and plant grows to three to four leaf after dates, gathers the blade of identical leaf age, for cultivation and the mensuration of powdery mildew of cucumber bacterium.
1.3.2 the cultivation of powdery mildew of cucumber bacterium and the preparation of spore suspension
The powdery mildew of cucumber bacterium adopts the plants method to cultivate under 20 ℃, the condition of 12h alternation of light and darkness, and every 30 d turn culture 1 time.During inoculation, with the conidium on sterile water wash-out incidence of leaf, being mixed with spore concentration is l * 10
6the suspension of individual/mL.
1.3.3 strains tested sensitivity testing
Adopt leaf dish moisturizing method to carry out toxicity test.First the blade of collection is prepared into to the leaf dish that diameter is 1.5cm, mix at random, be placed in respectively the series concentration liquid configured and soak lh, 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 blotting paper wetting in identical liquor strength, liquid on the leaf dish is blotted, the spore suspension l0L prepared is inoculated in to leaf dish central authorities, after room temperature is placed 5 min, is placed under 20 ℃, the condition of 1 2h alternation of light and darkness and cultivates, measure the onset area on the leaf dish after 10d, calculate EC
50.
On the basis of preliminary experiment, respectively single dose fluopicolide and cyflufenamid are carried out to toxicity test in order to upper method, the two EC
50value is respectively 4.82 ㎎/l and 4.73 ㎎/l
The percentage that accounts for the leaf disc area according to lesion area is divided sick level
0 grade: anosis;
1 grade: the sorus area accounts for below 5% of whole leaf area;
3 grades: the sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: the sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: the sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: the sorus area accounts for more than 50% of whole leaf area.
1.3.4 mixture toxicity test and interpretation of result
Carry out the toxicity test of mixture according to mixed ratio by single dose toxicity test method.
If contrast lethality<5%, do not proofread and correct, the contrast lethality, between 5%-20%, is proofreaied and correct by formula 2, the contrast lethality > 20%, test need be reformed.
The logarithm value of drug concentration (mg/L) of take is independent variable x, and the probability value of corrected mortality of take is dependent variable y, sets up respectively the virulence regression equation formula, adopts DPS software to calculate the EC of single dose and each proportioning mixture
50calculate co-toxicity coefficient (CTC) according to the abundant method of Sun Yun.Co-toxicity coefficient CTC, computing formula is as follows: (take fluopicolide as the standard medicament, its toxicity index is 100):
The EC of the toxicity index of kresoxim-methyl (TI)=fluopicolide
50the EC of/cyflufenamid
50* 100
The EC of the true toxicity index (ATI) of M=fluopicolide
50the LC of/M
50* 100
The TI of the TI of the theoretical toxicity index (TTI) of M=fluopicolide * P fluopicolide+cyflufenamid * P cyflufenamid
The TTI of the ATI/M of the co-toxicity coefficient of M (CTC)=M * 100.
In formula:
M is fluopicolide and the mixture of the different proportionings of cyflufenamid
The P fluopicolide is fluopicolide shared ratio in mixture
The P cyflufenamid is cyflufenamid shared ratio in mixture
2.1 toxicity test result
Table 1 fluopicolide and the cyflufenamid toxicity test to powdery mildew of cucumber
As can be seen from the table, the result of the test of different proportion proportioning shows, in the active ingredient ratio, is 6:42; 12:36; 18:30; 24:24; 30:18; 36:12; When 42:6 dilutes respectively, all show stronger synergistic effect, wherein take fluopicolide: cyflufenamid is synergistic effect the best as 24:24 the time, and its co-toxicity coefficient is 181.39.Suggestion is carried out further field control effectiveness test to suitable proportion 24:24 left and right mixture preparation, to estimate its field practical application effect.
3 field trials are prevented and treated powdery mildew of cucumber, the experimental result of late blight
3.1 field trial is prevented and treated powdery mildew of cucumber
3.1.1 test method
Test is at 4 points of Pingdu City cucumber Di，Mei community, Shandong investigation, and every some investigation 2 strains, put down in writing occurring degree by staging, and grade scale is as follows:
0 grade: anosis;
1 grade: the sorus area accounts for below 5% of whole leaf area;
3 grades: the sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: the sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: the sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: the sorus area accounts for more than 50% of whole leaf area.
3.1.2 control time and number of times
Test is investigated 4 times altogether, and radix investigation before medicine is investigated after 7 days, 7 days for the second time and medicine after medicine for the first time in 15 days.
3.1.3 drug effect computational methods
Sick leaf rate (%)=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 (%)=(disease index after disease index before 1-(blank district medicine * treatment region medicine)/(disease index before disease index after blank district medicine * treatment region medicine)) * 100.
3.1.4 poisoning investigation method
After dispenser, whether continuous 15d range estimation medicament has poisoning to crop.
3.1.5 result of the test and analysis
Each processes the effect of preventing and treating powdery mildew of cucumber.(table 2)
Each processes the effect of preventing and treating powdery mildew of cucumber table 2
As shown in Table 2 48% fluopicolide and cyflufenamid with 24:24 ratio composite bactericide for powdery mildew of cucumber control successful higher than Boscalid and kresoxim-methyl single dose, bactericidal effect increases progressively with the increase of dosage.According to the field range estimation, in the test dose scope, plant growth is normal, and the poisoning phenomenon to cucumber does not all appear in each treatment agent, illustrates that it is safe to cucumber.Advise that the bactericide different from the mechanism of action mixes use to delay the drug-fast generation of germ.
4.1 field trial control tomato late blight
4.1.1 test method
Test arrangement carries out in town Ying Shui village Zhang Qingxiang booth is jumped in the Tengchong County, Yunnan Province, it is serious that tomato late blight experimental field occurs over the years, tomato grows fine, the uniformities such as the soil types of each experimental plot, cultivation condition and water and fertilizer management, and test the last fortnight was not executed the bactericidal agent for preventing and treating disease.
Every community adopts 5 samplings, and whole blades of every strain are investigated in every some investigation 2-3 strain, with the number of the scab on every leaf, come classification to record total number of sheets, the sick number of sheets at different levels, calculate the blade incidence of disease, disease index, and contrast disease and refers to comparison, the calculating relative control effect.
Severity Scaling standard (take blade as unit)
0 grade: without scab;
1 grade: single blade has 3 of scabs;
3 grades: single blade has 4～6 of scabs;
5 grades: single blade has 7～10 of scabs;
7 grades: single blade has 11～20 of scabs, and part is intensive in flakes;
9 grades: single blade has the intensive leaf area that accounts for of scab more than 1/4th.
4.1.2 control time and number of times
Test is investigated 4 times altogether, radix investigation before medicine, after medicine 5 days for the first time, after medicine 5 days and after medicine, within 18 days, investigated for the third time for the second time.
4.1.3 drug effect computational methods
Sick leaf rate (%)=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 (%)=(disease index after disease index before 1-(blank district medicine * treatment region medicine)/(disease index before disease index after blank district medicine * treatment region medicine)) * 100.
4.1.4 poisoning investigation method
After dispenser, whether continuous 7d range estimation medicament has poisoning to crop.
4.1.5 result of the test and analysis
Each processes the effect (table 3) of preventing and treating anthracnose of tomato
As can be seen from Table 3,48% fluopicolide and cyflufenamid are better than with composite its control efficiency of anthracnose of tomato of preventing and treating of 24:24 ratio the preventive effect that fluopicolide and two kinds of single doses of cyflufenamid are processed with isoconcentration, there is good quick-acting, 48% fluopicolide and cyflufenamid have good lasting effect so that the 24:24 ratio is composite to anthracnose of tomato, can be good at controlling the generation of anthracnose.According to the field range estimation, in the test dose scope, plant growth is normal, and the poisoning phenomenon to tomato does not all appear in each treatment agent, illustrates that it is safe to tomato.
In sum, the present invention is the bactericidal composition that contains fluopicolide and cyflufenamid, powdery mildew, anthracnose of tomato etc. is all had to effect preferably, and it is to the target crop safety, with single dose, compare, bactericidal composition of the present invention has advantages of that quick-acting is good, the lasting period is long, is difficult for producing poisoning, so research and development of the present invention and popularization are of great significance social tool.
Claims (4)
1. a bactericidal composition that contains fluopicolide and cyflufenamid, it is characterized in that: two yuan of the active ingredient fluopicolide of this bactericidal composition and cyflufenamids are composite, all the other are auxiliary element, and wherein the mass ratio of active ingredient fluopicolide and cyflufenamid is 6～42: 42～6.
2. bactericidal composition according to claim 1, it is characterized in that: fluopicolide and the cyflufenamid gross weight in preparation accounts for 1%～80% of the whole quality of the pharmaceutical preparations.
3. bactericidal composition according to claim 2, it is characterized in that: fluopicolide and the cyflufenamid gross weight in preparation accounts for 15%～55% of the whole quality of the pharmaceutical preparations.
4. according to claim 1 or 2 or 3 described bactericidal compositions, it is characterized in that: the formulation of this bactericidal composition is missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion
.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104082303A (en) * | 2014-07-28 | 2014-10-08 | 陕西上格之路生物科学有限公司 | Bactericidal composition containing cyflufenamid and amides bactericide |
| CN106962346A (en) * | 2017-05-25 | 2017-07-21 | 陕西上格之路生物科学有限公司 | A kind of bactericidal composition containing cyflufenamid and Boscalid |
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| EP1552743A1 (en) * | 2002-08-07 | 2005-07-13 | Nippon Soda Co., Ltd. | Agricultural chemical composition in granular form |
| CN102365956A (en) * | 2011-11-03 | 2012-03-07 | 陕西美邦农药有限公司 | Sterilization composition containing fluopicolide and methoxyl acrylic acid ester compounds |
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2013
- 2013-01-22 CN CN2013100227966A patent/CN103070174A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1552743A1 (en) * | 2002-08-07 | 2005-07-13 | Nippon Soda Co., Ltd. | Agricultural chemical composition in granular form |
| CN102365956A (en) * | 2011-11-03 | 2012-03-07 | 陕西美邦农药有限公司 | Sterilization composition containing fluopicolide and methoxyl acrylic acid ester compounds |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104082303A (en) * | 2014-07-28 | 2014-10-08 | 陕西上格之路生物科学有限公司 | Bactericidal composition containing cyflufenamid and amides bactericide |
| CN104082303B (en) * | 2014-07-28 | 2015-11-18 | 陕西上格之路生物科学有限公司 | A kind of bactericidal composition containing cyflufenamid and acid amide fungicides |
| CN106962346A (en) * | 2017-05-25 | 2017-07-21 | 陕西上格之路生物科学有限公司 | A kind of bactericidal composition containing cyflufenamid and Boscalid |
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Application publication date: 20130501 |