CN104756988A - Trifloxystrobin and fludioxonil-containing sterilization composition - Google Patents
- ️Wed Jul 08 2015
CN104756988A - Trifloxystrobin and fludioxonil-containing sterilization composition - Google Patents
Trifloxystrobin and fludioxonil-containing sterilization composition Download PDFInfo
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- CN104756988A CN104756988A CN201510074236.4A CN201510074236A CN104756988A CN 104756988 A CN104756988 A CN 104756988A CN 201510074236 A CN201510074236 A CN 201510074236A CN 104756988 A CN104756988 A CN 104756988A Authority
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- fludioxonil
- bacterium ester
- oxime bacterium
- trifloxystrobin
- bactericidal composition Prior art date
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Abstract
The invention relates to a trifloxystrobin and fludioxonil-containing sterilization composition, active ingredients comprise compounded two components of trifloxystrobin and fludioxonil, and the mass ratio of trifloxystrobin to fludioxonil is 1 to 20: 20 to 1, the sterilization composition preparation comprises 1%-80% by mass of active ingredients of trifloxystrobin and fludioxonil, and balance of auxiliary components allowed to use and accept in pesticides, and the sterilization composition dosage form can be missible oil, a suspending agent, a wettable powder, a water agent, a water dispersion granule, an aqueous emulsion, a microemulsion, a granule and a capsule agent. The sterilization composition is mainly used for prevention and treatment of eumycetes (Ascomycetes, basidiomycetes, oomycetes and fungi imperfecti) diseases such as powdery mildew, rust disease, net blotch, downy mildew, rice blast and the like, especially used for prevention and treatment of gray mold.
Description
Technical field
The present invention relates to technical field of pesticide combination, particularly relate to a kind of bactericidal composition containing oxime bacterium ester and fludioxonil.
Background technology
Gray mold is the common and a kind of fungal disease of more difficult control of open country, protecting field crop, and belong to low temperature and high relative humidity type disease, growth of pathogenic bacteria temperature is 20 ~ 30 DEG C, is the disease high-incidence season when temperature 20 ~ 25 DEG C, humidity continue more than 90%.Gray mold, caused by the pathogen of Botrytis cinerea infects, belongs to fungal disease, and flower, really, leaf, stem all can fall ill.
Use the most effective means that chemical agent is controlling plant diseases.But long-term use single chemical bactericide continuously high dose, easily cause the problems such as the remaining of medicament, environmental pollution and resistance to pesticide resistance fungi development.Composite or the mixture of rational chemical bactericide has expansion fungicidal spectrum, improve control efficiency, extend the optimum period for applying fertilizer, reduce dosage, reduce poisoning, minimizing remains, delay Antifungal resistance and the actively feature such as drug-fast generation and development, bactericide compounded is one of the effective method the most solved the problem.Develop new product bactericide price constantly rises, and by contrast, exploitation is efficient with research, low toxicity, low-residual composite and mixture has small investment, the lead time is short and be subject to domestic and international attention, numerous and confused increasing develops dynamics.We are on the basis of lab screening and field trial, filter out oxime bacterium ester and fludioxonil carries out composite, have obvious synergistic effect.And about oxime bacterium ester and fludioxonil composite bactericidal composition and apply and there is no people at present and reported.
Oxime bacterium ester (Trifloxystrobin, No. CAS: 141517-21-7) is wide spectrum fungicides, characteristics such as having efficient, wide spectrum, protection, treat, root out, permeate, systemic activity, resistance of rainwater washing against, lasting period are long.Good activity is all had to nearly all Mycophytes (Ascomycetes, Basidiomycetes, Oomycete and Fungi Imperfecti) disease such as powdery mildew, rust, Ying's rot, net blotch, downy mildew, rice blast etc.
Fludioxonil (Fludioxonil; No. CAS: 70124-77-5; Fluoro-1, the 3-benzo dioxy-4-base of chemical name: 4-(2,2-bis-) pyrroles-3-nitrile) belong to the wide-spectrum bactericide of non-internal-absorting.Fludioxonil structure novel, by the transfer suppressing glucose phosphorylated relevant, and the mycelial growth of Antifungi, finally cause germ dead.The fludioxonil mechanism of action is unique, with existing biocide agent without cross resistance.Be mainly used in control snow rotten Fusariumsp, wheat net bunt bacterium, rhizoctonia solani etc., have special efficacy to gray mold.
Summary of the invention
Based on above situation, the object of the invention is to provide a kind of novelefficient pesticide sterilizing composite.Be mainly used in control Mycophytes (Ascomycetes, Basidiomycetes, Oomycete and Fungi Imperfecti) disease, as powdery mildew, rust, net blotch, downy mildew, rice blast etc., to be particularly useful for preventing and treating gray mold.
Technical scheme of the present invention is realized by following measures:
a kind of bactericidal composition containing oxime bacterium ester and fludioxonil, active ingredient oxime bacterium ester and the fludioxonil two yuan of this bactericidal composition are composite, and all the other are auxiliary element.In wherein said bactericidal composition, the mass ratio of active ingredient oxime bacterium ester and fludioxonil is 1 ~ 20: 20 ~ 1, described this brightly to killbacteria composition is through toxicity test experimental verification, and when the mass ratio of oxime bacterium ester and fludioxonil is 1 ~ 10: 10 ~ 1, synergistic effect is better.
Described this brightly to killthe formulations of pesticide that bacteria composition can be prepared are missible oil, suspending agent, wetting powder, aqua, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations.Wherein active ingredient oxime bacterium ester and fludioxonil gross mass in the formulation accounts for 1% ~ 80% of the whole quality of the pharmaceutical preparations, and when wherein accounting for 10% ~ 60%, toxicity reaches good balance with residual, and 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: oxime bacterium ester 1 ~ 50 part; Fludioxonil 1 ~ 50 part; Conventional emulsifier 10 ~ 30 parts; Conventional solvents 20 ~ 50 parts; Conventional synergist 1 ~ 5 part.The concrete production stage of this cream preparation be first active ingredient oxime bacterium ester and fludioxonil are added dissolve completely in solvent after add emulsifier again, synergist becomes transparent and homogeneous oily liquids after stirring, filling, namely can be made into the cream preparation of the present composition.
Described bactericidal composition is suspending agent, and the mass fraction of component is: oxime bacterium ester 1 ~ 50 part; Fludioxonil 1 ~ 50 part; Dispersant 5 ~ 20 parts; Antifreezing agent 1 ~ 5 part; Thickener 0.1 ~ 2 part; Defoamer 0.1 ~ 0.8 part; Penetrating agent 0 ~ 10 part; PH value regulator 0.1 ~ 5 part; Water, surplus.The concrete production stage of this suspending agent is for first to mix other auxiliary agents, mix through high speed shear, add active ingredient oxime bacterium ester and fludioxonil, abrading-ball 2 ~ 3 hours in ball crusher, make a diameter all at below 5mm, namely can be made into the aqueous suspension formulations of the present composition.
Described bactericidal composition is wetting powder, and the mass fraction of component is: oxime bacterium ester 1 ~ 50 part; Fludioxonil 1 ~ 50 part; Dispersant 3 ~ 10 parts; Wetting agent 1 ~ 5 part; Filler, surplus.The concrete production stage of this wetting powder is: mixed with fludioxonil and dispersant, wetting agent and filler by active ingredient oxime bacterium ester by above-mentioned formula, uniform stirring in stirred tank, mixing after airslide disintegrating mill, namely 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: oxime bacterium ester 1 ~ 50 part; Fludioxonil 1 ~ 50 part; Dispersant 3 ~ 10 parts; Wetting agent 1 ~ 10 part; Disintegrant 1 ~ 5 part; Filler, surplus.The concrete production stage of this water dispersible granules is: mixed with fludioxonil and dispersant, wetting agent, disintegrant and filler by active ingredient oxime bacterium ester by above-mentioned formula, pulverize with micro jet, through mediating, then add in fluidized-bed granulation dryer and to carry out after granulation, drying, screening, through sample analysis, namely 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: oxime bacterium ester 1 ~ 50 part; Fludioxonil 1 ~ 50 part; Emulsifier 3 ~ 30 parts; Solvent 5 ~ 15 parts; Stabilizing agent 2 ~ 15 parts; Antifreezing agent 1 ~ 5 part; Defoamer 0.1 ~ 8 part; Thickener 0.2 ~ 2 part; Water, surplus.The concrete production stage of this aqueous emulsion is: first oxime bacterium ester and fludioxonil, solvent and emulsifier, cosolvent are added together, and makes to be dissolved into uniform oil phase; By part water, antifreeze, other the insecticides adjuvant such as antimicrobial mixes uniformly aqueous phase; While high-speed stirred, oil phase is added aqueous phase in a kettle., slowly add water until reach 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, namely can be made into the aqueous emulsion of the present composition.
Described bactericidal composition is microemulsion, and the mass fraction of component is: oxime bacterium ester 1 ~ 50 part; Fludioxonil 1 ~ 50 part; Emulsifier 10 ~ 30 parts, antifreezing agent 1 ~ 8 part, stabilizing agent 0.5 ~ 10 part, Conventional solvents cosolvent 20 ~ 50 parts.Oxime bacterium ester and fludioxonil cosolvent are dissolved completely, then add other compositions such as emulsifier, antifreezing agent stabilizing agent, Homogeneous phase mixing, finally adds water, can be made into microemulsion after fully stirring.
Described bactericidal composition is granule, and the mass fraction of component is: oxime bacterium ester 1 ~ 50 part; Fludioxonil 1 ~ 50 part; Wetting dispersing agent 1 ~ 10 part; Thickener 0.1 ~ 5 part; Defoamer 0.1 ~ 5 part; Castor oil, surplus is supplied.Each components such as active ingredient oxime bacterium ester and fludioxonil, dispersant, stabilizing agent, defoamer and solvent are mixed in the ratio of filling a prescription, after putting into the grinding of sand milling still, sends into mixing in mixer for well-distribution and get product.
Described bactericidal composition is aqua, and the mass fraction of component is: oxime bacterium ester 1 ~ 50 part; Fludioxonil 1 ~ 50 part; Wetting dispersing agent 0.1 ~ 30 part; Antifreezing agent 2 ~ 8 parts; Defoamer 0.1 ~ 1 part; Thickener 0.1 ~ 3 part; Spreader-sticker 5 ~ 15 parts; Water, surplus is supplied.By active ingredient oxime bacterium ester and fludioxonil, dissolve completely with cosolvent, then add other compositions such as dispersant, antifreezing agent, defoamer, Homogeneous phase mixing, finally adds water, after fully stirring, finished product.
Described bactericidal composition is microcapsule formulations, and the mass fraction of component is: oxime bacterium ester 1 ~ 50 part; Fludioxonil 1 ~ 50 part; 5 ~ 20 parts, urea; 5 ~ 20 parts, formaldehyde; Emulsifying dispersant 5 ~ 20 parts; Antifreezing agent 1 ~ 5 part; Thickener 0.1 ~ 2 part; Defoamer 0.1 ~ 0.8 part; Water, surplus.Urea and formaldehyde (amount of substance ratio is about l:1.5 ~ 2.0) is added in the there-necked flask that agitating device is housed, regulate the pH value of solution to about 8 ~ 9 with sodium hydroxide solution, then be warming up to 70 ~ 80 DEG C, be obtained by reacting stable urea resin prepolymer.Get a certain amount of oxime bacterium ester and fludioxonil is dissolved in cyclohexane, and add emulsifying dispersant in the solution, with vigorous stirring, the O/W type stable emulsion that to be made into the aqueous solution containing emulsifying dispersant be aqueous phase.Above-mentioned urea resin prepolymer is added in emulsion, adjust ph, polymerization reaction take place under acid catalysed conditions, oil phase substance is wrapped, form microcapsule granule.Slow intensification, solidification, temperature controls at 40 ~ 50 DEG C, hardening time 1h.Select to add appropriate auxiliary agent, stable microcapsules.
Wherein above-described emulsifier is selected from calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, alkylphenol polyoxyethylene sulfosuccinate, styrylphenol polyoxyethylene ether, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base ester, any one in polyoxyethylene aliphatic alcohol ether or more than one any mixtures than composition.
Described solvent is dimethylbenzene or biodiesel, toluene, diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, turpentine-based vegetable oil code name is ND-45, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), one or more in water equal solvent are arbitrarily than the mixture of composition.
It is LG-3, GY-D1252, GY-D1256, SNWGF-01 that described dispersant is selected from polycarboxylate code name, lignosulfonates code name is 201107,201108, alkylphenol polyoxyethylene methyl ether condensate sulfate, alkylsulfonate calcium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol polyoxyethylene, polyoxyethylene carboxylate, aliphatic amine polyoxyethylene ether, one or more in fatty acid glyceride APEO.
Described wetting agent is selected from lauryl sodium sulfate, calcium dodecyl benzene sulfonate, Nekal BX, moistening bleeding agent F, alkylbenzenesulfonate polyoxyethylene triphen phosphenylic acid salt dimly, spaonin powder, silkworm excrement, one or more in 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, the one 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 10-20saturated 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 composite bactericide that the present invention is active ingredient with oxime bacterium ester and fludioxonil has obvious synergistic effect, delay the drug-fast generation in key, and reduce into product cost and use cost, be mainly used in control Mycophytes (Ascomycetes, Basidiomycetes, Oomycete and Fungi Imperfecti) disease, as powdery mildew, rust, net blotch, downy mildew, rice blast etc., to be particularly useful for preventing and treating gray mold.
Embodiment
For making technical scheme of the present invention, object and advantage are clearly understood, the following specific embodiment of the present invention is described, but the present invention is not limited to these examples.The mode that effect experimental of the present invention adopts indoor biometrics and field trial to combine, if no special instructions, the ratio below mentioned is all ratio of quality and the number of copies.
Embodiment: oxime bacterium ester and fludioxonil different ratio co-toxicity are tested.
1.1 reagent agent
The former medicine of 95% fludioxonil, the former medicine of 95% oxime bacterium ester, above-mentioned former medicine provides by research and development department of extra large rel medicine company limited company.
1.2 test targets
Never executed oxime bacterium ester and fludioxonil and cucumber of the same type to gather potted plantly be separated, for examination cucumber variety: Chang Chun Mi Ci from Shouguang, Shandong.
1.3 test method
1.3.1 medicament preparation
First use the former medicine of acetone solution, appropriate two former medicines are made into several different ratio by the result according to preliminary experiment, then it is stand-by with acetone, each process to be diluted to several concentration gradients respectively.
By susceptible cucumber variety Chang Chun Mi Ci cultivation in pot for growing seedlings, be placed in greenhouse and cultivate, plant grows to three to four leaf after dates, gathers the blade of identical leaf age, for cultivation and the mensuration of gray mold of cucumber germ.
1.3.2 the cultivation of gray mold of cucumber germ and the preparation of spore suspension
Gray mold of cucumber germ adopt plants method 20 DEG C, cultivate under the condition of 12h alternation of light and darkness, every 30 d turn culture 1 time.With the conidium on sterile water wash-out incidence of leaf during inoculation, being mixed with spore concentration is l × 10 6the suspension of individual/mL.
1.3.3 strains tested sensitivity testing
Leaf dish moisturizing method is adopted to carry out toxicity test.First the blade of collection is prepared into the leaf dish that diameter is 1.5cm, random mixing, be placed in the series concentration liquid configured respectively and soak lh, each concentration 50 leaf dishes, test with the process of not adding medicine as blank, after immersion terminates, leaf faces up and puts on the blotting paper that identical liquor strength is wetting, liquid on leaf dish is blotted, the spore suspension l0L prepared is inoculated in leaf dish central authorities, after room temperature places 5 min, is placed in 20 DEG C, cultivates under the condition of 1 2h alternation of light and darkness, measure the onset area on leaf dish after 10d, calculate EC 50.
The percentage accounting for leaf disc area according to lesion area divides disease level
0 grade: anosis;
1 grade: sorus area accounts for less than 5% of whole leaf area;
3 grades: sorus area accounts for below the 6%-10% of whole leaf area;
5 grades: sorus area accounts for below the 11%-20% of whole leaf area;
7 grades: sorus area accounts for below the 21%-50% of whole leaf area;
9 grades: 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%, does not correct, contrast lethality, between 5%-20%, corrects by formula 2, and contrast lethality >20%, test need be reformed.
Be independent variable x with the logarithm value of drug concentration (mg/L), with the probability value of corrected mortality for dependent variable y, set up virulence regression equation formula respectively, adopt DPS software to calculate the EC of single dose and each proportioning mixture 50co-toxicity coefficient (CTC) is calculated according to the abundant method of Sun Yun.Co-toxicity coefficient CTC, computing formula is as follows: (with oxime bacterium ester for standard agent, its toxicity index is 100):
The EC of toxicity index (the TI)=oxime bacterium ester of fludioxonil 50the EC of/fludioxonil 50× 100
The EC of true toxicity index (the ATI)=oxime bacterium ester of M 50the EC of/M 50× 100
TI × P fludioxonil of TI × P oxime bacterium ester+fludioxonil of theoretical toxicity index (the TTI)=oxime bacterium ester of M
TTI × 100 of the ATI/M of co-toxicity coefficient (the CTC)=M of M
In formula:
M is the mixture of oxime bacterium ester and fludioxonil different ratio
P oxime bacterium ester is the ratio of oxime bacterium ester shared by mixture
P fludioxonil is the ratio of fludioxonil shared by mixture.
2.1 toxicity test results
table 1fludioxonil and oxime bacterium ester are to the toxicity test of gray mold of cucumber
From in tablecan find out, the result of the test of different proportion proportioning shows, dilute respectively in active ingredient ratio and all show stronger synergistic effect, advise carrying out further field control effectiveness test to suitable proportion about 1:9 ~ 9:1 mixture preparation, to evaluate its field practical application effect.
3, the experimental result of field trial control gray mold of cucumber
3.1 test method
Test dispenser twice altogether, check plot spray equivalent clear water.When making up a prescription, after first medicament fully being dissolved with a small amount of water, then add suitable quantity of water carry out complete stool spraying process, even spraying.All adopt power driven sprayer during spray medicine, operating pressure is 0.3 ~ 0.4MPa, shower nozzle aperture 1.3mm.Community spouting liquid is 40 ~ 50kg/ mu, continuous dispenser twice, 10 days intervals, liquid is sprayed application to crop complete stool uniformly.
3.2 investigation method
Experimental field be located at Shouguang, Shandong, select the plastic tent cucumber of natural occurrence for experiment field, soil fertility is medium, and irrigation and drainage are convenient.Adopt bilinear sampling method, 5 points are got in every community, look into 5 caves at often, and during investigation, 2 blades in the fixing middle part of every strain carry out fixed point inspection.
Carry out classification according to gray mold of cucumber grade scale, record total strain number, diseased plant number, severity, calculate diseased plant rate, disease index and preventive effect.
Gray mold of cucumber grade scale is
0 grade: blade is without scab;
1 grade: lesion area accounts for less than 5% of whole leaf area;
3 grades: lesion area accounts for 6% ~ 10% of whole leaf area;
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 more than 50% of whole leaf area.
Test is investigated 3 times altogether, i.e. disease index investigation before medicine, preventive effect investigation in 5 days after the 1st medicine, 5 days and preventive effect investigation in 18 days after 2 medicines.
3.3 poisoning investigation
Whether after dispenser, continuous 7d estimates medicament has poisoning to crop.
3.4 drug effect computational methods
Sick leaf rate (%)=sick number of sheets/investigate the total number of sheets × 100
Disease index=∑ (the sick number of sheets × relative level numerical value at different levels)/(investigating the total number of sheets × 9) × 100
Control efficiency (%)=(before 1-(blank district medicine after disease index × treatment region medicine disease index)/(after blank district medicine before disease index × treatment region medicine disease index)) × 100.
3.5 field control effectiveness test result of the tests
The experiment effect of table 2 each test medicine control gray mold of cucumber
As shown in Table 2, it is remarkable that 20% oxime bacterium ester and fludioxonil mixture combine the effectiveness comparison preventing and treating gray mold of cucumber, the Be very effective of complex preparation is better than two kinds of single doses, not only significantly improve the control efficiency for gray mold, and extend its holding effect further, and produce without poisoning under the poisoning observation of continuous 7 days.
In sum, the present invention contains the bactericidal composition of oxime bacterium ester and fludioxonil, has good control efficiency to gray mold, and it is to Target crops safety.Complex preparation not only increases preventive effect, and expands fungicidal spectrum, widens the scope of application, reduces costs, and plays the double effect controlled of a medicine, alleviate manpower and materials to multiple diseases, improves productivity effect.So the invention of this complex preparation is of great significance social tool with popularization.
Claims (4)
1. one kind contains the bactericidal composition of oxime bacterium ester and fludioxonil, it is characterized in that: the active ingredient of this bactericidal composition is oxime bacterium ester and fludioxonil binary built, all the other are auxiliary element, and wherein the mass ratio of active ingredient oxime bacterium ester and fludioxonil is 1 ~ 20: 20 ~ 1.
2. bactericidal composition according to claim 1, is characterized in that: oxime bacterium ester and fludioxonil gross weight in the formulation accounts for 1% ~ 80% of the whole quality of the pharmaceutical preparations.
3. bactericidal composition according to claim 2, is characterized in that: oxime bacterium ester and fludioxonil gross weight in the formulation accounts for 5% ~ 60% of the whole quality of the pharmaceutical preparations.
4. the bactericidal composition according to claim 1 or 2 or 3, is characterized in that: the formulation of this bactericidal composition is missible oil, suspending agent, aqua, wetting powder, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations .
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CN107094766A (en) * | 2017-05-11 | 2017-08-29 | 深圳诺普信农化股份有限公司 | A kind of seed treatment |
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CN1871909A (en) * | 1996-12-13 | 2006-12-06 | 拜尔公开股份有限公司 | Plant protection agents |
US20140200140A1 (en) * | 2013-12-30 | 2014-07-17 | Sumitomo Chemical Company, Limited | Method of controlling pests |
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CN1240332A (en) * | 1996-12-13 | 2000-01-05 | 诺瓦提斯公司 | Plant protection agents |
CN1871909A (en) * | 1996-12-13 | 2006-12-06 | 拜尔公开股份有限公司 | Plant protection agents |
US20140200140A1 (en) * | 2013-12-30 | 2014-07-17 | Sumitomo Chemical Company, Limited | Method of controlling pests |
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