CN103202301A - Bactericidal composition containing pyraoxystrobin and mepanipyrim - Google Patents

Bactericidal composition containing pyraoxystrobin and mepanipyrim Download PDF

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CN103202301A
CN103202301A CN2012104324123A CN201210432412A CN103202301A CN 103202301 A CN103202301 A CN 103202301A CN 2012104324123 A CN2012104324123 A CN 2012104324123A CN 201210432412 A CN201210432412 A CN 201210432412A CN 103202301 A CN103202301 A CN 103202301A
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mepanipyrim
bactericidal composition
azoles bacterium
bacterium ester
cucumber
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葛大鹏
陈鹏
韩先正
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Hailir Pesticides and Chemicals Group Co Ltd
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Hailir Pesticides and Chemicals Group Co Ltd
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Abstract

The invention relates to a bactericidal composition containing pyraoxystrobin and mepanipyrim. The bactericidal composition is a binary complex of the effective components pyraoxystrobin and mepanipyrim, with the balance being auxiliary components. A mass ratio of pyraoxystrobin to mepanipyrim is 1-80: 80-1; the total mass of the effective components pyraoxystrobin and mepanipyrim in the composition accounts for 1 to 80% of the total mass of the composition. The pesticide formulation of the bactericidal composition provided by the invention can be a missible oil, a suspending agent, a wettable powder, a water dispersible granule, an emulsion in water and a microemulsion. The bactericidal composition is mainly used for preventing and controlling spot disease, powdery mildew and various botrytis and has excellent preventing and controlling effects on cucumber downy mildew, grape downy mildew, tomato late blight and cucumber anthracnose.

Description

A kind of bactericidal composition that contains azoles bacterium ester and mepanipyrim
Technical field
The present invention relates to the agriculture chemical compounding technical field, particularly relate to a kind of bactericidal composition that contains azoles bacterium ester and mepanipyrim.
Background technology
Azoles bacterium ester is the novel methoxy acrylic bactericide that Shenyang Chemical Engineering Inst develops.Azoles bacterium ester fungicidal spectrum is wide, bactericidal activity is high, and relatively more outstanding stripped bactericidal activity is arranged, and cucumber downy mildew, downy mildew of garpe, tomato late blight, cucumber anthracnose, powdery mildew of cucumber are had excellent control efficiency.Azoles bacterium esterification formal name used at school is called (E)-2-(2-((3-(4-chlorphenyl)-1-methyl isophthalic acid H-pyrazoles-5-oxygen base) methyl) phenyl)-3-methoxy-methyl acrylate.
Unique mechanism of action that has mepanipyrim namely suppresses the secretion of pathogen protein, comprises and reduces some hydrolase levels, and these enzymes advance the people host plant and cause that the necrosis of host tissue is relevant with pathogen by inference.No cross resistances such as the same triazole type of methyl mepanipyrim, dithiocarbamate, benzimidazole and the mould prestige of second, so it all has excellent activity to sensitivity or resistance pathogen.Be mainly used in preventing and treating star disease, powdery mildew and various gray mold, suitable crop reward plant, vegetables, fruit tree, grape etc.To crop safety crop safety, no poisoning.Mepanipyrim chemistry N-(4-methyl-6-third-alkynyl pyrimidine-2-base) aniline by name, its chemical structural formula is
Figure 692455DEST_PATH_IMAGE001
Using chemical agent is the most effectively means of controlling plant diseases.But long-term use single chemical bactericide continuously high dose, cause problems such as residual, the environmental pollution of medicament and anti-pesticide resistance fungi development easily.Reasonably chemical bactericide is composite or be mixed and have the expansion fungicidal spectrum, improve control efficiency, prolong the optimum period for applying fertilizer, reduce dosage, reduce poisoning, reduce residual, delay fungi drug resistance and positive characteristics such as drug-fast generation and development, bactericide compounded is one of the effective method the most that addresses 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 have small investment, the lead time is short and be subjected to domestic and international attention, strengthens the development dynamics one after another.We filter out azoles bacterium ester and mepanipyrim and carry out compositely on the basis of lab screening and field trial, have obvious synergistic effect.And about the composite bactericidal composition of azoles bacterium ester and mepanipyrim and use that still nobody reported at present.
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 star disease, powdery mildew and various gray mold, cucumber downy mildew, downy mildew of garpe, tomato late blight, cucumber anthracnose are also had excellent control efficiency.
Technical scheme of the present invention realizes by following measure:
A kind of bactericidal composition that contains azoles bacterium ester and mepanipyrim, active ingredient azoles bacterium ester and two yuan of the mepanipyrims of this bactericidal composition are composite, and all the other are auxiliary element.The mass ratio of active ingredient azoles bacterium ester and mepanipyrim is 1~80: 80~1 in the wherein said Pesticidal combination, and described bactericidal composition of the present invention is through the toxicity test experimental verification, and the mass ratio of azoles bacterium ester and mepanipyrim is 1~40: 40~1 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 azoles bacterium ester and the mepanipyrim gross mass in preparation accounts for 1%~80% of the whole quality of the pharmaceutical preparations, when wherein accounting for 5%-50%, 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: azoles bacterium ester 1~80; 1~80 part of mepanipyrim; 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 the oily liquids that becomes transparent and homogeneous after emulsifier, synergist stir after the dissolving fully again for earlier active ingredient azoles bacterium ester and mepanipyrim being added in the solvent, can 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: 1~80 part of azoles bacterium ester; 1~80 part of mepanipyrim; 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 earlier other auxiliary agents to be mixed, mix through high speed shear, add active ingredient azoles bacterium ester and mepanipyrim, abrading-ball is 2~3 hours in ball crusher, make a diameter all below 5mm, namely 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: 1~80 part of azoles bacterium ester; 1~80 part of mepanipyrim; 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 prescription active ingredient azoles bacterium ester is mixed with mepanipyrim and dispersant, wetting agent and filler, in stirred tank, evenly stir, behind airslide disintegrating mill, mixing, 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: 1~80 part of azoles bacterium ester; 1~80 part of mepanipyrim; 3~10 parts of dispersants; 1~10 part of wetting agent; 1~5 part of disintegrant; The filler surplus.
The concrete production stage of this water dispersible granules is: by above-mentioned prescription active ingredient azoles bacterium ester and mepanipyrim and dispersant, wetting agent, disintegrant and filler are mixed, pulverize with micro jet, through mediating, add then and carry out granulation, drying, screening in the fluidized bed prilling dryer by 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: 1~80 part of azoles bacterium ester; 1~80 part of mepanipyrim; 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 azoles bacterium ester and mepanipyrim, solvent and emulsifier, cosolvent are added together, make and be dissolved into uniform oil phase; With part water, antifreeze, other insecticides adjuvant such as antimicrobial mixes into uniform water; When the reactor high speed stirs, oil phase is added water, slowly add water until reaching the phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear half an hour approximately, form the aqueous emulsion of oil-in-water type, namely can be made into the aqueous emulsion of the present composition.
Wherein above-described emulsifier is selected from calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, the alkylphenol polyoxyethylene sulfosuccinate, styryl phenol APEO, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base ester, any or more than one any mixtures than composition in the 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 of forming.
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 the sodium bicarbonate.
Described thickener is selected from xanthans, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose, Magnesiumaluminumsilicate, in the polyvinyl alcohol one or more.
Described stabilizing agent is selected from sodium citrate, a kind of in the resorcinol.
Described antifreezing agent is selected from ethylene glycol, propane diols, one or more in the 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 the precipitated calcium carbonate.
The present invention is that the composite bactericide of active ingredient has obvious synergistic effect with azoles bacterium ester and mepanipyrim, 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 star disease, powdery mildew and various gray mold, cucumber downy mildew, downy mildew of garpe, tomato late blight, cucumber anthracnose are also had excellent control efficiency.
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 all is ratio of quality and the number of copies.
Embodiment: the different proportioning co-toxicity experiments with mepanipyrim of azoles bacterium ester.
1.1 reagent agent
The former medicine of 95.5% azoles bacterium ester, the former medicine of 97% mepanipyrim, above-mentioned former medicine provides by research and development department of extra large rel medicine company limited company.
1.2 test target
Never executed azoles bacterium ester and mepanipyrim and cucumber of the same type from Shouguang, Shandong and gather potted plantly and separate, for the examination cucumber variety: Chang Chun Mi Ci.
1.3 test method
1.3.1 medicament preparation
Earlier with the former medicine of acetone solution, according to the result of preliminary experiment two an amount of former medicines are made into 5 different proportionings, it is stand-by with acetone each processing to be diluted to 5 concentration gradients respectively again, and the ratio of 5 different proportioning active ingredients with mepanipyrim of azoles bacterium ester is respectively 12:28; 14:26; 16:24; 18:22; 20:20.
In pot for growing seedlings, place the greenhouse to cultivate susceptible cucumber variety Chang Chun Mi Ci cultivation, plant grows to three to four leaf after dates, gathers the blade of identical leaf age, is used for cultivation and the mensuration of powdery mildew of cucumber bacterium.
1.3.2 the cultivation of powdery mildew of cucumber bacterium and the preparation of spore suspension
The powdery mildew of cucumber bacterium adopts live body plant method to cultivate under 20 ℃, the condition of 12h alternation of light and darkness, and per 30 d change to be commissioned to train and support 1 time.With the conidium on the sterile water wash-out incidence of leaf, being mixed with spore concentration is l * 10 during inoculation 6The suspension of individual/mL.
1.3.3 strains tested sensitivity testing
Adopt the leaf dish method of preserving moisture to carry out toxicity test.Earlier the blade of gathering is prepared into the leaf dish that diameter is 1.5cm, mixing at random, place the series concentration soup that configures to soak lh respectively, 50 leaf dishes of each concentration, test is with the blank that is treated to of adding medicine not, after soaking end, leaf faces up and puts on the wetting blotting paper of identical liquor strength, soup on the leaf dish is blotted, the spore suspension l0L for preparing is inoculated in leaf dish central authorities, after room temperature is placed 5 min, places under 20 ℃, the condition of 1 2h alternation of light and darkness and cultivate, measure the onset area on the leaf dish behind the 10d, calculate EC 50
On the basis of preliminary experiment, respectively single agent azoles bacterium ester and mepanipyrim are carried out toxicity test, the two EC in order to last method 50Value is respectively 5.42 ㎎/l and 7.34 ㎎/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 whole below 5% of 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 whole more than 50% of leaf area;
1.3.4 mixture toxicity test and interpretation of result
Carry out the toxicity test of mixture according to mixed ratio with single agent toxicity test method.
If contrast lethality<5% is not proofreaied and correct, the contrast lethality by formula 2 is proofreaied and correct between 5%-20%, the contrast lethality〉20%, test need be reformed.
Logarithm value with drug concentration (mg/L) is independent variable x, is dependent variable y with the probability value of corrected mortality, sets up the virulence regression equation formula respectively, adopts DPS software to calculate the LC of single agent 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: (be standard medicament with azoles bacterium ester, its toxicity index is 100):
The LC of the toxicity index of mepanipyrim (TI)=azoles bacterium ester 50The LC of/mepanipyrim 50* 100
The LC of the true toxicity index (ATI) of M=azoles bacterium ester 50The LC of/M 50* 100
TI * P the mepanipyrim of the TI of the theoretical toxicity index (TTI) of M=azoles bacterium ester * P azoles bacterium ester+mepanipyrim
TTI * 100 of the ATI/M of the co-toxicity coefficient of M (CTC)=M
In the formula:
M is azoles bacterium ester and the mixture of the different proportionings of mepanipyrim
P azoles bacterium ester is azoles bacterium ester shared ratio in mixture
The P mepanipyrim is mepanipyrim shared ratio in mixture
2.1 toxicity test result
Table 1 azoles bacterium ester and mepanipyrim are to the toxicity test of powdery mildew of cucumber
Handle title Proportioning Virulence regression equation (Y=a+bX) The correlation coefficient r value LC 50(mg/L) Co-toxicity coefficient (CTC)
Azoles bacterium ester _____ Y=2.8994X+2.8719 0.9894 5.42 _______
Mepanipyrim _____ Y=2.6664X+2.6917 0.9882 7.34 _______
Azoles bacterium ester: mepanipyrim 12:28 Y=2.7422X+3.1826 0.9892 4.60 144.19
Azoles bacterium ester: mepanipyrim 14:26 Y=2.3354X+3.5493 0.9914 4.18 156.34
Azoles bacterium ester: mepanipyrim 16:24 Y=2.6462X+3.4809 0.9891 3.75 171.41
Azoles bacterium ester: mepanipyrim 18:22 Y=2.7323X+3.3820 0.9884 3.91 162.56
Azoles bacterium ester: mepanipyrim 20:20 Y=2.9733X+3.1347 0.9901 4.24 146.92
As can be seen from the table, the result of the test of different proportion proportioning shows, is 12:28 in the active ingredient ratio; 14:26; 16:24; 18:22; When 20:20 dilutes respectively, all show stronger synergistic effect, synergistic effect the best when wherein being 16:24 with azoles bacterium ester and mepanipyrim, its co-toxicity coefficient is 171.41.Suggestion is carried out further field control effectiveness test to suitable proportion 16:24 left and right sides mixture preparation, to estimate its field practical application effect.
3 field trials are prevented and treated powdery mildew of cucumber, the experimental result of gray mold.
3.1 field trial is prevented and treated powdery mildew of cucumber.
3.1.1 test method
Test is on Shandong Pingdu City cucumber ground, and 4 points of every residential quarter investigation are investigated 2 strains at every, put down in writing occurring degree with staging, and grade scale is as follows:
0 grade: anosis;
1 grade: the sorus area accounts for whole below 5% of 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 whole more than 50% of leaf area;
3.1.2 control time and number of times
Test is investigated 4 times altogether, and radix investigation before the medicine was investigated behind 3 days, 7 days and the medicine behind the medicine in 15 days.
3.1.3 drug effect computational methods
Sick leaf rate (the %)=sick number of sheets/investigate total number of sheets * 100
Disease index=∑ (the sick numbers of sheets at different levels * relative level numerical value)/(investigating total number of sheets * 9) * 100
Control efficiency (%)=(disease index behind disease index before the 1-(blank district medicine * treatment region medicine)/(disease index before disease index behind the blank district medicine * treatment region medicine)) * 100.
3.1.4 poisoning investigation method
Whether continuous 15d range estimation medicament has poisoning to crop after the dispenser.
3.1.5 result of the test and analysis
Each handles the effect of preventing and treating powdery mildew of cucumber.(table 2)
Each handles the effect of preventing and treating powdery mildew of cucumber table 2
Figure DEST_PATH_GDA0000274445402
40% azoles bacterium ester mepanipyrim SC(16:24 as shown in Table 2) composite bactericide is controlled effect apparently higher than azoles bacterium ester and the agent of mepanipyrim list for powdery mildew of cucumber, and 15 days bactericidal effect is respectively 91.12,92.43 behind medicine, and 93.54.Bactericidal effect increases progressively with the increase of dosage.According to field range estimation, in the test dose scope, plant growth is normal, and each is handled medicament and poisoning phenomenon to cucumber all do not occur, illustrates that it is safe to cucumber.Advise that the bactericide different with the mechanism of action mixes use to delay the drug-fast generation of germ.
4.1 field trial control gray mold of cucumber.
4.1.1 test method
Test is on Shandong Pingdu City cucumber ground, and 4 points of every residential quarter investigation are investigated 2 strains at every, put down in writing occurring degree with staging, and grade scale is as follows:
0 grade: anosis;
1 grade: the sorus area accounts for whole below 5% of 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 whole more than 50% of leaf area.
4.1.2 control time and number of times
Test is investigated 4 times altogether, radix investigation before the medicine, for the first time behind the medicine 7 days, investigated in 14 days and 21 days behind the medicine for the second time.
4.1.3 drug effect computational methods
Sick leaf rate (the %)=sick number of sheets/investigate total number of sheets * 100
Disease index=∑ (the sick numbers of sheets at different levels * relative level numerical value)/(investigating total number of sheets * 9) * 100
Control efficiency (%)=(disease index behind disease index before the 1-(blank district medicine * treatment region medicine)/(disease index before disease index behind the blank district medicine * treatment region medicine)) * 100.
4.1.4 poisoning investigation method
Observe continuously after the dispenser, whether the range estimation medicament has poisoning to crop.
4.1.5 result of the test and analysis
Each handles the effect of control gray mold of cucumber.(table 3)
Each handles the effect of control gray mold of cucumber table 3
Figure DEST_PATH_GDA0000309585571
As can be seen from Table 3,40% azoles bacterium ester mepanipyrim is very remarkable with the effect of 16:24 proportioning control gray mold of cucumber.The effect of complex preparation is significantly higher than single agent, its instant effect, and the lasting period is also better, is the desirable medicament of preventing and treating gray mold, and to cucumber safety, can effectively delays the drug-fast generation of germ.
In sum, the present invention contains the bactericidal composition of azoles bacterium ester and mepanipyrim, powdery mildew of cucumber and gray mold are had good control efficiency, and it is to the target crop safety.。Complex preparation has not only improved preventive effect, and has enlarged fungicidal spectrum, so this compounded combination has very important meaning in production practices.

Claims (5)

1. bactericidal composition that contains azoles bacterium ester and mepanipyrim, it is characterized in that: the active ingredient of this bactericidal composition is azoles bacterium ester and mepanipyrim binary built, and all the other are auxiliary element, and wherein the mass ratio of azoles bacterium ester and mepanipyrim is 1~80: 80~1.
2. bactericidal composition according to claim 1, it is characterized in that: the quality optimization ratio of azoles bacterium ester and mepanipyrim is preferably 1~40: 40~1.
3. bactericidal composition according to claim 1, it is characterized in that: azoles bacterium ester and the mepanipyrim gross mass in preparation accounts for 1%~80% of whole preparation gross mass.
4. bactericidal composition according to claim 3, it is characterized in that: azoles bacterium ester and the mepanipyrim gross mass in preparation accounts for 5%~50% of whole preparation gross mass.
5. according to claim 1 or 2 or 3 or 4 described bactericidal compositions, it is characterized in that: the formulations of pesticide that bactericidal composition of the present invention can be made are missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion.
CN2012104324123A 2012-11-02 2012-11-02 Bactericidal composition containing pyraoxystrobin and mepanipyrim Pending CN103202301A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101406191A (en) * 2007-10-09 2009-04-15 中国中化集团公司 Fungicidal compositions
CN100503576C (en) * 2004-02-20 2009-06-24 沈阳化工研究院 Substituted azole compounds, preparation and application thereof
WO2011017351A2 (en) * 2009-08-05 2011-02-10 E. I. Du Pont De Nemours And Company Mixtures of mesoionic pesticides

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100503576C (en) * 2004-02-20 2009-06-24 沈阳化工研究院 Substituted azole compounds, preparation and application thereof
CN101406191A (en) * 2007-10-09 2009-04-15 中国中化集团公司 Fungicidal compositions
WO2011017351A2 (en) * 2009-08-05 2011-02-10 E. I. Du Pont De Nemours And Company Mixtures of mesoionic pesticides

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