CN103004860A - Sterilization composition containing simeconazole and bupirimate - Google Patents
Sterilization composition containing simeconazole and bupirimate Download PDFInfo
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- CN103004860A CN103004860A CN2012104807576A CN201210480757A CN103004860A CN 103004860 A CN103004860 A CN 103004860A CN 2012104807576 A CN2012104807576 A CN 2012104807576A CN 201210480757 A CN201210480757 A CN 201210480757A CN 103004860 A CN103004860 A CN 103004860A
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Abstract
The invention relates to a sterilization composition containing simeconazole and bupirimate, and the effective ingredients are the simeconazole and the bupirimate, wherein the mass ratio of the simeconazole to the bupirimate is (1-80):(80-1), and in the preparation, the total mass of the effective ingredients ( the simeconazole and the bupirimate) is 1%-80% of the total mass of the whole preparation, and the balance is auxiliary components allowed to be used and acceptable in a pesticide. A pesticide formulation which can be prepared by using the sterilization composition can be milk oil, a suspending agent, wettable powder, a water dispersible granule, emulsion in water and microemulsion. The sterilization composition is mainly used for preventing and curing various powdery mildew, scab, rust diseases, damping off and banded sclerotial blight.
Description
Technical field
The present invention relates to the agriculture chemical compounding technical field, be specifically related to a kind of bactericidal composition that contains simeconazoles and bupirimate.
Background technology
Simeconazoles system Japan three common companies (now are three common A, company) in siliceous three series bactericidal agent of exploitation in 1991, it is the deep and remote pure biosynthesis inhibitor of a kind of ergot, destroy and stop the biosynthesis of the cell membrane important composition composition ergosterol of germ, cause cell membrane not form, make germ dead.Because absorption in having well, therefore can be promptly by plant absorbing, and in conducted inside; Have good protection and therapeutic activity.Can effectively prevent and treat disease due to numerous sac fungis, basidiomycetes and the imperfect fungus, especially all kinds of powdery mildews, scab, rust, damping off, banded sclerotial blight etc. be had excellent preventive effect.The chemistry of simeconazoles is called (R, S)-2-(4 fluorophenyl)-1-(1H-1,2,4-triazol-1-yl)-3-trimethyl silicane propane-2-alcohol, and its chemical structural formula is
Bupirimate belongs to the miazines systemic fungicide, has protection and therapeutic action.Can be absorbed rapidly by plant roots, stem, leaf, and in plant corpus, run to each position, so resistance of rainwater washing against.Have that consumption is few, efficient, low toxicity, powdery mildew had the advantage such as special efficacy, therefore replaced the agricultural chemicals such as the phonetic phenol of second and dimethirimol.Be suitable for ornamental plants, the field crops such as fruit tree, vegetables, flowers.The various powdery mildews of controlling object are such as apple, grape, cucumber, strawberry, rose, sweet Lay powdery mildew.The bupirimate chemistry is by name: 5-butyl-2-ethylamino-6-methylpyrimidine-4-base dimethylamino sulfuric ester, 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, cause easily 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, prolong 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 the most one of the effective method 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 subject to domestic and international attention, the numerous and confused dynamics that develops that strengthens.We filter out simeconazoles and bupirimate and carry out compositely on the basis of lab screening and field trial, have obvious synergistic effect.And about the composite bactericidal composition of simeconazoles and bupirimate and use and there is no at present the people and 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 all kinds of powdery mildews, scab, rust, damping off, banded sclerotial blight.
Technical scheme of the present invention realizes by following measures:
A kind of bactericidal composition that contains simeconazoles and bupirimate, two yuan of the active ingredient simeconazoles of this bactericidal composition and bupirimates are composite, and all the other are auxiliary element.The mass ratio of active ingredient simeconazoles and bupirimate is 1～80: 80～1 in the wherein said Pesticidal combination, described bactericidal composition of the present invention is through the toxicity test experimental verification, the mass ratio of simeconazoles and bupirimate 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 simeconazoles and the bupirimate 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 preferably balance 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: simeconazoles 1～80; 1～80 part of bupirimate; 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 after dissolving fully in the solvent again for first active ingredient simeconazoles and bupirimate being added, 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 simeconazoles; 1～80 part of bupirimate; 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 mixing other auxiliary agents first, mix through high speed shear, add active ingredient simeconazoles and bupirimate, 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 simeconazoles; 1～80 part of bupirimate; 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 the active ingredient simeconazoles is mixed with bupirimate and dispersant, wetting agent and filler, uniform stirring in stirred tank, 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 simeconazoles; 1～80 part of bupirimate; 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 simeconazoles and bupirimate and dispersant, wetting agent, disintegrant and filler are mixed, pulverize with micro jet, through mediating, then add 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 simeconazoles; 1～80 part of bupirimate; 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 simeconazoles and bupirimate, solvent and emulsifier, cosolvent are added together, make and be dissolved into uniform oil phase; With part water, antifreeze, other the insecticides adjuvant such as antimicrobial mixes into uniform water; When the reactor high speed stirs, oil phase is added water, slowly add water until reach the phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear approximately 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: 1～80 part of simeconazoles, 1～80 part of bupirimate, 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.Simeconazoles and bupirimate are dissolved fully with cosolvent, add again other compositions such as emulsifier, antifreezing agent stabilizing agent, evenly mix, add at last entry, can be made into microemulsion after fully stirring.
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 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 that forms.
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 composite bactericide of the present invention take simeconazoles and bupirimate as active ingredient has obvious synergistic effect, delays the drug-fast generation in key, and 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 all kinds of powdery mildews, scab, rust, damping off, banded sclerotial blight.
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 from bupirimate of simeconazoles.
1.1 reagent agent
The former medicine of 95 % simeconazoles, the former medicine of 95% bupirimate, above-mentioned former medicine provides by research and development department of extra large rel medicine company limited company.
1.2 test target
Never executed simeconazoles and bupirimate 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
Use first the former medicine of acetone solution, result according to preliminary experiment is made into 5 different proportionings with two an amount of former medicines, it is stand-by with acetone each processing to be diluted to respectively 5 concentration gradients again, and the ratio of 5 different proportioning active ingredients from bupirimate of simeconazoles is respectively 12:30; 16:26; 20:22; 24:18; 28:14.
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 the plants method to cultivate under 20 ℃, the condition of 12h alternation of light and darkness, and per 30 d turn culture 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 leaf dish moisturizing method to carry out toxicity test.First the blade that gathers is prepared into the leaf dish that diameter is 1.5cm, mixing at random, place respectively the series concentration liquid that configures to 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 wetting blotting paper of identical liquor strength, liquid 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 dose simeconazoles and bupirimate are carried out toxicity test in order to upper method, the two EC
50Value is respectively 5.58 ㎎/l and 6.69 ㎎/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 with single dose 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.
Take the logarithm value of drug concentration (mg/L) as independent variable x, take the probability value of corrected mortality as dependent variable y, set up respectively the virulence regression equation formula, adopt DPS software to calculate the LC 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 simeconazoles as the standard medicament, its toxicity index is 100):
The LC of the toxicity index of bupirimate (TI)=simeconazoles
50The LC of/bupirimate
50* 100
The LC of the true toxicity index (ATI) of M=simeconazoles
50The LC of/M
50* 100
The TI of the TI of the theoretical toxicity index (TTI) of M=simeconazoles * P simeconazoles+bupirimate * P bupirimate
The TTI of the ATI/M of the co-toxicity coefficient of M (CTC)=M * 100
In the formula:
M is simeconazoles and the mixture of the different proportionings of bupirimate
The P simeconazoles is simeconazoles shared ratio in mixture
The P bupirimate is bupirimate shared ratio in mixture.
2.1 toxicity test result
Table 1 simeconazoles and bupirimate are to the toxicity test of powdery mildew of cucumber
| Process title | Proportioning | Virulence regression equation (Y=a+bX) | The correlation coefficient r value | LC 50（mg/L） | Co-toxicity coefficient (CTC) |
| Simeconazoles | _____ | Y=3.9931X+2.0186 | 0.9894 | 5.58 | _______ |
| Bupirimate | _____ | Y=3.7534X+1.9018 | 0.9882 | 6.69 | _______ |
| Simeconazoles: bupirimate | 12：30 | Y=3.4964X+2.7958 | 0.9892 | 4.27 | 148.22 |
| Simeconazoles: bupirimate | 16：26 | Y=3.4521X+2.9829 | 0.9914 | 3.84 | 162.13 |
| Simeconazoles: bupirimate | 20：22 | Y=3.7478X+2.9749 | 0.9891 | 3.47 | 175.96 |
| Simeconazoles: bupirimate | 24：18 | Y=3.7906X+2.8373 | 0.9884 | 3.72 | 161.47 |
| Simeconazoles: bupirimate | 28：14 | Y=3.9592X+2.6206 | 0.9901 | 3.99 | 147.88 |
As can be seen from the table, the result of the test of different proportion proportioning shows, is 12:30 in the active ingredient ratio; 16:26; 20:22; 24:18; When 28:14 dilutes respectively, all show stronger synergistic effect, wherein take simeconazoles and bupirimate as 20:22 the time synergistic effect best, its co-toxicity coefficient is 175.96.Suggestion is carried out further field control effectiveness test to suitable proportion 20:22 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 pear scab
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 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, radix investigation before the medicine, for the first time behind the medicine 7 days, investigated in 15 days behind 7 days and the medicine behind the medicine for the second time.
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 7d range estimation medicament has poisoning to crop after the dispenser.
3.1.5 result of the test and analysis
Each processes the effect (table 2) of preventing and treating powdery mildew of cucumber
Each processes the effect of preventing and treating powdery mildew of cucumber table 2
As shown in Table 2,42% simeconazoles bupirimate is higher than simeconazoles and bupirimate single dose with the composite successful of controlling for powdery mildew of cucumber of the ratio of 20:22, and 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 is measured the control efficiency to pear scab
4.1.1 application method
Test is total to dispenser three times, check plot spray equivalent clear water.When making up a prescription, after with a small amount of water medicament fully being dissolved first, add again suitable quantity of water and carry out complete stool spraying processing, even spraying.All adopting power driven sprayer, operating pressure during the spray medicine is 2.0～2.3 kg/cm
2, shower nozzle aperture 1.2 mm.The residential quarter spouting liquid is used by 675 liters/hectare, and liquid is sprayed application to the positive and negative two sides of crop leaf uniformly.With the moistening blade of liquid, not lower is degree.
4.1.2 investigation method
Two strains of every residential quarter are all investigated, 5 samplings in every strain Fen Dong, south, west, the north, every 20 leaves and 20 fruit investigation of getting current-year branch.
The leaf stage division
0 grade: anosis;
1 grade: lesion area accounts for below 10% of one-piece blade area;
3 grades: lesion area accounts for 11%～25% of one-piece blade area;
5 grades: lesion area accounts for 26%～40% of one-piece blade area;
7 grades: lesion area accounts for 41%～65% of one-piece blade area;
9 grades: lesion area accounts for more than 65% of one-piece blade area.
The fruit stage division:
0 grade: on the fruit without scab;
1 grade: on each fruit 1 ~ 2 of scab is arranged;
3 grades: on each fruit 3 ~ 4 of scabs are arranged;
5 grades: on each fruit 5 ~ 6 of scabs are arranged;
7 grades: on each fruit 7 ~ 10 of scabs are arranged, the part scab links to each other, and accounts for about 1/5th of fruit area;
9 grades: scab is arranged more than 10 on each fruit, the part scab links to each other, and accounts for more than 1/4th of area of fruit.
4.1.3 control time and number of times
Test is investigated 4 times altogether, i.e. disease index investigation before the medicine, preventive effect investigation in 10 days behind the 1st medicine, 14 days preventive effect investigation behind 10 days and the 3rd (last) medicine behind the 2nd medicine.
4.1.4 drug effect computational methods
Sick leaf rate (%)=sick leaf (really) count/is investigated total leaf (really) number * 100
Disease index=∑ (sick leaves at different levels (really) number * relative level numerical value)/(investigating total leaf (really) number * 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
4.1.5 the direct impact on crop
Whether have poisoning produce, will record poisoning degree and type if any poisoning if observing crop.
4.1.6 result of the test and analysis
Each processes the effect of preventing and treating pear scab table 3
Interpretation of result: as can be seen from Table 3,42% simeconazoles bupirimate is more remarkable with the composite control efficiency to pear scab of the ratio of 20:22, and 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 pear tree does not all appear in each treatment agent, illustrates that it is safe to pear tree.Advise that the bactericide different from the mechanism of action mixes use to delay the drug-fast generation of germ.
In sum, the present invention is the bactericidal composition that contains simeconazoles and bupirimate, powdery mildew of cucumber, pear scab etc. all had preferably effect, and it is to the target crop safety, compare with single dose, bactericidal composition of the present invention has the advantage 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 (5)
1. bactericidal composition that contains simeconazoles and bupirimate, it is characterized in that: the active ingredient of this bactericidal composition is that simeconazoles and two yuan of bupirimates are composite, and wherein the mass ratio of active ingredient simeconazoles and bupirimate is 1～80: 80～1.
2. bactericidal composition according to claim 1, it is characterized in that: the quality optimization ratio of simeconazoles and bupirimate is 1～40: 40～1.
3. bactericidal composition according to claim 1, it is characterized in that: simeconazoles and bupirimate account for 1%～80% of the whole quality of the pharmaceutical preparations.
4. bactericidal composition according to claim 3, it is characterized in that: simeconazoles and bupirimate account for 5%～50% of the whole quality of the pharmaceutical preparations.
5. according to claim 1 and 2 or 3 or 4 described bactericidal compositions, it is characterized in that: the formulations of pesticide that this bactericidal composition can be prepared into are missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion.
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- 2012-11-23 CN CN2012104807576A patent/CN103004860A/en active Pending
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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 |
| WO2007083394A1 (en) * | 2006-01-19 | 2007-07-26 | Mitsui Chemicals, Inc. | Pest control composition containing diamine derivative |
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Application publication date: 20130403 |