CN103004817A - Insecticidal composition containing ethiprole and spirotetramat - Google Patents

Insecticidal composition containing ethiprole and spirotetramat Download PDF

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CN103004817A
CN103004817A CN2013100045402A CN201310004540A CN103004817A CN 103004817 A CN103004817 A CN 103004817A CN 2013100045402 A CN2013100045402 A CN 2013100045402A CN 201310004540 A CN201310004540 A CN 201310004540A CN 103004817 A CN103004817 A CN 103004817A
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ethyl ester
spiral shell
worm
spirotetramat
shell worm
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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 an insecticidal composition containing ethiprole and spirotetramat. The effective ingredients are compounded of ethiprole and spirotetramat, wherein the mass ratio of the ethiprole to the spirotetramat is (4-20):(44-28); the preparation contains 1-80% by weight of the effective ingredients ethiprole and spirotetramat, and the residual auxiliary ingredients permitted and acceptable in pesticide. The dosage form of the insecticidal composition disclosed by the invention is missible oil, suspending agent, wettable powder, water dispersible granule, emulsion in water and micro-emulsion. The insecticidal composition is mainly used for preventing and treating sucking mouthparts pest thrips, stinkbug, curculionid, asparagus caterpillar, aphid, plant hopper, locust, plant louse, mealybug, mealywing, and scale insect.

Description

A kind of Pesticidal combination that contains second worm nitrile and spiral shell worm ethyl ester
Technical field
The present invention relates to the agriculture chemical compounding technical field, particularly relate to a kind of Pesticidal combination that contains second worm nitrile and spiral shell worm ethyl ester.
Background technology
Second worm nitrile (Ethiprole) is the Insecticidal and acaricidal agent by rhone-poulenc is found, Beyer Co., Ltd develops, belong to effective to multiple chewing type and sucking pest under the low consumption of insecticide that the second generation acts on GABA, be mainly used in preventing and treating thrips, stinkbug, curculionid, beet armyworm, aphid, plant hopper and locust etc., some aleyrodid is also shown to activity, particularly the rice grub green rice bug of extremely difficult control had to very strong activity.The chemical name 1-of second worm nitrile (2,6-dichlor-4-trifluoromethyl phenyl)-3-cyano group-4-ethyl sulfinyl-5-amino-pyrazol, its chemical structural formula is
Figure 250729DEST_PATH_IMAGE001
.
Spiral shell worm ethyl ester is the tetronic acid compounds, and spiral shell worm ethyl ester has unique function Characteristics, is unique modern insecticide with two-way interior suction conductive performance so far.Spiral shell worm ethyl ester high-efficiency broad spectrum, can effectively prevent and treat various suckings pest, as aphid, thrips, wood louse, mealybug, aleyrodid and scale insect etc.Applicable chief crop comprises, cotton, soybean, oranges and tangerines, tropical fruit tree, nut, grape, lupulus, potato and vegetables etc.The chemical name of spiral shell worm ethyl ester: cis-3-(2,5-3,5-dimethylphenyl)-8-methoxyl group-2-oxo-1-azaspiro [4.5]-last of the ten Heavenly stems 3-alkene-4-guanidine-acetic acid ethyl ester, its chemical structural formula is
Figure 2013100045402100002DEST_PATH_IMAGE001
.
In the real process of agricultural production, using chemical agent is the most effectively means of control plant pest, but the problem the most easily produced by the chemical control insect is the generation of pest resistance to insecticide.And long-term use single chemical insecticide continuously high dose, easily cause the series of problems such as residual, environmental pollution of medicament.Reasonably chemical insecticide is composite or be mixed and have the expansion insecticidal spectrum, improve control efficiency, extend the optimum period for applying fertilizer, reduce dosage, reduce poisoning, reduce residual, delay pest resistance and the positive characteristics such as drug-fast generation and development, pesticide compositional or to be mixed be one of the effective method the most addressed the above problem.We filter out second worm nitrile and spiral shell worm ethyl ester is composite on the basis of lab screening and field trial, have obvious synergistic effect.And there is no at present the people about second worm nitrile and the composite Pesticidal combination of spiral shell worm ethyl ester 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 agricultural insecticide composition.Be mainly used in preventing and treating sucking pest thrips, stinkbug, curculionid, beet armyworm, aphid, plant hopper, locust, wood louse, mealybug, aleyrodid and scale insect.
Technical scheme of the present invention realizes by following measures:
A kind of Pesticidal combination that contains second worm nitrile and spiral shell worm ethyl ester, in this Pesticidal combination, the mass ratio of active ingredient second worm nitrile and spiral shell worm ethyl ester is 4~20: 44~28, described Pesticidal combination of the present invention is through the toxicity test experimental verification, the mass ratio of second worm nitrile and spiral shell worm ethyl ester is 4~20: 44~28 o'clock, synergistic effect was better.
The formulations of pesticide that described Pesticidal combination of the present invention can be prepared are the formulations such as missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion.Second worm nitrile and the gross mass of spiral shell worm ethyl ester in preparation account for 1%~80% of the whole quality of the pharmaceutical preparations, while wherein accounting for 15%~50%, and toxicity and the residual balance preferably that reaches, cost is also lower.
The specific embodiments of the formulations of pesticide that Pesticidal combination of the present invention is mixed with is as follows:
Described Pesticidal combination is cream preparation, and the mass fraction of component is: 1~40 part of second worm nitrile; 1~40 part of spiral shell worm ethyl ester; 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 second worm nitrile and spiral shell worm ethyl ester being added in solvent after dissolving fully, filling, can be made into the cream preparation of the present composition.
Described Pesticidal combination is suspending agent, and the mass fraction of component is: 1~40 part of second worm nitrile; 1~40 part of spiral shell worm ethyl ester; 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 second worm nitrile and spiral shell worm ethyl ester, 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 Pesticidal combination is wetting powder, and the mass fraction of component is: 1~40 part of second worm nitrile; 1~40 part of spiral shell worm ethyl ester; 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, active ingredient second worm nitrile is mixed with spiral shell worm ethyl ester 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 Pesticidal combination is water dispersible granules, and the mass fraction of component is: 1~40 part of second worm nitrile; 1~40 part of spiral shell worm ethyl ester; 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 formula, active ingredient second worm nitrile is mixed with spiral shell worm ethyl ester 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 Pesticidal combination is aqueous emulsion, and the mass fraction of component is: 1~40 part of second worm nitrile; 1~40 part of spiral shell worm ethyl ester; 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 second worm nitrile and spiral shell worm ethyl ester, 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 Pesticidal combination is microemulsion, and the mass fraction of component is: 1~40 part of second worm nitrile, 1~40 part of spiral shell worm ethyl ester, 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.Second worm nitrile and spiral shell worm ethyl ester 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 compounded pesticides that active ingredient is second worm nitrile and spiral shell worm ethyl ester and is had obvious synergistic effect, delay the drug-fast generation in key, and reduced to become to produce cost and use cost, be mainly used in preventing and treating sucking pest thrips, stinkbug, curculionid, beet armyworm, aphid, plant hopper, locust, wood louse, mealybug, aleyrodid and scale insect.
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: second worm nitrile proportioning co-toxicity experiments different from spiral shell worm ethyl ester.
1.1 reagent agent
The former medicine of 97 % second worm nitrile, the former medicine of 95% spiral shell worm ethyl ester, above-mentioned former medicine provides by research and development department of extra large rel medicine company limited company.
1.2 test target
The third-instar larvae of the responsive type beet armyworm that 5 generations of indoor continuous raising and its Individual Size are consistent with physiological status.Temperature (25 ± 2) ℃.Relative moisture 65% ± 5%, periodicity of illumination 12/12h (L/D).
1.3 experimental procedure
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 5 different proportionings, then it is stand-by with acetone, each processing to be diluted to respectively to 5 concentration gradients, 5 second worm nitriles are respectively 4:44 from the ratio of the different proportioning active ingredients of spiral shell worm ethyl ester; 8:40; 12:36; 16:32; 20:28.
1.3.2 chemicals treatment
The drop method that adopts NY/T1 154.1-2006 to recommend is measured.By micro intravenous drip device solvent clean, regulate dropper to stand-by state.Choose the examination worm CO of neat and consistent with writing brush 2slight paralysis is placed in the 9cm culture dish, then with the micro intravenous drip device by medicament by a belly that drips to polypide, every some drops physic liquor 0.1L, the corresponding acetone contained with drop 0.1L be treated to contrast, the examination worm after drop is moved to (28
Figure 105552DEST_PATH_IMAGE003
2) ℃, in the culture dish of relative moisture 75%, normally cultivate.Every processing repeats for 4 times, 20 examination worms of every repetition.
1.4 control time
After processing, 24h investigation examination worm death condition (judgement examination worm death standard is gently to sting without autonomic response with pin), record total borer population and dead borer population.
1.5 data statistics and analysis
According to investigation statistics, calculate the corrected mortality that each is processed.And adopt the abundant method of Sun Yun to calculate the co-toxicity coefficient (CTC value) of mixture with reference to NY/T1 154.7-2006.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 second worm nitrile as the standard medicament, its toxicity index is 100):
The EC of the toxicity index (TI) of spiral shell worm ethyl ester=second worm nitrile 50the EC of/spiral shell worm ethyl ester 50* 100
The EC of the true toxicity index (ATI) of M=second worm nitrile 50the LC of/M 50* 100
The TI of the TI of the theoretical toxicity index (TTI) of M=second worm nitrile * P second worm nitrile+spiral shell worm ethyl ester * P spiral shell worm ethyl ester
The TTI of the ATI/M of the co-toxicity coefficient of M (CTC)=M * 100
In formula:
The mixture that M is second worm nitrile and the different proportionings of spiral shell worm ethyl ester
P second worm nitrile is second worm nitrile shared ratio in mixture
P spiral shell worm ethyl ester is spiral shell worm ethyl ester shared ratio in mixture.
2.1 toxicity test result
Table 1 second worm nitrile, the spiral shell worm ethyl ester indoor measurement result to beet pretty young woman at night
Figure 321508DEST_PATH_IMAGE005
As can be seen from the table, in active ingredient second worm nitrile: spiral shell worm ethyl ester ratio is 4:44; 8:40; 12:36; 16:32; When 20:28 dilutes respectively, its co-toxicity coefficient all is greater than 120, shows certain synergistic effect, wherein second worm nitrile: the synergistic effect that spiral shell worm ethyl ester is 12:36 is the most obvious, and co-toxicity coefficient is 183.67.Result of the test shows, under indoor conditions, second worm nitrile and spiral shell worm ethyl ester are composite all has higher activity to beet armyworm, and suggestion is carried out further field control effectiveness test to suitable proportion 12:36 left and right mixture preparation, to estimate its field practical application effect.
The experimental result of 3 field trial control beet armyworms, Frankliniella occidentalis
3.1 field trial control beet armyworm
3.1.1 test method
Test is carried out at Kaiping City, Guangdong Province suburb truck garden.Process design concentration by each and carry out routine to water spray.Spraying equipment is WF-16 type knapsack hand sprayer, and shower nozzle is single fan nozzle, and operating pressure is 0.2-0.4Mpa, and spray amount is 0.36-0.48L/min, carries out the routine spraying, makes every effort to evenly thoughtful during the spray medicine.During dispenser, the field beet armyworm is 1~2 instar larvae peak period.
Duration of test weather is good, and daily mean temperature is 17.8~26.4 ℃.Dispenser same day is without rain.
3.1.2 investigation method
In dispenser Qian Mei community by 5 samplings of diagonal. every wild cabbage 2~3 strains (depending on insect density) of choosing Beet Armyworm Eggs and larva.Statistics is demarcated beet exigua larvae head number in strain. using this as dispenser before the insect population radix.After dispenser the 7th, 14,21d investigates respectively the beet exigua larvae number of determining residual survival in strain. and using and proofread and correct the insect population decline rate as control efficiency.
3.1.3 drug effect computational methods
Insect population decline rate (%)=(larva number after medicine prelarva number-medicine)/medicine prelarva number * 100
Preventive effect (%)=(treatment region insect population decline rate-contrast insect population decline rate)/(100-check plot insect population decline rate) * 100.
3.1.4 poisoning investigation method
Within 7,14,21 days after medicine, observe the wild cabbage growing state, the range estimation medicament to wild cabbage without poisoning.
3.1.5 field control effectiveness test result
The experimental result of table 2 treatment agent control beet armyworm
Figure 654400DEST_PATH_IMAGE007
The Mixed Pharmacy of different proportion, tested by different consumptions as can be seen from Table 2, and after medicine, its control to beet armyworm all is better than contrasting medicament.The insecticidal effect of 48% second worm nitrile (12%) spiral shell worm ethyl ester (36%) 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 wild cabbage does not all appear in each treatment agent, illustrates that it is safe to wild cabbage.Advise that the insecticide different from the mechanism of action mixes use to delay the generation of pest resistance to insecticide.
4.1 field experiment control Frankliniella occidentalis test
4.1.1 test method
Test in Liquan capsicum ground, Xianyang, Shanxi province city, thrips is contained the phase of sending out and carries out.Use WF-16 type knapsack hand sprayer, shower nozzle is single fan nozzle, and operating pressure is 0.2-0.4Mpa, and spray amount is 0.36-0.48L/min, carries out the routine spraying, makes every effort to evenly thoughtful during the spray medicine.
Duration of test weather is good, and daily mean temperature is 17.8~25.4 ℃.Dispenser same day is without rain.
4.1.2 investigation method
Investigation insect population radix ,,Mei 5 of communities sampling before dispenser, total number of thrips in every some random searching plant middle and upper part l0 piece spends, same method is 7d after dispenser for the first time, for the second time 7d after medicine, 14d, check the remaining borer population of living, and calculates insect population decline rate and control efficiency.
4.1.3 drug effect computational methods
Insect population decline rate (%)=(larva number after medicine prelarva number-medicine)/medicine prelarva number * 100
Preventive effect (%)=(treatment region insect population decline rate-contrast insect population decline rate)/(100-check plot insect population decline rate) * 100.
4.1.4 poisoning investigation method
Within 14 days after medicine, observe the chili growth situation, the range estimation medicament to capsicum without poisoning.
4.1.5 field control effectiveness test result
Figure 406455DEST_PATH_IMAGE009
As can be seen from Table 3, the Mixed Pharmacy of different proportion, carry out field experiment by different consumptions, after medicine, its control efficiency to the capsicum Frankliniella occidentalis is better than contrasting medicament, 48% second worm nitrile (12%) spiral shell worm ethyl ester (36%) control Frankliniella occidentalis instant effect, efficiency time is long, and control efficiency is good.Insecticidal effect increases progressively along with the increase of consumption.According to experimental observation, each medication is processed capsicum is not all produced to poisoning.The suggestion dispenser rests in the Frankliniella occidentalis occurance peak period, requires even spraying during dispenser, and it,, to spending safety, does not hinder flower.This is mixed, and can effectively control the harm of Frankliniella occidentalis to the host, to the raising of quality of vegetable with increase production significantly, stronger popularizing value is arranged.
Combine above result of the test described; the Pesticidal combination that the present invention contains second worm nitrile and spiral shell worm ethyl ester; beet armyworm, Frankliniella occidentalis are shown to good control efficiency; to the target crop safety; with single dose, compare; Pesticidal combination of the present invention has mechanism of action uniqueness; consumption is few; the advantage that quick-acting is good, the lasting period is long; so; in research and development of the present invention and popularization, great social effect is arranged, can produce very large economic worth, the increasing both production and income of peasant household and the protection tool of local environment are of great significance.

Claims (4)

1. a Pesticidal combination that contains second worm nitrile and spiral shell worm ethyl ester, it is characterized in that: the active ingredient of this Pesticidal combination is second worm nitrile and spiral shell worm ethyl ester binary built, all the other are auxiliary element, and wherein the mass ratio of active ingredient second worm nitrile and spiral shell worm ethyl ester is 4~20: 44~28.
2. Pesticidal combination according to claim 1, it is characterized in that: second worm nitrile and the gross weight of spiral shell worm ethyl ester in preparation account for 1%~80% of the whole quality of the pharmaceutical preparations.
3. Pesticidal combination according to claim 2, it is characterized in that: second worm nitrile and the gross weight of spiral shell worm ethyl ester in preparation account for 15%~50% of the whole quality of the pharmaceutical preparations.
4. according to claim 1 or 2 or 3 described Pesticidal combinations, it is characterized in that: the formulation of this Pesticidal combination is missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion .
CN2013100045402A 2013-01-07 2013-01-07 Insecticidal composition containing ethiprole and spirotetramat Pending CN103004817A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101489384A (en) * 2006-07-11 2009-07-22 拜尔农作物科学股份公司 Active ingredient combinations with insecticidal and acaricidal properties
US20100168090A1 (en) * 2006-07-11 2010-07-01 Bayer Cropscience Ag Active Ingredient Combinations With Insecticidal and Acaricidal Properties
CN102228039A (en) * 2011-05-11 2011-11-02 青岛海利尔药业有限公司 Pesticide composition containing spirotetramat and chlorfenapyr
CN103355325A (en) * 2012-03-28 2013-10-23 陕西韦尔奇作物保护有限公司 Insecticide composition containing spirotetramat and ethiprole

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101489384A (en) * 2006-07-11 2009-07-22 拜尔农作物科学股份公司 Active ingredient combinations with insecticidal and acaricidal properties
US20100168090A1 (en) * 2006-07-11 2010-07-01 Bayer Cropscience Ag Active Ingredient Combinations With Insecticidal and Acaricidal Properties
CN102228039A (en) * 2011-05-11 2011-11-02 青岛海利尔药业有限公司 Pesticide composition containing spirotetramat and chlorfenapyr
CN103355325A (en) * 2012-03-28 2013-10-23 陕西韦尔奇作物保护有限公司 Insecticide composition containing spirotetramat and ethiprole

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Application publication date: 20130403