CN103190434A - Pesticide composition with clothianidin and spirotetramat - Google Patents
Pesticide composition with clothianidin and spirotetramat Download PDFInfo
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- CN103190434A CN103190434A CN2013101377034A CN201310137703A CN103190434A CN 103190434 A CN103190434 A CN 103190434A CN 2013101377034 A CN2013101377034 A CN 2013101377034A CN 201310137703 A CN201310137703 A CN 201310137703A CN 103190434 A CN103190434 A CN 103190434A
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Abstract
The invention relates to a pesticide composition with clothianidin and spirotetramat. The effective components are the clothianidin and the spirotetramat. The mass ratio of the clothianidin to the spirotetramat is (1-40):(40-1); and the total mass of the effective components, namely the clothianidin and the spirotetramat, in the preparation accounts for 1-80 percent of the mass of the whole preparation, and the rests are auxiliary components which are allowed to be used and are accepted in pesticides. The pesticide composition can be missible oil, a suspending agent, wettable powder, a water scattering agent, water emulsion, microemulsion, granula and micro capsules and is mainly used for preventing and treating insects such as aphids, leafhopper, thrips, plant hopper, aleyrodid, phylloxera, mealybug and scale insect on rice, vegetables, cotton, soy beans, hops, potatoes, fruit trees and other crops.
Description
Technical field
The present invention relates to the agriculture chemical compounding technical field, particularly relate to a kind of Pesticidal combination that contains clothianidin and spiral shell worm ethyl ester.
Background technology
A kind of insecticide in the anabasine that clothianidin carries out the world market exploitation jointly by Beyer Co., Ltd and Japanese Takeda Wu Tian company, it is the novel pesticide of a class highly effective and safe, high selectivity, its effect is similar with nAChR, have tag, stomach toxicity and systemic activity.Be mainly used on paddy rice, vegetables, fruit tree and other crops anti-ly eliminating aphis, the insecticide of Semiptera, coleoptera, diptera and some Lepidoptera class pest such as leafhopper, thrips, plant hopper, there is efficient, wide spectrum, consumption is few, toxicity is low, the drug effect lasting period long, to crop without poisoning, use safety, with conventional pesticide without advantages such as cross resistances, remarkable interior suction and osmosis are arranged, and are the another kinds that substitutes high malicious organophosphorous pesticide.The chemical name of clothianidin is (E)-1-(the chloro-1,3-thiazoles of 2--5-ylmethyl)-3-methyl-2-2-nitroguanidine, and its chemical structural formula is
.
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
.
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 clothianidin 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 clothianidin 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 on paddy rice, vegetables, cotton, soybean, lupulus, potato, fruit tree and other crops anti-ly eliminating aphis, the insects such as leafhopper, thrips, plant hopper, wood louse, mealybug, aleyrodid and scale insect.
Technical scheme of the present invention realizes by following measures:
A kind of Pesticidal combination that contains clothianidin and spiral shell worm ethyl ester, in this Pesticidal combination, the mass ratio of active ingredient clothianidin and spiral shell worm ethyl ester is 1～40: 40～1, described Pesticidal combination of the present invention is through the toxicity test experimental verification, the mass ratio of clothianidin and spiral shell worm ethyl ester is 1～40: 40～1 o'clock, synergistic effect was better.
The formulations of pesticide that described Pesticidal combination of the present invention can be prepared are missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations.Clothianidin 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 5%～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 spiral shell worm ethyl ester; 1～40 part of clothianidin; 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 spiral shell worm ethyl ester and clothianidin 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 spiral shell worm ethyl ester; 1～40 part of clothianidin; 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 spiral shell worm ethyl ester and clothianidin, 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 spiral shell worm ethyl ester; 1～40 part of clothianidin; 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 spiral shell worm ethyl ester is mixed with clothianidin 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 spiral shell worm ethyl ester; 1～40 part of clothianidin; 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 spiral shell worm ethyl ester is mixed with clothianidin 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 spiral shell worm ethyl ester; 1～40 part of clothianidin; 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 spiral shell worm ethyl ester and clothianidin, 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 spiral shell worm ethyl ester; 1～40 part of clothianidin; 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.Spiral shell worm ethyl ester and clothianidin 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.
Described Pesticidal combination is granule, and the mass fraction of component is: 1～40 part of spiral shell worm ethyl ester; 1～40 part of clothianidin; 1～10 part of wetting dispersing agent; 0.1～5 part of thickener; 0.1～5 part of defoamer; Castor oil, surplus is supplied.Active ingredient spiral shell worm ethyl ester is mixed in the ratio of formula with each components such as clothianidin, dispersant, stabilizing agent, defoamer and solvents, after putting into the grinding of sand milling still, send in mixer for well-distribution and mix and get product.
Described Pesticidal combination is microcapsule formulations, and the mass fraction of component is: 1～40 part of spiral shell worm ethyl ester; 1～40 part of clothianidin; 5～20 parts, urea; 5～20 parts, formaldehyde; 5～20 parts of emulsifying dispersants; 1～5 part of antifreezing agent; 0.1～2 part of thickener; 0.1～0.8 part of defoamer; Water, surplus.In being housed, the there-necked flask of agitating device adds urea and formaldehyde (the amount of substance ratio is about l:1.5～2.0), with the pH value to 8 of sodium hydroxide solution regulator solution～9 left and right, then be warming up to 70～80 ℃, reaction obtains stable urea resin prepolymer.The former medicine of getting a certain amount of spiral shell worm ethyl ester and clothianidin is dissolved in cyclohexane, and adds emulsifying dispersant in solution, follows vigorous stirring, the O/W type stable emulsion that to be made into the aqueous solution of take containing emulsifying dispersant be water.Above-mentioned urea resin prepolymer is added in emulsion, regulate the pH value, polymerization reaction take place under the acid catalysis condition, be wrapped oil phase substance, forms microcapsule granule.Slowly heat up, solidify, temperature is controlled at 40～50 ℃, hardening time 1h.Selection adds appropriate auxiliary agent, the microcapsule suspending agent that gets final product stablely.
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 spiral shell worm ethyl ester and clothianidin and is had obvious synergistic effect, delay the drug-fast generation in key, and reduced and become to have produced cost and use cost, be mainly used in anti-ly on paddy rice, vegetables, cotton, soybean, lupulus, potato, fruit tree and other crops eliminating aphis, the insects such as leafhopper, thrips, plant hopper, 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: clothianidin proportioning co-toxicity experiments different from spiral shell worm ethyl ester.
1.1 reagent agent
95% the former medicine of spiral shell worm ethyl ester, the former medicine of 96% clothianidin, above-mentioned former medicine provides by research and development department of extra large rel medicine company limited company.
1.2 test target
Rice hoppers: indoor basin dress rice bud seedling is raised rice fulgorid 3 instar larvaes in 10 generations, temperature 27-29 degree, relative moisture 50% left and right, periodicity of illumination 14/10h (L/D) continuously.
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 several different proportionings, then it is stand-by with acetone, each processing to be diluted to respectively to several concentration gradients.
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.The examination worm of choosing neat and consistent with writing brush is placed in the 9cm culture dish by the slight paralysis of CO2, then with the micro intravenous drip device, medicament is dripped to the belly of polypide by head, 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
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 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 clothianidin as the standard medicament, its toxicity index is 100):
The EC of the toxicity index (TI) of spiral shell worm ethyl ester=clothianidin
50the EC of/spiral shell worm ethyl ester
50* 100
The EC of the true toxicity index (ATI) of M=clothianidin
50the LC of/M
50* 100
The TI of the TI of the theoretical toxicity index (TTI) of M=clothianidin * P clothianidin+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 clothianidin and the different proportionings of spiral shell worm ethyl ester
The P clothianidin is clothianidin 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 clothianidin and the spiral shell worm ethyl ester indoor measurement result to rice fulgorid
As can be seen from the table, in the active ingredient clothianidin: when spiral shell worm ethyl ester ratio is 1:40～40:1 dilution, its co-toxicity coefficient all is greater than 120, and show certain synergistic effect, wherein clothianidin: the synergistic effect that spiral shell worm ethyl ester is 4:40～40:4 is the most obvious.Result of the test shows, clothianidin under indoor conditions: spiral shell worm ethyl ester is composite all has higher activity to rice fulgorid, and suggestion is carried out further field control effectiveness test to suitable proportion 4:40～40:4 left and right mixture preparation, to estimate its field practical application effect.
3, the test of pesticide effectiveness of surveying control pear sucker, aphid is given birth in field
3.1, field give birth to survey the control pear sucker test of pesticide effectiveness
3.1.1 test method
Test is carried out in Liaoning Province young agricultural school orchard.Experimental field soil is sandy loam, and soil layer is deep, soil organic matter content 0.67%, and the test Pear Trees with Various Cultivars is 15 years living Jin Feng, distance between rows and hills 5m * 3m, the test region fruit tree growth is basically identical, and pear sucker occurs serious.
3.1.2 investigation method
5 processing are established in test, repeat 3 Ci，Mei community 10 strain trees, randomized arrangement.Fine during dispenser, duration of test is without rain.Spray before medicine every strain tree by East, West, South, North, in 5 orientation select 1 annotinous branch, investigate altogether 50 branches, the number of pest of living on statistics spray medicine front vane, and listing mark.Respectively before medicine, 7d, the 14d of spray after medicine, 21d checks the borer population alive on the listing mark blade, calculates each treatment region insect population decline rate and 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 continuous 7 days after medicine, observe the Growth of Pear Trees situation, the range estimation medicament to pear tree without poisoning.
3.1.5 field control effectiveness test result
As can be seen from Table 2, the Mixed Pharmacy of different proportion, carry out field experiment by different consumptions, after medicine, its control efficiency to pear sucker is better than contrasting medicament, with clothianidin: the spiral shell worm ethyl ester 32:16 ratio control pear sucker instant effect that is mixed, efficiency time is long, and insecticidal effect increases progressively along with the increase of consumption.According to experimental observation, each medication is processed pear tree is not all produced to poisoning.The suggestion dispenser rests in the pear sucker occurance peak period, to the raising of quality with increase production significantly, stronger popularizing value is arranged.
3.2 field experiment control cotton aphid test
3.2.1 test method
Test Zhang Wuzhuan village, the careless villages and small towns Cotton Fields in Chengwu County and carry out, soil is clay, the cultivation condition of middle fertility ，Ge community, water and fertilizer management uniformity.Cotton variety is the transgenic cotton against pests Lumianyan 15.
3.2.2 investigation method
5 samplings of experimental plot inner opposite angle line, fix 4 strains at every, and every strain is 3 of upper, middle and lower leaf fixedly, 60 leaves of fixing investigation 20 strain altogether, and 7d before medicine and after dispenser, 14,21d checks the remaining borer population of living, and calculates insect population decline rate and control efficiency.
3.2.3 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.
3.2.4 poisoning investigation method
Within 7 days after medicine, observe the cotton growth situation, the range estimation medicament to cotton without poisoning.
3.2.5 field control effectiveness test result
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 cotton aphid is better than contrasting medicament, clothianidin: the composite anti-instant effect that eliminates aphis of spiral shell worm ethyl ester 32:16 ratio, efficiency time is long, and control efficiency is good, and insecticidal effect increases progressively along with the increase of consumption.According to experimental observation, each medication is processed cotton is not all produced to poisoning.To the raising of cotton quality with increase production significantly, stronger popularizing value is arranged.
To sum up indoor biometrics and twice field experiment result are described, of the present inventionly take clothianidin and spiral shell worm ethyl ester and carry out two yuan of composite Pesticidal combinations as active ingredient, to rice fulgorid, pear sucker, the insects such as aphid show good control efficiency, to the target crop safety, with single dose, compare, Pesticidal combination of the present invention has mechanism of action uniqueness, the unit consumption is few, quick-acting is good, lasting period is long, the plurality of advantages such as the effect field is more wide in range, to plant diseases, insect pest can have better control, so, produce very large economic worth in research and development of the present invention and promotion conference, to vast vegetables, the protection tool of the increasing both production and income of the peasant household in fruit tree producing region and local environment is of great significance.
Claims (4)
1. a Pesticidal combination that contains clothianidin and spiral shell worm ethyl ester, it is characterized in that: the active ingredient of this Pesticidal combination is clothianidin and spiral shell worm ethyl ester binary built, all the other are auxiliary element, and wherein the mass ratio of active ingredient clothianidin and spiral shell worm ethyl ester is 1～40: 40～1.
2. Pesticidal combination according to claim 1, it is characterized in that: clothianidin and the gross mass 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: clothianidin and the gross weight of spiral shell worm ethyl ester in preparation account for 5%～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, granule, microcapsule formulations
.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114375962A (en) * | 2021-12-08 | 2022-04-22 | 赤天化科技集团有限公司 | Spirotetramat insecticidal composition and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101489393A (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 |
| CN101637159A (en) * | 2009-09-08 | 2010-02-03 | 深圳诺普信农化股份有限公司 | Pesticide composition with synergistic action |
-
2013
- 2013-04-20 CN CN2013101377034A patent/CN103190434A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101489393A (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 |
| CN101637159A (en) * | 2009-09-08 | 2010-02-03 | 深圳诺普信农化股份有限公司 | Pesticide composition with synergistic action |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114375962A (en) * | 2021-12-08 | 2022-04-22 | 赤天化科技集团有限公司 | Spirotetramat insecticidal composition and application |
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