CN110037033A - A kind of Pesticidal combination and its preparation containing capillary - Google Patents

A kind of Pesticidal combination and its preparation containing capillary Download PDF

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Publication number
CN110037033A
CN110037033A CN201910418978.2A CN201910418978A CN110037033A CN 110037033 A CN110037033 A CN 110037033A CN 201910418978 A CN201910418978 A CN 201910418978A CN 110037033 A CN110037033 A CN 110037033A
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CN
China
Prior art keywords
capillary
pesticidal combination
thymol
essential oil
wormwood
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CN201910418978.2A
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Chinese (zh)
Inventor
王龙宇
任承才
杜荣凯
朱明军
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BOSHIWEI AGRICULTURAL CHEMICAL Co Ltd HAINAN PROVINCE
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BOSHIWEI AGRICULTURAL CHEMICAL Co Ltd HAINAN PROVINCE
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Priority to CN201910418978.2A priority Critical patent/CN110037033A/en
Publication of CN110037033A publication Critical patent/CN110037033A/en
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N31/00Biocides, pest repellants or attractants, or plant growth regulators containing organic oxygen or sulfur compounds
    • A01N31/08Oxygen or sulfur directly attached to an aromatic ring system
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/36Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom five-membered rings

Abstract

The present invention relates to a kind of Pesticidal combination and its preparation containing capillary, effective component are capillary, Thymol, and the two proportion is 1:(0.1~0.3).The present invention has apparent synergistic effect using capillary, Thymol as the binary built insecticide of effective component, and quick-acting and lasting effect are good, and effective component dosage is less, the prevention and treatment suitable for thrips.

Description

A kind of Pesticidal combination and its preparation containing capillary
Technical field
The present invention relates to technical field of pesticide compounding, more particularly to a kind of Pesticidal combination and its system containing capillary Agent.
Background technique
Capillary is new pyrrole class compound, is acted on the mitochondria of insect bodies inner cell, intracorporal by insect Mixed-functional oxidase works, and mainly inhibits the conversion of adenosine diphosphate (ADP) (ADP) to atriphos (ATP).The medical instrument has stomach Poison and action of contace poison.Blade face permeability is strong, has certain systemic action, and with insecticidal spectrum is wide, preventive effect is high, holding effect is long, safety The characteristics of.
Thymol: chemical name is thymol, chemical formula C10H14O, molecular weight 150.22.Room temperature Lower is white to light yellow crystalline powder.Thymol has the function of antimycotic and helminth, due to phenols smell, It is usually used in pest repellant.The various agriculturals harmful mite such as Tetranychus cinnabarinus, Tetranychus piercei, Oligonychus biharensis can be effectively prevented, and safe, low Poison.
In terms of agricultural insecticidal, the single chemical agent of chronic administration, be easy to cause the residual of medicament, environmental pollution and Therefore the problems such as pest resistance to insecticide, is badly in need of developing a kind of with good insecticidal action and the good compounding of quick-acting and lasting effect is killed Worm agent.
Summary of the invention
Based on the above circumstances, it is an object of that present invention to provide a kind of Pesticidal combination and its preparation containing capillary is applicable in In the prevention and treatment of thrips.
The technical solution of the present invention is achieved by the following measures:
The present invention provides a kind of Pesticidal combination containing capillary, including capillary, Thymol, capillary and thyme The mass ratio of phenol is 1:(0.1~0.3).
It is a variety of that Pesticidal combination of the present invention can be made into missible oil, suspending agent, wettable powder, aqueous emulsion and microemulsion etc. Dosage form.Preferably microemulsion, in microemulsion also containing bamboo leaf essential oil, wormwood essential oil, cyclohexanone, 2201 emulsifiers, organosilicon and O-25 bleeding agent.The mass percent of each ingredient are as follows: capillary 12~20%, Thymol 1.2~6%, bamboo leaf essential oil 0.4~ 3.0%, wormwood essential oil 0.2~2.0%, cyclohexanone 25~35%, 2201 emulsifiers 18~23%, organosilicon 2~5% and O-25 Bleeding agent 2~5%, surplus are water.
The bamboo leaf essential oil is made by the following method:
1) leaf of bamboo is crushed to 10~30 mesh, obtains bamboo leaf powder;Every gram of bamboo leaf powder addition 20~40mL mass concentration 70~ 80% ethyl alcohol, 60~65 DEG C are stirred 1 hour;
2) solution of step 1) is subjected to microwave abstracting, setting microwave output power is 600w, the time 5~8 minutes, cooling After filter, collect filtrate, remove ethyl alcohol, obtain extract;
3) in every gram of extract be added 100~200mL mass ratio be 1:5~6 ethyl acetate and water mixed liquor in, Stirring 30~40 minutes, stratification, collected organic layer, concentration.
The wormwood essential oil is made by the following method:
(1) wormwood leaf crushed, cross 20~30 meshes, obtain wormwood powder;20~40mL mass concentration is added in every gram of wormwood powder 50~65% ethyl alcohol, 60~70 DEG C are stirred 1 hour;Cooled and filtered collects filtrate, removes ethyl alcohol, obtains extract;
2) mass ratio that 100~200mL is added in every gram of extract is to stir in the n-hexane of 1:5~7 and the mixed liquor of water It mixes 30~40 minutes, stratification, collected organic layer, is concentrated.
Pesticidal combination and its preparation of the present invention have obvious control efficiency to thrips.
The specific embodiment for the formulations of pesticide that Pesticidal combination of the present invention is configured to is as follows:
The Pesticidal combination is cream preparation, the mass percent of each component are as follows: capillary 12~20%, thyme Phenol 1.2~6%, emulsifier 8~20%, synergist 1~5% and solvent.The specific production stage of the cream preparation is will first have Emulsifier, synergist are added after mixing evenly at uniform after being completely dissolved in effect ingredient capillary, Thymol addition solvent Transparent oily liquids, it is filling, it can the missible oil preparation made into the composition of the present invention.
The Pesticidal combination is suspending agent, the mass percent of component are as follows: capillary 12~20%, Thymol 1.2~6%, dispersing agent 0~11%, antifreezing agent 1~3%, thickener 0.1~5%, defoaming agent 0.1~1%, wetting agent 2~ 8%, synergist 0~1% and solvent.The specific production stage of the suspending agent is first to mix other auxiliary agents, mixed through high speed shear Close uniformly, be added effective component capillary, Thymol, be sanded 2~3 hours in sand mill, make a diameter 5mm with Under, that is, it can be made into the aqueous suspension formulations of the present composition.
The Pesticidal combination is wettable powder, the mass percent of component are as follows: capillary 12~20%, thyme Phenol 1.2~6%, dispersing agent 3~15%, wetting agent 1~5% and filler.The specific production stage of the wettable powder are as follows: by upper It states formula to mix capillary, Thymol, dispersing agent, wetting agent and filler, in a stirring kettle uniform stirring, through air-flow crushing It is remixed after machine uniformly, that is, can be made into the wettable powder of the present composition.
The Pesticidal combination is aqueous emulsion, the mass percent of component are as follows: capillary 12~20%, Thymol 1.2~6%, emulsifier 3~25%, solvent 5~15%, stabilizer 2~10%, antifreezing agent 2~7%, defoaming agent 0.1~8%, Thickener 0.2~2% and water.The specific production stage of the aqueous emulsion are as follows: first by capillary, Thymol, solvent and emulsification Agent is added together, and makes to be dissolved into uniform oily phase;Other insecticides adjuvants such as part water, antifreezing agent are mixed into uniform Water phase;The oil phase is added to the aqueous phase while being stirred in the reactor at high speed, and slowly plus water is until reach phase inversion point, and unlatching is sheared Machine carries out high speed shear, and remaining water is added, and shearing about half an hour, forms the aqueous emulsion of oil-in-water type, that is, can be made into this hair The aqueous emulsion of bright composition.
The Pesticidal combination is microemulsion, and the mass percent of component is capillary 12~20%, Thymol 1.2 ~6%, emulsifier 18~28%, synergist 2~5%, cosolvent 25~35%, bleeding agent 2~5% can also include essential oil 0.6~5.0%, surplus is water.Capillary, Thymol, essential oil are completely dissolved with cosolvent, add emulsifier, synergy The other compositions such as agent uniformly mix, are eventually adding water, microemulsion can be made into after being sufficiently stirred.
Wherein above-described emulsifier is selected from calcium dodecyl benzene sulfonate, aliphatic acid polyethenoxy ether, alkyl phenol polyoxy Ethylene ether sulfosuccinates, styrylphenol polyoxyethylene ether, nonylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, The combination of one or more of aliphatic acid polyethenoxy base ester, polyoxyethylene aliphatic alcohol ether, 2201 emulsifiers, 700 emulsifiers.
The solvent is dimethylbenzene, toluene, methanol, ethyl alcohol, n-butanol, isopropanol, (code name is turpentine-based vegetable oil ND-60), one or more of solvent naphtha, dimethylformamide, dimethyl sulfoxide, water equal solvent combine.
The cosolvent be cyclohexanone, alcohols (methanol, ethyl alcohol etc.), phenols (phenol, cresols etc.), ethyl acetate, The combination of one or more of cosolvents such as dimethyl sulfoxide.
The dispersing agent be selected from polycarboxylate (code name YUS-WG5, TERSPERSE 2700, TERSPERSE2500), Lignosulfonates (code name YUS-WG4, YUS-207K, WLNOK, WLNO100, TERSPERSE2020), alkyl phenol polyoxy second Alkene ether methyl ether condensate sulfate, alkylsulfonate calcium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkyl phenol polyoxyethylene ether, rouge The combination of one or more of fat acid polyoxyethylene ester, aliphatic amine polyoxyethylene ether, glycerol fatty acid ester polyoxyethylene ethe.
The wetting agent be selected from lauryl sodium sulfate, calcium dodecyl benzene sulfonate, Nekal BX, TERWET1004, YUS-LXC, TERSPERSE 4894, TERSPERSE 2288, alkylbenzene sulfonate polyoxyethylene triphen dimly phosphenylic acid salt, One of spaonin powder, silkworm excrement, spaonin powder or multiple combinations.
The thickener be selected from xanthan gum, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose, aluminum magnesium silicate, One or more combinations in polyvinyl alcohol.
The stabilizer is selected from one or more of sodium citrate, resorcinol, epoxidized soybean oil, epoxychloropropane Combination.
The antifreezing agent is selected from one of ethylene glycol, glycerine.
The synergist select code name SP-4078, organosilicon, hypertonic anesthetic, except cured dose, one of transdermal element or more Kind combination.
The defoaming agent is selected from silicone oil, silicone compound, C10-20 saturated fat acid compounds, C8-10 fat One or more combinations of alcohol.
The filler is in kaolin, diatomite, bentonite, attapulgite, white carbon black, starch, precipitated calcium carbonate One or more combinations.
Pesticidal combination and its preparation of the present invention avoid applying at the nectariferous plant florescence.
The effect that the present invention obtains:
The present invention has apparent synergistic effect using capillary, Thymol as the compounded pesticides of effective component, quick-acting Property and lasting effect are good, the prevention and treatment especially suitable for thrips.
The insecticidal effect that microemulsion is made in the present composition is preferable, passes through rational proportion, better stability of preparation, quick-acting Good, efficiency time is long, and effective component dosage is few, environmental-friendly, is suitble to promote the use of.
Specific embodiment
For technical solution of the present invention, purpose and advantage is more clearly understood, the present invention is to kill Thysanoptera insect For thrips, it is described in the following specific embodiments through the invention.
Bamboo leaf essential oil is made by the following method in embodiment 2-8:
1) leaf of bamboo is crushed to 30 mesh, obtains bamboo leaf powder;The ethyl alcohol of every gram of bamboo leaf powder addition 40mL mass concentration 80%, 65 DEG C Stirring 1 hour;
2) solution of step 1) being subjected to microwave abstracting, setting microwave output power is 600w, the time 8 minutes, after cooling down Filtrate is collected in filtering, is removed ethyl alcohol, is obtained extract;
3) mass ratio that 200mL is added in every gram of extract is to stir 40 points in the ethyl acetate of 1:6 and the mixed liquor of water Clock, stratification, collected organic layer, concentration.
Wormwood essential oil is made by the following method in embodiment 2-8:
1) wormwood leaf crushed, cross 30 meshes, obtain wormwood powder;The second of 40mL mass concentration 65% is added in every gram of wormwood powder Alcohol, 70 DEG C are stirred 1 hour;Cooled and filtered collects filtrate, removes ethyl alcohol, obtains extract;
2) mass ratio that 200mL is added in every gram of extract is to stir 40 points in the n-hexane of 1:7 and the mixed liquor of water Clock, stratification, collected organic layer, concentration.
In the embodiment of the present invention, virulence test operating method:
Using leaf pipe medicine embrane method.Prick several apertures in 4mL centrifuge tube pipe lid and tube bottom, aperture with prevent thrips from escaping for It is quasi-.Then reagent agent is diluted with water to 5 concentration, under about 1mL medical fluid is added in centrifuge tube after reverse shaken several times Medical fluid is outwelled, naturally dry in pipe lid rear chamber is opened;Then fresh and tender cowpea beanpod is cut with a knife into the piece that length is about 2cm Section is placed in for naturally dry after dipping 10s in reagent liquid, is sandwiched in centrifuge tube, and suck 20 cowpea Jis with pest sucking device It is sprung into centrifuge tube after horse (the big thrips of beans) adult;It is (25 ± 2) DEG C that centrifuge tube, which is then placed in temperature, and L:D=is arranged in illumination Check that test worm death condition (touches polypide with small writing brush pen tip, motionless person is considered as extremely in the growth cabinet of 14h:10h, after 48h It dies).Every pipe is 1 repetition, and every concentration is repeated 3 times.Using clear water as blank control.Virulence equation and cause are calculated with least square method Concentration LC50, calculates the toxicity index and mixed co-toxicity coefficient (i.e. CTC value) of medicament in dead.
The synergistic effect of pharmacy mix is evaluated according to co-toxicity coefficient (CTC), i.e. CTC≤80 are antagonism, 80 < CTC < 120 is summation action, and CTC >=120 are synergistic effect.
Survey toxicity index (ATI)=(LC50 of the LC50/ reagent agent of standard agent) × 100;
The virulence of the percentage composition+B medicament of A medicament refers in toxicity index × mixture of theoretical toxicity index TTI=A medicament The percentage composition of B medicament in number × mixture;
Co-toxicity coefficient (CTC)=[mixture surveys toxicity index (ATI)/mixtures theoretical toxicity index (TTI)] × 100.
1 thrips virulence test of embodiment
Virulence test is carried out by the proportion of table 1, the results are shown in Table 1.
Table 1
Ingredient Proportion LC50(ug/ml) ATI TTI CTC
Capillary - 3.24 100 - -
Thymol - 16.23 19.96 - -
Capillary: Thymol 1:0.1 2.34 138.46 92.72 149.33
Capillary: Thymol 1:0.2 2.71 119.56 86.66 137.96
Capillary: Thymol 1:0.3 2.95 109.83 81.53 134.71
Capillary: Thymol 1:0.5 3.89 83.29 73.32 113.60
Capillary: Thymol 1:1 4.94 65.59 59.98 109.35
Table 1 is the results show that capillary: Thymol proportion is 1:(0.1~0.3) when, CTC is all larger than 120, illustrates at this In ratio range, Pesticidal combination of the present invention has synergistic function, shows apparent toxic effect to thrips.
2 26% capillary Thymol suspending agent of embodiment
By following weight proportion:
3 26% capillary Thymol missible oil of embodiment
By following weight proportion:
4 26% capillary Thymol microemulsion of embodiment
By following weight proportion:
5 13.2% capillary Thymol microemulsion of embodiment
By following weight proportion:
6 26% capillary Thymol microemulsion of embodiment
By following weight proportion:
7 22% capillary Thymol microemulsion of embodiment
By following weight proportion:
8 22% capillary Thymol microemulsion of embodiment
By following weight proportion:
Embodiment 9
The essential oil of embodiment 7 is replaced with into essential oil made from following methods:
Bamboo leaf essential oil is made by the following method:
The leaf of bamboo is crushed to 30 mesh, obtains bamboo leaf powder;The ethyl alcohol of 40mL mass concentration 50% is added in every gram of bamboo leaf powder, and 80 DEG C are stirred It mixes 1 hour;Cooled and filtered collects filtrate, removes ethyl alcohol, obtains extract;The mass ratio that 200mL is added in every gram of extract is 1: It in 6 n-hexane and the mixed liquor of water, stirs 40 minutes, stratification, collected organic layer, concentration.
Wormwood essential oil is made by the following method:
Wormwood leaf is crushed, crosses 30 meshes, obtains wormwood powder;The ethyl alcohol of 40mL mass concentration 80% is added in every gram of wormwood powder, 80 DEG C are stirred 1 hour;Cooled and filtered collects filtrate, removes ethyl alcohol, obtains extract;The quality of 200mL is added in every gram of extract It in mixed liquor than ethyl acetate and water for 1:5, stirs 40 minutes, stratification, collected organic layer, concentration.
1 20.4% chlorfenapyr microemulsion of comparative example
By following weight proportion:
The field control effectiveness test of the prevention and treatment thrips of embodiment 10
Experimental plot design is carried out according to China State Bureau of Quality and Technical Supervision's " pesticide field efficacy medicine test criterion (1) " standard, Each plot area is 20m2, 40 cells are set altogether, and the isolation strip of 1.2m is set between each cell.Insecticide-applying way uses spray-on process, With power spraye even spraying 1 time when application.
It participates in the experiment crop: cowpea
Reagent agent: embodiment 2~9, comparative example 1, clear water control.Every group of processing sets 4 repetitions.
Effective component dosage: 60g/hm2
Meteorological condition: weather is fine or cloudy, gentle breeze, and 23~32 DEG C of temperature.
Investigation method: adjusting Check insect population before application, is sampled with 5 points of every cell diagonal line, every solid point, which is seted the tone, looks into 10 plants of cowpeas Beans simultaneously mark.The work borer population on 50 plants of cowpeas is looked into altogether.1d, 3d, 7d and 14d carry out tune Check in the same way after application, Calculate preventive effect.
The field control effectiveness test of the prevention and treatment thrips of table 2
As the result is shown: average preventive effect reaches 82% or more after embodiment medicament application 3 days, and display embodiment medicament has speed Effect property;Average preventive effect reaches 87% or more after embodiment medicament application 7 days, shows synergistic effect, after embodiment medicament application 14d Preventive effect still maintains 75% or more, illustrates that lasting effect is good, wherein the quick-acting and holding effect of 7 microemulsion of embodiment 6 and embodiment Property it is obviously preferable, application 14 days after preventive effect still reach 95%.
In the embodiment of the present invention, effective component dosage is 60g/hm2When reaches good insecticidal effect, and (inventor will Effective component dosage is improved to 100g/hm2Shi Faxian, 1d, 3d, 7d, 14d preventive effect slightly rise), and the routine of capillary Dosage is generally 100g/hm2(test discovery, is increased to 100g/hm for the effective component dosage of comparative example 1 for left and right2Afterwards, 1d, 3d, 7d, 14d preventive effect are still significantly lower than each embodiment medicament), it can be seen that, pesticidal preparations of the present invention not only insecticidal effect compared with It is good, and effective component dosage is less, alleviates the influence to environment.
The above content is specific embodiment is combined, further detailed description of the invention, and it cannot be said that this hair Bright specific implementation is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, it is not taking off Under the premise of from present inventive concept, a number of simple deductions or replacements can also be made.

Claims (7)

1. the Pesticidal combination containing capillary, it is characterised in that: including capillary and Thymol, capillary and Thymol Mass ratio is 1:(0.1~0.3).
2. the Pesticidal combination according to claim 1 containing capillary, it is characterised in that: the dosage form of the Pesticidal combination For missible oil, suspending agent, wettable powder, aqueous emulsion and microemulsion.
3. the Pesticidal combination according to claim 1 containing capillary, it is characterised in that: the dosage form of the Pesticidal combination For microemulsion, also containing bamboo leaf essential oil, wormwood essential oil, cyclohexanone, 2201 emulsifiers, organosilicon and O-25 infiltration in microemulsion Agent.
4. the Pesticidal combination according to claim 3 containing capillary, it is characterised in that: the quality of each ingredient in microemulsion Percentage are as follows: capillary 12~20%, Thymol 1.2~6%, bamboo leaf essential oil 0.4~3.0%, wormwood essential oil 0.2~ 2.0%, cyclohexanone 25~35%, 2201 emulsifiers 18~23%, organosilicon 2~5% and O-25 bleeding agent 2~5%, surplus are Water.
5. the Pesticidal combination according to claim 4 containing capillary, it is characterised in that: the bamboo leaf essential oil passes through following Method is made:
1) leaf of bamboo is crushed to 10~30 mesh, obtains bamboo leaf powder;20~40mL mass concentration 70~80% is added in every gram of bamboo leaf powder Ethyl alcohol, 60~65 DEG C are stirred 1 hour;
2) solution of step 1) being subjected to microwave abstracting, setting microwave output power is 600w, the time 5~8 minutes, mistake after cooling down Filtrate is collected in filter, is removed ethyl alcohol, is obtained extract;
3) mass ratio that 100~200mL is added in every gram of extract is stirring in the ethyl acetate of 1:5~6 and the mixed liquor of water 30~40 minutes, stratification, collected organic layer, concentration.
6. the Pesticidal combination according to claim 4 containing capillary, it is characterised in that: the wormwood essential oil passes through following Method is made:
1) wormwood leaf crushed, cross 20~30 meshes, obtain wormwood powder;Every gram of wormwood powder addition 20~40mL mass concentration 50~ 65% ethyl alcohol, 60~70 DEG C are stirred 1 hour;Cooled and filtered collects filtrate, removes ethyl alcohol, obtains extract;
2) mass ratio that 100~200mL is added in every gram of extract is stirring 30 in the n-hexane of 1:5~7 and the mixed liquor of water ~40 minutes, stratification, collected organic layer, concentration.
7. described in any item Pesticidal combinations containing capillary according to claim 1~6, it is characterised in that: the desinsection group Object is closed for killing thrips.
CN201910418978.2A 2019-05-20 2019-05-20 A kind of Pesticidal combination and its preparation containing capillary Pending CN110037033A (en)

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CN113632797A (en) * 2021-08-30 2021-11-12 广西壮族自治区亚热带作物研究所(广西亚热带农产品加工研究所) Synergistic composition for preventing and treating papaya mites

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