CN102484996B - Synergy composition for matrine and tetronic acid pesticides - Google Patents
Synergy composition for matrine and tetronic acid pesticides Download PDFInfo
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Abstract
The invention belongs to the pesticide technology field, and relates to a synergy composition for matrine and tetronic acid pesticides. The mass ratio of matrine to tetronic acid is 50:1-1:50. The matrine in the composition comprises matrine, oxymatrine and a mixture of matrine and oxymatrine, or a series alkaloid extract and its preparation obtained from plants such as radix sophorae flavescentis, Sophora alopecuroides and Subprostrate Sophora Root. The tetronic acid pesticide can be one of spirotetramat, spirodiclofen and spirotetramat or its combination. The composition of the invention is capable of generating cooperation and synergy effects, overcoming harmful biological drug resistance, prolonging the service life of the pesticide, and enlarging the prevention and cure scope, can be used for preventing and treating a plurality of insect diseases on agriculture and gardening crops, especially suitable for insects possessing drug resistance on single pesticide, such as aphid, scale insect, leaf mites, leafhopper, planthopper or whitefly and thrips.
Description
Technical field
The invention belongs to technical field of pesticide, it is characterized in that relating to a kind of pesticide synergistic composition, particularly relate to a kind of preparation and application thereof of the synergistic composition that contains matrine and tetronic acid class agricultural chemicals.
Background technology
The problem often facing in control of insect is: how to make the active component dosage in agricultural chemicals reduce or avoid hostile environment or poisonous effect, and require still can effectively prevent and treat agricultural pest.Its two, avoid frequently and solely using a certain pesticide species, in order to avoid cause the quick selection of resistant insect or pathogene.Using the insecticide of the different mechanisms of action with synergistic effect to carry out composite in the compounded preparation of pesticide of maximum feature taking synergy, spread spectrum, double controlling, can reduce the dosage of each active ingredient, can be used for again the improvement of resistant insect or the generation of delaying drug resistance, be one of important channel solving above-mentioned two problems in control of insect.
Fly the homoptera pests such as (powder) lice, aphid, leafhopper, mealybug, the thrips insects such as thrips all have short, the feature such as breeding amount is large, generation overlap is obvious of breeding cycle, are easy to develop immunity to drugs; In addition, lepidopterous diamond-back moth, cabbage caterpillar etc., and harmful mite on some crops has also all produced serious pesticide resistance to the single agricultural chemicals of many obligates.For this reason, people have searched out some solutions from synergism compound preparation, Patents (application number) is as: 200910159604.X, 200510007412.9,200810211784.7,200910173094.1,200910173096.0,200910170818.7,200910173091.8,200910173097.5,200910190615 and 200910209737.3 etc., wherein the synergistic composition using matrine as active component has caused very large concern, and the built agent of matrine and other farm chemical ingredients has obvious synergy potentiality; On the other hand, the synergistic composition of the exclusive medicine spiral shell of emerging pesticide species sucking pest worm ethyl ester etc. is looked at from just starting to be just subject to parent.But, generally all concentrate on preventing and treating the close pesticide species of spectrum and combine (as, the combination of spiral shell worm ethyl ester and anabasine or pymetrozine) about the patent of matrine or spiral shell worm ethyl ester etc., be unfavorable for spread spectrum.Therefore, can prevent and treat the tetronic acid class pesticide new variety such as matrine and the exclusive medicine spiral shell of homoptera pest worm ethyl ester that Lepidoptera can prevent and treat again homoptera pest and carry out compositely, will play spread spectrum decrement, so that the object of protecting new varieties, increasing the service life.Matrine and tetronic acid class agricultural chemicals have no report as the composition pesticide of insecticidal constituent.
Natural source agricultural chemicals matrine (Matrine), to people and animals' low toxicity, uses safety, noresidue, has stomach toxicity and action of contace poison; Directly act on multiple action targets of polypide, paralysis nerve center, makes polypide protein coagulating then, blocks pore, death by suffocation; Can destroy the pesticide resistance system of insect, with other agricultural chemicals without cross resistance.Matrine is to vegetables lepidoptera pest cabbage caterpillar, tea caterpillar, diamond-back moth, and sucking pest aphid and tea lesser leafhopper, trialeurodes vaporariorum etc. all have desirable preventive effect.
Tetronic acid class insecticidal/acaricidal agent mechanism of action uniqueness, is lipid synthesis inhibitor, and larva, young mite and ovum are had to excellent control efficiency.And existing desinsection, kill between full agent without cross resistance, can effectively prevent and treat the worm mite that existing insecticidal/acaricidal agent is produced to resistance, meet modern crop protection requirement, Environmental compatibility is good, will have wide future develop in future.
Spiral shell worm ethyl ester (spirotetramat) belongs to tetronic acid class agricultural chemicals together with spiral shell mite ester (spirodiclofen) and spiral shell worm ester (spiromesifen).Spiral shell worm ethyl ester has unique function Characteristics, is unique modern insecticide with two-way interior suction conductive performance so far; Its another feature is that the lasting period is long, and the effective control that reaches 8 weeks can be provided; High-efficiency broad spectrum, can effectively prevent and treat various suckings pest, as aphid, thrips, wood louse, mealybug, aleyrodid and scale insect etc.The action of contace poison of spiral shell mite ester tool, does not have interior absorption, kills mite and composes wide, strong adaptability, all effective to each developmental stage of mite, comprises ovum.Spiral shell worm ester can effectively be prevented and treated ovum and the larva of tetranychid and aleyrodid.
Mechanism of action difference, the control differentiated matrine of spectrum and tetronic acid class agricultural chemicals are carried out composite, expand control spectrum, can be used for the control of multiple worm mite on agricultural and horticultural crop, there is obvious synergistic effect, be particularly useful for sucking mouth parts etc. and be easy to single agricultural chemicals to produce the insect evil mite of resistance.
Summary of the invention
The object of the invention is to make full use of plant resources, the advantage of performance botanical pesticide, it and the Chemical Pesticide Varieties of highly effective and safe are carried out to synergistic complex, to such an extent as to maximize favourable factors and minimize unfavourable ones, a kind of efficient, low toxicity, wide spectrum are provided and are difficult for causing drug-fast insecticidal/acaricidal agent---the synergistic composition of matrine and tetronic acid class agricultural chemicals.
The invention provides various preferred dosage form of the synergistic composition of described matrine and tetronic acid class agricultural chemicals and preparation method thereof.
Composition pesticide provided by the invention, is characterized in that: the mass ratio of active ingredient matrine and tetronic acid class agricultural chemicals is 50: 1～1: 50, is preferably 10: 1～1: 30, and the best is 10: 1～1: 20, and all the other are insecticides adjuvant.
Matrine described in the present invention comprises the mixture of matrine, oxymatrine and matrine and oxymatrine, or a series of alkaloid extracts and the preparation thereof that from the plants such as kuh-seng, Sophora alopecuroide, root of subprostrate sophora, obtain.Described tetronic acid class is spiral shell worm ethyl ester, spiral shell mite ester and spiral shell worm ester one or a combination set of.
The present invention, taking matrine and tetronic acid class agricultural chemicals as active ingredient, is mixed with the formulations such as suspending agent, microemulsion, aqueous emulsion, wetting powder, water dispersible granules and soluble liquid with insecticides adjuvant according to method known to those skilled in the art processing.
Described auxiliary agent is determined according to formulation.
In the time of preparation suspending agent, its auxiliary agent by the quality of the pharmaceutical preparations is: wetting dispersing agent 2%～10%, defoamer 0%～2%, antifreezing agent 2%～10%, preservative 0～1%, thickener 0.1%～1.5%, acidity regulator 0～1%, surplus deionized water.
In the time of preparation microemulsion, its auxiliary agent by the quality of the pharmaceutical preparations is: emulsifier 8%～28%, solvent 1%～20%, cosolvent 0～10%, defoamer 0.1%～1%, antifreezing agent 0～2%, surplus deionized water.
In the time of preparation aqueous emulsion, its auxiliary agent by the quality of the pharmaceutical preparations is: emulsifier 0.5%～10%, solvent 1%～50%, thickener 0～2%, defoamer 0～0.5%, preservative 0～2%, antifreezing agent 0～10%, surplus deionized water.
In the time of preparation wetting powder, its auxiliary agent by the quality of the pharmaceutical preparations is: wetting agent 3%～35%, dispersant 4%～30%, filler 10%～70%.
In the time of preparation water-dispersible granules, its auxiliary agent by the quality of the pharmaceutical preparations is: wetting agent 1%～5%, and dispersant 2%～8%, binding agent 0～10%, disintegrant 0～15%, filler adds to 100%.
In the time of preparation soluble liquid, its auxiliary agent is: surfactant 5%～15%, and antifreezing agent 0.5%～10%, solubilizer 3%～20%, solvent is mended to 100%.
Good effect of the present invention is: between botanical pesticide and chemical pesticide improved seeds, maximize favourable factors and minimize unfavourable ones, the mechanism of action complementation between the two of never poison and biosynthesis inhibitor, in addition, the composition of matrine and spiral shell worm ethyl ester integrate tag, stomach toxicity and systemic action, insect multiple action is had concurrently, really play the effect of synergy, spread spectrum, simultaneously, can reduce active ingredient dosage, reduce costs, the generation of the antagonism property of medicine has retarding action.
Embodiment
In order to understand better essence of the present invention, further illustrate technology contents of the present invention with example below, but content of the present invention is not limited to this.
Embodiment 1: preparation 5.5% matrine spiral shell worm ethyl ester microemulsion
Insecticidal active ingredient percentage by weight (%) is: matrine 5.0, spiral shell worm ethyl ester 0.5;
The each composition percentage by weight of auxiliary agent (%) is: emulsifier: polyoxyethylene alkyl amine 20.0; Cosolvent: ethyl acetate 0.05; Defoamer: efficient polysiloxanes 0.1～1.0; Antifreezing agent: glycerine 0.5; Solvent: Solvesso100 20.0; Surplus deionized water.
By proportioning, matrine and spiral shell worm ethyl ester are dissolved in solvent, emulsifier is joined in matrine spiral shell worm ethyl ester solution, stir, add deionized water and all the other auxiliary agents, put into and in homogenizer, give strong mixing homogenize and get final product.
Embodiment 2: preparation 5.1% matrine spiral shell worm ethyl ester aqueous emulsion
Insecticidal active ingredient percentage by weight (%) is: matrine 5.0, spiral shell worm ethyl ester 0.1;
The each composition percentage by weight of auxiliary agent (%) is: emulsifier: naphthalenesulfonic acid-formaldehyde condensate (NNO) 8.0; Solvent: S-15010.0; Thickener: xanthans 0.2, Magnesiumaluminumsilicate 1.0; Defoamer: EO-PO polymer 0.3%; Preservative: Sodium Benzoate 0.8%; Antifreezing agent: ethylene glycol 6.0; Surplus deionized water.
By proportioning, matrine and the former medicine of spiral shell worm ethyl ester are dissolved in solvent, emulsifier, cosolvent are joined in matrine and spiral shell worm ethyl ester solution, stir, said mixture is slowly added to the water, fully stirring and get final product.
Embodiment 3: preparation 33% matrine spiral shell mite ester suspending agent
Insecticidal active ingredient percentage by weight (%) is: matrine 30.0, spiral shell mite ester 3.0;
The each composition percentage by weight of auxiliary agent (%) is: wetting dispersing agent: NNO 2.0, D4251.5, agriculture breast 0201B 2.5; Defoamer: organic silicone 1.0; Antifreezing agent: propane diols 5; Preservative: paraformaldehyde 0.7; Thickener: xanthans 0.1, white carbon 1.0; Surplus deionized water.
By proportioning, matrine and the former medicine of spiral shell mite ester are pulverized, added various auxiliary agents and water except thickener, put into together high-shear emulsion machine and mix, add thickener further to mix, grind through skin grinder, after microscopy is qualified and get final product.
Embodiment 4: preparation 42% matrine spiral shell mite ester wetting powder
Insecticidal active ingredient percentage by weight (%) is: matrine is 2.0, and spiral shell mite ester is 40.0;
The each composition percentage by weight of auxiliary agent (%) is: wetting agent: bay alcohol radical sodium sulphate 20.0; Dispersant: M918.0; Filler: kaolin 20.0.
By proportioning, matrine and the former medicine of spiral shell mite ester are carried out joining in blender after air-flow crushing, in blender, add dispersant, filler respectively by proportioning, stir and get final product.
Embodiment 5: preparation 51% matrine spiral shell worm ester water-dispersible granules
Insecticidal active ingredient percentage by weight (%) is: matrine 1.0, and spiral shell worm ester is 50.0;
The each composition percentage by weight of auxiliary agent (%) is: wetting agent: saponin 3.0; Dispersant: GY-JZH-A 6.0; Binding agent: PEG 4.0; Disintegrant: soluble starch 3.0, bentonite 7.0, filler adds to 100.
See that by formula matrine and the former medicine of spiral shell worm ester and other auxiliary material one reinstate air-flow crushing etc. and carry out the fine pulverizing of dry type, obtain after the wetting powder of powdery, then by this water-dispersion type granula granulation, dry, screening, select the particle of certain particle size scope and get final product.
Embodiment 6: preparation 3.1% matrine spiral shell worm ester soluble liquid
Insecticidal active ingredient percentage by weight (%) is: matrine 0.1, spiral shell worm ester 3.0;
The each composition percentage by weight of auxiliary agent (%) is: surfactant: anhydrous sorbitol APEO 13.0; Antifreezing agent: glycerine 2.5; Solubilizer: ethyl acetate 15.0; Solvent is mended to 100.
In the there-necked flask that reflux condenser, agitator, attemperating unit are housed, add solvent, auxiliary agent and former medicine by formula requirement, open the former medicine of stirring and dissolving, auxiliary agent in solvent.As slow in dissolution velocity or dissolving can suitably be heated not completely, makes it to dissolve completely, is then cooled to room temperature.Finally solution filter is obtained to homogeneous phase transparent fluid sample.
The indoor virulence test that the present invention carries out the synergistic composition of matrine and tetronic acid class agricultural chemicals has adopted conventional method, and data are calculated and processing is carried out as follows:
By the each lethality of processing of Abbott formula correction, with DPS software calculating LC
50and virulence regression equation.Adopt the abundant method of Sun Yun to obtain the co-toxicity coefficient (CTC) of each mixed ratio with reference to NY/T1154.7-2006, and evaluate the two mixed synergistic effect.
Criterion: CTC≤80, show as antagonism; CTC:80～120, show as summation action; CTC >=120, show as synergistic effect.
Test example 1 matrine and the composite joint toxicity measuring of spiral shell worm ethyl ester
Examination worm: Brown Planthopper (Nilaparvata lugens (St 1))
Test method: adopt rice stem infusion process with reference to " the agricultural industry criteria NY/T1154.11-2008 of the People's Republic of China (PRC) " and " the agricultural industry criteria NY/T1154.7-2006 of the People's Republic of China (PRC) ".Extract with root the rice strain at healthy and strong tillering stage to booting initial stage, clean, be cut into the long band root rice stem of 15cm, 3 one group of strain, dry in the air to surface without washmarking in cool place place.Rice stem is soaked 30 seconds respectively in the medicament having diluted, after taking-up is dried, encase root put into cultivation cup with the absorbent cotton soaking, absorption nymph in 3 mid-term in age is put into and cultivates cup, 20 every glass, put temperature and be 27 DEG C, photoperiod and be in the incubator of 16h:18h (L:D) and raise.The cotton balls moisturizing that adds water of every two days bag rice root, clear water contrast, each concentration repeats 3 times.After 48 hours, check dead borer population, calculate lethality.
Result of the test is in table 1:
Table 1 matrine and the virulence result (48h) of the different proportionings of spiral shell worm ethyl ester to brown plant-hopper nymph in 3 age
*a is matrine, and B is spiral shell worm ethyl ester
As seen from Table 1, the composition of matrine and spiral shell worm ethyl ester is all greater than 120 to the co-toxicity coefficient of brown plant-hopper under each proportioning in table, the each proportioning mixing that shows matrine and spiral shell worm ethyl ester all produces synergistic effect, in for examination proportioning, proportioning matrine: spiral shell worm ethyl ester=1: the co-toxicity coefficient maximum of 10 pairs of brown plant-hoppers, its value is 223.05.
Test example 2 matrines and the composite joint toxicity measuring of spiral shell mite ester
Examination worm: Tetranychus cinnabarinus (Tetranychus cinnabarinus (Boisduval))
Test method: pre-configured various proportioning liquids are put respectively in beaker stand-by.By gathering the female one-tenth mite of Tetranychus cinnabarinus in indoor for subsequent use on Kidney bean in test booth.Test adopts slide infusion process, two-sided tape is bonded to one end of slide, provokes gently female one-tenth mite with writing brush, its back is bonded on adhesive tape to every sticky 3 row of slide, 10 of every row.At binocular stereo test under microscope acarid to be tried, reject dead and inactive individuality, supplement healthy individuals.The slide that is stained with female one-tenth mite is immersed in different liquids to be measured, after jog 5s, take out, suck unnecessary liquid with blotting paper, put into crisper, dry, add a cover and be placed under (26 ± 2) DEG C room temperature.3 repetitions are established in test, are treated to contrast with clear water, and 48h after medicine, in binocular stereo test under microscope Tetranychus cinnabarinus survival condition.
Result of the test is in table 2:
Table 2 matrine and the virulence result (48h) of the different proportionings of spiral shell mite ester to Tetranychus cinnabarinus
*a is matrine, and B is spiral shell mite ester
As seen from Table 2, the composition of matrine and spiral shell mite ester is all greater than 120 to the co-toxicity coefficient of Tetranychus cinnabarinus under each proportioning, the each proportioning mixing that shows matrine and spiral shell mite ester all produces synergistic effect, in for examination proportioning, proportioning matrine: spiral shell mite ester=1: the co-toxicity coefficient maximum of 10 pairs of Tetranychus cinnabarinus, its value is 156.27.Matrine has strengthened spiral shell mite ester Tetranychus cinnabarinus has been become the pesticide activity of mite greatly with spiral shell mite ester synergistic combination, prevent and treat into mite new approaches are provided for spiral shell mite ester.
Test example 3 matrines and the composite joint toxicity measuring of spiral shell worm ester
Examination worm: diamond-back moth (Plutella xylostella)
Test method: the cabbage leaves of fresh cleaning is cut into 3cm × 4cm small pieces, the culture dish that to put into diameter be 9cm, be lined with moisturizing filter paper, with Potter spray tower after liquid of dish leaf foliage-spray, upset blade, every ware access is for 10 of examination 3 instar larvaes, once, each spray amount is 10ml to spraying liquid again.Clear water according to same method spray equivalent is blank.After having sprayed, cover gauze in case larva escapes, then cover ware lid.Culture dish is placed in to insectary (25+2 DEG C), 24h " Invest, Then Investigate " death condition.3 repetitions of every processing.10 larvas of every repetition.
Result of the test is in table 3:
Table 3 matrine and the virulence result (24h) of the different proportionings of spiral shell worm ester to diamond-back moth 3 instar larvaes
*a is matrine, and B is spiral shell worm ester
As seen from Table 3, the composition of matrine and spiral shell worm ester is all greater than 120 to the co-toxicity coefficient of diamond-back moth under each proportioning, the each proportioning mixing that shows matrine and spiral shell worm ester all produces synergistic effect, in for examination proportioning, proportioning matrine: spiral shell worm ester=1: the co-toxicity coefficient maximum of 1 pair of diamond-back moth, its value is 190.52.
Claims (7)
1. a composition pesticide, it is characterized in that the matrine and the tetronic acid class agricultural chemicals that contain synergy effective dose, wherein tetronic acid class agricultural chemicals is any in spiral shell worm ethyl ester, spiral shell mite ester, spiral shell worm ester, and the weight ratio of matrine and tetronic acid class agricultural chemicals is 50: 1～1: 50.
2. composition pesticide according to claim 1, it is characterized in that matrine comprises the mixture of matrine, oxymatrine and matrine and oxymatrine, or a series of alkaloid extracts and the preparation thereof that from plant kuh-seng, Sophora alopecuroide, root of subprostrate sophora, obtain.
3. composition pesticide according to claim 1, is characterized in that the weight ratio of matrine and tetronic acid class agricultural chemicals is preferably 10: 1～1: 30.
4. composition pesticide according to claim 1, is characterized in that weight ratio the best of matrine and tetronic acid class agricultural chemicals is 10: 1～1: 20.
5. composition pesticide according to claim 1 can be processed into suspending agent, microemulsion, aqueous emulsion, wetting powder, water dispersible granules, soluble liquid in actual applications.
6. composition pesticide according to claim 1 can be used for the various pests on control agricultural and horticultural crop.
7. composition pesticide according to claim 1 can be used for lepidopterous insect pest and the sucking pest on control agricultural and horticultural crop.
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| CN102939978B (en) * | 2012-11-22 | 2014-05-28 | 海南正业中农高科股份有限公司 | Insecticidal composition containing oxymatrine and benzoylurea components |
| CN106818913A (en) * | 2016-12-13 | 2017-06-13 | 张世平 | A kind of insecticide for tea lesser leafhopper |
| CN108617675A (en) * | 2017-03-23 | 2018-10-09 | 浙江省化工研究院有限公司 | A kind of composition of ether compound containing loop coil and plant insecticide |
| CN110024803B (en) * | 2019-05-20 | 2020-06-23 | 海南博士威农用化学有限公司 | Spirotetramat-containing insecticidal composition and preparation thereof |
| CN110999693A (en) * | 2019-12-24 | 2020-04-14 | 山西省农业科学院植物保护研究所 | Water, fertilizer and pesticide integrated pesticide application method for fruit trees |
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| CN101361492A (en) * | 2007-08-09 | 2009-02-11 | 倪孟棣 | Biology plant pesticides and preparation technique thereof |
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