Pesticidal combination containing pirimiphos-methyl and microcapsule suspending agent thereof
Technical field
The present invention relates to a kind of composite composition pesticide and pesticide processing field, be specifically related to a kind of Pesticidal combination composite containing pirimiphos-methyl and insect growth regulator, IGR and its microcapsule suspending agent, be applied to hygienic insecticide field.
Background technology
Sanitary insect pest refers to that those can produce directly or indirectly harm to human health, affects all arthropodss of people's normal life, comprises two classes: Insecta and arachnids Acari.Mosquito, fly, cockroach (blattaria), termite, flea, bedbug all belong to Insecta.The main harm of sanitary insect pest is sucked blood and is harassed and parasitism, and the sanitary insect pest of some kind is the communication media of some infectious disease of the mankind, very large to the health hazard of people, once outburst, easily forms epidemic situation.
Pirimiphos-methyl (Pirimiphos-methyl).Chemical name: O-O-dimethyl-O-(2-diethylin-6-methylpyrimidine-4-base)-phosphorothionate.
Pirimiphos-methyl is a kind of wide spectrum of ICI company exploitation in 1974, quick-acting organophosphorus insecticides and miticide, belongs to anticholinesterase.Have and tag and fumigation action.Its mechanism of action suppresses the activity of cholinesterase in organism, and it is without interior absorption.Effective to the various pests of coleoptera, diptera, Lepidoptera, Homoptera and mite class, it not only can prevent and treat grain storage insect and domestic hygiene insect effectively.It is one of agricultural chemicals hygienic insecticide of controlling at sanitary insect pest of World Health Organization WHO recommendation.The control that WHO tropical disease controls administration editor, " chemical prevention and control method of important Vector factors " middle promotion pirimiphos-methyl of publication is used for the sanitary insect pests such as mosquito, fly, mouse flea, Pulex irritans, bedbug, cockroach and mite.
The fusing point of pirimiphos-methyl industrial goods is 15 ~ 18 DEG C; Decompose during distillation; Vapour pressure 2mpa (20 DEG C); Relative density 1.17 (20 DEG C); Solvability is 9.9 (PH5.2) in water, 8.6 (PH7.3), and 9.3 (PH9.3) (being mg/l30 DEG C entirely), can be dissolved in most of organic solution as ethanol, acetone, alkyl halide; Can by strong acid and basic hydrolysis, half life period 7.5d ~ 35d (between pH value scope 5.8 ~ 8.5, the most stable during PH7), under daylight, the half life period of its aqueous solution is 1d; Flash-point >46 DEG C; The common formulation in market has: pulvis, missible oil, aerosol, aqueous emulsion.
Pyriproxyfen, diflubenzuron, triflumuron, d ichlorbenzuron etc. belong to insect growth regulator, IGR, can be good at that interference insect grows normally, casts off a skin, delayed development, thus cause normally casting off a skin, to grow and dead.
Pyriproxyfen (pyriproxyfen) chemical name: 4-phenoxy phenyl (RS)-2-(2-pyridine radicals oxygen) propyl ether, physicochemical property: fusing point: 45-47 DEG C, density: 1.32, condition of storage: 0-6 DEG C, sterling is crystallization.Vapour pressure 0.29 × 10-3Pa (20 DEG C), relative density 1.23 (20 DEG C).Solvability is: dimethylbenzene 50g, hexane 40g.Pyriproxyfen is the insect growth regulator, IGR upsetting insect growth, and have interior suction transfer activity, low toxicity, the lasting period is long, to crop safety, to fish low toxicity, and the feature little to eco-environmental impact.This product has good control efficiency to the sanitary insect pest such as fly, mosquito.Have and suppress mosquito, fly larvae pupation and emergence effect.Mosquito, fly larva contact this medicament, substantially all dead in pupa time, can not sprout wings.This medicament lasting period reaches about 1 month, and easy to use, free from extraneous odour, is good kill mosquito, fly medicine.Common preparation has: 0.5% granule, 10% missible oil.
Diflubenzuron (Diflubenzuron) fusing point 230 DEG C ~ 232 DEG C.Solvability: water 0.08mg/L (pH5.5,200C), acetone 6.5g/L (20 DEG C), dimethyl formamide 104g/L (25 DEG C), moderate is dissolved in polar organic solvent.Insecticidal mechanism: Main Function is the chitin synthesis suppressing insect cuticle, has again damage destruction to the internal secretion such as fat-body, corporal allata and body of gland simultaneously, thus hinder the smooth molt metamorphosis of insect.Cause accumulation property poisoning after pests, owing to lacking chitin, larva can not form new epidermis, difficulty of casting off a skin, and pupates to be obstructed; Adult is difficult to sprout wings, lay eggs; Ovum can not normal development, hatching larva epidermis lack hardness and dead.To other biological safety in people and animals and environment, belong to low toxicity public nuisance-free agricultural chemicals.
Triflumuron (Triflumuron) is a kind of insect growth regulator, IGR.It, to insect mainly stomach poison function, has certain action of contace poison, but without systemic action, has good ovicidal action.Triflumuron belongs to low toxic pesticide, and suppress insect chitin synthesis, make casting off a skin of insect pupate to be obstructed, activity slows down, and takes food minimizing, even dead.Main based on stomach toxicity, have certain action of contace poison concurrently, to most animals and humans nonhazardous effect, and can be decomposed by Institute of Micro-biology, because it is efficient, low toxicity and wide spectrum, become the principal item of current conditioning agent class agricultural chemicals.
D ichlorbenzuron (chlorbenzuron) belongs to insect growth regulator, IGR.By suppressing the activity of insect cuticle chitin synthetase and urine nucleosides coenzyme, suppressing insect chitin to synthesize thus causing insect normally not cast off a skin and dead.Use in larval phase, the new epidermis of insect is formed and is obstructed, delayed development, or lack hardness, normally can not cast off a skin and cause death or form lopsided pupa dead.To the hymenopteran such as beneficial insect and honeybee and Forest birds almost harmless.Also special efficacy is had to the larvae in control lavatory fly maggot, stagnant water gulf.
Some active ingredients of the frequent use of public health insecticide are all mainly pyrethroids, due to Long-Time Service, under the sanitary insect pest colony being is in the selection pressure of this insecticides for a long time, the gene of target organism is undergone mutation, the susceptibility of insecticide is constantly declined, cause pesticide resistance to produce, the difficulty of control continues to increase.Pirimiphos-methyl, as important health pest control medicine, especially demonstrates higher biologically active to the sanitary insect pest that chrysanthemum ester class has produced resistance.Pirimiphos-methyl is to the micro-poison of mammal, and to environment non-target organism safety, be a kind of excellent sanitary insect pest insecticide of high-efficiency low-toxicity, its benefit is invisible.Pyriproxyfen, diflubenzuron, d ichlorbenzuron etc. are a kind of insect growth regulator, IGRs, the people in environment for use and livestock safety, and the mechanism of action of himself has the sanitary insect pest such as fly, mosquito to suppress mosquito, fly larvae pupation and emergence effect simultaneously.If mosquito, fly larva contact this pyriproxyfen, substantially all dead in pupa time, and adult can not be sprouted wings into.With the exception of this, insect growth regulator, IGR antagonism insect (to organic phosphor, carbamate, organochlorine, pyrethroid insectide) activity does not have difference, can not be subject to the impact of resistance.
In the prior art, publication number is a kind of public health insecticide and preparation method thereof disclosed in CN101715783A patent publications, and it is a kind of complex composition of pirimiphos-methyl and gamma cyhalothrin chrysanthemum ester.The effervescent tablet that it is is active ingredient with the gamma cyhalothrin of 2.5% and 6% pirimiphos-methyl.Gamma cyhalothrin has individual shortcoming as a kind of hygienic insecticide, be exactly that the former medicine of pyrethroid is general all with the sensitization to human body, especially the skin of gamma cyhalothrin to human body has very strong sensitization, cause itch, redness, concerning the comfort level affected operator and livestock when it uses.Publication number is that 102657160A discloses " insecticide pirimiphos-methyl micro-capsule suspension and preparation method ", and its product is single-dose product, and effect composition is single compound, and capsule material uses shitosan-aliphatic poly ester material.Be that CN101848642A discloses " pesticide compositions " and provides pesticide compositions at publication number, comprise the former medicine complex preparation containing pirimiphos-methyl and a kind of plants essential oil and chrysanthemum ester class.
At " Agriculture in Hunan science " 2002(4) in " pirimiphos-methyl and malathion are to the synergistic effect of corn weevil and application thereof " literary composition, disclose a kind of complex composition of pirimiphos-methyl and malathion, be mainly used in the control of grain pest, its controlling object is corn weevil, red flour beetle, mainly adopts the occupation mode to fumigation of grain.Malathion belongs to a kind of agricultural chemicals of organic phosphates, and former medicine itself has garlic odour taste, and industrial goods itself have strong impulse nature and flavor road, use so be generally used in closed granary, can not as the health medication of human settlement.
In " pesticide research and the application " time: 2011 issues: the 6th phase; Author: in the people such as Tu Ximao deliver " complex coacervation prepares the research of a pirimiphos-methyl micro-capsule suspension " literary composition, first be the unit dose preparation of a pirimiphos-methyl, have employed complex coacervation and prepare microcapsule suspending agent, Encapsulating materials is the natural wall material such as gelatin, gum Arabic, but this kind of natural polymer Encapsulating materials form the function that capsule casing material is difficult to realize active ingredient in Co ntrolled release micro-capsule, because complex coacervation is more difficult control in actual production process, therefore seldom to have in business-like micro-capsule and adopt the method, preparation is unitary agent.In " pesticide research and the application " time: 2010 issues: the 4th phase; Author: in the people such as Li Yan deliver " development of a 20% pirimiphos-methyl microcapsule suspending agent " literary composition, adopting situ aggregation method to prepare the pirimiphos-methyl microcapsules that Lauxite is wall material, is a kind of single dose about pirimiphos-methyl.
Summary of the invention
In order to solve the problem, the object of the present invention is to provide the Pesticidal combination containing pirimiphos-methyl and microcapsule suspending agent thereof, adopt the organic phosphates pirimiphos-methyl of efficient, low toxicity, wide spectrum and carry out composite as the low toxicity compounds pyriproxyfen of insect growth regulator, IGR (protecting young parahormone class), d ichlorbenzuron, diflubenzuron, triflumuron, effectively can delay the sanitary insect pest such as blattaria, mosquitos and flies to develop immunity to drugs, adult and the double effect controlled of larva can be reached again.
Technical solution of the present invention is as follows:
The invention provides the Pesticidal combination containing pirimiphos-methyl, described Pesticidal combination comprises component A and B component, described component A is pirimiphos-methyl, described B component is selected from the one in pyriproxyfen, d ichlorbenzuron, diflubenzuron and triflumuron, and the mass ratio of described component A and B component is 100:1 ~ 2:1.
Pesticidal combination containing pirimiphos-methyl of the present invention, preferably the mass ratio of described component A and B component is 50:1 ~ 20:1, and synergistic effect is especially obvious.
Pesticidal combination containing pirimiphos-methyl of the present invention, most preferably the mass ratio of described component A and B component is 50:1, now co-toxicity coefficient 224.1, and synergistic effect is the most obvious.
Pesticidal combination containing pirimiphos-methyl of the present invention, preferably, the mass ratio of described pirimiphos-methyl and pyriproxyfen is 50:1 ~ 20:1, has good control efficiency to mosquitos and flies.
Pesticidal combination containing pirimiphos-methyl of the present invention, further preferably, the optimum quality ratio of described pirimiphos-methyl and pyriproxyfen is 50:1, and now co-toxicity coefficient is 224.1.
The present invention also provides a kind of and comprises the described microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination, comprises the component of following proportioning, by percentage to the quality:
Described active components A is pirimiphos-methyl, and described active component B is selected from the one in pyriproxyfen, d ichlorbenzuron, diflubenzuron and triflumuron.
The invention provides the microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination described in a kind of comprising, preferably, comprise the component of following proportioning, by percentage to the quality:
Described active components A is pirimiphos-methyl, and described active component B is selected from the one in pyriproxyfen, d ichlorbenzuron, diflubenzuron and triflumuron.
The invention provides the microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination described in a kind of comprising, most preferably, comprise the component of following proportioning, by percentage to the quality:
Described active components A is pirimiphos-methyl, and described active component B is selected from the one in pyriproxyfen, d ichlorbenzuron, diflubenzuron and triflumuron.
Microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination of the present invention, preferably, described solvent is selected from the one in methyl esters soybean oil, corn methyl esters oil, methyl esters palm oil, methyl esters cocoa butter, turpentine-based vegetable oil and fatty acid ester; Most preferably methyl esters soybean oil, methyl esters palm oil, turpentine-based vegetable oil.
Microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination of the present invention, preferably, described stabilizing agent is selected from the one in epoxidized soybean oil, 2,6-toluene di-tert-butyl phenols (BHT), butylated hydroxy anisole (BHA), triphenyl phosphite and potassium dihydrogen phosphate.
Microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination of the present invention, preferably, described attractant is selected from the one in 1-octyne-3-alcohol, fatty glyceride, glyceride lactate, lactolactone and amino acid.
Microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination of the present invention, preferably, described cyst material is selected from carbamide resin, melamine resin, polyurethane, polyesteramide, the one in aliphatic polyamide resin, polyvinyl acetate resin and polystyrene resin.
Microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination of the present invention, preferably, described dispersant is selected from the one in aromatic sulphonate, acrylic acid and acrylic ester copolymers, formaldehyde condensate sulfonate, copolymer-maleic anhydride sodium salt, polymerization of carboxylic acid sodium salt class, styrene alkyl polyoxyethylene ether phosphate and sodium lignin sulfonate.
Microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination of the present invention, preferably, described emulsifier is selected from the one of anhydrous sorbitol laurate, polyoxyethylene laurel ether, fatty alcohol-polyoxyethylene ether, polyoxyethylene monopalmitate and Emulsifier EL-60.
Microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination of the present invention, preferably, described antifreeze is selected from the one in ethylene glycol, propane diols, glycerine, isopropyl alcohol and urea, preferred propane diols.
Microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination of the present invention, preferably, described preservative is selected from the one in Sodium Benzoate and KF88.
Microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination of the present invention, preferably, described viscosity-controlling agent is selected from the one in xanthans, carragheen, gelatin, aluminium-magnesium silicate and bentonite, preferred xanthans.
Microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination of the present invention, preferably, described PH acid-base modifier is selected from the one in glacial acetic acid, citric acid, ammoniacal liquor, triethanolamine and sodium hydroxide.
Microcapsule suspending agent containing pirimiphos-methyl Pesticidal combination of the present invention, preferably, described water is deionized water or distilled water.
The application's Pesticidal combination itself has the insecticidal effect of good sanitary insect pest, said composition is after microencapsulation simultaneously, after being prepared into microcapsule suspending agent, good lasting effect is had when residual spray, the efficacy data of embodiment all illustrates this point, and this effect than common microcapsule suspending agent is well a lot.
The invention provides the microcapsule suspending agent formulation form being prepared applicable Pesticide use by above-mentioned composition, above-mentioned dosage formulation can also be prepared by known method, and the present composition also can be prepared as granule GR, wetting powder WP, suspension emulsion SE, microemulsion ME, aqueous emulsion EW or water dispersible granules WDG etc.
The invention provides a kind of hygienic insecticide for preventing and treating sanitary insect pest mosquito, fly, it is the complex preparation containing pirimiphos-methyl, its active ingredient comprises active components A and active component B, wherein active components A is pirimiphos-methyl, and active component B is any one in following insect growth regulator, IGR: pyriproxyfen, diflubenzuron, d ichlorbenzuron, triflumuron;
Embodiment of the present invention microcapsule suspending agent comprises the component of following weight proportion: be prepared into microcapsule suspending agent, is made up of active component, stabilizing agent, attractant, emulsifier, Encapsulating materials, dispersant, antifreeze, preservative, water; Basic components is as follows:
Component |
Mass percent |
Active components A |
0.1%~60% |
Active component B |
0.01%~10% |
Solvent |
0.5%~5% |
Stabilizing agent |
0.1%~3% |
Attractant |
0.01%~1% |
Emulsifier |
1%~3% |
Encapsulating materials |
3%~10% |
Dispersant |
1%~8% |
Antifreeze |
1%~5% |
Preservative |
0.1%~0.3% |
Thickener |
0.01%~0.3% |
Water |
Complement to ~ 100% |
Active components A in formula is pirimiphos-methyl, and the high-purity former medicine that former medicine purity is greater than more than 95%, almost do not make us unjoyful stink;
Active component B in formula is: wipe out the flies and mosquitoes, one in diflubenzuron, d ichlorbenzuron and triflumuron;
Solvent in formula does not use the dimethylbenzene, aromatic solvent naphtha, polar solvent etc. that use in traditional pesticidal preparations, and is the use of solvent methylated vegetable oil (as: methyl esters soybean oil, corn methyl esters oil, methyl esters palm oil, methyl esters coconut wet goods plant resource methyl esters oil), turpentine-based vegetable oil, the fatty acid ester etc. of environmental protection;
With the addition of stabilizing agent in the present invention, mainly because the special physico-chemical character of the former medicine of pirimiphos-methyl, pirimiphos-methyl is the same with other organophosphorus insecticide, and at memory period, also objective reality active ingredient holds labile problem.And then cause the decline of properties of product, cause product not reach pesticide supplying effect.As everyone knows, the factor mainly purity of former medicine and the stability of chemical constitution of organic phosphor phosphate pesticide stability is affected.The stabilizing agent Main Function of this recipe determination is: 1. the physics and the chemical stability that keep and strengthen the former medicine of pirimiphos-methyl; 2. be prevent gentle decomposition of separating the former medicine of pirimiphos-methyl.Mainly from following material, select one: epoxidized soybean oil, 2,6-toluene di-tert-butyl phenols (BHT), butylated hydroxy anisole (BHA), triphenyl phosphite, potassium dihydrogen phosphate;
Attractant: the insecticide that the present invention relates to a kind of sanitary insect pest, so add some attractants wherein, its action principle is the odiferous information of sex attractant and the secretion of simulation domestic animal, so that better to the attracting action of mosquitos and flies after administration, what attract the contact of mosquito and fly licks probability, thus improves insect killing efficiency.Select from following component: 1-octyne-3-alcohol, fatty glyceride, glyceride lactate, lactolactone, amino acid etc.;
Cyst material in formula is carbamide resin, melamine resin, polyurethane, polyesteramide, aliphatic polyamide resin, polyvinyl acetate resin, polystyrene resin;
Dispersant in formula selects the one in aromatic sulphonate, acrylic acid and acrylic ester copolymers, formaldehyde condensate sulfonate, copolymer-maleic anhydride sodium salt, polymerization of carboxylic acid sodium salt class, styrene alkyl polyoxyethylene ether phosphate, sodium lignin sulfonate;
The one of anhydrous sorbitol laurate, polyoxyethylene laurel ether, fatty alcohol-polyoxyethylene ether, polyoxyethylene monopalmitate, Emulsifier EL-60 selected by emulsifier in formula;
The antifreeze used in formula is ethylene glycol, propane diols, glycerine, isopropyl alcohol, urea, preferred propane diols;
Preservative in formula: the one in Sodium Benzoate, KF88;
Viscosity-controlling agent in formula is selected from xanthans, carragheen, gelatin, aluminium-magnesium silicate, bentonite, our preferred xanthans;
The PH acid-base modifier used in formula is glacial acetic acid, one in citric acid, ammoniacal liquor, triethanolamine, sodium hydroxide;
The water adopted in this production technology: be deionized water or distilled water.
The technique effect that the present invention is useful:
Pesticidal combination containing pirimiphos-methyl provided by the invention and microcapsule suspending agent thereof adopt that organic phosphates is efficient, the low toxicity compounds pyriproxyfen of the pirimiphos-methyl of low toxicity, wide spectrum and insect growth regulator, IGR (protecting young parahormone class), d ichlorbenzuron, diflubenzuron, triflumuron are composite, effectively can delay the sanitary insect pest such as blattaria, mosquitos and flies to develop immunity to drugs, adult and the double effect controlled of larva can be reached again.
Instant invention overcomes the deficiency containing single-activity component insecticide, to the blattaria developed immunity to drugs because of long-term prescription, mosquito, fly, termite, flea etc., there is double anti-effect, reduce formulation rate simultaneously, reduce drug cost and the pollution to environment.
The microcapsule suspending agent tool of the Pesticidal combination containing pirimiphos-methyl provided by the invention has the following advantages: by (1) after this Pesticidal combination after microencapsulation owing to thus having the longer lasting period to the Co ntrolled release of active ingredient pirimiphos-methyl, reduces the number of times of dispenser; (2) active ingredient is wrapped in cyst wall and improves safety, makes preparation reduce toxic grade; (3) active component B belongs to insect growth regulator, IGR steroids former medicine, and after being wrapped in capsule casing material, slow releasing contributes to extending and controls mosquito, the emergence time of fly and larvae pupation in the environment; (4) some unhappy smells and skin irritating substances is effectively reduced; (5) minimizing brings the loss of active ingredient because steam volatilizees.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, the following specific embodiment of the present invention is described, but the present invention is limited to absolutely not these examples.The following stated is only the good embodiment of the present invention, only for explaining the present invention, therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that all any amendments done within the spirit and principles in the present invention, be equal to alternative and improvement etc., all should be included within protection scope of the present invention.
Preparation of the present invention is the processing method by existing formulations of pesticide comparative maturity, by pirimiphos-methyl and the common method such as pyriproxyfen, auxiliary agent, make the preparations such as glue bait formulation, wetting powder, aqueous emulsion, suspension emulsion, missible oil, microemulsion, microcapsule suspending agent, ultra low volume spraying agent in the ratio in embodiment.The preferred microcapsule suspending agent of the present invention is inventive embodiments.Reagent used is commercial.In these embodiments apart from outside specified otherwise, all percentage is weight ratio
The determination of activity report of embodiment 1 laboratory:
Experiment purpose:
To make a living mark target with the monochromatic Ability of Culex Pipiens Larvae of laboratory rearing, the mixed agent measuring each single dose and pirimiphos-methyl and pyriproxyfen, to the virulence of monochromatic Ability of Culex Pipiens Larvae, calculates composite mixture co-toxicity coefficient, determines that synergistic effect is strong and weak.
Assay method:
Measure the larva eradicative rate of each process, calculate composite mixture co-toxicity coefficient.The index of correlation that comprehensive analysis is managed everywhere, the proportioning that selective advance effect is strong.By mosquito larvae being immersed in the 24h lethality obtained in different liquids, obtain LC50.
1, test material: test tools: dilute liquid medicine with 50ml volumetric flask several, some, adjustable pipette, some, the beaker of all size, the suction pipe number selecting larva props up.Insecticide: the preparation selecting pure medicine or high concentration take acetone as solvent, first medicament is configured to 1% mother liquor control Refrigerator store for subsequent use.Be configured to the mother liquor of 0.1% during experiment again, when configuration needs concentration, all press active ingredient calculating; For test worm: monochromatic culex, 4 instar larvaes.
2. method of testing: immersion method, selects 4 instar larvaes to put into small beaker, 20 every glass, then supplies water yield 50ml.Each large beaker adds 200ml dechlorination running water.Every beaker is answered labeled test medicine name and concentration value.Then, the liquid of the variable concentrations be configured in volumetric flask, therefrom draw 1ml respectively with pipette, in liquid instillation water, then stir evenly with glass bar.At this moment larva in measuring cup is all poured in beaker together with 50ml water, add up to into the 250ml aqueous solution.Each concentration has 3 repetitions at least, and arranges control group, same instillation blank solvent liquid.Death toll is checked after 24h.When checking dead larvae quantity, available tip tweezers touch lose favour head and afterbody respiratory siphon gently, if slow in reacting and can not floating to level, or the larva of the thick seemingly-dead dress of language, calculate in the lump in death toll.Error Pass Test requirement, then available Abbott knows together corrected mortality calculate LD50.
Carry out statistical analysis with DPS data processing software, calculate the LC50(half lethal concentration of each medicament) and reagent agent EC50(half-maximal effect concentration), then press the abundant method of Sun Yun and calculate co-toxicity coefficient (CTC).
When CTC≤80, then composition shows as antagonism, works as 80<CTC<120, then composition shows as summation action, and when CTC >=120, then composition shows as synergistic effect.
Actual measurement toxicity index (ATI)=(standard agent EC50/ reagent agent EC50) × 100;
In theoretical toxicity index (TTI)=A medicament toxicity index × mixture A percentage composition+B medicament toxicity index × mixture in the percentage composition of B;
Co-toxicity coefficient (CTC)=[the theoretical toxicity index (TTI) of mixture actual measurement toxicity index (ATI)/mixture] × 100;
Different disposal is to the Toxicity Determination result of monochromatic Ability of Culex Pipiens Larvae
Four, discussion of results
In the scope of the weight proportion 100:1 ~ 2:1 of pirimiphos-methyl and pyriproxyfen, between the obvious weight proportion 50:1 ~ 20:1 of synergistic effect, methyl Midinyanglin and pyriproxyfen complex preparation (50:1) monochromatic Ability of Culex Pipiens Larvae is selected to carry out toxicity test, its co-toxicity coefficient is 224.1, and synergistic effect is especially obvious.
The determination of activity report of embodiment 2 laboratory:
Control mosquito, fly indoor pharmacodynamic test; Test target: Culex pipiens pallens, the 3rd day ~ female insect of not sucking blood for the 5th day after sprouting wings; Housefly, the adult sprouted wings latter 3rd ~ 4 days, female, hero half and half; Test method: with reference to GB T13917.10-2009, cage test; Experiment process: preparation diluent is to equal working concentration.
Result of the test shows: the single dose missible oil of control sample 9,10 for the drug effect of mosquito, fly at the composite sample of knocking down property not as 1 ~ 8, but the composite sample of pirimiphos-methyl and pyriproxyfen is fine to the down effect of mosquitos and flies, and good lethality rate in addition.
Data result can be found out: at pirimiphos-methyl and pyriproxyfen is composite all reaches more than 95% to mosquitos and flies 24h lethality rate preventive effect, kills mosquitos and flies respond well.Meet 24h mosquitos and flies lethality rate and reach 100%, simultaneously in knocking down property KT50min reasonable weight proportion between 50:1 ~ 20:1.
This combines composite preparation, reasonable control efficiency is had to the sanitary insect pest such as mosquito, fly, there is good rate of knockdown to have again good lethality rate simultaneously, put at control sanitary insect pest and exempt to have significant synergies, the usage amount of preparation can be reduced, cost-saving, delay the drug-fast generation of sanitary insect pest simultaneously.
Embodiment 1:
Active components A pirimiphos-methyl 6g, active component B d ichlorbenzuron 0.06g joins in solvent 2g methyl esters soybean oil and stirs, after add stabilizing agent epoxidized soybean oil 0.2g, emulsifier fatty alcohol-polyoxyethylene ether 1g again, attractant 1-octyne-3-alcohol 0.02%, adds encystation monomer toluene di-isocyanate(TDI) 2g and stirs and obtain oil phase; Dispersant polymerization of carboxylic acid sodium salt class 2g and antifreeze ethylene glycol 5%, preservative KF88 0.1%, thickener xanthans 0.3%g are added to the water (water complements to 100g) stir and obtain aqueous phase; By oil, water preheat to 40 DEG C, then pour oil phase into aqueous phase and open emulsify at a high speed, by the time stable emulsion, keeps temperature 6 hours, adopts interfacial polymerization to obtain the 6.06% pirimiphos-methyl d ichlorbenzuron microcapsule suspending agent (active components A: active component B=100:1) that carbamide resin is capsule material.
Embodiment 2:
Active components A pirimiphos-methyl 24g, active component B pyriproxyfen 0.3g joins in solvent 4g rosinweed oil and stirs, after add stabilizing agent triphenyl phosphite 0.3g, emulsifier polyoxyethylene castor oil 1g again, attractant glyceride lactate 0.1g, adds encystation monomer toluene di-isocyanate(TDI) 4g and stirs and obtain oil phase; Dispersant acrylic acid and acrylic ester copolymers 5g and antifreeze propane diols 5%, preservative sodium benzoate 0.1%, thickener xanthans 0.2g are added to the water (water complements to 100g) stir and obtain aqueous phase; By oil, water preheat to 45 DEG C, then pour oil phase into aqueous phase and open emulsify at a high speed, by the time stable emulsion, keeps temperature 4 hours, adopts interfacial polymerization to obtain the 24.3% pirimiphos-methyl pyriproxyfen microcapsule suspending agent (active components A: active component B=80:1) that carbamide resin is capsule material.
Embodiment 3:
Active components A pirimiphos-methyl 30g, active component B pyriproxyfen 0.6g joins in solvent 2.5g rosinweed oil and stirs, after add emulsifier polyoxyethylene bay ether 2g again, attractant fatty glyceride 0.1g stirs and obtains oil phase; Antifreeze glycerine 3g, stabilizing agent potassium dihydrogen phosphate 0.2g, encystation performed polymer formaldehyde-urea performed polymer 10g be added to the water (water complements to 100g) stir and obtain aqueous phase; By oil, water preheat to 60 DEG C, then pour oil phase into aqueous phase and open emulsify at a high speed, by the time stable emulsion, adding watery hydrochloric acid in batches regulates pH=2.5 that polycondensation reaction occurs, keep temperature 4 hours, again dispersant sodium lignin sulfonate 6g, thickener carragheen 0.2%g, preservative sodium benzoate 0.2% are added and stir, change example and adopt situ aggregation method to obtain the 30.6% pirimiphos-methyl pyriproxyfen microcapsule suspending agent (active components A: active component B=50:1) that Lauxite is capsule material.
Embodiment 4:
Active components A pirimiphos-methyl 60g, active component B diflubenzuron 2g joins in solvent 2g methyl esters palm oil and stirs, after add stabilizing agent BHA0.3g, emulsifier anhydrous sorbitol laurate 1g again, attractant lactolactone 0.1, add Encapsulating materials 4,4-methyl diphenylene diisocyanate 6g to stir and obtain oil phase; Dispersant copolymer-maleic anhydride sodium salt 2g and antifreeze ethylene glycol 1g, preservative KF88 0.1%, thickener xanthans 0.01g are added to the water (water complements to 100g) stir and obtain aqueous phase; By oil, water preheat to 40 DEG C, then pour oil phase into aqueous phase and open emulsify at a high speed, by the time stable emulsion, keeps temperature 8 hours, adopts interfacial polymerization to obtain the 62% pirimiphos-methyl diflubenzuron microcapsule suspending agent (active components A: active component B=30:1) that carbamide resin is capsule material.
Embodiment 5:
Active components A pirimiphos-methyl 40g, active component B pyriproxyfen 2g joins in solvent 4g methyl esters cocoa butter and stirs, after add stabilizing agent BHT0.1g, emulsifier polyoxyethylene monopalmitate 2g again, attractant amino acid 0.1g stirs and obtains oil phase; Dispersant lignosulfonates 4g and antifreeze glycerine 3g, preservative KF88 0.2g, Encapsulating materials polyvinyl acetate emulsion 4g, thickener xanthans 0.05g are added to the water (water complements to 100g) stir and obtain aqueous phase; By oil, water preheat to 60 DEG C, then pour oil phase into aqueous phase and open emulsify at a high speed, by the time stable emulsion, keep temperature 4 hours, adopt suspension polymerization to obtain the 42% pirimiphos-methyl pyriproxyfen microcapsule suspending agent (active components A: active component B=20:1) that polyvinyl acetate resin is capsule material.
Embodiment 6:
Active components A pirimiphos-methyl 10g, active component B triflumuron 1g joins in solvent 1g corn methyl esters oil and stirs, after add emulsifier fatty alcohol-polyoxyethylene ether 1g again, attractant 1-octyne-3-alcohol 0.1g stirs and obtains oil phase; Antifreeze propane diols 5g, stabilizing agent potassium dihydrogen phosphate 0.1g, encystation performed polymer melamine-formaldehyde performed polymer 5g be added to the water (water complements to 100g) stir and obtain aqueous phase; By oil, water preheat to 45 DEG C, then pour oil phase into aqueous phase and open emulsify at a high speed, by the time stable emulsion, adding watery hydrochloric acid in batches regulates pH=3.5 that polycondensation reaction occurs, keep temperature 6 hours, again dispersant sodium lignin sulfonate 3g, thickener xanthans 0.3%g, preservative sodium benzoate 0.2% are added and stir, change example and adopt situ aggregation method to obtain the 11% pirimiphos-methyl triflumuron microcapsule suspending agent (active components A: active component B=10:1) that melamine resin is capsule material.
Embodiment 7:
Active components A pirimiphos-methyl 0.5g, active component B diflubenzuron 0.1g joins in solvent 10g methyl esters cocoa butter and stirs, after add stabilizing agent epoxidized soybean oil 0.2g, emulsifier anhydrous sorbitol laurate 2g again, attractant amino acid 0.1g stirs and obtains oil phase; By dispersant according to carboxylate 3g and antifreeze ethylene glycol 5g, preservative KF88 0.2g, triethanolamine 0.1g, thickener xanthans 0.3g, encystation monomer styrene emulsion 0.4g be added to the water (water complements to 100g) stir and obtain aqueous phase; By oil, water preheat to 35 DEG C, then pour oil phase into aqueous phase and open emulsify at a high speed, by the time stable emulsion, keeps temperature 8 hours, adopts suspension polymerization to obtain the 0.6% pirimiphos-methyl diflubenzuron microcapsule suspending agent (active components A: active component B=5:1) that polystyrene resin is capsule material.
The residual spray pharmacodynamic results of embodiment 1 ~ 7 pair of housefly, Culex pipiens pallens:
Assay method: carry out according to GB13917.1-92.By sample by a certain percentage with after distilled water diluting, effective dose is recommended to be coated on breadboard face routinely, the breadboard face of dispenser is at room temperature deposited, and with dispenser after the 1st day, 7 days, 30 days, employing forces contact method, makes examination worm contact plate face 30min with the contactor that forces being parallel to plate face, then examination worm is moved to clean raising in cylinder, clean cage and raises, observed and recorded Culex pipiens pallens 24h lethality, housefly 24h lethality.Test in triplicate, carries out blank test, gets rid of error.With Abbott formulae discovery corrected mortality.
Pharmacodynamic results: the active component A pirimiphos-methyl active component B microcapsule suspending agent that this embodiment 1 ~ 7 prepares is applied to the control of Culex pipiens pallens, housefly.Embodiment medicament is coated on plate face by recommendation concentration ratio thin up, recommended density 1 ~ the 2g(a.i of residual spray control housefly, Culex pipiens pallens pirimiphos-methyl preparation active ingredient)/m2,1 day, 7 days and 30 days control efficiency to sanitary insect pest after statistics medicine.Result is as follows:
As can be seen from the table, by pirimiphos-methyl by composite pyriproxyfen, diflubenzuron, triflumuron etc., good synergistic effect is obtained to sanitary insect pest, the low resistance delaying insect and produce pesticide control can effectively be fallen, can effectively extend the control time by the complex preparation after microencapsulation, obtain good residual spray effect.To in the quick-acting killed of mosquitos and flies and lasting effect significantly better than single dose.
The composite microcapsule suspending agent of combination of the present invention contrasts with the 30% pirimiphos-methyl microcapsule suspending agent single dose contrasted, be not difficult to find out composite after composition to the control efficiency of mosquitos and flies more, time (7d, 30d) same after residual spray, control efficiency is all better than microcapsule suspending agent single dose.Expand desinsection pedigree by composite, delayed the pesticide resistance of sanitary insect pest, improve the lasting effect of residual spray.