CN114568435A - Pesticide composition containing spiromesifen and application thereof - Google Patents
Pesticide composition containing spiromesifen and application thereof Download PDFInfo
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- CN114568435A CN114568435A CN202210282033.4A CN202210282033A CN114568435A CN 114568435 A CN114568435 A CN 114568435A CN 202210282033 A CN202210282033 A CN 202210282033A CN 114568435 A CN114568435 A CN 114568435A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/06—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings
- A01N43/12—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings condensed with a carbocyclic ring
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention discloses a pesticide composition containing spiromesifen, which comprises active ingredients A and B, wherein the active ingredients A are spiromesifen, the active ingredients B are compounds shown in a formula I, and the mass ratio of the active ingredients A to the active ingredients B is 1: 25-25: 1. The pesticide composition disclosed by the invention is safe to target organisms, has good quick-acting property and can effectively prevent and control various plant pests.
Description
Technical Field
The invention relates to the technical field of pesticide compounding, and particularly relates to a pesticide composition containing spiromesifen and application thereof.
Background
Greenhouse whitefly (Westwood), which belongs to insects in the family of homoptera whitefly, is distributed and harmed all over the world and is a main pest cultivated in a protected area, and the juice of adult and nymph sucking plants of greenhouse whitefly is faded green and yellowed by harmful leaves. The greenhouse trialeurodes vaporariorum has strong reproductive capacity, high propagation speed, large population quantity and cluster hazard, and can secrete a large amount of honeydew to pollute leaves, hinder photosynthesis and respiration of plants, cause leaf wilting and reduce commodity value of vegetables.
Pear Psylla (Psylla chinensis), belonging to the homoptera and psyllidae, is widely distributed in Shandong, Hebei, Henan and other areas, and is mainly used for weakening the vigor of pear trees, early leaf fall and fruit pollution to cause thickening of peels and reduction of quality by piercing and sucking leaves, fruits and twigs of the pear trees, so that the pear Psylla is more serious in disease incidence in northern pear areas, influences flower bud formation and next-year yield and becomes a main pest in pear producing areas.
The spiromesifen is a spirocyclic tetronic acid type insecticidal and acaricidal agent developed by Bayer company, has a unique spirocyclic tetronic acid structure, a novel action mechanism and excellent insecticidal and acaricidal activity, can penetrate into the cuticles of plant leaves, has the performance of rain wash resistance, has the action mechanism of influencing the development of pests, interfering the biosynthesis of liposomes of the pests, particularly having better biological activity on larval stages, and simultaneously can generate the closing action of ovarian ducts, reduce the reproductive capacity of the pests and greatly reduce the number of spawning. The structural formula is as follows:
the chemical name of the compound of the formula (I) is 3-bromo-1- (3-chloropyridin-2-yl) -N- [4, 6-dichloro-3-fluoro-2- (methylcarbamoyl) phenyl]-1H-pyrazole-5-carboxamide, empirical formula: c17H10BrCl3FN5O2. Belongs to benzamide pesticide, can efficiently activate an insect ryanodine (muscle) receptor to excessively release calcium ions in a calcium reservoir in cells, and leads the insects to die by paralysis. High activity to lepidoptera pest larva, broad spectrum and high durability. The structural formula is as follows:
chemical control is used as a main control means in agricultural pest control, but long-term application of the pesticide results in that target pests have different degrees of drug resistance to various pesticides. The chemical agent is scientifically and reasonably compounded or mixed, the development of the drug resistance of pests can be delayed to a certain extent, the insecticidal activity of the effective components can be obviously improved, and the service life of the agent is prolonged. Through a large number of experiments, the applicant finds that the combination of the spiromesifen and the 3-bromo-1- (3-chloropyridine-2-yl) -N- [4, 6-dichloro-3-fluoro-2- (methylcarbamoyl) phenyl ] -1H-pyrazole-5-formamide has an obvious synergistic effect on various target pests, the dosage is reduced, and the drug residue is reduced.
Disclosure of Invention
Based on the situation, the invention aims to provide a pesticide composition containing spiromesifen and a preparation thereof, which are mainly used for controlling plant pests, particularly hemiptera pests, and can enhance the pesticide effect and reduce the dosage.
In order to achieve the purpose, the invention provides a pesticide composition containing spiromesifen, which comprises an active component A and an active component B, wherein the active component A is the spiromesifen, and the active component B is a compound shown as a formula (I):
further, the mass ratio of the active ingredient A to the active ingredient B is 1: 15-15: 1;
further, the mass ratio of the active ingredient A to the active ingredient B is 1: 12-10: 1;
further, the sum of the content of the active ingredient A and the content of the active ingredient B in the pesticide composition is 1-80 wt% based on 100 wt% of the total weight of the pesticide composition;
further, the pesticide composition comprises an auxiliary agent besides the active ingredient, wherein the auxiliary agent is selected from one or more of a wetting agent, a dispersing agent, an emulsifying agent, a thickening agent, a disintegrating agent, an antifreezing agent, an antifoaming agent, a solvent, a preservative, a stabilizing agent, a synergist or a carrier;
further, the wetting agent is selected from one or more of a wetting agent selected from alkyl benzene sulfonate, alkyl naphthalene sulfonate, lignosulfonate, sodium dodecyl sulfate, dioctyl sodium sulfosuccinate, alpha-olefin sulfonate, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol ethoxylate, fatty alcohol polyoxyethylene ether sodium sulfate, silkworm excrement, Chinese honeylocust powder, soapberry powder, SOPA, a detergent, an emulsifier 2000 series and a wetting penetrating agent F; and/or
The dispersing agent is selected from one or more of lignosulfonate, alkyl naphthalene sulfonate formaldehyde condensate, naphthalene sulfonate, tristyrylphenol ethoxylate phosphate ester, fatty alcohol ethoxylate, alkylphenol polyoxyethylene ether methyl ether condensate sulfate, fatty amine polyoxyethylene ether, glycerol fatty acid ester polyoxyethylene ether, polycarboxylate, polyacrylic acid, phosphate, EO-PO block copolymer and EO-PO graft copolymer; and/or
The thickening agent is selected from one or more of xanthan gum, polyvinyl alcohol, organic bentonite, magnesium aluminum silicate and carboxymethyl cellulose; and/or
The disintegrating agent is selected from one or more of sodium sulfate, ammonium sulfate, aluminum chloride, sodium chloride, ammonium chloride, bentonite, glucose, sucrose, starch, cellulose, urea, sodium carbonate, sodium bicarbonate, citric acid and tartaric acid; and/or
The emulsifier is selected from one or more of fatty alcohol polyoxyethylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, phenethyl phenol polyoxyethylene polyoxypropylene ether, alkylphenol polyoxyethylene, fatty amine polyoxyethylene ether, alkylbenzene sulfonate, styryl phenol polyoxyethylene ether and fatty acid polyoxyethylene ester; and/or
The defoaming agent is selected from silicone oil and C10~C20Saturated fatty acid compound, C8~C10One or more of fatty alcohol compounds or silicone compounds; and/or
The preservative is selected from one or more of sorbic acid, sorbic acid sodium salt, sorbic acid potassium salt, benzoic acid sodium salt, parahydroxybenzoic acid sodium salt and parahydroxybenzoic acid methyl ester; and/or
The stabilizer is selected from one or more of disodium hydrogen phosphate, oxalic acid, succinic acid, adipic acid, borax, 2, 6-di-tert-butyl-p-cresol, epoxidized vegetable oil; and/or
The synergist is selected from synergistic phosphorus and synergistic ether; and/or
The carrier is selected from one or more of kaolin, bentonite, attapulgite, light calcium carbonate, diatomite and white carbon black; and/or
The solvent is selected from one or more of benzene, toluene, xylene, methanol, ethanol, isopropanol, N-butanol, diesel oil, N-dimethylformamide, cyclohexanone, ethyl acetate, N-methylpyrrolidone, propanol, butanol, ethylene glycol, diethylene glycol, ethylene glycol methyl ether, butyl ether, solvent oil, vegetable oil derivatives and deionized water; and/or
Further, the pesticide composition can be prepared into any agriculturally acceptable dosage form, and the dosage form is a solid preparation, a liquid preparation or a seed treatment preparation;
further, the solid preparation is a direct-use solid preparation, a dispersible solid preparation or a soluble solid preparation;
further, the directly used solid preparation is powder, granules, pellets, tablets or bars;
the dispersible solid preparation is wettable powder, oil dispersible powder, emulsion powder, water dispersible granules, emulsion granules or water dispersible tablets;
the soluble solid preparation is soluble powder, soluble tablets or soluble granules;
further, the liquid preparation is a solution preparation, a dispersion liquid preparation, an emulsion preparation, a suspension preparation or a multi-phase preparation;
further, the solution preparation is soluble agent, soluble colloid, oil agent or spreading oil agent;
the dispersion liquid preparation is missible oil, latex, dispersible agent or paste;
the emulsion preparation is an aqueous emulsion, an oil emulsion, a microemulsion or a fat agent;
the suspension preparation is a suspending agent, a microcapsule suspending agent, an oil suspending agent or a dispersible oil suspending agent;
the multi-phase preparation is a suspending emulsion, a microcapsule suspension-suspending agent, a microcapsule suspension-water emulsion or a microcapsule suspension-suspending emulsion;
further, the seed treatment preparation comprises a seed treatment solid preparation or a seed treatment liquid preparation;
further, the seed treatment solid preparation is seed treatment dry powder or seed treatment dispersible powder;
the seed treatment liquid preparation is a seed treatment liquid agent, a seed treatment emulsion or a seed treatment suspending agent;
furthermore, the dosage form is a liquid preparation which is a suspending agent or an aqueous emulsion, and the solid preparation is wettable powder.
The invention also discloses application of the pesticide composition in controlling plant pests.
Further, the plant pest is a Hemiptera (Hemiptera) pest;
further, said Hemiptera (Hemiptera) pests include, but are not limited to, aphids (Aphis), scale (scales), whiteflies (whiteflies), leafhoppers (leafhoppers), pea aphids (acrythophon pisum) (pisum aphid), coccidiodes species (adegels spp), Aleurodes brassicae (Aleurodes proteella), Aleurodicus spirifera (Aleurodicus disperceus), aleuropilus velocus (aleurothrix florosus), verticillium species (aleurospira spp.), red round beetles (Aonidiella aurantiani), aphids species (Aphis spp.), cotton aphids (Aphis gossypii), apple aphids (Aphis pomphoides), potato aphids (asparagus aphid), aphids (apple aphid), aphid (aphid sporus), cotton aphid (aphid gossypii), cotton aphid (aphid gossypium), cotton aphid (aphid) and aphid), cotton plant (beard), cotton plant (aphid), rice plant louse (aphid), rice plant (rice plant), rice plant louse (rice plant, rice, long pipe aphid species (Macrosiphum spp.), Long pipe aphid (Macrosiphum euphocae), Long pipe aphid (Macrosiphum grandiflora), Long pipe aphid (Macrosiphum grandirum), Long pipe aphid (Macrosiphum rosae), Mahanarva frimyola, Nephophora graminis (Metholophilum dirhodum), Micts longicornis, Ottura nodorum species (Myzus spp.), Myzus persicae (Myzus persicae), Nephophora species (Nephotettix spp.), Nephotephophora nigra (Nephotettx cinctipes), Nilavata lugens), Pisca pellus (Parapelothyria pergami), Myxophysa species (Pholeys spp.), Photinus spp., Rhizopus spp.), Photinus spp
(Pseudococcus spp.), Verticillium brevicornum (Pseudococcus braviceps), Pieris piricola (Quadraspidium perniciosus) (Pieris pyrena (San Jose scale)), Aphis pellucida (Rhopalosiphum spp.), Zea mays (Rhopalosiphum maida), Aphis graminearum (Rhaparosiphum padi), Paralymus species (Saissetia spp.), Sclerotia elegans (Saissetia oleraceae), Schizophilus graminis (Schizophis graminum), Aphis graminis (Sitobion avenae), Pecticola (Sogatella furcifera), Paralygus paraguas (Rhizopus pyla), Paralygus viridis (Trigonococcus spp.), Trigonopsis viridis (Trigonopsis viridis), Trigonopsis viridis (Trigonopsis farina), Trigonopsis fargeum spp.).
Further, the hemipteran pest is a sternorrhyncha (sternorrhynchha) pest;
further, the pests of the suborder sternorrhyncha are pests of the family Psyllidae (Psyllidae) and/or pests of the family Aleyrodidae (Aleyrodidae);
furthermore, the pests of the psyllidae are psyllids pyricularis, and the pests of the whitefly family are greenhouse trialeurodes vaporariorum.
Further, the pesticide composition is applied to the pests or the medium in which the pests need to be controlled in an effective dose.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) the insecticidal composition obtained by compounding the spiromesifen and the compound shown in the formula I has an obvious synergistic effect, and can effectively control various plant pests;
(2) the insecticidal composition has good quick-acting property and long lasting period, and can effectively delay the generation of drug resistance of pests;
(3) the insecticidal composition is safe to crops and non-target organisms, and simultaneously reduces the use amount of pesticides and the use cost.
Detailed Description
Preparation examples of the formulations
Preparation example 1: 36% spiromesifen-compound wettable powder (3:1) of formula I
27% of spiromesifen, 9% of a compound of formula I, 8% of sodium lignosulphonate, 3% of sodium dodecyl sulfate, 4% of a dispersant NNO and the balance of kaolin.
The preparation method comprises the following steps: the active ingredients, the dispersing agent, the wetting agent and the filler are mixed according to the formula proportion, evenly stirred in a stirring kettle, and smashed and evenly mixed for many times by a jet mill, so as to prepare the wettable powder.
Preparation example 2: 30% spiromesifen-compound wettable powder (1:2) of formula I
The composition comprises, by weight, 10% of spiromesifen, 20% of a compound of formula I, 10% of calcium lignosulfonate, 2% of a naphthalenesulfonate formaldehyde condensate sodium salt, 3% of nekal BX, and the balance kaolin.
The preparation method comprises the following steps: the same as in preparation example 1.
Preparation example 3: 10% spiromesifen-compound aqueous emulsion of formula I (3:2)
The composition comprises, by weight, 6% of spiromesifen, 4% of a compound of formula I, 8% of tristyrylphenol polyoxyethylene ether polyoxypropylene ether, 2% of phenethylphenol polyoxyethylene ether phosphate, 15% of cyclohexanone, 0.1% of xanthan gum, 5% of ethylene glycol, 0.2% of benzoic acid and the balance of deionized water.
The preparation method comprises the following steps: adding the active ingredients, a solvent, an emulsifier and a cosolvent together according to the formula proportion to dissolve the active ingredients into a uniform oil phase; mixing part of water, antifreeze and other pesticide auxiliaries together to form a uniform water phase; adding the oil phase into the water phase while stirring at high speed in the reaction kettle, and after uniformly stirring, starting a shearing machine to shear at high speed for about half an hour to form the oil-in-water emulsion in water.
Preparation example 4: 12% spiromesifen-compound aqueous emulsion of formula I (1:1)
The composition comprises, by weight, 6% of spiromesifen, 6% of a compound of formula I, 16% of acetophenone, 5% of alkylaryl polyoxyethylene polyoxypropylene ether, 0.1% of xanthan gum, 5% of ethylene glycol, 0.1% of benzoic acid and deionized water for balancing.
The preparation method comprises the following steps: the same as in preparation example 3.
Preparation example 5: 20% of spiromesifen, a compound of formula I suspending agent (2:3)
The composition comprises, by weight, 8% of spiromesifen, 12% of a compound of formula I, 2% of fatty alcohol-polyoxyethylene ether, 3% of sodium lignosulfonate, 3% of alkylphenol polyoxyethylene phosphate, 2% of sodium polycarboxylate, 5% of glycerol, 1% of magnesium aluminum silicate, 0.2% of xanthan gum, 2% of sodium sorbate, 0.5% of silicone oil and the balance deionized water.
The preparation method comprises the following steps: according to the formula proportion, the active ingredients, the surfactant and other functional additives are sequentially placed in a reaction kettle, water is added for uniform mixing, and the product is obtained through high-speed shearing, wet sanding and finally homogeneous filtration.
Preparation example 6: 16% spiromesifen, Compound of formula I suspension (1:7)
The composition comprises, by weight, 2% of spiromesifen, 14% of a compound of formula I, 4% of alkylphenol polyoxyethylene, 3% of styryl phenol polyoxyethylene ether phosphate, 3% of a naphthalenesulfonate formaldehyde condensate, 0.5% of magnesium aluminum silicate, 0.2% of xanthan gum, 5% of ethylene glycol, 0.01% of benzisothiazolinone potassium, 0.5% of silicone oil and the balance of deionized water.
The preparation method comprises the following steps: the same as in preparation example 5.
Indoor activity test:
example 1: indoor activity test of spiromesifen and compound of formula I on psylla chinensis
The test method comprises the following steps: the leaf soaking method is adopted.
Test targets: chinese pear Psylla (Psylla chinensis Yang et Li) imago, a test insect source is a population for continuously breeding and propagating multiple generations indoors by a group research and development center.
Test reagents: 95% of the compound of formula I and 98% of the spiromesifen are provided by the Helier pharmaceutical industry group research and development center.
Preparing a medicament: preparing single-dose mother liquor respectively, designing proper proportion according to the mixing purpose and the medicament activity, and preparing the single dose and each group of proportion mixed dose into required series of mass concentrations.
The test steps are as follows:
(1) preparing a test material: selecting the insect-free pear leaves which grow well, are complete in shape and uniform in growth, washing off surface dust, and drying in the shade for later use.
(2) Medicament treatment: the method comprises the steps of soaking clean pear leaves in liquid medicine with various concentrations for 10s, setting a Tween 80 aqueous solution which does not contain a medicament and contains a corresponding solvent as a blank control, drying in the shade, placing in a culture dish with the diameter of 9cm for standby (1 leaf per dish), wrapping petioles of the pear leaves with wet absorbent cotton for moisturizing, placing absorbent paper containing a proper amount of water at the bottom of the culture dish, and keeping the appropriate humidity in the culture dish.
(3) Inoculating insects: picking 3-year nymphs which are consistent in size and lively in action by using a writing brush, inoculating the nymphs to the leaves of each treatment, testing 20 nymphs of each leaf, covering the nymphs with a dish cover, and repeating each treatment for 4 times.
(4) And (3) investigation:
after 48 hours of treatment, the number of live insects treated each time is checked one by one, the brush pen slightly touches the insect body, and the tested insects are considered to die after the test insects do not move or can not normally move. From the survey data, corrected mortality for each treatment was calculated.
(6) Data statistics and analysis:
the corrected mortality is calculated according to the formulas (1) and (2), and the calculation results are both reserved to the last two decimal points:
in the formula:
p-mortality, in percent (%);
k-represents the number of dead insects in units of heads;
n-represents the total number of insects treated, in heads.
In the formula:
P1corrected mortality in% is reported;
Pt-treatment mortality in percent (%);
P0blank mortality in percent (%).
If the control mortality rate is less than 5%, correction is not needed; the control mortality rate is between 5% and 20%, and the correction is carried out according to the formula (2); control mortality was > 20%, and the test was redone.
And processing the data by adopting a method of analyzing a few rate value. Analyzing by SPSS statistical analysis system to obtain virulence regression line and LC50Value and its 95% confidence limit and correlation coefficient R2The activity of the test agent on the biological sample is evaluated.
The co-toxicity coefficient (CTC value) of the mixture is calculated according to the formulas (3), (4) and (5):
in the formula:
ATI-actually measured toxicity index of mixed agent;
S-LC of Standard Agrochemical50In milligrams per liter (mg/L);
LC of M-mixtures50In milligrams per liter (mg/L).
TTI=TIA*PA+TIB*PB·······(4)
In the formula:
TTI-mixture theory virulence index;
TIA-agent virulence index a;
PA-the percentage of agent a in the mixture in percent (%);
TIB-agent B virulence index;
PB-the percentage of the agent B in the mixture is given in percentage (%).
In the formula:
CTC-co-toxicity coefficient;
ATI-actually measured toxicity index of mixed agent;
TTI-mixture theory virulence index.
The compounded co-toxicity coefficient CTC is more than or equal to 120, and the synergistic effect is shown; CTC is less than or equal to 80 and shows antagonism; 80 < CTC < 120 showed additive effects.
The results of the tests are given in the following table:
TABLE 1 indoor Activity test results of spiromesifen and Compounds of formula I against Pear psylla
As can be seen from Table 1, the spiromesifen has high toxicity to the psylla chinensis and LC thereof50The ratio of the spiromesifen to the compound of the formula I is 0.621mg/L, the mass ratio of the spiromesifen to the compound of the formula I is in a range of 1: 25-25: 1, the co-toxicity coefficient is more than 120, and the combined effect is represented as a synergistic effect; the mass ratio of the spiromesifen to the compound of the formula I is 1: 7-7: 1, the co-toxicity coefficient is more than 150, and the synergistic effect is obvious. The mass ratio of the spiromesifen to the compound of the formula I is 3:2, and the co-toxicity coefficient is 192.743 at the maximum.
Example 2: indoor activity test of spiromesifen and compound of formula I on whitefly
The test method comprises the following steps: soaking leaves in agar for keeping moisture.
Test targets: greenhouse whitefly (Westwood) adults, a source of test insects, breed populations of multiple generations in indoor continuous breeding for group research and development centers.
Test agents: 95% of the compound of formula I and 98% of the spiromesifen are provided by the Helier pharmaceutical industry group research and development center.
The test steps are as follows:
(1) preparing liquid agar:
placing agar powder in a triangular flask, adding water, placing in a microwave oven, and heating until agar is completely dissolved. After slightly cooling, 2mL of liquid agar is sucked by a pipette and added to the bottom of the flat-bottomed glass tube, and after the liquid agar is cooled and solidified, steam on the tube wall is completely volatilized for later use. In the cooling process, agar is prevented from being stained on the tube wall and solidified agar generates bubbles.
(2) Preparing a medicament: preparing single-dose mother liquor respectively, designing proper proportion according to the mixing purpose and the medicament activity, and preparing the single dose and each group of proportion mixture into required series of mass concentrations.
(3) Medicament treatment:
the fresh and flat cucumber leaves are beaten into leaf dishes by a puncher. And (3) immersing the leaf disk into the liquid medicine to be detected for 10s, taking out and drying, and spreading the leaf disk with the front face facing downwards in a flat-bottom glass tube added with agar by using a pair of tweezers, wherein the leaf disk is tightly attached to the agar and the tube wall without leaving a gap. Each treatment was repeated 4 times and the treatment without agent was used as a blank.
(3) Inoculating insects: and (3) inclining the glass tube with the laid leaf disc on cucumber leaves for culturing whiteflies, slightly flapping the leaves to enable the whiteflies to enter the glass tube, inserting 20 whiteflies into each glass tube, enabling the tube openings to face downwards until the whiteflies fly into the leaf disc at the bottom of the tube, and plugging the leaf disc at the position which is 15mm away from the bottom of the tube by using a cotton plug to enable the whiteflies to be forcibly positioned on the leaf disc at the bottom of the tube. After the test insects are inoculated for about 10min, the number of the live insects in each tube is checked and recorded one by one.
(4) Feeding and observing:
and (3) the treated test insects are placed upside down at the temperature of (25 +/-1) DEG C, the relative humidity of 65% +/-5%, and the photoperiod of L: D: 14:10h for feeding and observation.
(5) And (3) investigation:
after 48 hours of treatment, the number of live insects in each tube is checked and recorded one by one, and the test insects are considered to die when the test insects do not move or can not normally move. From the survey data, corrected mortality for each treatment was calculated.
(6) Data statistics and analysis:
the corrected mortality is calculated according to the formulas (1) and (2), and the calculation results are both reserved to the last two decimal points:
in the formula:
p-mortality in percent (%);
k-represents the number of dead insects, in head;
n-represents the total number of insects treated, in heads.
In the formula:
P1corrected mortality in percent (%);
Pttreatment mortality in% by weight;
P0blank mortality in percent (%).
If the control mortality rate is less than 5%, no correction is needed; the control mortality rate is between 5% and 20%, and the correction is carried out according to the formula (2); control mortality was > 20%, and the test was redone.
And processing the data by adopting a method of analyzing a few rate value. Analyzing by SPSS statistical analysis system to obtain virulence regression line and LC50Value and its 95% confidence limit and correlation coefficient R2The activity of the test agent on the biological sample is evaluated.
The co-toxicity coefficient (CTC value) of the mixture is calculated according to the following formula (3), formula (4) and formula (5):
in the formula:
ATI-actually measured toxicity index of mixed agent;
S-LC of Standard Agrochemical50In milligrams per liter (mg/L);
LC of M-mixtures50In milligrams per liter (mg/L).
TTI=TIA*PA+TIB*PB·······(4)
In the formula:
TTI-mixture theory virulence index;
TIA-agent virulence index a;
PA-the percentage of agent a in the mixture in percent (%);
TIB-agent B virulence index;
PB-the percentage of the agent B in the mixture is given in percentage (%).
In the formula:
CTC-co-toxicity coefficient;
ATI-actually measured toxicity index of mixed agent;
TTI-mixture theory virulence index.
The compounded co-toxicity coefficient CTC is more than or equal to 120, and the synergistic effect is shown; CTC is less than or equal to 80 and shows antagonism; 80 < CTC < 120 shows additive effects.
The results of the tests are given in the following table:
TABLE 2 results of the indoor activity test of spiromesifen and the compound of formula I against whitefly
As can be seen from table 2, it is,the spiromesifen has higher toxicity to the whitefly and LC thereof501.893mg/L, the mass ratio of the spiromesifen to the compound of the formula I is in the range of 1: 12-10: 1, the co-toxicity coefficient is more than 120, and the combined effect is represented as a synergistic effect; the mass ratio of the spiromesifen to the compound of the formula I is in the range of 1: 7-7: 1, the co-toxicity coefficient is more than 140, and the synergistic effect is obvious. The mass ratio of the spiromesifen to the compound of the formula I is 1:2, and the co-toxicity coefficient is 175.857 at the maximum.
And (3) field efficacy test:
example 3: test of field efficacy of spiromesifen and compound of formula I on greenhouse trialeurodes vaporariorum
The test basis is as follows: the test refers to GB/T17980.16-2000 'pesticide field efficacy test criterion (I) for controlling greenhouse trialeurodes vaporariorum';
and (3) test crops: cucumber (cucumber No. 1 of green research).
Test targets: greenhouse whitefly.
Test site: in the greenhouse vegetable greenhouse in the ink area, Qingdao city, Shandong province, the soil of the test field is sandy loam, the soil fertility is medium, and the fertilizer and water management is consistent. The cultivation density of the cucumber is 4.5 ten thousand plants/hm2。
The test method comprises the following steps: the test adopts a leaf surface spraying method, and the test medicament is uniformly sprayed on the front and back surfaces of the leaf. Each cell area is 20m2Each treatment was repeated 4 times. The test is carried out for 1 time, the application time is 6 months and 10 days in 2019, and the greenhouse trialeurodes vaporariorum is in the early stage of adult generation.
Investigation time and investigation method: the population base number is investigated before application, the number of live insects is investigated after application of the pesticide for 3d and 7d, the test is carried out when the adult insects do not move greatly in the morning, and the front and back sides of the leaf blade are inspected under the condition that the insects are not frightened. The test adopts a five-point sampling method for sampling, 5 cucumbers are fixed at each point, the middle-upper part of each cucumber is marked with 2 leaves, 25 cucumbers are surveyed in each cell, and the population base number and the number of residual and living insects of the greenhouse trialeurodes vaporariorum on the fixed-point plants are respectively surveyed.
The drug effect calculation method comprises the following steps:
two decimal points are reserved in the calculation result.
Effects on crops and other non-target organisms: in the test process, no chemical injury of the test medicament to the cucumber is found, and no adverse effect on non-target organisms of the cucumber is found.
The results of the tests are given in the following table:
TABLE 3 field efficacy test results of spiromesifen and the compound of formula I against greenhouse whitefly
According to the results of the field pesticide effect test, the spiromesifen and the compound shown in the formula I are mixed to show good control effect on the greenhouse trialeurodes vaporariorum. After 3d, the prevention and treatment effect of the preparation compounded by the spiromesifen and the compound of the formula I on the greenhouse trialeurodes vaporariorum is above 80.80%, and each preparation example shows good prevention and treatment effect.
After the pesticide is applied, the control effects of 7d, 12% of spiromesifen and the compound aqueous emulsion (1:1) of the formula I, 30% of spiromesifen and the compound wettable powder (1:2) of the formula I, 10% of spiromesifen and the compound aqueous emulsion (3:2) of the formula I and 16% of spiromesifen and the compound suspending agent (1:7) of the formula I are respectively 88.72%, 90.83%, 85.02% and 87.81%, and the pesticide has better lasting effect.
Example 4: field efficacy test of spiromesifen and compound of formula I on psylla chinensis
The test basis is as follows: the test refers to GB/T17980.10-2000 'pesticide field efficacy test criterion (I) for controlling pear psylla'.
Test targets: psyllium (Psylla chinensis).
And (3) test crops: pear trees (jade).
Test site: in a pear garden in Liangshan county, Jining city, Shandong province, pear trees are 5-year-old emerald pears, the soil fertility is medium, and the fertilizer and water management is consistent.
And (3) experimental design: the experiment designed a total of 5 agent treatments and 1 clear water control, each treatment was repeated 4 times. The treatment of the test agent, the control agent and the blank control cell adopts random block arrangement, each cell is 5 pear trees, and the periphery of the adjacent cell is provided with a protection row.
The application method comprises the following steps: the test is carried out in 2019, 5 months and 15 days, a leaf surface spraying method is adopted in the test, the front and back surfaces of each leaf are sprayed, and 200kg of liquid medicine is sprayed per mu.
Survey time and survey method: 2 pear trees are investigated in each cell, 5 short branches are randomly fixed in east, west, south, north and middle 5 directions of each pear tree before spraying, the number of active insects on 10 leaves is randomly investigated in each branch, the number of nymphs treated is not less than 200, the number of the living insects of the psylla chinensis on the leaves is counted, and the number of the adult psylla chinensis and the number of the nymphs are respectively counted. Each of 5d, 10d and 15d after application was examined once.
The drug effect calculation method comprises the following steps:
effects on crops and non-target organisms: irregular observations during the trial showed that all trial agents had no adverse effect on pear growth and no effect on other non-target organisms.
The results of the tests are shown in the following table.
TABLE 4 field efficacy test results of spiromesifen and the compound of formula I on psylla chinensis
The results of field experiments on the psylla chinensis by mixing the spiromesifen and the compound of the formula I and single dose show that the pesticide composition obtained by compounding the spiromesifen and the compound of the formula I has better control effect on the psylla chinensis.
Through indoor toxicity measurement and field pesticide effect tests, the pesticide composition and/or the preparation thereof has a good control effect on hemiptera pests, the pesticide composition has a long lasting period, no phytotoxicity of the compound pesticide on crops is found in the tests, and the pesticide composition is safe to the crops.
The above embodiments are only for illustrating the technical concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention accordingly, and not to limit the protection scope of the present invention accordingly. All equivalent changes or modifications made in accordance with the spirit of the present disclosure are intended to be covered by the scope of the present disclosure.
Claims (10)
1. A pesticide composition containing spiromesifen is characterized in that: the compound comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is spiromesifen, and the active ingredient B is a compound shown as a formula (I):
2. The pesticide composition as claimed in claim 1, wherein the mass ratio of the active ingredient A to the active ingredient B is 1: 15-15: 1.
3. The pesticide composition as claimed in claim 1, wherein the mass ratio of the active ingredient A to the active ingredient B is 1: 12-10: 1.
4. The pesticide composition as set forth in claim 1, wherein the sum of the contents of the active ingredient A and the active ingredient B in the pesticide composition is 1 to 80 wt% based on 100 wt% of the total weight of the pesticide composition.
5. The pesticidal composition according to claim 1, characterized by comprising, in addition to the active ingredient, an adjuvant selected from one or more of a wetting agent, a dispersing agent, an emulsifier, a thickener, a disintegrant, an antifreeze, an antifoaming agent, a solvent, a preservative, a stabilizer, a synergist or a carrier.
6. The pesticide composition as set forth in claim 1, wherein the pesticide composition can be prepared in any agriculturally acceptable dosage form, such dosage form being a solid preparation, a liquid preparation or a seed treatment preparation;
preferably, the liquid preparation is a suspending agent or an aqueous emulsion, and the solid preparation is wettable powder.
7. Use of a pesticidal composition according to any one of claims 1 to 6 for controlling plant pests.
8. Use according to claim 7, wherein the plant pest is a hemipteran (Hemiptera) pest.
9. The use of claim 8, wherein said hemipteran pest is a sternorrhyncha (sternorrhynchha) pest;
preferably, said pests of the suborder sternorrhyncha are pests of the family Psyllidae (Psyllidae) and/or of the family Aleyrodidae (Aleyrodidae);
more preferably, the pests of the psyllidae are psyllids pyricularis, and the pests of the whitefly family are greenhouse trialeurodes vaporariorum.
10. The use according to claim 7, wherein the pesticidal composition is applied in an effective amount to a pest or to a medium in which it is desired to control the pest.
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CN109845745A (en) * | 2019-01-19 | 2019-06-07 | 海利尔药业集团股份有限公司 | A kind of composition containing fluorine chlorine worm bisamide and process for preparation of benzoylurea compounds |
CN113331198A (en) * | 2021-06-28 | 2021-09-03 | 海利尔药业集团股份有限公司 | Use of bifloramide for improving plant quality |
CN113693070A (en) * | 2021-09-06 | 2021-11-26 | 海利尔药业集团股份有限公司 | Use of bifloramide for increasing plant reproductive activity |
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CN109845745A (en) * | 2019-01-19 | 2019-06-07 | 海利尔药业集团股份有限公司 | A kind of composition containing fluorine chlorine worm bisamide and process for preparation of benzoylurea compounds |
CN113331198A (en) * | 2021-06-28 | 2021-09-03 | 海利尔药业集团股份有限公司 | Use of bifloramide for improving plant quality |
CN113693070A (en) * | 2021-09-06 | 2021-11-26 | 海利尔药业集团股份有限公司 | Use of bifloramide for increasing plant reproductive activity |
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