CN114568435B - Pesticide composition containing spiromesifen and application thereof - Google Patents

Pesticide composition containing spiromesifen and application thereof Download PDF

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CN114568435B
CN114568435B CN202210282033.4A CN202210282033A CN114568435B CN 114568435 B CN114568435 B CN 114568435B CN 202210282033 A CN202210282033 A CN 202210282033A CN 114568435 B CN114568435 B CN 114568435B
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active ingredient
pesticide composition
pest
spiromesifen
test
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CN114568435A (en
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葛尧伦
杨志鹏
张永芳
王伟香
刘金玲
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Hailir Pesticides and Chemicals Group Co Ltd
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Hailir Pesticides and Chemicals Group Co Ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02Biocides, 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
    • A01N43/04Biocides, 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
    • A01N43/06Biocides, 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
    • A01N43/12Biocides, 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
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/561,2-Diazoles; Hydrogenated 1,2-diazoles
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against 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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  • Life Sciences & Earth Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • General Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
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  • Environmental Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a pesticide composition containing spiromesifen, which comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is spiromesifen, the active ingredient B is a compound shown in a formula I, and the mass ratio of the active ingredient A to the active ingredient B is 1:25-25:1. The pesticide composition provided by the invention is safe to target organisms, has good quick-acting property, and can effectively control various plant pests.

Description

Pesticide composition containing spiromesifen and application thereof
Technical Field
The invention relates to the technical field of pesticide compounding, in particular to a pesticide composition containing spiromesifen and application thereof.
Background
The white fly (Trialeurodes vaporarirum) belongs to the homoptera aleyrodid, is distributed and harmful throughout the world, is a main pest cultivated in the protected area, and the imago and nymphs of the white fly absorb the sap of plants and the harmful leaves fade green and turn yellow. The white fly in the greenhouse has strong fertility, high propagation speed, large population quantity and cluster hazard, can secrete a large amount of honeydew to pollute the leaves, prevent photosynthesis and respiration of plants, cause leaf wilting and reduce commodity value of vegetables.
Pear psyllids (psyllids) belong to homoptera, are widely distributed in areas such as Shandong, hebei and Henan, and mainly cause the vigor of pear trees to be weakened, the leaves to fall early and the fruits to be polluted by sucking the leaves, the fruits and the tender branches of the pear trees, so that the fruit peel is thickened and the quality is reduced, the pear psyllids are serious in the northern pear area, the flower bud formation and the next year yield are affected, and the pear psyllids become main pests in the pear producing area.
The spiromesifen is a spirotetramic acid insecticidal and acaricidal agent developed by Bayer company, has a unique spirotetramic acid structure, a novel action mechanism and excellent insecticidal and acaricidal activity, can penetrate into the plasma layer of plant leaves, has rain wash resistance, has the action mechanism of affecting the development of pests, interfering the biosynthesis of liposome, particularly has better biological activity on larva stages, can also generate ovarian duct closing action, reduces the reproductive capacity of the pests, and greatly reduces the spawning quantity. The structural formula is as follows:
Figure BDA0003558147720000011
chemical name of the compound of formula (I)Is 3-bromo-1- (3-chloropyridin-2-yl) -N- [4, 6-dichloro-3-fluoro-2- (methylcarbamoyl) phenyl]-1H-pyrazole-5-carboxamide, experimental formula: c (C) 17 H 10 BrCl 3 FN 5 O 2 . Belongs to benzamide pesticides, can efficiently activate insect ryanodine (muscle) receptors so as to excessively release calcium ions in intracellular calcium libraries, and causes paralysis death of insects. Has high activity on larvae of lepidoptera pests, broad insecticidal spectrum and good persistence. The structural formula is as follows:
Figure BDA0003558147720000021
chemical control is used as the main control means in agricultural pest control, but long-term application of pesticides leads to different degrees of resistance of target pests to various pesticides. The chemical agent is scientifically and reasonably compounded or mixed, so that the development of 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 spiromesifen and 3-bromo-1- (3-chloropyridine-2-yl) -N- [4, 6-dichloro-3-fluoro-2- (methylcarbamoyl) phenyl ] -1H-pyrazole-5-carboxamide compound combination has obvious synergistic effect on various target pests, reduces the dosage and reduces the medicament residue.
Disclosure of Invention
Based on the above circumstances, the present 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 the pesticide composition or the preparation thereof can enhance the pesticide effect and reduce the dosage.
In order to achieve the above purpose, the invention provides a pesticide composition containing spiromesifen, which 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 in a formula (I):
Figure BDA0003558147720000022
the mass ratio of the active component A to the active component B is 1:25~25:1;
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 contents of the active ingredient A and the active ingredient B in the pesticide composition is 1 to 80 weight percent based on 100 weight percent of the total weight of the pesticide composition;
further, the pesticide composition comprises an auxiliary agent in addition to the active ingredient, wherein the auxiliary agent is selected from one or more of wetting agents, dispersing agents, emulsifying agents, thickening agents, disintegrating agents, antifreezing agents, antifoaming agents, solvents, preservatives, stabilizers, synergists or carriers;
further, the wetting agent is selected from one or more of alkylbenzene sulfonate, alkyl naphthalene sulfonate, lignin sulfonate, sodium dodecyl sulfate, dioctyl sodium succinate, alpha-olefin sulfonate, alkylphenol ethoxylate, castor oil polyoxyethylene ether, alkylphenol ethoxylate, fatty alcohol polyoxyethylene ether sodium sulfate, silkworm excrement, chinese honeylocust fruit powder, soapberry powder, SOPA, detergent, emulsifier 2000 series and 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, fatty alcohol ethoxylate, alkylphenol polyoxyethylene ether methyl ether condensate sulfate, fatty amine polyoxyethylene ether, glycerin fatty acid ester polyoxyethylene ether, polycarboxylate, polyacrylic acid, phosphate, EO-PO block copolymer and EO-PO graft copolymer; and/or
The thickener is one or more selected from xanthan gum, polyvinyl alcohol, organic bentonite, magnesium aluminum silicate and carboxymethyl cellulose; and/or
The disintegrating agent is one or more selected from 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 one or more selected from fatty alcohol polyoxyethylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, phenethyl phenol polyoxyethylene polyoxypropylene ether, alkylphenol polyoxyethylene ether, fatty amine polyoxyethylene ether, alkylbenzene sulfonate, styrylphenol polyoxyethylene ether and fatty acid polyoxyethylene ester; and/or
The defoamer is selected from silicone oil and C 10 ~C 20 Saturated fatty acid compound, C 8 ~C 10 One or more of fatty alcohol compounds or silicone compounds; and/or
The preservative is one or more of sorbic acid, sodium sorbate, potassium sorbate, benzoic acid, sodium benzoate, sodium p-hydroxybenzoate and methyl p-hydroxybenzoate; and/or
The stabilizer is one or more selected from disodium hydrogen phosphate, oxalic acid, succinic acid, adipic acid, borax, 2, 6-di-tert-butyl-p-cresol, epoxidized vegetable oil; and/or
The synergistic agent is selected from synergistic phosphorus and synergistic ether; and/or
The carrier is one or more selected from 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 pesticidal composition can be prepared into any agriculturally acceptable dosage form, which 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, granule, sphere, tablet or strip;
the dispersible solid preparation is wettable powder, oil dispersion powder, emulsion powder, water dispersible granule, emulsion granule or water dispersible tablet;
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 multiphase preparation;
further, the solution preparation is a soluble agent, an oil agent or a film spreading oil agent;
the dispersion liquid preparation is emulsifiable concentrate, emulsion, dispersible agent or paste;
the emulsion preparation is aqueous emulsion, oil emulsion, microemulsion or fat agent;
the suspension preparation is suspending agent, microcapsule suspending agent, oil suspending agent or dispersible oil suspending agent;
the multiphase preparation is a suspension 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, a seed treatment emulsion or a seed treatment suspending agent;
further, the preparation 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, the Hemiptera (Hemipera) pests include, but are not limited to, aphids (Aphis), scales, white flies (white flies), leafhoppers (leaf hoppers), pea aphids (Acrythosiphon pisum) (pea aphids), genus Bemisia (Adelges) and cabbage whiteflies (Aleurodes proletella), spiral white flies (Aleurodicus disperses), silk velvet flies (Aleurothrixus floccosus), genus Bemisia (Aluaca) and red scales (Aonidiella aurantii), aphids (Aphis spp.), cotton aphids (Aphis gossypii), apple aphids (Aphis pomi), potato aphids (Aulacorthum solani) (foxglove aphid), white flies (Bemisia spp.), silver leaf aphids (Bemisia argentifolii), white flies (Bemisia tabaci), wheat two-tailed aphids (apple aphid) and apple aphids (3986), cotton hoppers (24), leaf hoppers (35), leaf hoppers (35, and other than the genus Bemisia (35), the plant aphids (P., the genus Pachyrhizus (Philaenus spp.), rhizopus vitis (Phylloxera vitifoliae), leptosphaeria sequoyis (Physokermes piceae), leptosphaeria species (Planococcus spp.), leptosphaeria species
(Pseudococcus spp.), mealybugs (Pseudococcus brevipes), meadow bugs (Quadraspidiotus perniciosus) (pear garden bugs (San Jose scale)), rhopalespedeza species (Rhopalespedeza spp.), corn aphids (Rhopalosiphum maida), gramineae spillway aphids (Rhapalosiphum padi), ericerus pela species (Saissetia spp.), elemi cerus pela (Saissetia oleae), mylabris (Schizaphis graminum), sitopon avena (Sitobion avene), beacon planthoppers (Sogatella furcifera), ericerus species (Theriopolis spp.), tourella species (Toumerella spp.), aphis species (Toxoptera spp.), bemisia species (Trialeurodes spp.), bemisia tsetus (Trialeurodes vaporariorum), bemisia nodosa (Trialeurodes abutiloneus), bemisia species (Una spp.) and Tocop (Unaspis yanonensis).
Further, the hemipteran pests are the sub-thoracic (sternorhyncha) pests;
further, the sub-thoracic pest is a Psyllidae (Psyllidae) pest and/or a Aleyrodidae (Aleyrodidae) pest;
furthermore, the psyllidae pests are pear psyllids, and the whitefly pests are greenhouse white flies.
Further, the pesticidal composition is applied to a pest to be controlled or a medium on which it grows 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 obvious synergistic effect and can effectively control various plant pests;
(2) The insecticidal composition disclosed by the invention 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 meanwhile, the use amount of pesticides is reduced, and the use cost is reduced.
Detailed Description
Preparation example of the formulation
Preparation example 1:36% spiromesifen-Compound wettable powder of formula I (3:1)
The weight percentage is that the spiromesifen is 27 percent, the compound of the formula I is 9 percent, the sodium lignin sulfonate is 8 percent, the sodium dodecyl sulfate is 3 percent, the dispersant NNO is 4 percent, and the kaolin is the balance.
The preparation method comprises the following steps: mixing the active ingredients, the dispersing agent, the wetting agent and the filler according to the formula proportion, uniformly stirring in a stirring kettle, and carrying out multiple crushing and uniform mixing by a jet mill to obtain the wettable powder.
Preparation example 2:30% spiromesifen-Compound wettable powder of formula I (1:2)
According to the weight percentage, the spiromesifen is 10 percent, the compound of the formula I is 20 percent, the calcium lignosulfonate is 10 percent, the naphthalene sulfonate formaldehyde condensate sodium salt is 2 percent, the nekal BX is 3 percent, and the kaolin is used for the balance.
The preparation method comprises the following steps: the same as in preparation example 1.
Preparation example 3:10% spiromesifen-Compound emulsion in water of formula I (3:2)
The composition comprises, by weight, 6% of spiromesifen, 4% of a compound shown in a formula I, 8% of tristyrylphenol polyoxyethylene ether polyoxypropylene ether, 2% of phenethyl phenol 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 emulsifying agent and a cosolvent together according to the formula proportion, so as to dissolve the active ingredients into a uniform oil phase; mixing part of water, an antifreeze agent and other pesticide auxiliary agents together to form a uniform water phase; adding the oil phase into the water phase while stirring at high speed in a reaction kettle, and after stirring uniformly, starting a shearing machine to conduct high-speed shearing for about half an hour to form the oil-in-water type aqueous emulsion.
Preparation example 4:12% spiromesifen-Compound emulsion in water of formula I (1:1)
The weight percentage is that spiromesifen is 6%, compound of formula I is 6%, acetophenone is 16%, alkylaryl polyoxyethylene polyoxypropylene ether is 5%, xanthan gum is 0.1%, ethylene glycol is 5%, benzoic acid is 0.1%, and deionized water is used for balancing.
The preparation method comprises the following steps: the same as in preparation example 3.
Preparation example 5:20% spiromesifen-Compound suspending agent of formula I (2:3)
According to the weight percentage, 8 percent of spiromesifen, 12 percent of compound in the formula I, 2 percent of fatty alcohol polyoxyethylene ether, 3 percent of sodium lignin sulfonate, 3 percent of alkylphenol polyoxyethylene ether phosphate, 2 percent of polycarboxylic acid sodium salt, 5 percent of glycerol, 1 percent of magnesium aluminum silicate, 0.2 percent of xanthan gum, 2 percent of sodium sorbate, 0.5 percent of silicone oil and the balance of deionized water.
The preparation method comprises the following steps: according to the formula proportion, the active ingredients, the surfactant and other functional auxiliary agents are sequentially placed in a reaction kettle, water is added and mixed uniformly, and the product is obtained through high-speed shearing, wet sanding and homogenizing and filtering.
Preparation example 6:16% spiromesifen-Compound suspending agent of formula I (1:7)
According to the weight percentage, the spiromesifen is 2 percent, the compound of the formula I is 14 percent, alkylphenol ethoxylates is 4 percent, the styrol polyoxyethylene ether phosphate is 3 percent, the naphthalene sulfonate formaldehyde condensate is 3 percent, the magnesium aluminum silicate is 0.5 percent, the xanthan gum is 0.2 percent, the ethylene glycol is 5 percent, the benzisothiazolinone potassium is 0.01 percent, the silicone oil is 0.5 percent, and the balance is 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 pear psyllids
The test method comprises the following steps: the leaf dipping method is adopted.
Test target: the Chinese pear psylla (Psylla chinensis Yang et Li) adults are the population which is continuously bred and propagated for multiple generations in the room by the group research and development center as a test insect source.
Test agent: 95% of the compound raw medicine of the formula I and 98% of the spiromesifen raw medicine are provided by a research and development center of a sea li pharmaceutical industry group.
And (3) preparation of a medicament: the mother solution of each single agent is prepared respectively, and the proper proportion is designed according to the mixing purpose and the medicament activity, and each single agent and each group of proportion are mixed to prepare the required series of mass concentration.
The test steps are as follows:
(1) Preparing a test material: selecting insect-free pear leaves with good growth, complete shape and uniform growth vigor, washing off surface dust, and drying in the shade for later use.
(2) And (3) medicament treatment: immersing clean pear leaves in the liquid medicine with each concentration for 10s, setting Tween 80 water solution without medicament and containing corresponding solvent as blank control, drying in the shade, placing in a culture dish with diameter of 9cm for standby (1 leaf per dish), wrapping the petiole of the pear leaves with moist absorbent cotton for moisturizing, placing water absorbing paper with proper amount of water at the bottom of the culture dish, and keeping the humidity in the culture dish proper.
(3) And (3) insect inoculation: the 3-year nymphs with consistent size and active actions are picked by a writing brush and connected to the leaves treated by the above steps, 20 heads of the insects are tested on each leaf, a dish cover is covered, and each treatment is repeated for 4 times.
(4) Investigation:
and (4) checking and recording the number of living insects treated each time after the treatment for 48 hours, wherein the writing brush touches the bodies of the insects, and the insects are considered to be dead after the insects are not moved 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 formulas (1) and (2), and the calculated results are reserved to two positions after decimal point:
Figure BDA0003558147720000071
wherein:
p-mortality in percent (%);
k-represents the number of dead insects in units of heads;
n-represents the total number of insects treated in units of heads.
Figure BDA0003558147720000072
Wherein:
P 1 -correct mortality in percent (%);
P t mortality rate in percent (%);
P 0 blank mortality in percent (%).
If the control mortality is less than 5%, correction is not needed; the control mortality is between 5% and 20%, and correction is carried out according to the formula (2); control mortality was > 20% and the test was reworked.
And processing the data by adopting a probability value analysis method. Analyzing by SPSS statistical analysis system to obtain virulence regression line and LC 50 Value and 95% confidence limit and correlation coefficient R thereof 2 The activity of the test agent on the biological test material was evaluated.
The co-toxicity coefficient (CTC value) of the mixture is calculated according to the formulas (3), (4) and (5):
Figure BDA0003558147720000073
wherein:
ati—actual measured virulence index of the mixture;
S-LC of Standard agricultural Agents 50 Milligrams per liter (mg/L);
M-LC of the mixture 50 Units are milligrams per liter (mg/L).
TTI=TI A *P A +TI B *P B ·······(4)
Wherein:
TTI-the theoretical toxicity index of the mixture;
TI A -a medicament virulence index;
P A -the percentage of agent a in the mix, in percent (%);
TI B -B agent virulence index;
P B the percentage of the B medicament in the mixture is expressed as percentage (%).
Figure BDA0003558147720000081
Wherein:
ctc—co-toxicity coefficient;
ati—actual measured virulence index of the mixture;
TTI-the theoretical toxicity index of the mixture.
The compound co-toxicity coefficient CTC is more than or equal to 120 and shows synergistic effect; ctc.ltoreq.80 shows antagonism; 80 < CTC < 120 shows additive effect.
The test results are shown in the following table:
TABLE 1 results of indoor Activity test of spiromesifen and Compound of formula I on pear psyllids
Figure BDA0003558147720000082
Figure BDA0003558147720000091
As can be seen from Table 1, spiromesifen has high toxicity to pear psyllids and LC thereof 50 The mass ratio of the spiromesifen to the compound in the formula I is 0.621mg/L, and is in the range of 1:25-25:1, the co-toxicity coefficient is more than 120, and the combined action is shown as a synergistic effect; the mass ratio of spiromesifen to the compound in the formula I is in the range of 1:7-7:1, the co-toxicity coefficient is more than 150, and the synergy is remarkable. The mass ratio of spiromesifen to the compound in the formula I is 3:2, and the co-toxicity coefficient is the largest and is 192.743.
Example 2: indoor activity test of spiromesifen and formula I compound on whitefly
The test method comprises the following steps: the leaf soaking method by agar moisture preservation.
Test target: the greenhouse trialeurodes vaporariorum (Trialeurodes vaporarirum (Westwood)) adults, and the source of the test insects is a population which is continuously bred and propagated for multiple generations indoors by a group development center.
Test agent: 95% of the compound raw medicine of the formula I and 98% of the spiromesifen raw medicine are provided by a research and development center of a sea li pharmaceutical industry group.
The test steps are as follows:
(1) Preparing liquid agar:
putting agar powder into a triangular flask, adding water, transferring into a microwave oven, and heating until agar is completely dissolved. After cooling, 2mL of liquid agar is sucked by a pipette, the liquid agar is added to the bottom of the flat-bottom glass tube, and after the liquid agar is cooled and solidified, the tube wall steam volatilizes cleanly for later use. And in the cooling process, the agar is prevented from being stained with the pipe wall and solidified agar to generate bubbles.
(2) And (3) preparation of a medicament: the mother solution of each single agent is prepared respectively, and the proper proportion is designed according to the mixing purpose and the medicament activity, and each single agent and each group of proportion are mixed to prepare the required series of mass concentration.
(3) And (3) medicament treatment:
fresh and flat cucumber leaves are punched into leaf discs by a puncher. And immersing the leaf disc into the liquid medicine to be detected for 10s, taking out, airing, spreading the leaf in a flat-bottom glass tube with agar in which the front face of the leaf is downward by using tweezers, and tightly attaching the leaf disc to the agar and the tube wall without leaving gaps. Treatments were repeated 4 times for each group and treatments without agent were set as blank.
(3) And (3) insect inoculation: the glass tube paved with leaf discs is inclined on cucumber leaves for culturing whiteflies, the leaves are gently beaten, so that the whiteflies enter the glass tube, 20 whiteflies are connected into each tube, the mouth of the tube faces downwards, the whiteflies are placed into the leaf discs at the bottom of the tube, and the position, which is about 15mm away from the bottom of the tube, of the cotton plug is plugged, so that the whiteflies are forcedly positioned on the leaf discs at the bottom of the tube. After about 10min of insect test access, the number of live insects in each tube was checked and recorded one by one.
(4) Feeding and observing:
the treated test insects are inverted to a temperature of (25+/-1) DEG C and a relative humidity of 65% +/-5%, and the light period is L:D=14:10 h, and are fed and observed.
(5) Investigation:
the number of live insects in each tube is checked and recorded one by one 48 hours after the treatment, and the death is considered if the test insects are motionless or can not normally act. From the survey data, corrected mortality for each treatment was calculated.
(6) Data statistics and analysis:
the corrected mortality is calculated according to formulas (1) and (2), and the calculated results are reserved to two positions after decimal point:
Figure BDA0003558147720000101
wherein:
p-mortality in percent (%);
k-represents the number of dead insects in units of heads;
n-represents the total number of insects treated in units of heads.
Figure BDA0003558147720000102
Wherein:
P 1 -correct mortality in percent (%);
P t mortality rate in percent (%);
P 0 blank mortality in percent (%).
If the control mortality is less than 5%, correction is not needed; the control mortality is between 5% and 20%, and correction is carried out according to the formula (2); control mortality was > 20% and the test was reworked.
And processing the data by adopting a probability value analysis method. Analyzing by SPSS statistical analysis system to obtain virulence regression line and LC 50 Value and 95% confidence limit and correlation coefficient R thereof 2 The activity of the test agent on the biological test material was evaluated.
The co-toxicity coefficient (CTC value) of the mixture is calculated according to the formulas (3), (4) and (5):
Figure BDA0003558147720000103
wherein:
ati—actual measured virulence index of the mixture;
S-LC of Standard agricultural Agents 50 Milligrams per liter (mg/L);
M-LC of the mixture 50 Units are milligrams per liter (mg/L).
TTI=TI A *P A +TI B *P B ·······(4)
Wherein:
TTI-the theoretical toxicity index of the mixture;
TI A -a medicament virulence index;
P A -the percentage of agent a in the mix, in percent (%);
TI B -B agent virulence index;
P B the percentage of the B medicament in the mixture is expressed as percentage (%).
Figure BDA0003558147720000111
Wherein:
ctc—co-toxicity coefficient;
ati—actual measured virulence index of the mixture;
TTI-the theoretical toxicity index of the mixture.
The compound co-toxicity coefficient CTC is more than or equal to 120 and shows synergistic effect; ctc.ltoreq.80 shows antagonism; 80 < CTC < 120 shows additive effect.
The test results are shown in the following table:
TABLE 2 results of indoor Activity test of spiromesifen and Compound of formula I on whitefly
Figure BDA0003558147720000112
As can be seen from Table 2, spiromesifen has higher toxicity to whiteflies and LC thereof 50 The mass ratio of the spiromesifen to the compound shown in the formula I is 1.893mg/L, and is in the range of 1:12-10:1, the co-toxicity coefficient is more than 120, and the combined action shows a synergistic effect; the mass ratio of spiromesifen to the compound in the formula I is in the range of 1:7-7:1, the co-toxicity coefficient is more than 140, and the synergy is remarkable. The mass ratio of spiromesifen to the compound in the formula I is 1:2, and the co-toxicity coefficient is the largest and is 175.857.
And (3) field efficacy test:
example 3: field efficacy test of spiromesifen and Compound of formula I on greenhouse trialeurodes vaporariorum
The test is based on: the test refers to GB/T17980.16-2000 pesticide field efficacy test guidelines (one) for controlling greenhouse trialeurodes vaporariorum;
test crop: cucumber (Qing yan cucumber No. 1).
Test target: white fly in greenhouse.
Test site: greenhouse vegetable greenhouse in ink-free region of Qingdao city in Shandong province, sandy loam soil as test soil, medium soil fertility and consistent fertilizer and water management. Cucumber cultivation density is 4.5 ten thousand plants/hm 2
The test method comprises the following steps: the test adopts a foliar spray method, and the test agent is uniformly sprayed on the front and back surfaces of the leaves. Each cell area is 20m 2 Each treatment was repeated 4 times. The experiment is carried out for 1 time, the administration time is 2019, 6 months and 10 days, and the greenhouse trialeurodes vaporariorum is in the initial stage of adult occurrence.
Investigation time and investigation method: the number of insect population was investigated before the application, the number of living insects was investigated after the application for 3d and 7d, the test was carried out in the morning when the adults were not active, and the front and back sides of the leaves were examined without surprise. The test adopts a five-point sampling method to sample, 5 cucumber plants are fixed at each point, 2 leaves at the middle and upper parts of the cucumber plants are marked in a hanging manner, 25 plants are investigated in each cell, and the root numbers of the white fly and the number of residual living insects on the greenhouse white fly on the fixed plants at the fixed points are respectively checked.
The drug effect calculation method comprises the following steps:
Figure BDA0003558147720000121
Figure BDA0003558147720000122
the result of the calculation retains two decimal places.
Effects on crops and other non-target organisms: no phytotoxicity of the test agent to cucumber was found during the test, and no adverse effect on the non-target organism was found.
The test results are shown in the following table:
table 3 results of field efficacy test of spiromesifen and Compound of formula I on greenhouse trialeurodes vaporariorum
Figure BDA0003558147720000123
As shown by the field efficacy test results, the spiromesifen and the compound shown in the formula I are mixed to show good control effect on the greenhouse trialeurodes vaporariorum. The control effect of the preparation compounded by the spiromesifen and the compound shown in the formula I on the greenhouse trialeurodes vaporariorum after 3d is above 80.80%, and each preparation example shows good control effect.
After the medicine is taken, the control effects of 7d,12% spiromesifen-formula I compound aqueous emulsion (1:1), 30% spiromesifen-formula I compound wettable powder (1:2), 10% spiromesifen-formula I compound aqueous emulsion (3:2) and 16% spiromesifen-formula I compound suspending agent (1:7) are 88.72%, 90.83%, 85.02% and 87.81%, respectively, and the medicine shows good lasting effect.
Example 4: field efficacy test of spiromesifen and Compound of formula I on pear psyllids
The test is based on: the test refers to GB/T17980.10-2000 pesticide field efficacy test criterion (one) for controlling pear psyllids.
Test target: pear psyllids (psyllids).
Test crop: pear tree (emerald).
Test site: the pear garden in the mountain county of Jining city in Shandong province is a 5-year-old green pear, the soil fertility is medium, and the fertilizer and water management is consistent.
And (3) test design: the experiment was designed with a total of 5 drug treatments and 1 clear water control, each treatment being repeated 4 times. The cell treatment of the test agent, the control agent and the blank control adopts random group arrangement, each cell is 5 pear trees, and the periphery of the adjacent cells is provided with protection rows.
The application method comprises the following steps: the test is carried out on the 5 th month and 15 th day of 2019, the test adopts a foliar spray method, the front and the back of each plant of leaves are sprayed, and 200kg of liquid medicine is sprayed per mu.
Investigation time and investigation method: 2 pear trees are investigated in each district, 5 short branches are randomly fixed in 5 directions of east, west, south, north and middle 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 pear psyllium active insects on the leaves is counted, and the number of pear psyllium adults and nymphs is counted respectively. Each of 5d, 10d, and 15d was investigated once after administration.
The drug effect calculation method comprises the following steps:
Figure BDA0003558147720000131
Figure BDA0003558147720000132
impact on crops and non-target organisms: the test period showed that all test agents did not adversely affect pear growth and were not found to have an effect on other non-target organisms by irregular observations.
The test results are shown in the following table.
Table 4 results of field efficacy test of spiromesifen and compounds of formula I on pear psyllids
Figure BDA0003558147720000133
Figure BDA0003558147720000141
The field test result of the single dose of the compound of the formula I on the pear psyllids shows that the pesticide composition obtained by compounding the spiromesifen and the compound of the formula I has better control effect on the pear psyllids.
Through indoor toxicity measurement and field efficacy test, the pesticide composition and/or the preparation thereof provided by the invention have good control effect on hemiptera pests, and the pesticide composition has long lasting period, and no drug damage to crops caused by the compound preparation is found in the test, so that the pesticide composition is safe to crops.
The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the content of the present invention and implement the same, and are not intended to limit the scope of the present invention. All equivalent changes or modifications made in accordance with the spirit of the present invention are intended to be included within the scope of the present invention.

Claims (13)

1. A pesticide composition containing spiromesifen is characterized in that: 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 in a formula (I):
Figure FDA0004180185920000011
the mass ratio of the active ingredient A to the active ingredient B is 1:25-25:1.
2. A pesticide composition as set forth in claim 1, characterized in that the mass ratio of the active ingredient a to the active ingredient B is 1:15 to 15:1.
3. A pesticide composition as set forth in claim 1, characterized in that the mass ratio of the active ingredient a to the active ingredient B is 1:12 to 10:1.
4. A 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% by weight based on 100% by weight of the total weight of the pesticide composition.
5. A pesticide composition as set forth in claim 1, characterized in that said pesticide composition comprises, in addition to the active ingredient, an adjuvant selected from one or more of wetting agents, dispersants, emulsifiers, thickeners, disintegrants, antifreeze agents, defoamers, solvents, preservatives, stabilizers, synergists or carriers.
6. A pesticide composition as set forth in claim 1, wherein said pesticide composition is capable of being prepared in any of agriculturally acceptable dosage forms, said dosage forms being solid, liquid or seed treatment formulations.
7. A pesticide composition as set forth in claim 6 wherein said liquid formulation is a suspension or aqueous emulsion and said solid formulation is a wettable powder.
8. Use of the pesticidal composition according to any one of claims 1 to 7 for controlling plant pests.
9. The use according to claim 8, wherein the plant pest is a hemipteran (Hemiptera) pest.
10. The use according to claim 9, wherein the hemipteran pest is a sub-thoracic (sternorhyncha) pest.
11. The use according to claim 10, wherein the thoracic subgenera pest is a Psyllidae (Psyllidae) pest and/or a Aleyrodidae (Aleyrodidae) pest.
12. The use according to claim 11, wherein the psyllidae is psyllid and the aleurodidae is trialeurodes vaporariorum.
13. The use according to claim 8, wherein the pesticidal composition is applied in an effective dose to the pest or medium in which it is growing to be controlled.
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