CN112219852A - Application of insecticidal composition containing nicotinamide compound in controlling honeysuckle insect pests - Google Patents

Application of insecticidal composition containing nicotinamide compound in controlling honeysuckle insect pests Download PDF

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CN112219852A
CN112219852A CN202011121241.3A CN202011121241A CN112219852A CN 112219852 A CN112219852 A CN 112219852A CN 202011121241 A CN202011121241 A CN 202011121241A CN 112219852 A CN112219852 A CN 112219852A
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formula
honeysuckle
compound
insecticidal composition
matrine
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张芳
王伟香
王玉
隋书婷
王均竹
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Qingdao Tengrunxiang Testing And Evaluation Co ltd
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Qingdao Tengrunxiang Testing And Evaluation 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
    • A01N43/48Biocides, 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
    • 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
    • A01N43/90Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system

Abstract

The invention belongs to the technical field of pesticide compounding, and relates to application of an insecticidal composition containing a nicotinamide compound in controlling honeysuckle insect pests. The insecticidal composition or the preparation thereof can increase insecticidal effect, reduce dosage and improve crop quality.

Description

Application of insecticidal composition containing nicotinamide compound in controlling honeysuckle insect pests
Technical Field
The invention relates to the technical field of pesticide compounding, in particular to an insecticidal composition containing a nicotinamide compound, emamectin benzoate and matrine.
Background
Honeysuckle is a dried flower bud or a flower which is just bloomed in the honeysuckle of the Caprifoliaceae family, and is an important traditional Chinese medicinal material. The planting of the traditional Chinese medicinal materials can remarkably promote the development of local agriculture, and due to the fact that China pays attention to and supports the planting of the traditional Chinese medicinal materials, the honeysuckle flower is planted in various places, the vigorous development of the honeysuckle flower industry is greatly promoted, the situation of comprehensive development of a suitable area is presented, and the planting range and the production scale of the honeysuckle flower are continuously expanded. With the continuous expansion of planting area, the problems of difficult pest control and the like caused by large-area large-scale planting are solved, and simultaneously, the problems of pesticide abuse and overproof pesticide residues of products are not avoidable.
At present, chemical agents are still the main means for controlling honeysuckle pests, and commonly used agents such as beta-cypermethrin, chlorpyrifos and the like. In the process of preventing and controlling pests, the pesticide resistance of pests is continuously accumulated due to long-term unreasonable use of organic phosphorus medicaments and pyrethroid medicaments, and the prevention and control effect of the medicaments is reduced year by year. Research reports indicate that various lepidoptera larvae have strong resistance to pyrethrins and organophosphorus medicaments, the organophosphorus medicaments and the pyrethroid medicaments are the medicaments applied most in the honeysuckle pest control process, and the problems of single medicament and over-standard medicament consumption are very common. In addition, the medicament has serious environmental pollution after long-term application, kills natural enemies and beneficial organisms, pollutes water sources, and is limited to use at present.
The chemical name of the nicotinamide compound shown in the formula I is 2-chloro-N-cyclopropyl-5- (1- (2,6-dichloro-4- (perfluoropropane-2-yl) phenyl) -1H-pyrazol-4-yl) -N-methylnicotinamide, and the English chemical name is as follows: 2-Chloro-N-cyclopropyl-5- (1- (2, 6-dichoro-4- (perfluoropropan-2-yl) phenyl) -1H-pyrazol-4-yl) -N-methylnicotinamide, the chemical structural formula of which is as follows:
Figure BDA0002732058380000011
emamectin benzoate, abbreviated as emamectin benzoate, is a novel high-efficiency semi-synthetic antibiotic pesticide synthesized from a fermentation product, namely, abamectin B1, is widely applied to the control of various pests on crops such as fruit trees, vegetables, cotton and the like, and has the characteristics of safety, high efficiency, low residue, no public nuisance and other biological pesticides.
Matrine is plant pesticide, is prepared from dried root, plant and fruit of Sophora flavescens ait of Leguminosae by extracting with organic solvent, and is alkaloid. The general matrine is total matrine, and the main components of the total matrine comprise various alkaloids such as matrine, sophocarpine, oxysophocarpine, sophoridine and the like, and the content of the matrine and the oxysophocarpine is the highest.
Unreasonable medication causes serious pesticide residue in honeysuckle, reduces the quality of medicinal materials and influences the health of people. The reasonable compounding or mixing of the chemical agents has the positive characteristics of expanding the insecticidal spectrum, improving the control effect, prolonging the application period, reducing the dosage, reducing the phytotoxicity, reducing the residue, delaying the occurrence of the drug resistance and the drug resistance of pests and the like.
The honeysuckle has strong adaptability, mild living conditions and good plantability, the honeysuckle in the market at present has large demand and wide planting distribution, the quality is greatly reduced while the yield is pursued, the phenomenon of rough preparation occurs, the drug property of the honeysuckle cannot be exerted, the demand on the honeysuckle is difficult to meet, in view of the high ornamental value, economic value and medicinal value of the honeysuckle, an insecticide which can improve the pest control effect of the honeysuckle and does not influence the drug property and the content of beneficial components of the honeysuckle is urgently needed, the insecticide has great significance for perfecting the scientific control of honeysuckle pests, and the applicant surprisingly discovers 2-chloro-N-cyclopropyl-5- (1- (2,6-dichloro-4- (perfluoropropane-2-yl) phenyl) -1H-pyrazol-4-yl) -N-one-phase through indoor toxicity experiments and field efficacy experiments The compound combination of the methylnicotinamide, the emamectin benzoate and the matrine has obvious synergistic effect, and the pesticide composition compounded by the 2-chloro-N-cyclopropyl-5- (1- (2,6-dichloro-4- (perfluoropropane-2-yl) phenyl) -1H-pyrazol-4-yl) -N-methylnicotinamide, the emamectin benzoate and the matrine and the application thereof are not reported at present.
Disclosure of Invention
Based on the situation, the invention aims to provide a pesticide insecticidal composition containing 2-chloro-N-cyclopropyl-5- (1- (2,6-dichloro-4- (perfluoropropane-2-yl) phenyl) -1H-pyrazol-4-yl) -N-methylnicotinamide and a preparation thereof, which are mainly used for controlling plant pests.
In order to achieve the purpose, the invention provides an insecticidal composition containing a nicotinamide compound shown as the formula I, which comprises an active ingredient A and an active ingredient B, wherein the active ingredient A is a compound shown as the formula (I)
Figure BDA0002732058380000021
The active component B is any one of emamectin benzoate and matrine;
further, the mass ratio of the active ingredient A to the active ingredient B is 50: 1-1: 50;
further, the mass ratio of the active ingredient A to the emamectin benzoate is 20: 1-1: 30, preferably 5: 1-1: 20;
further, the mass ratio of the active ingredient A to the matrine is 16: 1-1: 30, preferably 4: 1-1: 25;
further, the sum of the contents of the active ingredient A and the active ingredient B in the insecticidal composition is 1-95 wt%, preferably 5-80 wt%, based on the total weight of the insecticidal composition being 100 wt%;
further, the insecticidal composition further comprises 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 and a carrier;
the wetting agent is selected from one or more of 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 fruit powder, soapberry powder, SOPA, detergent, emulsifier 2000 series and wetting penetrant 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, glycerol fatty acid ester polyoxyethylene ether, polycarboxylate, polyacrylic acid, phosphate, EO-PO block copolymer and EO-PO graft copolymer; and/or
The emulsifier is selected from one or more of calcium dodecylbenzene sulfonate, alkylphenol formaldehyde resin polyoxyethylene ether, phenethyl phenol polyoxyethylene polyoxypropylene ether, fatty alcohol ethylene oxide-propylene oxide copolymer, styryl phenol polyoxyethylene ether, castor oil polyoxyethylene ether and alkylphenol ether phosphate; and/or
The thickener is one or more selected from xanthan gum, organic bentonite, gum arabic, sodium alginate, magnesium aluminum silicate, carboxymethyl cellulose and white carbon black; and/or
Disintegrant the disintegrant 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 antifreezing agent is selected from one or more of alcohols, alcohol ethers, chlorohydrocarbons and inorganic salts; and/or
The defoaming agent is selected from C10-C20Saturated fatty acid compound, silicone oil, silicone compound, C8-C10One or more of fatty alcohols; and/or
The solvent is selected from one or more of benzene, toluene, xylene, methanol, ethanol, isopropanol, n-butanol, dimethyl sulfoxide, dimethylformamide, cyclohexanone, alkylene carbonate, diesel oil, solvent oil, vegetable oil derivative and deionized water; and/or
The preservative is selected from one or more of propionic acid, sodium propionate, sorbic acid, sodium sorbate, potassium sorbate, benzoic acid, sodium benzoate, sodium parahydroxybenzoate, methyl parahydroxybenzoate, carbazone and 1, 2-benzisothiazoline 3-one; 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, triethanolamine oleate, epoxidized vegetable oil, kaolin, bentonite, attapulgite, white carbon black, talcum powder, montmorillonite and starch; and/or
The synergist is selected from synergistic phosphorus and synergistic ether; and/or
The carrier is selected from one or more of ammonium salt, ground natural mineral, ground artificial mineral, silicate, resin, wax, solid fertilizer, water, organic solvent, mineral oil, vegetable oil and vegetable oil derivative.
An insecticidal composition containing the nicotinamide compound shown in the formula I, wherein the active ingredient and the auxiliary agent can be prepared into any agriculturally acceptable dosage form;
further, the dosage form comprises any one of powder, granules, soluble powder, soluble granules, soluble tablets, water dispersible granules, wettable powder, microcapsule granules, powder, water dispersible tablets, microcapsule suspending agents, dispersible agents, emulsifiable solutions, emulsions in water, microemulsions, suspending agents, suspoemulsions, soluble agents and ultra-low volume solutions;
further, the preparation is any one of wettable powder, microemulsion and suspending agent;
wettable powders are mixtures of the compositions in a certain proportion with suitable surfactants and inert substances. Wettable powders are formulations which are uniformly dispersible in water and which contain, in addition to the active substance and inert substance, a certain amount of an anionic or nonionic surfactant. The wettable powder does not use solvent and emulsifier, is safe to plants, is not easy to generate phytotoxicity and is safe to the environment.
When the insecticidal composition is wettable powder, the components in parts by weight are as follows: 1-40 parts of a compound shown in the formula I; 1-40 parts of emamectin benzoate or matrine; 3-10 parts of a dispersing agent; 1-5 parts of a wetting agent; the filler makes up the balance. The wettable powder has the specific production steps as follows: the compound of the formula I as an effective component is mixed with emamectin benzoate or matrine, a dispersing agent, a wetting agent and a filler according to the formula, uniformly stirred in a stirring kettle, and uniformly mixed after air flow crushing, so that the wettable powder of the composition can be prepared.
The microemulsion is a homogeneous liquid preparation with transparent appearance and composed of oil-soluble raw medicine, an emulsifier and water. The suspended liquid drops in the system are fine, the particle size is 0.01-0.1 mu m, the colloidal range is achieved, and the target body has strong permeability and good adhesion. In addition, the microemulsion takes water as a medium and contains no or little organic solvent, so that the microemulsion is non-inflammable and non-explosive, is safe in production and operation, and storage and transportation, has little environmental pollution, and saves a large amount of organic solvent.
When the insecticidal composition is a microemulsion, the components in parts by weight are as follows: 1-40 parts of a compound of formula I, 1-40 parts of emamectin benzoate or matrine, 2-20 parts of an emulsifier, 0.1-8 parts of an antifreezing agent, 0.5-10 parts of a stabilizer, 5-20 parts of a solvent and the balance of deionized water. Dissolving the compound of formula I and emamectin benzoate or matrine completely with cosolvent, adding emulsifier, antifreeze, stabilizer, etc., mixing, adding water, and stirring to obtain microemulsion.
The suspending agent is prepared by mixing the composition with appropriate surfactant and water according to a certain proportion, uniformly grinding by a colloid mill, and grinding for 1-2 times by a sand mill to a certain fineness. The suspending agent is divided into an aqueous suspending agent and an oil suspending agent, and has small particle size, high biological activity, no dust flying problem, and no flammability and explosion. The suspending agent consists of active ingredients, a dispersing agent, a thickening agent, an anti-settling agent, a defoaming agent, an antifreezing agent, water and the like.
When the insecticidal composition is a suspending agent, the insecticidal composition comprises the following components in parts by weight: 1-40 parts of a compound shown in the formula I; 1-40 parts of emamectin benzoate or matrine; 1-10 parts of a dispersing agent; 0.1-5 parts of an antifreezing agent; 0.1-2 parts of a thickening agent; 0.1-0.8 part of defoaming agent; 1-5 parts of a stabilizer; and deionized water is used for complementing the balance. The compound of formula I, emamectin benzoate or matrine, a dispersant and part of water are subjected to wet grinding by a sand mill to obtain D90 (the particle size of 90% of particles) is less than 10 mu m, and the mixture is fully and uniformly mixed with the rest water dissolved with an antifreezing agent, a thickening agent and a defoaming agent under the action of the sand mill to obtain the suspension preparation of the composition.
An application of the pesticide insecticidal composition containing the compound of formula I and the preparation thereof in preventing and controlling plant pests in agriculture, forestry and gardening;
further, the plant pests are pests on cash crops and food crops;
further, the cash crop is honeysuckle;
further, the plant pests are piercing-sucking pests and chewing pests;
further, the piercing-sucking pests are Microaphis carotovora (Semiaphis heraclei Takahashi), and the chewing pests are geometrid (Heterophajinyhuahaga Chu);
further, the pesticidal composition is applied to a pest or a medium in which it grows in need of control in an effective amount.
With the rapid development of the traditional Chinese medicine industry, honeysuckle is used as a widely used traditional Chinese medicine, and the honeysuckle is not only used for traditional Chinese medicines, but also has great development in the food health care and green tourism industries. The planting area is continuously enlarged, the problems of difficult pest control and the like caused by large-area large-scale planting are solved, and the use of pesticides and honeysuckle pesticide residues is an unavoidable problem. Honeysuckle geometrid (Heteroochajinoyhuahaga Chu) and carrot microdyster aphid (Semiaaphis heraclei Takahashi) are important leaf-eating pests which are harmful to honeysuckle in recent years and are also dominant species of honeysuckle pests in Shandong province, and the two pests are also serious in Henan province, Anhui province and other provinces.
Honeysuckle inchworm (Heterophasha jinyuahaga Chu) belongs to Lepidoptera family insects of the family Endomastoideae, is an oligotrophic insect, only eats a plant of the family Caprifoliaceae, mainly takes the fact that larvae bite leaves, and causes the yield of honeysuckle to be sharply reduced and even a large number of plants to die when the damage is serious. The insect is grown for 3 generations in 1 year in Shandong province, and the peak period of the insect is the harmful growth of the larva in the middle of 5 months to the end of 6 months, in the middle of 7 months to the end of 8 months, and in the middle of 9 months to the end of 10 months; the aphids (Semiaphis heraclei Takahashi) of homoptera, Aphidae, are widely distributed in many provinces such as Shandong, Hebei, Henan, Anhui, Guangdong, Guangxi, Chongqing, Yunnan, Fujian and the like, the aphids (carrot) grow 10-20 generations annually, eggs are used for overwintering on branches such as honeysuckle of Lonicera and the like, the eggs are hatched from 3 months to 4 months in the next year, and the honeysuckle is seriously damaged from 4 months to 5 months. In the period of taking golden honeysuckle flowers in positive value, the aphid propagation speed is extremely high and the life cycle is short. The pesticide residue of the product is extremely easy to exceed the standard, the traditional Chinese medicine components of the honeysuckle are reduced, and even the yield is reduced due to improper medicament selection of farmers during the flower picking period.
The specific implementation scheme of the pesticide formulation prepared by the insecticidal composition is as follows:
the insecticidal composition obtained by compounding the active ingredient compound shown in the formula I with any one of emamectin benzoate and matrine has an obvious synergistic effect, can delay the generation of insect resistance, can reduce the production cost and the use cost, and can effectively prevent and treat plant pests.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) by compounding the compound shown in the formula I with any one of emamectin benzoate and matrine, the composition obtains excellent control effect and has synergistic effect;
(2) the using amount of pesticides is reduced, and the agricultural cost is reduced;
(3) the pesticide is friendly to crops, non-target organisms and environment, increases the quick-acting property of the pesticide to pests, delays the generation of pesticide resistance of the pests and prolongs the pesticide persistence.
Detailed Description
To make the technical solutions, objects, and advantages of the present invention more apparent, the present invention is described with the following specific examples, but the present invention may be implemented in various forms and should not be limited by the embodiments set forth herein.
Preparation example 1: 16% wettable powder of the compound of the formula I matrine (1:7)
Adding 2g of compound raw medicine of the formula I, 14g of matrine mother medicine, 5g of sodium dodecyl sulfate, 2g of sodium lignosulphonate and 100g of kaolin, pre-crushing and uniformly mixing, and crushing by using an airflow crusher until the fineness meets the requirement that at least 98 wt% passes through a 45-micrometer test sieve to prepare wettable powder with the mass content of the effective component of 16 wt%.
Preparation example 2: 12% wettable powder of compound of formula I and emamectin benzoate (1:5)
2g of compound raw drug of formula I, 10g of emamectin benzoate raw drug, 5g of sodium lignosulfonate, 3g of sodium dodecyl sulfate and 100g of kaolin are added, pre-crushed and mixed uniformly, and then crushed by an airflow crusher until the fineness meets the requirement that at least 98 wt% passes through a 45-micrometer test sieve, so as to prepare wettable powder with the mass content of active ingredients of 12 wt%.
Preparation example 3: 15% wettable powder of the compound of formula I matrine (1:2)
5g of compound raw medicine of the formula I, 10g of matrine mother medicine, 6g of sodium dodecyl sulfate, 2g of sodium lignosulphonate and starch are added to 100g, the mixture is pre-crushed and mixed uniformly, and then the mixture is crushed by an airflow crusher until the fineness meets the requirement that at least 98 wt% passes through a 45-micron test sieve, so as to prepare wettable powder with the mass content of active ingredients of 15 wt%.
Preparation example 4: 16% wettable powder of compound I and emamectin benzoate (1:7)
2g of compound raw drug of formula I, 14g of emamectin benzoate raw drug, 5g of sodium lignosulfonate, 3g of sodium dodecyl sulfate and attapulgite are added to 100g, the mixture is pre-crushed and mixed uniformly, and then the mixture is crushed by a jet mill until the fineness meets the requirement that at least 98 wt% passes a 45 mu m test sieve, so as to prepare wettable powder with the mass content of the active ingredient of 16 wt%.
Preparation example 5: 10% Compound of formula I Emamectin benzoate microemulsion (1:4)
2g of a compound raw material medicine of a formula I, 8g of a emamectin benzoate raw material medicine, 10g of dimethyl sulfoxide, 5g of calcium dodecyl benzene sulfonate and 2g of ethylene glycol are fully dissolved and mixed to form a uniform and transparent oil phase, deionized water is slowly added under stirring to form W/O type emulsion, then stirring and heating are carried out to enable the W/O type emulsion to rapidly convert into O/W type, cooling to room temperature, standing and filtering are carried out to obtain O/W type microemulsion, and the microemulsion with the mass content of active ingredients of 10 wt% is prepared.
Preparation example 6: 14% Compound of formula I Emamectin benzoate microemulsion (1:6)
2g of a compound raw material medicine of a formula I, 12g of a emamectin benzoate raw material medicine, 6g of cyclohexanone, 4g of styrylphenol polyoxyethylene ether and 2g of ethylene glycol are fully dissolved and mixed to form a uniform and transparent oil phase, deionized water is slowly added under stirring to form W/O type emulsion, then stirring and heating are carried out to enable the W/O type emulsion to rapidly convert into O/W type, cooling is carried out to room temperature, standing and filtering are carried out to obtain O/W type microemulsion, and the microemulsion with the effective component mass content of 14 wt% is obtained.
Preparation example 7: 12% of the compound of formula I matrine microemulsion (1:4)
2.4g of the compound original drug of the formula I, 9.6g of matrine parent drug, 7.9g of isopropanol, 5g of fatty acid polyoxyethylene ether and 2g of glycerol are fully dissolved and mixed to form a uniform and transparent oil phase, the oil phase is slowly added into deionized water which is supplemented with 100g of the mixture under stirring to form W/O type emulsion, then the W/O type emulsion is stirred and heated to quickly convert the phase into O/W type, the O/W type microemulsion is obtained after cooling to room temperature and standing and filtering, and the microemulsion with the mass content of the active ingredients of 12 wt% is prepared.
Preparation example 8: 18% of the compound of formula I matrine microemulsion (1:8)
2g of compound raw material of the formula I, 16g of matrine, 4g of isopropanol, 4g of ethanol, 4.5g of calcium dodecyl benzene sulfonate, 4.5g of polyoxyethylene fatty acid ether, 1g of polyoxyethylene fatty acid ester and 2g of ethylene glycol are fully dissolved and mixed to form a uniform and transparent oil phase, the oil phase is slowly added into deionized water which is supplemented with 100g of the oil phase under stirring to form W/O type emulsion, then the W/O type emulsion is stirred and heated to rapidly convert the phase into O/W type, the O/W type emulsion is cooled to room temperature and is kept stand and filtered to obtain the O/W type microemulsion with the mass content of the active ingredients of 18wt percent.
Preparation example 9: 12% of the compound of formula I matrine microemulsion (1:5)
2g of compound raw material of the formula I, 10g of matrine, 9g of dimethyl sulfoxide, calcium dodecyl benzene sulfonate, 5g of fatty acid polyoxyethylene ether and 2g of ethylene glycol are fully dissolved and mixed to form a uniform and transparent oil phase, deionized water is slowly added under stirring to form W/O type emulsion, then stirring and heating are carried out to ensure that the W/O type emulsion is rapidly converted into O/W type, cooling to room temperature is carried out, standing and filtering are carried out to obtain O/W type microemulsion, and the microemulsion with the mass content of the effective components of 12 wt% is prepared.
Preparation example 10: 25% Compound of formula I Emamectin benzoate suspension concentrate (1:4)
3g of an alkylnaphthalenesulfonate formalin condensate, 1g of an EO-PO block copolymer, 2g of sodium laurylsulfate, and 0.5g of an organosilicon antifoaming agent were dispersed in 50g of water, and 5g of a dispersed type I compound drug and 20g of a emamectin benzoate were wet-pulverized with a sand mill to D90 (particle diameter of 90% of particles) < 10 μm to obtain a pulverized slurry. Adding 0.2g of xanthan gum, 1g of magnesium aluminum silicate, 5g of ethylene glycol and 0.5g of sodium benzoate into the crushed slurry, uniformly mixing, complementing deionized water to 100g, and uniformly shearing at high speed to obtain the suspending agent with the mass content of the effective component of 25 wt%.
Preparation example 11: 30% Compound of formula I Emamectin benzoate suspension concentrate (1:5)
4g of lignosulfonate, 1g of EO-PO block copolymer, 3g of sodium alkylphenol polyoxyethylene ether methyl ether condensate sulfate and 0.7g of silicone oil were dispersed in 50g of water, and 5g of dispersed type I compound drug and 25g of emamectin benzoate were wet-pulverized with a sand mill to D90 (particle diameter of 90% of particles) < 10 μm to obtain a pulverized slurry. Adding 0.15g of sodium alginate, 1g of magnesium aluminum silicate, 5g of ethylene glycol and 0.5g of sodium benzoate into the crushed slurry, uniformly mixing, complementing deionized water to 100g, and uniformly shearing at high speed to obtain the suspending agent with the mass content of the effective component of 30 wt%.
Preparation example 12: 18% of the compound of formula I matrine suspension (1:8)
3g of an alkylnaphthalenesulfonate formaldehyde condensate, 1.5g of an aliphatic alcohol ethoxylate, 2g of sodium laurylsulfate and 0.5g of an organosilicon antifoaming agent were dispersed in 50g of water, and 2g of a dispersed type I compound crude drug and 16g of a matrine base drug were wet-pulverized with a sand mill to D90 (particle diameter of 90% of particles) < 10 μm to obtain a pulverized slurry. Adding 0.2g of xanthan gum, 1g of magnesium aluminum silicate, 5g of ethylene glycol and 0.55g of propionic acid into the crushed slurry, uniformly mixing, complementing deionized water to 100g, and uniformly shearing at high speed to obtain the suspending agent with the mass content of the effective component of 22 wt%.
Indoor toxicity test
Examples reference indoor bioassay test guidelines for pesticides part 6: an insect soaking method NT/T1154.6-2006; section 7: the combined effect of compounding was determined for NT/T1154.7-2008.
90% of a compound raw drug of the formula I, 95% of an emamectin benzoate raw drug and 10% of a matrine raw drug, wherein the test drugs are provided by group research and development centers.
The indoor test is prepared from the above raw materials, emulsifier is 0.1% Tween 80, and solvent is acetone.
Inchworm indoor toxicity test
Test targets: heterophaea jinyhuahaga Chu of honeysuckle flower geometrid
The insect source to be tested is honeysuckle planted in a teaching base of Shandong agriculture university in Taian city, 1-3 instar larvae are collected and continuously fed and bred with honeysuckle leaves indoors, and indoor population is established.
Honeysuckle leaves are used as feed for larvae. Feeding conditions are as follows: the temperature is 25 +/-1 ℃, the temperature is constant, the relative humidity is 65 +/-5%, and the illumination L: D is 14:10 h.
The determination method comprises the following steps: preparing single-dose mother liquor respectively, designing 5 groups of proportioning according to the mixing purpose and the medicament activity, and preparing 5 series of mass concentrations of each single dose and each group of proportioning mixing agent according to an equal ratio method. Selecting 2-instar larvae with consistent physiological state, soaking in the medicinal liquid for 5s with an insect soaking device, repeating for 4 times every 20 times, treating the control group with 0.1% Tween 80 water solution, transferring the treated larvae into culture dish with diameter of 9.0cm and laid with filter paper, placing 2 fresh folium Lonicerae slices in each dish, continuously feeding, and changing fresh folium Lonicerae slices every day. Then placing the mixture in an illumination incubator at 25 +/-1 ℃, wherein the relative humidity is 65% +/-5%, and the illumination L: D is 14:10 h.
And (5) checking the death condition of the test insects 48 hours after treatment, and respectively recording the total number of the insects and the number of the dead insects. From the survey data, corrected mortality for each treatment was calculated. Calculating according to the formulas (1) and (2), and reserving the calculation results to the last two decimal points:
Figure BDA0002732058380000091
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.
Figure BDA0002732058380000092
In the formula:
P1corrected mortality in percent (%);
Pt-treatment mortality in percent (%);
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. Can be analyzed by an IBM SPSS Statistics2.0 statistical analysis system to obtain a virulence regression line and LC50The value and its 95% confidence limit and the correlation coefficient r, and the activity of the test agent on the biological test material. The co-toxicity coefficient (CTC value) of the mixture is calculated according to the following formula (3), formula (4) and formula (5):
Figure BDA0002732058380000101
in the formula:
ATI-actually measured toxicity index of mixed agent;
S-LC of Standard insecticide50In 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 hundred of the A medicament in the mixtureFractional content in percent (%);
TIB-agent B virulence index;
PB-the percentage of the agent B in the mixture in percent (%).
Figure BDA0002732058380000102
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.
Aphid indoor toxicity test
Test targets: carrot microtubule aphid (Semiaphis heraclei Takahashi)
Aphids are raised on potted honeysuckle plants, and wingless adult aphids are used as test insects. And selecting the wingless adult aphids which are fed indoors and have consistent physiological state. The temperature is 25 +/-1) DEG C, the relative humidity is 65% +/-5%, and the illumination period is 16/8h (L/D);
preparing a medicament: the water soluble medicine is directly dissolved in water, and other medicines are dissolved in organic solvent acetone, and then diluted with 0.1% Tween-80 aqueous solution. Respectively preparing single-dose mother liquor, designing 5 groups of proportioning according to the mixing purpose and the medicament activity, and preparing 5 series of mass concentrations of each single dose and each group of proportioning mixture according to an equal ratio method, wherein the liquid medicine amount of each mass concentration is not less than 50 mL.
The determination method comprises the following steps: selecting representative fresh honeysuckle tender tips (about 5cm in length), and keeping about 50 tips of the uniform developed wingless adult aphids as test insects. Soaking the tender tips of the honeysuckle with the insects in the liquid medicine for 5s by adopting a soaking method for determination, taking out and airing, using soaked absorbent cotton and a preservative film to protect the cuts of the tender tips, keeping 80 insects with consistent development, and placing the insects into an insect-raising box. The control group was treated with 0.1% aqueous tween 80 and repeated 4 times per treatment. Then placing the mixture in an incubator at the temperature of 25 +/-1 ℃ and the relative humidity of 65% +/-5% and with the illumination period of 16/8h (L/D) for breeding.
Data statistics and analysis:
and (5) checking the death condition of the test insects 48 hours after treatment, and respectively recording the total number of the insects and the number of the dead insects. From the survey data, corrected mortality for each treatment was calculated. Calculating according to the formulas (1) and (2), and reserving the calculation results to the last two decimal points:
Figure BDA0002732058380000111
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.
Figure BDA0002732058380000112
In the formula:
P1corrected mortality in percent (%);
Pt-treatment mortality in percent (%);
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. Can be analyzed by an IBM SPSS Statistics2.0 statistical analysis system to obtain a virulence regression line and LC50The value and its 95% confidence limit and the correlation coefficient r, and the activity of the test agent on the biological test material.
The co-toxicity coefficient (CTC value) of the mixture is calculated according to the following formula (3), formula (4) and formula (5):
Figure BDA0002732058380000121
in the formula:
ATI-actually measured toxicity index of mixed agent;
S-LC of Standard insecticide50In 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 in percent (%).
Figure BDA0002732058380000122
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.
Example 1
The combined toxicity of the compound of the formula I and emamectin benzoate in different proportions on inchworm is determined:
honeysuckle looper is an oligotrophic insect, only eating the plant of Caprifoliaceae, mainly biting the leaves by the larvae, and when the damage is serious, the yield of the honeysuckle is sharply reduced and even a large number of plants die. As can be seen from the results in Table 1, compounds of formula IThe product and emamectin benzoate have good insecticidal activity on honeysuckle loopers. The results of the combined toxicity measurement of the compounds of formula I and emamectin benzoate in different proportions on honeysuckle geometrid show that the emamectin benzoate has high toxicity on the honeysuckle geometrid and LC50A value of 0.347 mg/L; LC of compound of formula I on honeysuckle inchworm50The value was 2.284 mg/L. The mass ratio of the compound in the formula I to the emamectin benzoate is within 1: 50-50: 1, and the compound in the formula I and the emamectin benzoate both show additive action or synergistic action; the compound of the formula I has the highest toxicity to honeysuckle loopers, LC50The value is 0.296mg/L, the co-toxicity coefficient is 136.527, and the synergistic effect is shown; the compound of formula I, emamectin benzoate 1:1, also shows synergistic effect on honeysuckle loopers, LC50The value was 0.474mg/L and the cotoxicity coefficient was 127.103.
TABLE 1 toxicity test results of different proportions of compounds of formula I and emamectin benzoate on honeysuckle geometrid
Figure BDA0002732058380000131
Figure BDA0002732058380000141
TABLE 2 Joint toxicity assay for honeysuckle geometrid with different proportions of compound of formula I and emamectin benzoate
Figure BDA0002732058380000142
Figure BDA0002732058380000151
Example 2
The joint toxicity of the compound of the formula I and the matrine in different proportions is determined:
as shown in the results in Table 3, the compound of formula I and matrine have better insecticidal activity on the looper worm of honeysuckle. The combined toxicity measurement results of the compounds of formula I and matrine in different proportions on honeysuckle geometrid in Table 4 show that the sophora flavescensThe toxicity of the alkali and the compound of the formula I on the honeysuckle looper is similar, LC50The values were 2.414mg/L and 2.284mg/L, respectively. The mass ratio of the compound in the formula I to the matrine is within 1: 50-50: 1, and the compound shows additive action or synergistic action; the compound of the formula I and the matrine have synergistic effect within the mass ratio of 1: 8-1: 4, the compound of the formula I and the matrine have the highest toxicity to honeysuckle geometrid 1:8, and LC50The value is 1.556mg/L, and the cotoxicity coefficient is 154.166; compound of formula I matrine 1:4 pair honeysuckle looper LC50The value was 1.774mg/L, and the cotoxicity coefficient was 134.545.
TABLE 3 toxicity test results of compounds of formula I and matrine in different ratios for honeysuckle looper
Figure BDA0002732058380000152
Figure BDA0002732058380000161
TABLE 4 Joint toxicity assay for honeysuckle looper with different proportions of compound of formula I and matrine
Figure BDA0002732058380000162
Figure BDA0002732058380000171
Example 3
The combined toxicity of the compound of the formula I and emamectin benzoate on aphids is determined according to different ratios:
the honeysuckle aphids can directly eat the damaged honeysuckle and suck tender tips and tender leaves of the thorn honeysuckle, so that the damaged leaves contract and turn yellow, and flower buds of the honeysuckle are deformed due to damage in bud period; honeydew is secreted in the damage process, so that soot diseases of the honeysuckle occur, the photosynthesis of honeysuckle plants is seriously influenced, and the yield and the quality of the honeysuckle are influenced. As can be seen from the results in Table 5, the compounds of formula IThe compound and matrine have good insecticidal activity on honeysuckle aphids. Table 6 shows that the compound of formula I and emamectin benzoate have high toxicity to honeysuckle aphids and LC (liquid chromatography) of the emamectin benzoate is higher than that of the compound of formula I50The value is 1.381mg/L, and the compound of the formula I is applied to honeysuckle aphid LC50The value was 14.309 mg/L. The mass ratio of the compound in the formula I to the emamectin benzoate is within 1: 50-50: 1, and the compound in the formula I and the emamectin benzoate both show additive action or synergistic action; wherein the mass ratio of the compound of the formula I to the emamectin benzoate is 1: 10-1: 1, and the synergistic effect is shown.
TABLE 5 toxicity test results of compounds of formula I and emamectin benzoate on honeysuckle aphid
Figure BDA0002732058380000172
Figure BDA0002732058380000181
Figure BDA0002732058380000191
TABLE 6 Joint virulence determination of honeysuckle aphids with different proportions of compounds of formula I and emamectin benzoate
Figure BDA0002732058380000192
Example 4
The combined toxicity of the compound of the formula I and matrine in different proportions on aphids is determined:
as shown in the results in Table 7, the compound of the formula I and matrine have better insecticidal activity on honeysuckle aphids. The combined toxicity test results of honeysuckle aphids with different proportions of the compound shown in the formula I and matrine in the table 8 show that the toxicity of the compound shown in the formula I to the honeysuckle aphids is 2 times that of the matrine, LC50The values were 14.309mg/L and 31.861mg/L, respectively. The mass ratio of the compound of the formula I to the matrine is within the range of 1: 50-50: 1, and the compound of the formula I and the matrine are all expressedAdditive or synergistic effects; the compound of the formula I and the matrine have synergistic effect within the mass ratio of 1: 16-1: 1, the compound of the formula I and the matrine have the highest toxicity to honeysuckle aphids within the mass ratio of 1:4, and LC50The value is 17.481mg/L, and the cotoxicity coefficient is 146.356; compound of formula I matrine 1:1 pair honeysuckle looper LC50The value is 15.323mg/L, and the cotoxicity coefficient is 128.883; compound of formula I matrine 1:8 pair honeysuckle looper LC50The value was 22.301mg/L, and the cotoxicity coefficient was 125.732.
TABLE 7 toxicity test results of compounds of formula I and matrine in different ratios on honeysuckle aphid
Figure BDA0002732058380000193
Figure BDA0002732058380000201
Figure BDA0002732058380000211
TABLE 8 Joint virulence determination of honeysuckle aphids with different ratios of compounds of formula I and matrine
Figure BDA0002732058380000212
Test of field drug effect
Field pesticide effect test for controlling honeysuckle inchworm by different agents
The test object is honeysuckle inchworm, the test crop is honeysuckle, and the variety is honeysuckle of all seasons.
The test site is a Shandong province fat city tide spring town honeysuckle plantation, honeysuckle is planted in a test field all year round, and inchworm is common. All test plot cultivation conditions (soil type, fertilization, cultivation, row spacing, etc.) were uniform and consistent with local agricultural cultivation practices (GAP).
Test ofThe cells are arranged in random block, the adjacent cells are provided with guard lines, and the area of each cell is 20m2The test was carried out in mid 7 th of 2020 using a conventional spray method (cone spray head, flow 540 ml/min) with 4 repetitions. The application is carried out for 1 time, and the period of the low-age larvae of the honeysuckle looper is the full-blown period.
The weather is fine at the same day of pesticide application, the temperature is 18.2-29.8 ℃, the relative humidity is 70%, the weather is good during the test period, and no disastrous weather exists.
The investigation method comprises the steps of investigating population base before medicine, investigating residual insect quantity 3, 7 and 14 days after medicine, and investigating 4 times.
Sampling is carried out at 5 random points in each cell, 1 plant is fixedly investigated at each point, and the number of loopers and larvae on each branch is investigated.
The drug effect calculation method comprises the following steps: the drug effect is calculated by the following formula (6) and formula (7):
Figure BDA0002732058380000221
Figure BDA0002732058380000222
example 5 field test of the Compound of formula I with Emamectin benzoate on Lonicera japonica geometrid
The test results of the treatment agents for controlling honeysuckle inchworm:
the field test results of different test agents on honeysuckle inchworm show that the pesticide composition obtained by compounding the compound of the formula I and the emamectin benzoate has good control effect on the honeysuckle inchworm, 3d after the pesticide is applied, the control effect of each treatment in the preparation examples is more than 80%, wherein 14% of the compound of the formula I and the emamectin benzoate microemulsion (1:6) has the best control effect of 85.75%, the quick action is good, the test data is processed by using Duncan method through IBM SPSS data processing software, and the analysis result of variance shows that the compounding treatments have no significant difference under the levels of 0.01 and 0.05. With the increase of time, the insecticidal effect of each compound insecticide is increased, and after the insecticide is applied, the 14% compound of formula I and emamectin benzoate microemulsion (1:6) has the best control effect, and the control effect is 90.73%, but under the 0.01 level, the control effect is not obviously different from the control effects of 12% compound of formula I and emamectin benzoate wettable powder (1:5), 14% compound of formula I and emamectin benzoate microemulsion (1:6) and 25% compound of formula I and emamectin benzoate suspending agent (1: 4). After the pesticide is applied, the control effects of the 12% compound of the formula I, emamectin benzoate wettable powder (1:5) and the 14% compound of the formula I, emamectin benzoate microemulsion (1:6) are higher than 90%, respectively are 90.23% and 92.26%, and under the 0.01 level, no significant difference exists between the control effects of the 14d after the 4 preparation examples on the honeysuckle inchworm.
TABLE 9 field test results of different test reagents on Lonicera japonica geometrid
Figure BDA0002732058380000223
Figure BDA0002732058380000231
Note: the control (%) in the table above is the average of each repetition. Lower case letters represent 5% level difference and upper case letters represent 1% level difference.
Example 6 field test of the Compound of formula I and matrine on Lonicera japonica geometrid
The test results of the treatment agents for controlling honeysuckle inchworm:
the field test results of the compound of the formula I and the matrine in table 10 and the single dose of the compound of the formula I on the honeysuckle loopers show that the pesticide composition obtained by compounding the compound of the formula I and the matrine has better control effect on the honeysuckle loopers, the control effect of each preparation example is more than 80% after 3d of application, the control effect of each compounding treatment is more than 89% after 7d of application, the test data is processed by a Duncan method through IBM SPSS data processing software, and the variance analysis results show that the control effects of the preparation examples 3d after application and 7d after application are not significantly different at the level of 0.01 and 0.05, and the control effects are significantly different from those of a 5% microemulsion of the compound of the formula I and a 0.3% aqueous solution of the matrine. The control effect of each medicament is increased after 14 days, and the 18 percent of the compound of the formula I and the matrine suspending agent (1:8) has the best control effect, namely 93.72 percent, and shows better lasting effect. The control effects of two mixed medicaments of 14 percent of compound of formula I and matrine wettable powder (1:7) and 12 percent of compound of formula I and matrine microemulsion (1:5) are respectively 90.55 percent and 91.28 percent, and the control effects of the three mixed medicaments have no difference under the level of 0.05.
TABLE 10 field test results of different test agents on Lonicera japonica geometrid
Figure BDA0002732058380000232
Note: the control (%) in the table above is the average of each repetition. Lower case letters represent 5% level difference and upper case letters represent 1% level difference.
Field pesticide effect test for controlling honeysuckle aphids by different medicaments
The test object is honeysuckle flower carrot aphid microtubular aphid, the test crop is honeysuckle flower, and the variety is honeysuckle flower No. 3.
The test site is carried out in a zibo city Boshan area pond town pond Xincun honeysuckle field, and the test field has medium soil fertility, smooth terrain, uniform fertility and good irrigation conditions. All test plot cultivation conditions (soil type, fertilization, cultivation, row spacing, etc.) were uniform and consistent with local agricultural cultivation practices (GAP).
The test cells are arranged in random blocks, guard rows are arranged between adjacent cells, and the area of each cell is 20m2The test was carried out in 5 months of 2020 using a conventional spray method (cone spray head, flow rate 540 ml/min) every 4 repetitions. The application is carried out for 1 time, and the honeysuckle is in vegetative growth phase.
The day of pesticide application, the weather is sunny, 3-4 levels of east wind, the temperature is 8-23 ℃, the relative humidity is 66%, the weather is good during the test period, and no disastrous weather exists.
The investigation method comprises the steps of investigating population base before medicine, investigating residual insect quantity 3, 7 and 14 days after medicine, and investigating 4 times.
Sampling is carried out at 5 random points in each cell, 1 aphid is fixedly surveyed at each point, and the number of the aphids living on 5 branches (the length of the top end is 10 cm) is recorded according to 4 directions and the specification of a middle hanging plate (taking the base number of the surveyed aphids not less than 500 as a standard).
The drug effect calculation method comprises the following steps: the drug effect is calculated by the following formula (6) and formula (7):
Figure BDA0002732058380000241
Figure BDA0002732058380000242
during the test period, the honeysuckle grows well in each treatment cell, and no phytotoxicity is generated in each treatment.
Example 7 field test of the Effect of Compounds of formula I and emamectin benzoate on aphids in honeysuckle
The test results of each treatment medicament for preventing and treating honeysuckle aphids are as follows:
the field test results of different test agents on honeysuckle aphids show that the pesticide composition obtained by compounding the compound of the formula I and emamectin benzoate has a good control effect on honeysuckle aphids, the control effects of 3d after application are 82.25%, 84.39%, 84.94% and 85.96% of 10% compound-emamectin benzoate microemulsion (1:4), 14% compound-emamectin benzoate microemulsion (1:6) and 25% compound-emamectin benzoate suspending agent (1:4), respectively, IBM SPSS data processing software is used for processing test data by a Duncan method, and the analysis result of variance shows that the compound pesticides do not have a significant difference when processed at a 0.01 level. The control effect of the 5% compound of formula I-emamectin benzoate microemulsion (1:4) is the best 90.97% at 7d after the drug is applied, but the microemulsion has no difference with other three complex treatments, and is obviously superior to two control microemulsions of the compound of formula I and 5% emamectin benzoate microemulsions. The maximum control effect is achieved 14 days after the pesticide is applied, the control effects of 10 percent of the compound of formula I and emamectin benzoate microemulsion (1:4), 12 percent of compound of formula I and emamectin benzoate wettable powder (1:5), 14 percent of the compound of formula I and emamectin benzoate microemulsion (1:6) and 25 percent of compound of formula I and emamectin benzoate suspending agent (1:4) are respectively 95.14 percent, 95.00 percent, 90.91 percent and 93.09 percent, and are all more than 90 percent.
TABLE 11 field test results of different test agents on aphids of honeysuckle
Figure BDA0002732058380000243
Figure BDA0002732058380000251
Note: the control (%) in the table above is the average of each repetition. Lower case letters represent 5% level difference and upper case letters represent 1% level difference.
Example 8 field test of the Effect of Compounds of formula I and matrine on aphids in honeysuckle
The test results of each treatment medicament for preventing and treating honeysuckle aphids are as follows:
the results of field experiments on honeysuckle aphids by compounding the compound of the formula I and the matrine and single dose of the compound of the formula I and the matrine in the table 12 show that the pesticide composition obtained by compounding the compound of the formula I and the matrine has better control effect on the honeysuckle aphids, the control effect of each treatment in the preparation example 3d after application is more than 80%, the control effects of 5% of the microemulsion of the compound of the formula I and 0.3% of the aqueous matrine are 77.07% and 75.17% respectively, and the compounded medicaments are obviously better than the control medicaments. The control effect of the compound of the formula I and the matrine microemulsion (1:4) is 91.26 percent at 7d after the drug is applied to the maximum extent in 12 percent; after the pesticide is applied, the control effect of 12 percent of the compound of the formula I and the matrine microemulsion (1:4) is increased to 95.18 percent, and the compound of the formula I and the matrine microemulsion show higher quick-acting property and lasting effect on honeysuckle aphids. 14d after the drug is taken, the control effect of 18 percent of the compound of the formula I and the matrine suspending agent (1:8) is 94.830 percent, and the control effect is not different from that of 12 percent of the compound of the formula I and the matrine microemulsion (1: 4). The quick-acting property and the lasting property of the compounded insecticidal composition on the honeysuckle aphids are superior to the control effect of a single agent, which shows that the compounded insecticidal composition or the preparation thereof has obvious control effect.
TABLE 12 field test results of different test agents on aphids of honeysuckle
Figure BDA0002732058380000252
Note: the control (%) in the table above is the average of each repetition. Lower case letters represent 5% level difference and upper case letters represent 1% level difference.
Example 9
Safety test for controlling honeysuckle with different medicaments
Honeysuckle variety: the variety of the jatropha, the siji flower and the hirsute flower is 4-5 years old, the pruning degree of the honeysuckle in winter is consistent, and the growth period is the spring honeysuckle stripping period. The test field is the planting base of Zheng town honeysuckle in Pingyi county, Shandong province.
The test method comprises the following steps: uniformly spraying the liquid medicine on honeysuckle plant leaves by using a sprayer, and treating 4 honeysuckle plants in total by using the treatment concentration of each medicament of each honeysuckle variety as a control without application of the medicament. Before the test, 10 branches with consistent growth vigor are selected from each honeysuckle, the length of each branch is marked with a distance of 5cm from the top end, and the damage conditions of leaves and branches are respectively checked 3d after the application of the pesticide.
The calculation method comprises the following steps: and calculating the growth rate inhibition rate of each treatment according to survey data by referring to the agricultural industry standard NY/T1965.1-2010.1 of the people's republic of China. Calculating according to the formulas (1) and (2), and reserving the calculation results to the last two decimal points:
R=L/D……(8)
in the formula:
r-growth rate/cm. d-1
L is the new height or length/cm of the plant or branch or the new root system;
d-is time/D.
RI=(RCK-RT)/RCK×100……(9)
In the formula:
RI-growth rate inhibition/%;
RCKblank growth rate/%;
RTgrowth rate/%, of the agent treatment.
The inhibition rate of the growth rate is within 10 percent after the application for 21 days; after the pesticide is applied, the inhibition rate of the growth rate is 11% -20% of the inhibition rate of the growth rate in 21 days, which is slight phytotoxicity; after the pesticide is applied, the inhibition rate of the growth rate in 21 days is 21% -50%, and the moderate phytotoxicity is obtained; after the application, the inhibition rate of the growth rate in 21 days is more than 50 percent, which is serious phytotoxicity.
Safety test results:
as can be seen from the safety test results of different test agents on different varieties of honeysuckle in Table 13, the compound preparation of the compound of the formula I and emamectin benzoate or matrine and a single agent show safety on three varieties tested, and after 3d after application, the treated leaves are consistent with the control and have no phytotoxicity symptom. And 14d after the application, the honeysuckle branches grow normally after each treatment, and each treatment has no obvious difference compared with a clear water control and does not show obvious growth inhibition.
TABLE 13 safety test results of different test agents on different varieties of honeysuckle
Figure BDA0002732058380000261
Figure BDA0002732058380000271
Note: the length of the upper shoot is the average length of 10 shoots with 4 repetitions.
The test results show that the compound of the formula I, emamectin benzoate and matrine has good control effect on honeysuckle aphids, and has low toxicity and low residue, and the phenomena of phytotoxicity and natural enemy insect killing of honeysuckle in each application treatment area are not seen.
Through indoor toxicity measurement and experiments on field honeysuckle, the insecticidal composition compounded by the compound of the formula I, emamectin benzoate and matrine has a good control effect on honeysuckle loopers or aphids. The insecticidal composition or the preparation thereof obtained by compounding the insecticidal composition has obvious control effect, and is superior to a single preparation in the aspects of delaying the generation of drug resistance and prolonging the drug-holding property. And the compound pesticide is not found to cause phytotoxicity to crops in the test, which shows that the production cost and the use cost can be reduced and the crop safety can be realized under the condition that the insecticidal synergy of the obtained insecticidal composition or preparation is improved.

Claims (10)

1. An insecticidal composition containing a nicotinamide compound, which is characterized in that: comprises an active component A and an active component B, wherein the active component A is a nicotinamide compound shown in a formula (I):
Figure FDA0002732058370000011
the active ingredient B is any one of emamectin benzoate and matrine.
2. The insecticidal composition according to claim 1, wherein the mass ratio of the active ingredient A to the active ingredient B is 50: 1-1: 50.
3. The insecticidal composition according to claim 1, wherein the mass ratio of the formula (I) to the emamectin benzoate is 20: 1-1: 30, preferably 5: 1-1: 20.
4. The insecticidal composition according to claim 1, wherein the mass ratio of the compound of formula (I) to the matrine is 16: 1-1: 30, preferably 4: 1-1: 25.
5. An insecticidal composition according to any one of claims 1 to 4, wherein the sum of the contents of active ingredient A and active ingredient B in the insecticidal composition is 1 to 95 wt%, preferably 5 to 80 wt%, based on 100 wt% of the total weight of the insecticidal composition.
6. An insecticidal composition according to any one of claims 1 to 5 further comprising an adjuvant selected from one or more of wetting agents, dispersing agents, emulsifiers, thickeners, disintegrants, antifreeze agents, antifoam agents, solvents, preservatives, stabilisers, synergists and carriers.
7. An insecticidal composition according to any one of claims 1 to 6, characterized in that the active ingredient and adjuvants can be prepared in any agriculturally acceptable dosage form;
preferably, the dosage form comprises any one of powder, granules, soluble powder, soluble granules, soluble tablets, water dispersible granules, wettable powder, microcapsule granules, powder, water dispersible tablets, microcapsule suspending agents, dispersible agents, missible oil, emulsion in water, microemulsion, suspending agents, suspoemulsion, soluble agents and ultra-low volume liquid agents;
more preferably, the formulation is any one of wettable powder, microemulsion and suspending agent.
8. Use of the pesticidal composition of any one of claims 1 to 6 or the formulation of claim 7 for controlling plant pests in agriculture, forestry, horticulture;
preferably, the plant pests are pests on cash crops and food crops;
more preferably, the cash crop is honeysuckle (Lonicera japonica).
9. The use of claim 8, wherein the plant pests are piercing-sucking pests, chewing pests;
preferably, the piercing-sucking pest is Microaphis carotovora (Semiaphis heraclei Takahashi) and the chewing pest is geometrid (Heterophajinyhuahaga Chu).
10. The use according to any one of claims 8 to 9, wherein the pesticidal composition is applied in an effective amount to the pest or to the medium in which it is to be controlled.
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