阅读说明：本技术 含蓖麻杀虫活性物质的提取方法及其与氨基甲酸酯类杀虫剂的组合应用 (Method for extracting castor-containing insecticidal active substance and combined application of castor-containing insecticidal active substance and carbamate insecticide ) 是由 张开心 雒珺瑜 崔金杰 朱香镇 姬继超 王丽 于 2018-03-02 设计创作，主要内容包括：本发明属于植物保护领域,涉及农药组合物及其应用领域,具体的说是以蓖麻杀虫物质和常规杀虫剂为组合物,主要用于农作物有害节肢动物的防治。本发明首先公开了一种蓖麻杀虫物质的提取方法,其次公开了一种蓖麻杀虫物质与常规杀虫剂组合物及其应用。本发明乙醇溶液热浸提与超声波浸提组合的方式得到蓖麻杀虫物质,所得蓖麻杀虫物质对多种杀虫剂有显著的增效作用,本发明所述的组合物使用方法简单,便于推广应用,对棉叶螨、斜纹夜蛾、甜菜夜蛾、小菜蛾、蚜虫、粉虱、蓟马和叶螨等多种靶标节肢动物有较好的防效,能在很大程度上降低农药施用量,延缓靶标节肢动物对杀虫剂的抗性发展,符合目前农药减量化和环境友好的要求。(The invention belongs to the field of plant protection, relates to a pesticide composition and an application field thereof, and particularly relates to a composition which is mainly used for preventing and treating harmful arthropods of crops and takes castor bean insecticidal substances and conventional insecticides as the composition. The invention discloses a method for extracting a castor insecticidal substance, and further discloses a castor insecticidal substance and conventional insecticide composition and application thereof. The castor insecticidal substance is obtained by combining ethanol solution hot extraction and ultrasonic extraction, and has obvious synergistic effect on various insecticides.)

1. An insecticidal composition containing a castor insecticidal substance comprises a castor insecticidal substance and an insecticide, and is characterized in that 1) the mass ratio of the castor insecticidal substance to the insecticide is 1: 5-80: 1; 2) the castor bean insecticidal substance is extracted from castor bean tissues by a mode of combining hot extraction with ultrasonic extraction of an ethanol solution, wherein the castor bean tissues comprise one or more of old leaves, stem barks, root barks, seed hulls and castor bean cakes of castor beans, the specific extraction mode is that the castor bean tissues are dried, crushed and sieved by a 100-150-mesh fine sieve, the castor bean tissue dry powder is soaked in an ethanol water solution with the mass concentration of 50-75% according to the mass ratio of the castor bean tissue dry powder to the ethanol water solution of 1: 6-15, the castor bean tissue dry powder is soaked in the ethanol water solution with the mass concentration of 40-90 ℃ for 8-12 hours, then ultrasonic oscillation is carried out for 20-45 minutes under the water bath condition of 50-80 ℃, and primary filtrate is obtained after filtration; soaking the filter residue obtained after the first filtration in 50-75% ethanol water solution with the mass ratio of the filter residue to the castor tissue dry powder of 1: 2-20, performing ultrasonic oscillation for 10-35 min under the water bath condition of 50-80 ℃, and filtering to obtain a second filtrate; mixing the two filtrates to obtain an extracting solution containing the castor bean insecticidal substance, performing rotary evaporation concentration on the extracting solution containing the castor bean insecticidal substance under the water bath condition of 40-90 ℃ to obtain a paste-shaped castor bean insecticidal substance, drying at 40-90 ℃ to constant weight, and crushing and sieving to obtain castor bean insecticidal substance powder; 3) the pesticide is a conventional variety and dosage form used in the agricultural field, and specifically is one or more carbamate pesticides.

2. An insecticidal composition containing a castor bean insecticidal substance according to claim 1, wherein the conventional insecticide species comprises one or more of carbofuran, carbosulfan, pirimicarb, methomyl; the conventional formulation of the pesticide comprises one or more of an emulsifiable concentrate, a microemulsion, an aqueous emulsion, granules, wettable powder and a suspending agent.

3. A method for using an insecticidal composition containing a castor insecticidal substance is characterized in that an extracting solution containing the castor insecticidal substance is mixed with an insecticide mother liquor, or a pasty castor insecticidal substance is diluted by a surfactant solution with the mass concentration of 0.01-10.00% and mixed with the insecticide mother liquor, or dried castor insecticidal substance powder is diluted by the surfactant solution with the mass concentration of 0.01-10.00% and mixed with the insecticide mother liquor, and the mixed liquor is diluted again and then applied to an area where harmful arthropods of crops occur or are likely to occur in a spraying, root irrigation or seed dressing mode.

4. The use method of the castor-oil plant insecticidal composition according to claim 3, wherein the surfactant comprises one or more of alkyl benzene sulfonate, alkylphenol ethoxylates, phenethyl phenol ethoxylates polyoxypropylene ethers and the like, span series, and tween.

5. The use method of the insecticidal composition containing castor bean insecticidal substance according to claim 3, wherein said crop harmful arthropods comprise one or more of cotton spider mites, prodenia litura, beet armyworm, diamond back moth, aphids, whiteflies and thrips.

Technical Field

The invention belongs to the field of plant protection, relates to the field of pesticide compositions and application thereof, and particularly relates to an extraction method of castor-containing insecticidal active substances and combined application of the castor-containing insecticidal active substances and an insecticide.

Background

Although there are many emerging and environment-friendly technologies for treating diseases and pests in modern agriculture, chemical pesticides still play a significant role due to factors such as cost and control effect. However, the existing pesticide also has the defects of large using amount, easy generation of resistance, serious environmental pollution and the like, and the defects also limit the development of the pesticide industry and agricultural production. The plant secondary metabolite not only can provide a lead compound with excellent activity for synthesis and screening of pesticide molecules with novel structures, but also can be directly developed into a natural product pesticide which is friendly to the environment, can prevent and treat plant diseases and insect pests, reduces the problems of residue and pollution caused by using chemical pesticides, and has positive significance for promoting the sustainable development of agriculture. However, the single use of plant secondary metabolites, namely plant-derived pesticides, has some irreparable disadvantages, such as short duration, slow effect, relatively poor control effect and the like. The pesticide and the plant secondary metabolites are used in combination, so that the defects of the pesticide and the plant secondary metabolites can be effectively overcome, the product effective period of the pesticide can be prolonged, the using amount of the pesticide can be reduced, and the resistance development of target organisms to the pesticide can be delayed, and the method is a direction for the development of the current pesticide industry.

Ricinus communis L, a dicotyledonous annual or perennial herbaceous plant of the genus Ricinus of the family Euphorbiaceae, has strong stress resistance, can grow on saline-alkali and barren lands, and is a dominant crop in barren areas of China. The main product of castor is castor seed, which contains 50% of castor oil, is used for producing industrial products such as lubricating oil, paint, emulsifier, etc., and is widely applied to the industries such as chemical industry, light textile industry, medicine industry, etc. The seeds, roots, stems, leaves and flowers of castor beans and the cake meal after the castor seeds are pressed contain ricin, and the ricinine and allergen content in the castor cake meal are high, so that the application of the castor cake meal in the feed industry is prevented, and a large amount of protein is wasted. The research on the biological activity of the castor extract is more focused on the activity measurement of pests in the agricultural field, and the castor extracts with different tissues and different solvents have various biological activities of contact poisoning, stomach poisoning, food refusal, fumigation, avoidance, attraction and the like on different pests. However, the castor extract has a large difference in biological activity according to the extraction method, which limits the application of the castor extract in the field of plant protection.

In the process of deeply researching the castor bean insecticidal substances, the inventor surprisingly discovers that the castor bean insecticidal substances extracted according to a certain method can be compatible with various organic phosphorus, carbamates, pyrethroids, neonicotinoids and microbial insecticides, has obvious synergistic effect in a certain compounding ratio range, and has good control effect on harmful arthropods of crops. The present invention has been completed through further studies.

According to the data search made by the inventor, no patent and other published data conflicting with the present invention are found.

Disclosure of Invention

In view of the above, an object of the present invention is to provide an insecticide composition containing castor bean insecticide, which has the advantages of reasonable components, significant synergistic effect, excellent insecticidal effect, long duration, low medication cost, and safety to crops, and can delay the generation of drug resistance by pests.

The invention also aims to provide an extraction method for extracting the castor bean insecticidal substance which has good compatibility with various insecticides and has good synergistic effect.

Another object of the present invention is to provide a method of using a castor-containing insecticidal material in combination with an insecticide.

In order to achieve the purpose, the invention adopts the following technical solutions to realize:

the pesticide composition containing the castor insecticidal substance comprises the castor insecticidal substance and a pesticide, and is characterized in that the mass ratio of the castor insecticidal substance to the pesticide is 1: 10-100: 1; the castor insecticidal substance is extracted from castor tissue by a mode of combining ethanol solution hot extraction and ultrasonic extraction; the pesticide is a conventional variety and dosage form used in the agricultural field.

Preferably, the pesticide composition containing the castor insecticidal substance comprises the castor insecticidal substance and a pesticide, and is characterized in that the mass ratio of the castor insecticidal substance to the pesticide is 1: 5-80: 1.

The extraction method of the castor-oil plant insecticidal substances is characterized by comprising the steps of drying and crushing castor-oil plant tissues, sieving the crushed castor-oil plant tissues by a 50-200-mesh fine sieve, soaking the castor-oil plant tissue dry powder in an ethanol water solution with the mass concentration of 30-90% according to the mass ratio of the castor-oil plant tissue dry powder to the ethanol water solution of 1: 2-20, soaking for 5-12 hours in a water bath at 40-90 ℃, then ultrasonically oscillating for 10-45 min in the water bath at 40-90 ℃, and filtering to obtain a first filtrate; soaking the filter residue obtained after the first filtration in 30-90% ethanol water solution with the mass concentration of 1: 2-20 of the castor tissue dry powder, performing ultrasonic oscillation for 10-45 min under the water bath condition of 40-90 ℃, and filtering to obtain a second filtrate; mixing the two filtrates to obtain an extracting solution containing the castor bean insecticidal substance, performing rotary evaporation concentration on the extracting solution containing the castor bean insecticidal substance under the water bath condition of 40-90 ℃ to obtain a paste-shaped castor bean insecticidal substance, drying at 40-90 ℃ to constant weight, and crushing and sieving to obtain castor bean insecticidal substance powder.

Preferably, the method for extracting the castor-oil plant insecticidal substances is characterized by comprising the steps of drying and crushing castor-oil plant tissues, sieving the crushed castor-oil plant tissues by a 100-150-mesh fine sieve, soaking the castor-oil plant tissue dry powder in an ethanol water solution with the mass concentration of 50-75% according to the mass ratio of the castor-oil plant tissue dry powder to the ethanol water solution of 1: 6-15, soaking for 8-10 hours in a 50-80 ℃ water bath, then ultrasonically oscillating for 20-35 min in a 50-80 ℃ water bath, and filtering to obtain a first filtrate; soaking the filter residue obtained after the first filtration in 50-75% ethanol water solution with the mass ratio of the filter residue to the castor tissue dry powder of 1: 2-20, performing ultrasonic oscillation for 20-35 min under the water bath condition of 50-80 ℃, and filtering to obtain a second filtrate; mixing the two filtrates to obtain an extracting solution containing the castor bean insecticidal substance, performing rotary evaporation concentration on the extracting solution containing the castor bean insecticidal substance under the water bath condition of 40-90 ℃ to obtain a paste-shaped castor bean insecticidal substance, drying at 40-90 ℃ to constant weight, and crushing and sieving to obtain castor bean insecticidal substance powder.

The castor tissue is characterized by comprising one or more of old leaves, inflorescences, stems, roots, husks and castor bean cakes of castor beans.

Preferably, the castor tissue is characterized by comprising one or more of old leaves, root barks, seed hulls and castor seed cakes of castor beans.

The pesticide is characterized in that the conventional variety comprises one or more of trichlorfon, dichlorvos, omethoate, malathion, phoxim, chlorpyrifos, carbofuran, carbosulfan, pirimicarb, methomyl, imidacloprid, nitenpyram, acetamiprid, thiamethoxam, clothianidin, dinotefuran, abamectin, emamectin benzoate, ivermectin, spinosad and liuyangmycin; the conventional preparation formulation comprises one or more of an emulsifiable concentrate, a microemulsion, an aqueous emulsion, a granule, a wettable powder and a suspending agent.

A combined application method of a castor-containing insecticidal substance and an insecticide is characterized in that an extracting solution containing the castor-containing insecticidal substance is mixed with an insecticidal mother liquor, or a pasty castor insecticidal substance is diluted by a surfactant solution with the mass concentration of 0.01-10.00% and mixed with the insecticide mother liquor, or dried castor insecticidal substance powder is diluted by the surfactant solution with the mass concentration of 0.01-10.00% and mixed with the insecticide mother liquor, and then the mixed liquor is diluted again and applied to an area where harmful arthropods of crops occur or can occur in a spraying, root irrigation or seed dressing mode.

The surfactant is characterized by comprising one or a mixture of a plurality of alkyl benzene sulfonate, alkylphenol polyoxyethylene ether, phenethyl phenol polyoxyethylene ether polyoxypropylene ether and similar substances, span series and Tween.

The harmful arthropods of crops are characterized in that the harmful arthropods of crops comprise one or more of cotton bollworms, prodenia litura, beet armyworm, diamond back moth, aphids, whiteflies, thrips and spider mites.

The invention has the technical characteristics and advantages that:

1. the castor insecticidal substance extracted by the method disclosed by the invention has more excellent bioactivity on harmful arthropods of crops than a pure product of ricinine. 2. The castor bean insecticidal substance is a natural active substance, is easy to degrade in the environment, has low toxicity to mammals such as human and livestock, and is safe to natural enemies of pests and other beneficial organisms. 3. The obtained castor bean insecticidal substance has good compatibility with various insecticides, has obvious synergistic effect on the various insecticides, can reduce the use cost on the premise of greatly improving the pesticide effect, can reduce the application amount of the pesticide to a great extent, and is favorable for further reducing the pressure of the insecticides on the environment. 4. The combined application method of the castor-containing insecticidal substance and the insecticide has the advantages of simple use method and convenience in popularization and application. 5. The composition has good control effect on various target arthropods such as cotton bollworms, prodenia litura, beet armyworms, diamond back moths, aphids, whiteflies, thrips, spider mites and the like, delays the resistance development of the target arthropods to insecticides, and meets the requirements of current pesticide reduction and environmental friendliness.

Detailed Description

The invention will be described in further detail with reference to specific embodiments for the purpose of making clear the objects, technical solutions and advantages thereof, which should not be construed as limitations of the invention, but is for explanation and modification, substitutions or improvements made without departing from the spirit and principle of the invention are within the scope of the invention as claimed.

In recent years, with the enhancement of environmental awareness and the requirement of agricultural sustainability development, the extraction of plant secondary metabolites and the prevention and control effects on harmful arthropods become research hotspots in the field of plant protection, and particularly, the combined use of the plant secondary metabolites with biological activity and the existing pesticide is an effective way for rapidly applying the plant secondary metabolites and reducing the use of the existing pesticide.

In the process of deeply researching the castor insecticidal substances, the inventor surprisingly discovers that the castor insecticidal substances extracted by the method of combining ethanol solution hot leaching and ultrasonic leaching can be compatible with various organic phosphorus, carbamates, pyrethroids, neonicotinoids and microbial insecticides, the mass ratio of the castor insecticidal substances to the insecticides is 1: 10-100: 1, the castor insecticidal substances have a remarkable synergistic effect on the insecticides, and the castor insecticidal substances have a good control effect on harmful animals of crops such as cotton bollworms, prodenia litura, beet armyworms, diamond back moths, aphids, whiteflies, thrips, spider mites and the like.

For better understanding of the essence of the present invention, the technical contents of the present invention will be described in detail with examples, but the present invention is not limited to these examples.

A first part: extraction test of castor bean insecticidal substance

Example 1 extraction of Castor insecticidal substances

Drying and crushing 500g of old castor leaves, sieving the crushed old castor leaves by a 100-mesh fine sieve, soaking the old castor leaves dry powder in 50% ethanol water solution according to the mass ratio of the castor tissue dry powder to the ethanol water solution of 1:10 for 8 hours under the condition of 50 ℃ water bath, then ultrasonically oscillating the old castor leaves for 20 minutes under the condition of 50 ℃ water bath, and filtering the old castor leaves to obtain a first filtrate; soaking the filter residue obtained after the first filtration in 50% ethanol water solution with the mass ratio of the filter residue to the castor tissue dry powder of 1:10, performing ultrasonic oscillation for 20min under the condition of 50 ℃ water bath, and filtering to obtain a second filtrate; mixing the filtrates to obtain extractive solution containing fructus Ricini insecticidal substance, rotary evaporating at 60 deg.C in water bath to concentrate the extractive solution containing fructus Ricini insecticidal substance to obtain pasty fructus Ricini insecticidal substance, oven drying at 70 deg.C to constant weight, pulverizing, and sieving to obtain fructus Ricini insecticidal substance powder (TQW-1).

The extraction rate of the castor bean insecticidal substance is calculated to be 10% according to the following formula after the castor bean insecticidal substance powder is weighed, and the content of the ricinine in the castor bean insecticidal substance powder is measured to be 60% by utilizing liquid chromatography (ACQUITY UPLC, Waters; a detector is a diode array detector, a chromatographic column is a C18 column, and a mobile phase is water/acetonitrile).

Example 2 extraction of Castor insecticidal substances

Drying 300g of castor seed shells, crushing, sieving with a 150-mesh fine sieve, soaking the old castor leaf dry powder in an ethanol water solution with the mass concentration of 70% according to the mass ratio of the castor tissue dry powder to the ethanol water solution of 1:15 for 7h under the condition of 60 ℃ water bath, then ultrasonically shaking for 15min under the condition of 60 ℃ water bath, and filtering to obtain a first filtrate; soaking the filter residue obtained after the first filtration in 70% ethanol water solution with the mass ratio of the filter residue to the castor tissue dry powder of 1:15, performing ultrasonic oscillation for 15min under the water bath condition of 60 ℃, and filtering to obtain a second filtrate; mixing the filtrates to obtain extractive solution containing fructus Ricini insecticidal substance, rotary evaporating at 70 deg.C in water bath to concentrate the extractive solution containing fructus Ricini insecticidal substance to obtain pasty fructus Ricini insecticidal substance, oven drying at 65 deg.C to constant weight, pulverizing, and sieving to obtain fructus Ricini insecticidal substance powder (TQW-2).

The extraction rate of the castor bean insecticidal substance was calculated to be 18% by the following formula after the castor bean insecticidal substance powder was weighed, and the ricinine content in the castor bean insecticidal substance powder was measured to be 70% by liquid chromatography (ACQUITY UPLC, Waters; detector is diode array detector, chromatographic column is C18 column, mobile phase is water/acetonitrile).

Example 3 extraction of Castor insecticidal substances

Drying 600g of castor bean cake, crushing, sieving with a 80-mesh fine sieve, soaking old castor leaf dry powder in an ethanol water solution with the mass concentration of 60% according to the mass ratio of castor tissue dry powder to ethanol water solution of 1:20, soaking for 8 hours in a water bath at 60 ℃, then ultrasonically oscillating for 15min in the water bath at 60 ℃, and filtering to obtain a first filtrate; soaking the filter residue obtained after the first filtration in 60% ethanol water solution with the mass ratio of the filter residue to the castor tissue dry powder of 1:20, performing ultrasonic oscillation for 15min under the water bath condition of 60 ℃, and filtering to obtain a second filtrate; mixing the filtrates to obtain extractive solution containing fructus Ricini insecticidal substance, rotary evaporating at 70 deg.C in water bath to concentrate the extractive solution containing fructus Ricini insecticidal substance to obtain pasty fructus Ricini insecticidal substance, oven drying at 65 deg.C to constant weight, pulverizing, and sieving to obtain fructus Ricini insecticidal substance powder (TQW-3).

The extraction rate of the castor bean insecticidal substance is calculated to be 25% according to the following formula after the castor bean insecticidal substance powder is weighed, and the content of the ricinine in the castor bean insecticidal substance powder is determined to be 75% by utilizing liquid chromatography (ACQUITY UPLC, Waters; a diode array detector, a C18 column and water/acetonitrile as a mobile phase).

Comparative example 1 extraction of Castor plant insecticidal substances

Drying 300g of castor seed shells, crushing, sieving with a 150-mesh fine sieve, soaking old castor leaf dry powder in an ethanol water solution with the mass concentration of 95% according to the mass ratio of castor tissue dry powder to ethanol water solution of 1:15, soaking for 7h under the condition of 60 ℃ water bath, then ultrasonically oscillating for 15min under the condition of 60 ℃ water bath, and filtering to obtain a first filtrate; soaking the filter residue obtained after the first filtration in 95% ethanol water solution with the mass ratio of 1:15 to the castor tissue dry powder again, ultrasonically oscillating for 15min under the water bath condition of 60 ℃, and filtering to obtain a second filtrate; mixing the filtrates to obtain extractive solution containing fructus Ricini insecticidal substance, rotary evaporating at 70 deg.C in water bath to concentrate the extractive solution containing fructus Ricini insecticidal substance to obtain pasty fructus Ricini insecticidal substance, oven drying at 65 deg.C to constant weight, pulverizing, and sieving to obtain fructus Ricini insecticidal substance powder (TQW-4).

The extraction rate of the castor bean insecticidal substance is calculated to be 10% according to the following formula after the castor bean insecticidal substance powder is weighed, and the content of the ricinine in the castor bean insecticidal substance powder is measured to be 50% by utilizing liquid chromatography (ACQUITY UPLC, Waters; a diode array detector, a C18 column and water/acetonitrile as a mobile phase).

Comparative example 2 extraction of Castor insecticidal substances

Drying 600g of castor bean cake, crushing, sieving with a 80-mesh fine sieve, soaking old castor leaf dry powder in 10% ethanol water solution according to the mass ratio of castor tissue dry powder to ethanol water solution of 1:20, soaking for 8h under the condition of 60 ℃ water bath, then ultrasonically oscillating for 15min under the condition of 60 ℃ water bath, and filtering to obtain a first filtrate; soaking the filter residue obtained after the first filtration in 10% ethanol water solution with the mass ratio of the filter residue to the castor tissue dry powder of 1:20, performing ultrasonic oscillation for 15min under the water bath condition of 60 ℃, and filtering to obtain a second filtrate; mixing the filtrates to obtain extractive solution containing fructus Ricini insecticidal substance, rotary evaporating at 70 deg.C in water bath to concentrate the extractive solution containing fructus Ricini insecticidal substance to obtain pasty fructus Ricini insecticidal substance, oven drying at 65 deg.C to constant weight, pulverizing, and sieving to obtain fructus Ricini insecticidal substance powder (TQW-4).

The extraction rate of the castor bean insecticidal substance was calculated to be 14% by the following formula after the castor bean insecticidal substance powder was weighed, and the ricinine content in the castor bean insecticidal substance powder was measured to be 45% by liquid chromatography (ACQUITY UPLC, Waters; detector is diode array detector, chromatographic column is C18 column, mobile phase is water/acetonitrile).

A second part: indoor synergy test of castor bean insecticidal substance on insecticide

EXAMPLE 4 indoor synergy test for the combination of 4TQW-2 with insecticides for Cotton bollworm control

The castor bean insecticide dry powder TQW-2 prepared in example 2 was prepared into 1000mg/L castor bean insecticide solution with 0.5% tween-20 aqueous solution, the castor bean insecticide dry powder TQW-4 prepared in comparative example 1 was prepared into 1000mg/L castor bean insecticide solution with 0.5% tween-20 aqueous solution, Ricinine (Ricinine, CAS accession No. 524-40-3, available from carbofuran technologies Co., Ltd.) was prepared into 1000mg/L castor bean insecticide solution with 0.5% tween-20 aqueous solution, the abamectin chlorpyrifos, methomyl, fenpropathrin, dinotefuran, and methylaminomycin benzoate (abbreviated as "emamectin benzoate") to be tested were dissolved with a small amount of analytically pure acetone and then prepared into 100mg/L insecticide solution with 0.5% tween-20 aqueous solution, the method is characterized in that 3-instar cotton bollworm larvae which are harvested from the institute of cotton research (Anyang) of Chinese academy of agricultural sciences are raised indoors for 5-6 generations to serve as test targets of harmful arthropods.

TQW-2, TQW-4, ricinine, chlorpyrifos, methomyl, fenpropathrin, dinotefuran, emamectin benzoate single agent, TQW-2, TQW-4, ricinine and insecticide composition (the mass ratio of the effective components is 1:15, 1:5, 1:1, 20:1, 50:1 and 110:1 respectively) are carried out according to the indoor bioassay test criteria of pesticides (NYT 1154.10-2008) to achieve indoor toxicity to target harmful arthropods. Evaluating the toxicity effect of the composition on target harmful arthropods by using a co-toxicity coefficient method (CTC method), wherein the CTC value is less than 80, and antagonism is formed between two components of the composition; a CTC value greater than 80 and less than 120, an additive effect between the two components of the composition; the CTC value is more than 120, and the two components of the composition have a synergistic effect; the CTC value is more than 150, and the two components of the composition have obvious synergistic effect.

The method for calculating the co-toxicity coefficient of the binary mixture comprises the following steps:

setting the mixing agent as m, and respectively setting the two single agents as a and b; a. the lethal mid-concentrations of b and m on the target are LC₅₀a、LC₅₀b and LC₅₀The virulence indexes of m, a and b are Ka and Kb respectively, and the theoretical value and the actual value of the virulence index of m are Km respectively_thAnd Km_obThe proportions of a and b in the mixture are Pa and Pb respectively; if the single agent a is taken as a standard, the following components are added:

Km_th＝Ka×Pa+Kb×Pb；

TQW-2 and the pesticide have synergistic effects on controlling Helicoverpa armigera at different ratios as shown in Table 1. TQW-2, chlorpyrifos, methomyl, fenpropathrin, dinotefuran and emamectin benzoate are mixed according to the mass ratio of 1:5, 1:1, 20:1 and 50:1 to have good control effect on cotton bollworms, TQW-2 shows synergistic effect on insecticides such as chlorpyrifos, methomyl, fenpropathrin, dinotefuran and emamectin benzoate, wherein the synergistic effect is obvious when the mass ratio is 1:1, 20:1 and 50: 1; TQW-2 and the insecticide are mixed in a mass ratio of 1:15 and 110:1 to only show additive effect.

The prevention effect of the ricinine and the insecticide after being mixed is slightly worse than that of the ricinine and the insecticide after being mixed with TQW-2, and the ricinine and the insecticide are mixed according to the mass ratio of 1:5, 1:1, 20:1 and 50:1 to show the synergistic effect; the mixing in mass ratios of 1:15 and 110:1 only showed additive effects. TQW-4 has additive effect on the control effect of cotton bollworm after being mixed with the insecticide according to the mass ratio of 1:15, 1:5, 1:1, 20:1 and 50:1, and has antagonistic effect on the control effect of cotton bollworm after being mixed with chlorpyrifos, fenpropathrin and emamectin benzoate according to the mass ratio of 110: 1.

TABLE 1 synergistic effect of 1 TQW-2 composition with insecticide for prevention and control of bollworm in different proportions

Note: "+" indicates synergistic effect; ". indicates significant synergy.

EXAMPLE 5 indoor synergistic test for the control of Aphis gossypii with a combination of 5 TQW-2 and an insecticide

The castor disinsection dry powder TQW-2 prepared in example 2 was prepared into 1000mg/L castor disinsection substance solution with 1% sodium dodecyl benzene sulfonate aqueous solution, the castor disinsection dry powder TQW-4 prepared in comparative example 1 was prepared into 1000mg/L castor disinsection substance solution with 1% sodium dodecyl benzene sulfonate aqueous solution, Ricinine (Ricinine, CAS accession number 524-40-3, available from Bailingwei science and technology Co., Ltd.) was prepared into 1000mg/L castor alkali solution with 1% sodium dodecyl benzene sulfonate aqueous solution, the original drug chlorpyrifos, methomyl, fenpropathrin, dinotefuran, and emamectin benzoate (abbreviated as "emamectin benzoate") to be tested were dissolved with a small amount of analytically pure acetone and then prepared into 100mg/L insecticide solution with 1% sodium dodecyl benzene sulfonate aqueous solution, the method is characterized in that cotton aphids collected from a cotton research institute experimental base (river) of Chinese academy of agricultural sciences are raised indoors for 5-6 generations to serve as test targets of harmful arthropods.

TQW-2, TQW-4, ricinine, chlorpyrifos, methomyl, fenpropathrin, dinotefuran, emamectin benzoate single agent, TQW-2, TQW-4, ricinine and insecticide composition (the mass ratio of the effective components is 1:15, 1:5, 1:1, 20:1, 50:1 and 110:1 respectively) are carried out according to the indoor bioassay test criteria of pesticides (NYT 1154.10-2008) to achieve indoor toxicity to target harmful arthropods. Evaluating the toxicity effect of the composition on target harmful arthropods by using a co-toxicity coefficient method (CTC method), wherein the CTC value is less than 80, and antagonism is formed between two components of the composition; a CTC value greater than 80 and less than 120, an additive effect between the two components of the composition; the CTC value is more than 120, and the two components of the composition have a synergistic effect; the CTC value is more than 150, and the two components of the composition have obvious synergistic effect.

The method for calculating the co-toxicity coefficient of the binary mixture comprises the following steps:

setting the mixing agent as m, and respectively setting the two single agents as a and b; a. the lethal mid-concentrations of b and m on the target are LC₅₀a、LC₅₀b and LC₅₀The virulence indexes of m, a and b are Ka and Kb respectively, and the theoretical value and the actual value of the virulence index of m are Km respectively_thAnd Km_obThe proportions of a and b in the mixture are Pa and Pb respectively; if the single agent a is taken as a standard, the following components are added:

Km_th＝Ka×Pa+Kb×Pb；

TQW-2 and the pesticide composition in different proportions have synergistic effects on preventing and controlling Aphis gossypii Glover as shown in Table 2. TQW-2, chlorpyrifos, methomyl, fenpropathrin, dinotefuran and emamectin benzoate are mixed according to the mass ratio of 1:5, 1:1, 20:1 and 50:1 to have good control effect on cotton aphids, TQW-2 shows synergistic effect on insecticides such as chlorpyrifos, methomyl, fenpropathrin, dinotefuran and emamectin benzoate, wherein the synergistic effect is obvious when the mass ratio is 1:1, 20:1 and 50: 1; TQW-2 and the insecticide are mixed in a mass ratio of 1:15 and 110:1 to only show additive effect.

After being mixed with the insecticide, the ricinine has slightly poorer control effect on cotton aphids than that of TQW-2, and is mixed with the insecticide according to the mass ratio of 1:5, 1:1, 20:1 and 50:1 to show synergistic effect; the mixing in mass ratios of 1:15 and 110:1 only showed additive effects. TQW-4, the prevention and control effects of the pesticide and the insecticide are only additive effect after being mixed according to the mass ratio of 1:15, 1:5, 1:1, 20:1 and 50:1, and the prevention and control effects of the pesticide and the chlorpyrifos, methomyl and fenpropathrin are antagonistic effect after being mixed according to the mass ratio of 110: 1.

TABLE 2 synergistic effect of the compositions of 2 TQW-2 and insecticide for controlling Aphis gossypii with different ratios

Note: "+" indicates synergistic effect; ". indicates significant synergy.

EXAMPLE 6 indoor synergism test for the combination of 6TQW-2 and insecticide against Tetranychus urticae

Preparing 1000mg/L castor insecticidal substance solution from 5% nonylphenol polyoxyethylene ether aqueous solution for TQW-2 of castor insecticidal substance prepared in example 2, 1000mg/L castor insecticidal substance solution from 5% nonylphenol polyoxyethylene ether aqueous solution for TQW-4 of castor insecticidal substance prepared in comparative example 1, 1000mg/L castor insecticidal substance solution from 5% nonylphenol polyoxyethylene ether aqueous solution for ricine (CAS accession No. 524-40-3, available from Bailingwei science and technology Co., Ltd.), 1000mg/L castor aqueous solution from 5% nonylphenol polyoxyethylene ether aqueous solution for ricine, original pesticide chlorpyrifos, methomyl, fenpropathrin, dinotefuran and emamectin benzoate (abbreviated as "emamectin benzoate") to 100mg/L insecticide solution from 5% nonylphenol polyoxyethylene ether aqueous solution after dissolving a small amount of analytically pure acetone, the method is characterized in that cotton spider mites which are harvested from the cotton research institute test base (Aksu) of Chinese academy of agricultural sciences are raised indoors for 5-6 generations to serve as test targets of harmful arthropods.

TQW-2, TQW-4, ricinine, chlorpyrifos, methomyl, fenpropathrin, dinotefuran, emamectin benzoate single agent, TQW-2, TQW-4, ricinine and insecticide composition (the mass ratio of the effective components is 1:15, 1:5, 1:1, 20:1, 50:1 and 110:1 respectively) are carried out according to the indoor bioassay test criteria of pesticides (NYT 1154.10-2008) to achieve indoor toxicity to target harmful arthropods. Evaluating the toxicity effect of the composition on target harmful arthropods by using a co-toxicity coefficient method (CTC method), wherein the CTC value is less than 80, and antagonism is formed between two components of the composition; a CTC value greater than 80 and less than 120, an additive effect between the two components of the composition; the CTC value is more than 120, and the two components of the composition have a synergistic effect; the CTC value is more than 150, and the two components of the composition have obvious synergistic effect.

The method for calculating the co-toxicity coefficient of the binary mixture comprises the following steps:

setting the mixing agent as m, and respectively setting the two single agents as a and b; a. the lethal mid-concentrations of b and m on the target are LC₅₀a、LC₅₀b and LC₅₀The virulence indexes of m, a and b are Ka and Kb respectively, and the theoretical value and the actual value of the virulence index of m are Km respectively_thAnd Km_obThe proportions of a and b in the mixture are Pa and Pb respectively; if the single agent a is taken as a standard, the following components are added:

Km_th＝Ka×Pa+Kb×Pb；

TQW-2 and the pesticide composition with different proportions have the synergistic effect of controlling tetranychus urticae koch shown in Table 3. TQW-2, chlorpyrifos, methomyl, fenpropathrin, dinotefuran and emamectin benzoate are mixed according to the mass ratio of 1:5, 1:1, 20:1 and 50:1 to have good control effect on cotton spider mites, TQW-2 shows synergistic effect on insecticides such as chlorpyrifos, methomyl, fenpropathrin, dinotefuran and emamectin benzoate, wherein the synergistic effect is obvious when the mass ratio is 1:1, 20:1 and 50: 1; TQW-2 and the insecticide are mixed in a mass ratio of 1:15 and 110:1 to only show additive effect.

The control effect of the ricinine and the insecticide after being mixed is slightly worse than that of TQW-2, and the ricinine and the insecticide are mixed according to the mass ratio of 1:5, 1:1, 20:1 and 50:1 to show the synergistic effect; the mixing in mass ratios of 1:15 and 110:1 only showed additive effects. TQW-4 has additive effect on the control effect of the cotton spider mites after being mixed with the insecticide according to the mass ratio of 1:15, 1:5, 1:1, 20:1 and 50:1, and has antagonistic effect on the control effect of the cotton spider mites after being mixed with the fenpropathrin according to the mass ratio of 110: 1.

TABLE 3 synergistic effect of the compositions of 3 TQW-2 and insecticides for controlling Tetranychus urticae Koch in different ratios

Note: "+" indicates synergistic effect; ". indicates significant synergy.

EXAMPLE 7 TQW-3 composition with insecticide indoor synergy test for controlling Bemisia tabaci

The castor bean insecticide dry powder TQW-3 prepared in example 3 was prepared into 1000mg/L castor bean insecticide solution with 2% of agricultural milk 600# aqueous solution, the castor bean insecticide dry powder TQW-5 prepared in comparative example 2 was prepared into 1000mg/L castor bean insecticide solution with 2% of agricultural milk 600# aqueous solution, Ricinine (CAS accession No. 524-40-3, available from Bailingwei science and technology Co., Ltd.) was prepared into 1000mg/L castor bean insecticide solution with 2% of agricultural milk 600# aqueous solution, and the original pesticide chlorpyrifos, methomyl, fenpropathrin, dinotefuran and emamectin benzoate (abbreviated as "emamectin benzoate") to be tested was dissolved with a small amount of analytically pure acetone and then prepared into 100mg/L insecticide solution with 2% of agricultural milk 600# aqueous solution, and the insecticide solution was collected from cotton breeding base (Mao) of China academy of agriculture sciences, and feeding tobacco whitefly for 5-6 generations indoors as a test target harmful arthropod.

TQW-3, TQW-5, ricinine, chlorpyrifos, methomyl, fenpropathrin, dinotefuran, emamectin benzoate single agent, TQW-3, TQW-5, and ricinine and pesticide composition (the mass ratio of the effective components is 1:15, 1:5, 1:1, 20:1, 50:1 and 110:1 respectively) are carried out according to the indoor bioassay test criteria of pesticides (NYT 1154.10-2008) to achieve indoor toxicity to target harmful arthropods. Evaluating the toxicity effect of the composition on target harmful arthropods by using a co-toxicity coefficient method (CTC method), wherein the CTC value is less than 80, and antagonism is formed between two components of the composition; a CTC value greater than 80 and less than 120, an additive effect between the two components of the composition; the CTC value is more than 120, and the two components of the composition have a synergistic effect; the CTC value is more than 150, and the two components of the composition have obvious synergistic effect.

The method for calculating the co-toxicity coefficient of the binary mixture comprises the following steps:

setting the mixing agent as m, and respectively setting the two single agents as a and b; a. the lethal mid-concentrations of b and m on the target are LC₅₀a、LC₅₀b and LC₅₀The virulence indexes of m, a and b are Ka and Kb respectively, and the theoretical value and the actual value of the virulence index of m are Km respectively_thAnd Km_obThe proportions of a and b in the mixture are Pa and Pb respectively; if the single agent a is taken as a standard, the following components are added:

Km_th＝Ka×Pa+Kb×Pb；

TQW-3 and the pesticide composition in different proportions have synergistic effects on controlling bemisia tabaci as shown in Table 4. TQW-3, chlorpyrifos, methomyl, fenpropathrin, dinotefuran and emamectin benzoate are mixed according to the mass ratio of 1:5, 1:1, 20:1 and 50:1 to achieve good control effect on bemisia tabaci, TQW-3 shows synergistic effect on insecticides such as chlorpyrifos, methomyl, fenpropathrin, dinotefuran and emamectin benzoate, wherein the synergistic effect is obvious when the mass ratio is 1:1, 20:1 and 50: 1; TQW-3 and the pesticide are mixed according to the mass ratio of 1:15 and 110:1 and only show additive effect.

The control effect of the ricinine and the pesticide after being mixed is slightly worse than that of TQW-3 and the pesticide after being mixed, and the ricinine and the pesticide are mixed according to the mass ratio of 1:5, 1:1, 20:1 and 50:1 to show the synergistic effect; the mixing in mass ratios of 1:15 and 110:1 only showed additive effects. TQW-5 and the pesticide are mixed according to the mass ratio of 1:15, 1:5, 1:1, 20:1 and 50:1, and the control effect on the bemisia tabaci is only additive, and the control effect on the bemisia tabaci is antagonistic after the pesticide is mixed with the chlorpyrifos and the methomyl according to the mass ratio of 110: 1.

TABLE 4 synergistic effect of 4 TQW-3 composition with insecticide against Bemisia tabaci at different ratios

Note: "+" indicates synergistic effect; ". indicates significant synergy.

EXAMPLE 8 indoor synergy test for the combination of 8TQW-3 and insecticide against thrips tabaci

The castor insecticide dry powder TQW-3 prepared in example 3 was prepared into a 1000mg/L castor insecticide solution using a 10% span-20 aqueous solution, the castor insecticide dry powder TQW-5 prepared in comparative example 2 was prepared into a 1000mg/L castor insecticide solution using a 10% span-20 aqueous solution, Ricinine (Ricinine, CAS registry No. 524-40-3, available from Bailingwei science and technology Co., Ltd.) was prepared into a 1000mg/L castor alkali solution using a 10% span-20 aqueous solution, the original pesticide chlorpyrifos, methomyl, fenpropathrin, dinotefuran, and methylamino avermectin benzoate (abbreviated as "emamectin benzoate") to be tested was dissolved with a small amount of analytically pure acetone and then prepared into a 100mg/L insecticide solution using a 10% span-20 aqueous solution, the method takes cotton thrips collected from the experimental base (Tanjiang) of the institute of Cotton, academy of agricultural sciences, China, and after 5-6 generations of breeding indoors as a target for testing harmful arthropods.

TQW-3, TQW-5, ricinine, chlorpyrifos, methomyl, fenpropathrin, dinotefuran, emamectin benzoate single agent, TQW-3, TQW-5, and ricinine and pesticide composition (the mass ratio of the effective components is 1:15, 1:5, 1:1, 20:1, 50:1 and 110:1 respectively) are carried out according to the indoor bioassay test criteria of pesticides (NYT 1154.10-2008) to achieve indoor toxicity to target harmful arthropods. Evaluating the toxicity effect of the composition on target harmful arthropods by using a co-toxicity coefficient method (CTC method), wherein the CTC value is less than 80, and antagonism is formed between two components of the composition; a CTC value greater than 80 and less than 120, an additive effect between the two components of the composition; the CTC value is more than 120, and the two components of the composition have a synergistic effect; the CTC value is more than 150, and the two components of the composition have obvious synergistic effect.

The method for calculating the co-toxicity coefficient of the binary mixture comprises the following steps:

setting the mixing agent as m, and respectively setting the two single agents as a and b; a. the lethal mid-concentrations of b and m on the target are LC₅₀a、LC₅₀b and LC₅₀The virulence indexes of m, a and b are Ka and Kb respectively, and the theoretical value and the actual value of the virulence index of m are Km respectively_thAnd Km_obThe proportions of a and b in the mixture are Pa and Pb respectively; if the single agent a is taken as a standard, the following components are added:

Km_th＝Ka×Pa+Kb×Pb；

TQW-3 and the synergistic effect of the pesticide composition in different proportions for controlling thrips is shown in Table 5. TQW-3, chlorpyrifos, methomyl, fenpropathrin, dinotefuran and emamectin benzoate are mixed according to the mass ratio of 1:5, 1:1, 20:1 and 50:1 to achieve good effect of controlling the cotton thrips, TQW-3 shows synergistic effect on insecticides such as chlorpyrifos, methomyl, fenpropathrin, dinotefuran and emamectin benzoate, wherein the synergistic effect is obvious when the mass ratio is 1:1, 20:1 and 50: 1; TQW-3 and the pesticide are mixed according to the mass ratio of 1:15 and 110:1 and only show additive effect.

The control effect of the ricinine and the pesticide is slightly worse than that of TQW-3 after being mixed with the pesticide, and the ricinine and the pesticide are mixed according to the mass ratio of 1:5, 1:1, 20:1 and 50:1 to show the synergistic effect; the mixing in mass ratios of 1:15 and 110:1 only showed additive effects. TQW-5 has additive effect on the control effect of the cotton thrips after being mixed with the insecticide according to the mass ratio of 1:15, 1:5, 1:1, 20:1 and 50:1, and has antagonistic effect on the control effect of the cotton thrips after being mixed with the chlorpyrifos, the methomyl and the fenpropathrin according to the mass ratio of 110: 1.

TABLE 5 TQW-3 synergistic Effect of different proportions of insecticide composition for prevention and treatment of thrips tabaci

Note: "+" indicates synergistic effect; ". indicates significant synergy.

A second part: field test of insecticidal composition containing castor insecticidal substance

Example 9 field control of Cotton bollworm with insecticidal composition containing Castor insecticidal Material

In order to clarify the field efficacy of the composition in the above examples, the applicant performed a field plot efficacy test for the composition against bollworms in 2017 in the second generation period of bollworms (cotton bud period) at the experimental farm of cotton institute of the academy of agricultural sciences (Anyang).

The test agent is castor bean insecticidal substance dry powder TQW-2 prepared in example 2 and 40% chlorpyrifos emulsifiable concentrate produced by Jiangsu Baoling chemical company Limited, a castor bean insecticidal substance and chlorpyrifos are prepared into a composition mother solution by 0.5% of tween-20 aqueous solution according to the mass ratio of effective components of 5:0, 4:1, 3:2, 2:3, 1:4 and 0:5, and the composition mother solution is sprayed on a cotton field according to the effective component of 675.00g/ha and the dosage. A clear water control was also set, each treatment was repeated 4 times, and each cell had an area of 333.33m²All cells are randomly arranged in groups. Investigating the population basal number and egg number of the cotton bollworm before applying the pesticide for prevention, investigating and recording the live cotton bollworm number at a fixed point 3, 7 and 14 days after pesticide application, and calculating the population decline rate and the prevention effect; counting the damage rate of the buds and the bolls and the bud protection effect during the last investigation after pesticide application; SPSS 19.0 statistical software was used to analyze the control of each treatment and Duncan New Bipolar error (DMRT) was used to test the significance of the differences between treatments.

The calculation formula of the correction control effect (%) and the bud protection effect (%) is as follows:

the 3 rd day oral cavity decline rate (%) - (predrug larvae number + predrug egg number + hatchability) -postdrug larvae number + black egg number + yellow egg number + hatchability)/(predrug larvae number + predrug egg number + hatchability) ]. 100; the control effect (%) was corrected on day 3 (treatment zone oral decline rate ± blank zone oral decline rate)/(100-blank zone oral decline rate) × 100.

On day 7, the oral decline rate (%) is { [ number of larvae before the drug + (number of eggs before the drug + number of eggs after 3 days after the drug) × hatchability ] -number of remaining live larvae }/[ (number of eggs before the drug + number of eggs after 1 day after the drug) × hatchability ] × 100; the control effect (%) was corrected on day 7 (treatment zone oral decline rate ± blank zone oral decline rate)/(100 ± blank zone oral decline rate) × 100.

On day 14, the oral decline rate (%) is [ number of pre-drug larvae + (number of pre-drug eggs + number of eggs 3 days after the drug + number of eggs 7 days after the drug). ] hatchability-number of surviving residual insects ]/[ number of pre-drug larvae + (number of pre-drug eggs + number of eggs 3 days after the drug + number of eggs 7 days after the drug) ] hatchability ] 100; the control effect (%) was corrected on day 14 (treatment zone oral decline rate ± blank zone oral decline rate)/(100-blank zone oral decline rate) × 100.

Bud damage ratio (%) — cumulative damaged bud number/total number of investigated buds 100; bud protection effect (%) (bud damage rate in placebo zone-bud damage rate in treated zone)/bud damage rate in placebo zone 100.

The field control effect statistical analysis results and the bell protecting effect are shown in the table 6. The results show that: the composition of the castor insecticidal substance and the chlorpyrifos has better prevention effect on the second-generation cotton bollworms compared with a single agent, and also has better bud protection effect on cotton. Under the condition of ensuring the prevention effect and the bud protection effect not to be reduced, the application amount of the chlorpyrifos is reduced, the lasting period is prolonged, the prevention and treatment cost of the cotton bollworm is reduced, and the pressure of the chemical prevention and treatment of the cotton bollworm on the environment is reduced.

TABLE 6 composition of castor oil plant insecticide and chlorpyrifos for preventing and controlling bollworm field effect (%) and bud-keeping effect (%)

Note: the control effect (%) and the bud-retaining effect (%) in the above table are the average values of the respective repetitions. Lower case letters in the same column represent significant differences at the 0.05 level.

In conclusion, the castor bean insecticidal substance obtained by combining the ethanol solution hot leaching and the ultrasonic leaching has excellent biological activity, is well compatible with various insecticides, and has remarkable synergistic effect on various insecticides. The insecticidal composition containing the castor insecticidal substance is simple in use method and convenient to popularize and apply. The insecticidal composition containing the castor insecticidal substance has a good control effect on various target arthropods, can reduce the use cost on the premise of greatly improving the pesticide effect, can reduce the application amount of pesticides to a great extent, is beneficial to delaying the development of the resistance of the target arthropods to pesticides, is beneficial to further reducing the pressure of the pesticides on the environment, and meets the requirements of reduction of pesticides and environmental friendliness at present.