CN103548886B - Use of Ferula bungeanaemulsion oil or microemulsion as insecticide and acaricide - Google Patents

Abstract

The invention discloses a ferula bungeana insecticidal acaricide and a preparation method thereof. The prepared ferula bungeana insecticidal acaricide is formed by a ferula bungeana extract serving as a main component and auxiliary ingredients. The ferula bungeana insecticidal acaricide can be missible oil or a microemulsion, has a good pesticide effect and is safe to the environment, humans, livestock, natural enemies of pest mites and other beneficial organisms, and pest mites are unlikely to generate drug resistance to the pistacia chinensis acaricide. The insecticidal acaricide manufacturing technology is simple, low in cost and suitable for popularization and application.

Description

Application of hard ferulic emulsifiable oil or microemulsion for killing insects and mites

technical field

The invention belongs to the technical field of pesticides, specifically relates to the field of pesticide preparation and processing, in particular to the application of hard ferulic emulsifiable oil or microemulsion for killing insects and acarids.

Background technique

Hard Ferula (Ferula bungeana Kitagawa) is a plant of the genus Ferula in Umbelliferae (Illustrated Handbook of Higher Plants in China), also known as Fennel (Inner Mongolia, Western Liaoning), Pepper, Flower Tiao (Northern Shaanxi), Wild Fennel (Minqin, Gansu) , Fangfeng, Gangqianhu, Han-Temuri, Niumingmo, Niumingmo, Adenophora, Shaqianhu, fennel, wild fennel, are perennial herbaceous plants. Distributed in Heilongjiang, Jilin, Liaoning, Inner Mongolia, Hebei, Henan, Shanxi, Shaanxi, Gansu, Ningxia and other provinces. It grows in sand dunes, sandy land, Gobi Desert gullies, dry fields, roadsides and gravel hillsides (Editorial Committee of Flora of China, Chinese Academy of Sciences: "Flora of China", Volume 55(3), Science Press, 1992, P.102-103).

Active ingredients: volatile oil contained in the whole plant and fruit of Ferula ferulae, the main components of which are: anisole, accounting for 50-60%, dex-anisone, accounting for 18-20%, D- and L-limonene, dipentene, anisaldehyde etc., the endosperm contains about 15% of fatty oil and about 20% of protein, in addition, it also contains vitamin A-like substances, starch, carbohydrates and mucus.

As a common Chinese herbal medicine, the research on ferulicum mainly focuses on its medicinal activity. Its roots are used for medicinal purposes, and folks are used for clearing heat and detoxification, reducing swelling, and relieving pain (Inner Mongolia); it is also used for nourishing yin and clearing lungs, removing asthenic heat, eliminating phlegm and relieving cough (Shaanxi). The whole herb and its seeds can be used as medicine. It has pungent and warm nature and has the effects of promoting qi and relieving pain, invigorating the stomach and dispersing cold, eliminating phlegm, relieving cough, and relieving exterior syndrome; it is mainly used to treat colds, bronchial pneumonia, tuberculosis, and chest pain , stomach pain, dysmenorrhea and other diseases, especially for the prevention and treatment of tuberculosis has a significant effect.

In terms of agricultural activity, Han Jianhua et al. reported that the acetone extract of hard Ferulicum stems and leaves has certain effects on wheat scab (Gibberella zeae), corn leaf spot (Exserohilum turcicum) and pepper phytophthora (Phytophthora capsici) Bacteriostatic activity. But so far, there is no relevant literature on the research on the insecticidal and acaricidal effects of its deployment system, and no product has been formed and used in production.

Contents of the invention

The purpose of the present invention is to provide a high efficacy, pollution-free, low-cost ferulicum insecticide and acaricide and a preparation method thereof for the application of hard ferulic emulsifiable oil or microemulsion for insecticidal and acaricidal applications.

In order to achieve the above tasks, the present invention takes the following technical solutions to achieve:

An application of hard ferulic emulsifiable oil or microemulsion for killing insects and acarids, characterized in that the prepared hard ferulic emulsifiable oil or microemulsion is processed from hard ferulic extract as main component and added with auxiliary agents, Wherein: described hard Ferulic emulsifiable oil is formulated by weight percentage by following raw material:

Hard Ferulicum extract: 10% to 50%, surfactant: 5% to 20%, the balance is solvent, and the sum of the weight percentages of raw materials is 100%;

Described solvent is one or more mixtures in methanol, ethanol, acetone, n-propanol, ethyl acetate or solvents known in the art;

The surfactant is selected from octylphenol polyoxyethylene ether, calcium dodecylbenzenesulfonate, nonylphenol polyoxyethylene ether, styrene phenol polyoxyethylene polyoxypropylene ether, stearyl polyoxyethylene ether One or more mixtures of phosphate esters;

Described hard Ferulic microemulsion is formulated by weight percentage by following raw material:

Hard ferulic extract: 10% to 30%, emulsifier: 10% to 20%, co-emulsifier: 0.5% to 5%, the balance is water, and the weight percentage of raw materials is 100%;

The emulsifier is calcium dodecylbenzenesulfonate, and the co-emulsifier is nonylphenol polyoxyethylene ether.

Described hard ferulic emulsifiable oil or microemulsion adopts following steps to prepare:

A) Mixing the whole ferulae ferulae, and pulverizing it into a coarse pulverization of 1 mm to 5 mm with a plant tissue pulverizer;

B) The coarse pulverized matter obtained in step A is leached with a solvent, and the extract is concentrated in vacuum to be equivalent to 1kg dry powder/kg concentrated solution; the solvent is ethanol, acetone, ethyl acetate, chloroform, petroleum ether, water Any one or more of them, the extraction temperature is 30-40°C, and the extraction time is 6h-12h;

C) Mix the concentrated solution, solvent and surfactant obtained in step B in proportion, stir evenly in the reactor, the temperature of the reactor is 35°C-60°C, the reaction stirring time is 30 minutes, and the hard molasses is obtained after quality inspection. Wei butter;

D) The concentrate, emulsifier, co-emulsifier and water obtained in step B are stirred evenly in a mixing tank in proportion. The temperature of the mixing tank is 35-60 ° C, and the stirring time is 30 minutes. Ferulic microemulsion.

The hard Ferulic insecticide and acaricide made by the present invention has the following advantages:

1. It has strong poisonous activity against Lepidoptera pests, especially diamondback moth, and has high insecticidal effect; it has good effect on mites, especially against wood sorrel such as spider mites, and has good acaricidal effect;

2. The biologically active ingredients contained are complex, and pests and mites are not easy to develop resistance to them;

3. Safe for the environment, humans, animals, natural enemies of pests and other beneficial organisms;

4. No residual toxicity after use;

5. The resource is abundant, the preparation method is simple, the cost is low, and it is suitable for popularization and use.

Detailed ways

In order to better understand the essence of the invention, the technical content of the invention will be described in detail below in conjunction with examples, but the invention is not limited to these examples.

The present invention uses whole ferulicum as raw material, and through a certain processing process, can be made into an insecticide and acaricide, and the preparation forms are emulsifiable concentrate and microemulsion.

A. Obtaining of Hard Ferulic Extract:

Use a plant tissue grinder to pulverize the whole feruli herb to a coarse pulverization of 1 to 5 mm.

The obtained coarse pulverized product is leached with a solvent, and the extracted product is concentrated in vacuum to an amount corresponding to 1 kg of dry powder/kg of concentrated liquid.

The above-mentioned solvent is any one or more of ethanol, acetone, ethyl acetate, chloroform, petroleum ether (60-90°C), water, the extraction temperature is 30-40°C, and the extraction time is 6h-12h;

B, the preparation of hard Ferulic insecticide and acaricide

The concentrated solution obtained in step A (i.e. ferulicum extract) and auxiliary agents are formulated into emulsifiable concentrates and microemulsions for preventing and controlling harmful organisms. The weight percent of each raw material in above-mentioned various dosage forms is:

EC: ferulicum extract 10%-50%, surfactant 5%-20%, solvent added to 100%;

Mix hard ferulic extract, solvent and surfactant in proportion, stir evenly in the reaction kettle, the temperature of the reaction kettle is 35°C-60°C, the reaction stirring time is 30 minutes, and the hard ferulic insecticide is obtained after quality inspection Acaricide cream;

Above-mentioned solvent is one or more mixtures in methanol, ethanol, acetone, n-propanol, ethyl acetate or solvents known in the art;

The above surfactants are selected from octylphenol polyoxyethylene ether, calcium dodecylbenzenesulfonate, nonylphenol polyoxyethylene ether, styrene phenol polyoxyethylene polyoxypropylene ether, stearyl polyoxyethylene ether phosphate One or a mixture of more than one of them.

Microemulsion: 10%-30% extract, 10%-20% emulsifier, 0.5%-5% co-emulsifier, 100% water;

Stir the hard Ferulic extract, emulsifier, co-emulsifier and water in a mixing tank evenly in proportion. The temperature of the mixing tank is 35-60°C, and the stirring time is 30 minutes. After the quality inspection, the hard Ferulic Insect and acaricide microemulsion.

The emulsifier is calcium dodecylbenzenesulfonate, and the co-emulsifier is nonylphenol polyoxyethylene ether.

The following are examples given by the inventors.

1. Example of preparation of hard Ferulic insecticide and acaricide

Embodiment 1: the preparation of 20% hard ferulic emulsifiable oil:

Weigh 20kg of hard Ferula concentrate, dissolve in 30kg of acetone, then add 15kg of calcium dodecylbenzenesulfonate, 5kg of nonylphenol polyoxyethylene ether, and acetone to make up to 100kg. After being fully mixed, the acaricide emulsifiable concentrate is obtained. After quality inspection, the stability and appearance of the preparation meet the requirements of commercial preparations.

The inventor's test proves that the above-mentioned calcium dodecylbenzenesulfonate and nonylphenol polyoxyethylene ether can also be made of octylphenol polyoxyethylene ether, styrene phenol polyoxyethylene polyoxypropylene ether, stearyl polyoxyethylene ether, etc. Oxyethylene ether phosphate can also be made into an emulsifiable concentrate that meets the requirements of commercial preparations.

Embodiment 2: the preparation of 10% hard Ferulicum microemulsion

Weigh 10kg of hard ferulicum concentrate, dissolve it in 20kg of acetone, then add 15kg of calcium dodecylbenzenesulfonate and 5kg of nonylphenol polyoxyethylene ether, mix under high-speed stirring, and heat to about 30°C; high-speed stirring Add 50kg of deionized water dropwise, control the rate of addition of water, and keep the temperature at about 30°C; after the addition of water, the temperature is raised to 40°C and stirred for 1 hour to obtain 20% hard microemulsion of ferulicum. After quality inspection, the stability and appearance of the preparation meet the requirements of commercial preparations.

2. Indoor Bioassay Example 1:

In this experiment, the poisonous activity of ferulicum acetone extract on wood sorrel such as spider mite and spider mite was determined. The test method and test results are as follows:

1. Test pest mites

Wood sorrel such as Tetranychina harti Ewing and Tetranychus cinnabrinus Boiduval are kept indoors (T=(25±1)℃, RH=(40±10)%, D/L=16h/8h) The population was provided by the Pollution-free Pesticide Research Service Center of Yangling University of Agricultural Science and Technology. Female adult mites with uniform individual size and strong activity were selected for testing.

2. Test method

Toxic activity determination adopts slide immersion method recommended by FAO (1980), and slightly improved, the specific method is as follows: paste 2cm long double-sided adhesive tape on one end of the glass slide, peel off the paper, and pick up the large and small pieces with a brush. Consistent and active female adult mites, stick their backs on double-sided adhesive tape, and ensure that the mites' feet, mouthparts and pedicles can move freely, and stick 30 to 40 heads per piece. Use a binocular dissecting microscope to perform microscopic examination on the sticky test mites, remove unqualified test mites, and make up. Then immerse one end of the glass slide with the test mite stuck in the prepared medicinal solution, shake it lightly for 5 seconds, take it out, quickly absorb the medicinal solution around the mite body with a small piece of absorbent paper, and then move it in at a temperature of (25 ± 1 )°C, relative humidity of (40±10)%, and light conditions of (L/D=18h/6h) in a biochemical incubator. After 24 hours (using wood sorrel such as spider mite as the test mite) and 48 hours later (using Tetranychus cinnabarinus as the test mite), check the results, record the number of dead mites, lightly touch the body of the mites with a brush during microscopic examination, and check the mites without moving their feet considered dead. The test was repeated 3 times, with 0.5% Tween-80 aqueous solution (adding an appropriate amount of acetone and controlling the amount of acetone to be consistent with that in the treatment liquid) as a control. When determining the toxicity, 5 to 7 concentrations of the medicinal solution were set.

The test data was statistically analyzed using SPSS 20.0 software, and the linear regression analysis was carried out according to the probability value analysis method, and the toxicity regression equation, chi-square value χ ² , lethal intermediate concentration LC ₅₀ and its 95% confidence limit were calculated. Adjusted mortality was calculated using Abbott's formula.

Mortality rate (%) = number of dead mites/total number of mites × 100

Adjusted mortality rate (%) = (treatment mortality rate - control mortality rate) / (1 - control mortality rate) × 100

3. Test results

Using the glass slide dipping method, the poisonous activity of ferulicum acetone extract to wood sorrel such as spider mite (24h) and spider mite (48h) was measured, and the toxicity curve was obtained. The results are shown in Table 1 and Table 2 .

Table 1: Toxic activity of ferulicum acetone extracts against wood sorrel such as Tetranychus (24h) and Tetranychus cinnabarinus (48h)

Table 2: Toxicity of acetone extracts of hard ferulicum to wood sorrel such as Tetranychus (24h) and Tetranychus cinnabarinus (48h)

Pest mite Virulence regression equation Lethal intermediate concentration LC ₅₀ (95% confidence limit)/g DW/mL Chi-square value χ ² wood sorrel like spider mite y=2.55+1.77x 0.03(0.01-0.06) 2.09 Tetranychus cinnabarinus y=2.92+2.69x 0.08(0.04-0.11) 1.60

From the data in Table 1 and Table 2, it can be seen that under the concentration of 0.2g DW/mL and 0.1g DW/mL, the acetone extract of ferulicum ferulus has strong poisonous activity against sorrel such as Tetranychus cinnabarinus and Tetranychus cinnabarinus Toxicity test shows that the acetone extract of ferulicum is more toxic to wood sorrel such as Tetranychus cinnabarinus than to Tetranychus cinnabarinus, and _LC50 is 0.03g DW/mL and 0.08g DW/mL respectively.

3. Indoor Biotest Example 2:

Measured the poisonous activity of hard ferulicum acetone extract to armyworm and diamondback moth, test method and test result are as follows:

1. Insects to be tested

Armyworm (Mythimna separata W.) and diamondback moth (Plutella xylostella L.) were kept indoors (T=(25±1)°C, RH=(75±5)%, D/L=12h/12h). Provided by the Pollution-free Pesticide Research Service Center of Northwest Agriculture and Forestry University, healthy and lively 3rd instar larvae of uniform size were selected for the test.

2. Test method

Toxic activity was determined by adding small leaf dish. Cut fresh cabbage or corn leaves into small leaf discs (corn leaves 1cm×1cm, cabbage leaves 0.5cm×0.5cm), soak in the test plant extract for 5s, dry naturally, and put them into a petri dish (D= 9 cm) or a plastic culture box (H=7.5 cm, D=5 cm), insert the test worms starved for 4 h. Each treatment was repeated 3 times, and every repetition of 10 test insects was used as a control with 0.5% Tween-80 aqueous solution (adding an appropriate amount of acetone and controlling the amount of acetone to be consistent with that in the treatment liquid). The results were checked after 48h and 72h of treatment, and the mortality rate was counted (death standard: the test insects could not eat, could not touch or could not crawl normally). When determining the toxicity, the acetone extract of ferulicum ferulae was diluted with 0.5% Tween-80 aqueous solution to the required concentration. The adjusted mortality of armyworm and diamondback moth was calculated according to the following formula.

3. Test results

The toxicity of ferulicum acetone extract to armyworm and Plutella xylostella 3rd instar larvae at 48h and 72h was determined by adding the small leaf dish, the results are shown in Table 3.

Table 3: Toxicity determination of the acetone extract of ferulicum ferulae to the 3rd instar larvae of Plutella xylostella xylostella and armyworm

From the data in Table 3, it can be seen that the virulence of Ferulica ferulae extract to armyworm and diamondback moth at 48h and 72h are different. Among them, the toxicity of Ferulica ferulae extract to Plutella xylostella was higher than that to Armyworm, the LC ₅₀ of 48h was 0.09g DW/mL and 0.15g DW/mL, and the LC ₅₀ of 72h was 0.07g DW/mL respectively. mL and 0.10g DW/mL.

Four, field efficacy test embodiment 1:

In order to verify the field efficacy of hard ferulic emulsifiable oil and hard ferulic microemulsion against Tetranychus cinnabarinus, the applicant controlled two hard ferulic preparations against cinnabar leaf Field plot efficacy test of mites.

1. Drugs to be tested

20% hard ferulic emulsifiable oil and 10% hard ferulic microemulsion are provided by the Pollution-free Pesticide Research Service Center of Yangling University of Agricultural Science and Technology;

1.8% Abamectin EC (Hebei Jindelun Biochemical Technology Co., Ltd.).

2. Test items

3 syringes (10ml), 2 knapsack sprayers, hang tags (300 pcs), 1 enamel tank (1000ml), 3 pencils, 1 record book, some setting needles, and a camera.

3. Test crops

corn.

4. Experimental design and methods

The plot test is randomly arranged, and the area of the plot depends on the actual situation. Carry out foliage constant spray with 250, 500 and 750 times of the test agent, the contrast agent is 1.8% abamectin 3000 times of liquid, and set clear water control, a total of 8 treatments, each treatment repeated 3 times, each repeated for a district. The test was applied on July 20, 2012, and the front and back sides of the corn leaves were evenly sprayed with Gongnong-16 sprayer until the leaves began to drip. The weather was fine when the pesticide was applied, and there was no rain during the test. Mark 5-10 leaves with mites in each plot, and investigate the amount of spider mites (the number of insects in each plot should be no less than 100). Investigate the base number of mite mouths before the drug treatment, and investigate the number of residual living mites 1, 3, and 7 days after the drug treatment. According to the survey results, the control effect of each treatment area was calculated in chronological order, and the difference in effect among the treatments was compared using the DMRT method.

Calculated as follows:

Control effect (%)={1-(Ta·Cb)/(Tb·Ca)}×100

Ta: the number of live mites in the chemical treatment area after treatment; Tb: the number of live mites in the chemical treatment area before treatment;

Ca: the number of live mites in the blank control area after treatment; Cb: the number of live mites in the blank control area before treatment

5. Experimental results and statistics

The control effects of 20% hard ferulic EC and 10% hard ferulic microemulsion on Tetranychus cinnabarinus were measured, and the results are shown in Table 3.

Table 4: Control effect of two kinds of hard ferulic acaricides on Tetranychus cinnabarinus

Note: The data in the table is the average value of 3 repetitions; in the column of "control effect", the same letter after the value in the same column means that the difference is not significant at the level of α=0.05 (DMRT method). The table below is the same.

It can be seen from Table 4 that both hard ferulic emulsifiable oil and hard ferulic microemulsion have good control effects on Tetranychus cinnabarinus. After 3 days of application, the 250 times and 500 times of the two preparations had better control effects on Tetranychus cinnabarinus, especially the 250 times of the two preparations had the best effect, and there was no significant difference with the 3000 times of 1.8% avermectin EC. difference. After 7 days of spraying, the control effects of the two preparations decreased, but the control effects of the 250-fold and 500-fold solutions were still above 80%, which indicated that they had good long-lasting effects. Considering factors such as economy, it is recommended to use hard ferulic emulsifiable oil and hard ferulic microemulsion 500 times.

Five, field test embodiment 2:

In order to clarify the field efficacy of the two hard Ferulic preparations on Plutella xylostella, the applicant conducted a field plot to control Plutella xylostella with two hard Ferulic preparations in the vegetable field of Dongni Village, Nianqiao Township, Weinan City, Shaanxi Province in 2012. Drug efficacy test.

1. Drugs to be tested

20% hard ferulic emulsifiable oil and 10% hard ferulic microemulsion are provided by the Pollution-free Pesticide Research Service Center of Yangling University of Agricultural Science and Technology;

20% fenvalerate emulsifiable concentrate (Jiangsu Tongzhou Xinhua Pesticide Factory).

2. Test crops

kale.

3. Objects of prevention and control

Diamondback moth (Plutella xylostella L.).

4. Experimental design and methods

The plot test is randomly arranged, and the area of the plot depends on the actual situation. Use 250, 500 and 750 times of the liquid volume of the test agent for constant spraying on the leaves, and use 1000 times of 20% fenvalerate EC as the control agent, and set up water as a control, a total of 8 treatments, each treatment set 3 repetitions, Each repetition is a plot. The investigation method of fixed-point and fixed-plant was adopted, and 5 points were investigated in each plot, and 5 plants were investigated in each point, and a total of 25 plants were investigated in each plot. The day of spraying was sunny and there was no rain during the test. Investigate the base number of insect population before spraying, and investigate the number of insect population 1, 3, and 7 days after spraying. Calculate the control effect, and use the DMRT method to analyze the significance of the difference among the treatments. Calculated as follows:

5. Experimental results and statistics

The control effects of 20% hard ferulic EC and 10% hard ferulic microemulsion on Plutella xylostella were measured, and the results are shown in Table 5.

Table 5: The control effect of two hard ferulic preparations on Plutella xylostella

It can be seen from Table 5 that the two preparations of ferulicum feruli had good control effects on Plutella xylostella. After 3 days of spraying, the 250 times of the two preparations had the best control effect on diamondback moth, both above 80%. difference. In this field efficacy test, the control effect of the 500-fold solution of the two preparations was also more than 70%, which also had a good control effect, while the control effect of the 750-fold solution was poor.

Claims (2)

1. An application of hard ferulic emulsifiable oil or microemulsion for killing insects and acarids, characterized in that the prepared hard ferulic emulsifiable oil or microemulsion is processed by hard ferulic extract as main component and added auxiliary agent , wherein: the hard ferulic emulsifiable oil is prepared by the following raw materials by weight percentage: Hard Ferulicum extract: 10% to 50%, surfactant: 5% to 20%, the balance is solvent, and the sum of the weight percentages of raw materials is 100%; Described solvent is the mixture of one or more in methanol, ethanol, acetone, normal isopropanol and ethyl acetate; The surfactant is selected from octylphenol polyoxyethylene ether, calcium dodecylbenzenesulfonate, nonylphenol polyoxyethylene ether, styrene phenol polyoxyethylene polyoxypropylene ether and stearyl polyoxyethylene ether One or a mixture of two or more phosphate esters; Described hard Ferulic microemulsion is formulated by weight percentage by following raw material: Hard ferulic extract: 10% to 30%, emulsifier: 10% to 20%, co-emulsifier: 0.5% to 5%, the balance is water, and the weight percentage of raw materials is 100%; The emulsifier is calcium dodecylbenzenesulfonate, and the co-emulsifier is nonylphenol polyoxyethylene ether. 2. the application of hard ferulic emulsifiable oil or microemulsion as claimed in claim 1 is used for killing insects and acarids, it is characterized in that, described hard ferulic emulsifiable oil or microemulsion adopts the following steps to prepare: A) Mixing the whole ferulae ferulae, and pulverizing it to a coarse pulverization of 1-5 mm with a plant tissue pulverizer; B) The coarse pulverized matter obtained in step A is extracted with a solvent, and the extract is concentrated in vacuum to be equivalent to 1kg dry powder/kg concentrated solution; the solvent is ethanol, acetone, ethyl acetate, chloroform, petroleum ether and water The extraction temperature is 30-40°C, and the extraction time is 6-12 hours; C) Mix the concentrated solution, solvent and surfactant obtained in step B in proportion, stir evenly in the reactor, the temperature of the reactor is 35-60°C, the reaction stirring time is 30 minutes, and the hard ferulicum is obtained after quality inspection Cream; D) Stir the concentrate, emulsifier, co-emulsifier and water obtained in step B evenly in a mixing tank in proportion. The temperature of the mixing tank is 35-60°C, and the stirring time is 30 minutes. After the quality inspection, the hardened Ferulic microemulsion.