Compound low-toxicity insecticidal liquid as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of insecticides, and particularly provides a compound low-toxicity insecticidal solution which comprises the following components in percentage by mass: 2-5% of allicin, 1-10% of essential oil, 2-5ppm of methoprene and the balance of water. The compound low-toxicity insecticidal liquid provided by the invention is in a liquid dosage form and has effective insect expelling and killing effects, the used active components are non-toxic to livestock, the compound low-toxicity insecticidal liquid can be sprayed in a breeding environment and feed for disinfection in a spraying manner, the compound low-toxicity insecticidal liquid is convenient and rapid to use, and the compound low-toxicity insecticidal liquid has the effects of improving the breeding environment, reducing the ammoniacal odor of a breeding house and facilitating the growth of livestock and poultry.

Description

Technical Field

[0001] The present invention belongs to the technical field of insecticides, and in particular relates to a compound low-toxic insecticide liquid, a preparation method and an application thereof. Background Art

[0002] In the livestock and poultry industry, flies are known vectors of disease. By carrying pathogens and parasites that contaminate feed, they can spread dozens of livestock and poultry diseases, accelerating the spread of epidemics. Furthermore, the harassment and nuisance of large numbers of flies can cause restlessness in livestock and poultry, preventing them from getting adequate rest and affecting their feed intake. This can, at best, affect growth and development, feed utilization, hinder fattening, and result in economic losses. In worse cases, it can weaken livestock and poultry's immune system and lead to epidemics. Furthermore, large numbers of flies pose serious public health risks to the surrounding environment.

[0003] Currently, fly control in the aquaculture industry is still primarily based on chemical control. However, the extensive use of chemical pesticides has led to the development of pest resistance, resulting in a series of problems such as increased pesticide application, reduced control effectiveness, the resurgence of pests, and environmental pollution. Summary of the Invention

[0004] The purpose of the present invention is to overcome the problems in the prior art of fly insecticides having obvious drug resistance and being toxic to non-target organisms.

[0005] To this end, the present invention provides a composite low-toxic insecticide liquid, which comprises, by mass percentage, 2-5% of allicin, 1-10% of essential oil, 2-5ppm of methoprene, and the balance is water.

[0006] Specifically, the essential oils include camphor essential oil and citrus essential oil.

[0007] Specifically, the above-mentioned compound low-toxic insecticide liquid further comprises 5-10% of a protective agent; the protective agent comprises β-cyclodextrin.

[0008] Specifically, the above-mentioned compound low-toxic insecticide solution further includes 5-20% of a cosolvent; the cosolvent includes one or more of acetone, DMSO, ethyl acetate, and anhydrous ethanol.

[0009] Specifically, the compound low-toxic insecticide liquid further comprises 1-2% of a suspending agent; the suspending agent comprises at least one of carboxymethyl cellulose and glycerol.

[0010] Specifically, the compound low-toxic insecticide solution further comprises 1-2% of a stabilizer; the stabilizer comprises one or more of H2SO4, H3PO4, and acetic acid.

[0011] The present invention also provides a method for preparing a compound low-toxic insecticide liquid, comprising the following steps:

[0012] (1) dissolving the essential oil in a cosolvent and ultrasonically obtaining reagent A;

[0013] (2) dissolving allicin and a suspending agent in water and adjusting the pH to obtain reagent B;

[0014] (3) dissolving methoprene in a cosolvent to obtain reagent C;

[0015] (4) Dissolve the protective agent in water, add reagent B, sonicate until there is no precipitation in the liquid, add reagents A and C, and sonicate again to obtain a compound low-toxic insecticide solution.

[0016] Compared with the prior art, the present invention has the following advantages and beneficial effects:

[0017] The compound low-toxic insecticide provided by the present invention is a liquid dosage form, has effective anthelmintic and insecticidal effects, and the active ingredients used are non-toxic to poultry and livestock. It can be sprayed on the breeding environment and feed for disinfection by spraying. It is convenient and quick to use, has the effect of improving the breeding environment, reducing the ammonia smell in the breeding house, and is beneficial to the growth of livestock and poultry. DETAILED DESCRIPTION

[0018] The technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Although the representative embodiments of the present invention have been described in detail, it will be understood by those skilled in the art that various modifications and changes can be made to the present invention without departing from the scope of the present invention. Therefore, the scope of the present invention should not be limited to the embodiments, but should be defined by the appended claims and their equivalents.

[0019] The invention provides a compound low-toxic insecticide liquid, which comprises, by mass percentage, 2-5% of allicin, 1-10% of essential oil, 2-5ppm of methoprene, and the balance is water.

[0020] Among them, preferably include 0.5-5% camphor essential oil and 0.5-5% citrus essential oil.

[0021] In a detailed embodiment, the compounded low-toxic insecticide solution further comprises 5-10% of a protective agent, 5-20% of a cosolvent, 1-2% of a suspending agent, and 1-2% of a stabilizer. The protective agent comprises β-cyclodextrin; the cosolvent comprises one or more of acetone, DMSO, ethyl acetate, and anhydrous ethanol; the suspending agent comprises at least one of carboxymethyl cellulose and glycerol, with glycerol also being able to adjust the viscosity of the essential oil preparation and improve the preparation's adhesion; and the stabilizer comprises one or more of H2SO4, H3PO4, and acetic acid.

[0022] The present invention also provides a method for preparing a compound low-toxic insecticide liquid, comprising the following steps:

[0023] (1) Dissolve the surfactant in water and stir evenly; dissolve the essential oil in the cosolvent, add 7.5% Tween 80 solution, and sonicate to obtain reagent A;

[0024] (2) dissolving allicin and a suspending agent in pure water and adjusting the pH to 5.5 to 6.5 to obtain reagent B;

[0025] (3) dissolving methoprene in a cosolvent to obtain reagent C;

[0026] (4) Dissolve the protective agent in water, add reagent B, sonicate until there is no precipitation in the liquid, add reagents A and C, and sonicate again to obtain a compound low-toxic insecticide solution.

[0027] The effects of the compound low-toxic insecticide liquid, preparation method and application of the present invention are studied through specific examples below.

[0028] Example 1:

[0029] 1. Toxic effect of plant essential oils on fly maggot larvae

[0030] 1.1 Pretreatment of housefly larvae

[0031] In the experiment, housefly larvae from the end of the second instar to the beginning of the third instar were selected. The healthy larvae with the same weight and body length were picked out from the culture medium, cleaned, and placed in a culture dish containing 2 ml of physiological saline for later use.

[0032] 1.2 Agarose Preparation

[0033] In a 1 L beaker, add: 10 g agarose, 20 g skim milk powder, 20 g brown sugar, and 20 g cornstarch;

[0034] Add pure water to prepare 1000 ml of solution, heat, boil, and cool. After the agar block solidifies, use a sterilized scalpel to cut it into 0.2 cm thick pieces, and use a 1 cm diameter hollow tube to cut cylindrical agar particles.

[0035] 1.3 Screening of essential oils

[0036] Cinnamon essential oil, cinnamon essential oil, citrus essential oil and citronella oil (all purchased from Shanghai Yuanye Biotechnology Co., Ltd.) were prepared into 100 μL / mL stock solution using acetone as solvent.

[0037] The essential oil was diluted with physiological saline containing 1% Tween 80 to an essential oil content of 1 μL / mL, 10 μL / ml, 25 μL / ml, and 50 μL / ml.

[0038] Soak the agar block in essential oil of corresponding concentration for 1 hour and wipe off the surface moisture.

[0039] Housefly larvae were evenly divided into 17 treatment groups, with 20 larvae per replicate. The larvae were placed in a 150 mm culture dish and evenly placed with 30 essential oil agar blocks. The control group was placed with agar blocks soaked with equal concentrations of acetone and DMSO. The larvae were evenly placed in the culture dish and cultured in a dark incubator at 28℃±0.5℃, 55%±3% humidity for 2 days. Ten agar blocks of the corresponding group were added every 8 hours. The dead larvae were cleaned and recorded, and the mortality rate was counted after 2 days.

[0040] 1.4 Data Processing

[0041] Mortality rate = (number of dead insects / total number of insects) × 100%

[0042] Corrected mortality rate = 100% × [treatment mortality rate (%) - control mortality rate (%)] / [1 - control mortality rate (%)]

[0043] 1.5 Test results

[0044] Table 1 Corrected mortality of housefly larvae with different essential oil contents, %

[0045]

[0046] The results of the fly maggot killing test showed that camphor essential oil, citronella oil and citrus essential oil had better killing effects on fly maggots.

[0047] 2. The killing effect of essential oil combined with methoprene on housefly adults

[0048] 2.1 Reagent Configuration

[0049] Mix camphor essential oil, citronella oil, and citrus essential oil in pairs.

[0050] Methoprene (purchased from Shanghai Maokang Biotechnology Co., Ltd., effective content ≥98%) was prepared into a 1000 mg / L stock solution with DMSO for later use, and then diluted to 100 mg / L with 0.1% Tween 80 in sterile saline.

[0051] The compound essential oil was compounded with methoprene, and diluted with acetone to a concentration of 5 μL / ml of plant essential oil and 2 mg / L or 20 mg / L of methoprene in the preparation.

[0052] 2.2 Experimental Animal Preparation

[0053] 600 adult houseflies 2 days after eclosion were collected and placed in a sealed transparent box. Ether vapor was introduced into the box. After 80% of the houseflies were anesthetized, they were randomly divided into 10 groups with equal weight, half male and half female, with 3 replicates per group and 20 houseflies per replicate. The grouped houseflies were placed in a clean culture dish for processing.

[0054] 2.3 Microdrip method for determination of toxicity of essential oil preparations to houseflies

[0055] House flies were placed on an operating table and the essential oil preparation was dripped onto their outer skin at a rate of 0.2 μL per fly. After the drip, the flies were placed in a cage and considered dead if they fell on their backs and could not crawl. The number of dead flies was counted every 8 hours and any dead flies were removed. Observation continued for 1 day.

[0056] 2.4 Test results

[0057] Table 2 Lethality of housefly corrected by different proportions of essential oil compounded with methoprene, %

[0058]

[0059] The same letters in the same row indicate no significant difference (P < 0.05), and different letters indicate significant difference (P > 0.05).

[0060] A 1:1 mixture of camphor essential oil and citrus essential oil diluted to 5 μL / ml and compounded with 2 mg / L methoprene had a good fly-killing effect.

[0061] 3. The effect of adding allicin to compound low-toxic insecticide on repelling houseflies

[0062] 3.1 Reagent Configuration

[0063] The camphor essential oil and citrus essential oil are compounded in a 1:1 ratio to obtain a mixed essential oil.

[0064] Methoprene (purchased from Shanghai Maokang Biotechnology Co., Ltd., effective content ≥98%) was prepared into a 1000 mg / L stock solution with DMSO for later use, and then diluted to 100 mg / L with 0.1% Tween 80 in sterile saline.

[0065] The compound essential oil, methoprene and allicin were compounded and diluted with acetone to a preparation containing 5 μL / ml of plant essential oil, 2 mg / L of methoprene and 50 g / L of allicin, to prepare a compound essential oil preparation A containing allicin and a compound essential oil preparation B not containing allicin.

[0066] 3.2 Experimental Animal Preparation

[0067] Take 100 healthy and vigorous housefly adults 2 days after emergence, place them in a sealed transparent box No. ①, and cover it with black cloth.

[0068] Take two other breathable boxes of the same size, No. 2 and No. 3, and connect them to the bifurcation of the Y-shaped tube. Spray 5 ml of each of the A and B agents inside the breathable boxes, mark them, and cover them with a black cloth. Attach No. 1 box to the starting end of the Y-shaped tube and gently tap the box to force all houseflies into the tube. Carefully remove No. 1 box and seal the Y-shaped tube. Let it sit for 4 hours. Then remove No. 2 and No. 3 boxes and count the number of houseflies in each box. Calculate the avoidance rate. Repeat the experiment three times.

[0069] Avoidance rate = (1-total number of flies in the box / total number of flies in the two boxes) * 100

[0070] 3.3 Test results

[0071] Table 3. The repellency rate of houseflies to essential oils with allicin, %

[0072]

[0073] The same letters in the same row indicate no significant difference (P < 0.05), and different letters indicate significant difference (P > 0.05).

[0074] The experimental results show that adding allicin to the compound essential oil can improve the repellent rate of houseflies.

[0075] (P>0.05).

[0076] Example 2:

[0077] This embodiment provides a composite low-toxic insecticide liquid, including 5 ml of mixed essential oil (camphor essential oil and citrus essential oil in a 1:1 ratio), 25 g of β-cyclodextrin, 20 ml of acetone, 2 mg of methoprene, 15 g of carboxymethyl cellulose, 50 g of allicin, 10 ml of DMSO, 15 ml of Tween 80, and 950 ml of pure water.

[0078] The compound low-toxic insecticide solution is prepared by the following steps:

[0079] (1) Dissolve Tween 80 in 200 ml of pure water and stir evenly;

[0080] (2) Dissolve the mixed essential oil in acetone, add 7.5% Tween 80 solution, and sonicate for 20 minutes to obtain reagent A;

[0081] (3) Dissolve allicin and carboxymethyl cellulose in 250 ml of pure water, add 1 M H2SO4 to adjust the pH to 5.5, and obtain reagent B;

[0082] (4) dissolving methoprene in DMSO to obtain reagent C;

[0083] (5) Dissolve β-cyclodextrin in 500 ml of cold water, add reagent B, and sonicate for more than 25 min until there is no precipitation in the liquid. Add reagents A and C, and sonicate for another 10 min.

[0084] (6) The preparation is filtered through a 0.22 μm filter membrane to obtain a compound low-toxic insecticide solution.

[0085] Example 3:

[0086] This embodiment provides a composite low-toxic insecticide liquid, including 10 ml of mixed essential oil (camphor essential oil and citrus essential oil in a ratio of 1:1), 20 ml of anhydrous ethanol, 2 mg of methoprene, 100 ml of glycerol, 100 g of allicin, 10 ml of ethyl acetate, 6060 ml of Span, and 800 ml of pure water.

[0087] The compound low-toxic insecticide solution is prepared by the following steps:

[0088] (1) Dissolve the mixed essential oil in anhydrous ethanol, add Span 60 solution, and sonicate for 20 minutes to obtain reagent A;

[0089] (2) Dissolve allicin in 500 ml of pure water, add 1 M H2SO4 to adjust the pH to 5.5, add glycerol, and mix well to obtain reagent B;

[0090] (3) Dissolve methoprene in ethyl acetate and add 200 ml of pure water to obtain reagent C;

[0091] (4) Mix reagent A and reagent C, sonicate for more than 30 minutes until there is no obvious precipitation in the solvent, add reagent B, and sonicate for another 10 minutes.

[0092] (5) The preparation is filtered through a 0.22 μm filter membrane to obtain a compound low-toxic insecticide solution.

[0093] Comparative Example 1:

[0094] In this comparative example, an insecticide solution was prepared using the method of Example 2, except that carboxymethyl cellulose was not added in step (3).

[0095] Comparative Example 2:

[0096] In this comparative example, an insecticide solution was prepared using the method of Example 2, except that β-cyclodextrin was not added in step (5).

[0097] Comparative Example 3:

[0098] In this comparative example, an insecticide solution was prepared using the method of Example 3, except that Span 60 was not added in step (1).

[0099] Comparative Example 4:

[0100] In this comparative example, an insecticide solution was prepared using the method of Example 2, except that H2SO4 was not used to adjust the pH in step (2).

[0101] Example 4:

[0102] Insecticidal solutions are sensitive to temperature and light. Therefore, 30 ml of each of the insecticide solutions of Examples 2-3 and Comparative Examples 1-4 were placed in 50 ml EP tubes, the sampling time was marked, and the samples were placed in darkness at a temperature of 25°C ± 2°C and a humidity of 60% ± 5% for 6 months. The uniformity of the samples was observed at 0, 1, 2, 3, and 6 months. A clear solution was marked as "0", a slightly turbid solution with no stratification or no precipitation was marked as "+", a relatively turbid solution with unclear stratification or partial precipitation was marked as "++", and a sample with turbidity, stratification, and significant precipitation was marked as "+++". The results are shown in Table 4.

[0103] Table 4 Uniformity of essential oil preparations under different configurations

[0104]

[0105] The compound low-toxic insecticide provided by the present invention can ensure stability for 1 to 3 months.

[0106] The above examples are merely illustrative of the present invention and do not limit the scope of protection of the present invention. Any design that is identical or similar to the present invention falls within the scope of protection of the present invention.

Claims

1. A compound low-toxic insecticide, characterized by: Calculated by mass percentage, the invention comprises 2-5% of allicin, 1-10% of essential oil, 2-5ppm of methoprene, and the balance is water.

2. The compound low-toxic insecticide according to claim 1, characterized in that: The essential oils include camphor essential oil and citrus essential oil.

3. The compound low-toxic insecticide according to claim 1, characterized in that: The invention also comprises 5-10% of a protective agent; the protective agent comprises β-cyclodextrin.

4. The compound low-toxic insecticide according to claim 1, characterized in that: The invention also includes 5-20% of a co-solvent; the co-solvent includes one or more of acetone, DMSO, ethyl acetate and anhydrous ethanol.

5. The compound low-toxic insecticide according to claim 1, characterized in that: The invention also includes 1-2% of a suspending agent; the suspending agent includes at least one of carboxymethyl cellulose and glycerol.

6. The compound low-toxic insecticide according to claim 1, characterized in that: The invention also includes 1-2% of a stabilizer; the stabilizer includes one or more of H2SO4, H3PO4 and acetic acid.

7. A method for preparing a compound low-toxic insecticide, characterized in that: The following steps are involved: (1) dissolving the essential oil in a cosolvent and ultrasonically obtaining reagent A; (2) dissolving allicin and a suspending agent in water and adjusting the pH to obtain reagent B; (3) dissolving methoprene in a cosolvent to obtain reagent C; (4) Dissolve the protective agent in water, add reagent B, sonicate until there is no precipitation in the liquid, add reagents A and C, and sonicate again to obtain a compound low-toxic insecticide solution.

8. Use of the compound low-toxic insecticide according to any one of claims 1 to 6 in improving aquaculture environment.

9. The use according to claim 8, characterized in that: Spray the compound low-toxic insecticide on the breeding environment and feed.

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