Suspoemulsion composition for preventing and treating cockroaches and preparation method of suspoemulsion composition

Abstract

The invention discloses a suspension emulsion composition for preventing and controlling cockroaches and a preparation method thereof. The cockroach insecticide is composed of a pre-dissolved main drug A, a solid main drug B, a solid main drug C, a dispersing agent, a thickening agent, a thixotropic agent, a defoaming agent, a preservative, an anti-freezing agent and cockroach pheromone, the main drug A is a chloride ion channel inhibitor, the solid main drug B is an acetylcholine receptor agonist, the solid main drug C is an acetylcholine enzyme inhibitor, and the insecticidal effect is remarkably improved through the multi-target synergistic effect; the pest resistance is reduced. In the preparation process, high-speed shearing and particle grinding technologies are adopted, so that uniform distribution and stability of the medicine in the suspoemulsion are ensured. The suspoemulsion shows excellent insecticidal performance under various environmental conditions, has short lethal time and lasting killing effect, is high in safety to human and livestock, is environment-friendly, is suitable for cockroach control in household and commercial environments, and is a convenient, economical and efficient sanitary pest control solution.

Description

Technical Field

[0001] The present invention relates to the field of cockroach control insecticides, and in particular to a suspoemulsion composition for controlling cockroaches and a preparation method thereof. Background Art

[0002] Cockroaches are ancient insects, dating back over 350 million years. They are widely distributed worldwide and are particularly common in warm, humid environments. Cockroaches are typically flat, oval, have a hard exoskeleton, and long antennae. They are primarily nocturnal and highly adaptable to a variety of environments. Because they not only spread disease but also destroy food and other organic materials, they are considered important pests. There are many species of cockroaches, but the German cockroach and the American cockroach are the most common indoor pests.

[0003] Cockroaches are highly adaptable and have strong survival abilities, making them resistant to many traditional insecticides. This has prompted researchers to focus on how to improve the effectiveness and safety of cockroach drugs through new compounds or unique delivery systems to reduce their harm to human health and the environment.

[0004] A wide variety of cockroach control drugs are currently available on the market, including common chemical drugs such as acephate, imidacloprid, propoxur, chlorpyrifos, and fipronil, as well as biological cockroach killers such as avermectin, cockroach viruses, and Metarhizium anisopliae. In addition, pyrethroids, boric acid, mothballs, and natural substances such as garlic cloves, onions, and Sichuan peppercorns are also widely used.

[0005] Suspoemulsions can impart unique dispersion systems to main drugs with different solubility characteristics. This multiphase dispersion system ensures the uniform distribution of various drugs in the spoemulsion, allowing their respective effects to be fully exerted, achieving a synergistic effect. By adjusting the viscosity of the spoemulsion (such as by adding thickeners or stabilizers), solid particles can be kept suspended in the emulsion while preventing the sedimentation of solid components. Advanced micronization or nanometerization technologies are used to micronize the solid phase components, increasing the surface area in contact with the target organism and improving the stability of the drug efficacy. Its stability not only extends the storage time of the product but also ensures the uniform exertion of drug efficacy. The dispersed state of the solid phase particles further reduces the risk of precipitation while increasing the resistance of the preparation to environmental influences. The spoemulsion can be used directly through ordinary spray equipment, has good dispersibility, and evenly covers the target area. The micro-high efficiency characteristics reduce the amount of drug used and meet environmental requirements.

[0006] Phenylpyrazole broad-spectrum insecticides affect specific receptors (such as γ-aminobutyric acid receptors) in the insect central nervous system, leading to abnormal nerve conduction and thus causing insect death. Existing cockroach control technologies mainly include chemical insecticides and pheromone luring, but both have certain limitations. In terms of chemical control, CN114868758A discloses a cockroach control composition compounded with pyrethroids and organophosphorus. Although it has a fast knockdown rate, it has a risk of accidental killing of non-target organisms (such as pets and beneficial insects), and long-term use may lead to environmental residues. In order to reduce the negative impact of chemical agents, CN10614750A has developed a cockroach pheromone-based luring technology, which enhances the trapping efficiency by extracting cockroach aggregation pheromones (such as nonanoic acid and decanoic acid); however, this method relies on the purity and stability of the pheromone, and is easily affected by temperature and humidity in actual application, resulting in fluctuations in the luring effect. Nicotine insecticides are widely used because of their neurotoxic mechanism. For example, CN104663701A discloses a synergistic suspoemulsion containing imidacloprid, which achieves rapid lethality by blocking cockroach acetylcholine receptors. However, the prior art does not address the problem of drug resistance that may be caused by long-term single use. In order to improve drug efficacy, CN101978830A further developed a compound wettable powder of nicotine and highly effective chlorflucythrinate, but its compounding ratio needs to be strictly regulated, otherwise there may be problems of stratification or unstable drug efficacy. Carbamate insecticides work by inhibiting acetylcholinesterase. CN110074125A and CN107372554A have developed preparations with propoxur and benomyl as main ingredients, respectively. Although they have a dual effect of contact and stomach poisoning, the mammalian toxicity mentioned in the patents limits their application in domestic environments. Furthermore, CN1100500786A attempts to extend the duration of efficacy by compounding cypermethrin with carbamates into a suspoemulsion. However, this compounding may increase degradation in soil and water, posing a potential risk of environmental accumulation. In summary, while existing technologies have achieved breakthroughs in cockroach killing efficiency, further optimization is still needed in terms of environmental compatibility, resistance management, and formulation stability.

[0007] Although the existing technology is effective in killing cockroaches, the current prevention and control situation shows that single-dose medication will produce obvious resistance problems over time, causing the required dosage to increase continuously, which is unfavorable for ecological and environmental safety. This problem has been alleviated by using one or two of the above-mentioned insecticide combinations. However, after years of environmental screening, the problem of drug resistance has gradually emerged. In addition, the dosage forms of existing cockroach medicines include but are not limited to baits, suspensions, and emulsifiable concentrates, all of which achieve certain cockroach killing effects by virtue of their advantages. For example, the effect of baits is long-lasting, easy to use, and can expand the scope of killing indirectly, while suspensions are quick to take effect, have a wide range of spraying, and are adaptable to various environments. However, baits have long waiting times, are prone to failure, and are highly environmentally polluting. Suspensions require high professional requirements for spraying technology or equipment, and have unstable sedimentation and stratification phenomena. The fillers in wettable agents have a problem of soil compaction, and low-boiling-point solvents such as xylene in emulsifiable concentrates have high environmental polluting properties. Suspoemulsions can stably suspend high-concentration drugs of different solubilities through solid-liquid suspension, and are suitable for preparing multi-component high-concentration compound preparations. However, there are few precedents for the preparation of cockroach drug suspoemulsions. Summary of the Invention

[0008] To solve the above problems, the object of the present invention is to provide a suspoemulsion composition for preventing and treating cockroaches and a preparation method thereof, by combining the three main components of chloride channel inhibitor A, acetylcholine receptor agonist B, and acetylcholine enzyme inhibitor C and using them as the main drug for compounding, that is, nerve signal transmission, receptor activation and enzyme activity regulation related types of nerve agents act together, in order to reduce the drug resistance of cockroaches, improve the cockroach killing effect of the agent, and even expand the insecticide spectrum, improve the secondary killing rate, and avoid the situation of multiple administration. A large amount of pre-screening work is carried out on the auxiliary agent system, and the dosage form is selected as a suspoemulsion. Through the coordinated combination of various auxiliary agents such as dispersants, emulsifiers, and low-toxic organic solvents, in order to evenly disperse the main drug, reduce the solvent dosage, ensure the high efficiency and broad-spectrum adaptability of the suspoemulsion, and enhance stability. It has good application prospects.

[0009] In order to solve the existing technical problems, the technical problems adopted by the present invention are:

[0010] A suspoemulsion composition for controlling cockroaches comprises a pre-dissolved main drug A, a solid main drug B, a solid main drug C, a dispersant, a thickener, a thixotropic agent, a defoaming agent, a preservative, an antifreeze agent, and a cockroach pheromone. The main drug A is a chloride ion channel inhibitor, the solid main drug B is an acetylcholine receptor agonist, and the solid main drug C is an acetylcholinesterase inhibitor. The mass fraction of the main drug A in the suspoemulsion composition is 5-20%, the mass fraction of the solid main drug B in the composition is 5-20%, and the mass fraction of the solid main drug C in the composition is 5-20%, and the mass ratio thereof is 1:1:-1:5:5.

[0011] As an improvement, the chloride channel inhibitor is any one of fipronil, ethiprole, fipronil and acetamiprid; the acetylcholinesterase inhibitor is any one of propoxur, benzylpyrid, carbaryl, carbosulfan, methiocarb and methylaminocarb; the acetylcholine receptor agonist is any one of acetamiprid, clothianidin, cyclohexidine, dinotefuran, imidacloprid, nitrazepam, thiacloprid and thiamethoxam.

[0012] As an improvement, the mass fraction of the dispersant is 1.0-15.0%, and the dispersant includes one or more of polymer polycarboxylate, dispersant NNO, dispersant MF, sodium lignin sulfonate, sodium lauryl sulfate, castor oil polyoxyethylene ether, and polyoxyethylene ether carboxylate.

[0013] As an improvement, the mass fraction of the thickener is 0.5-1.0%, and the thickener includes one or more of starch, gum arabic, pectin, agar, gelatin, sodium alginate, carrageenan, xanthan gum, methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, polyacrylamide, polyvinyl alcohol or sodium polyacrylate.

[0014] As an improvement, the mass fraction of the thixotropic agent is 0.1-0.5%, and the thixotropic agent is one or more of fumed silica, organic bentonite, hydrogenated castor oil, and polyamide wax; the mass fraction of the defoaming agent is 1.0-1.5%, and the defoaming agent is one or more of polydimethylsiloxane, polyoxypropylene glycerol ether, palmitic acid, isopropyl ester, octanoate, and polyether-modified polysiloxane; the mass fraction of the preservative is 0.1-0.5%, and the preservative includes one or two of benzoic acid, sodium benzoate, and sodium phenylpropionate; the mass fraction of the antifreeze is 1.0-5.0%, and the antifreeze includes one or two of propylene glycol and ethylene glycol; the mass fraction of the cockroach pheromone is 0.5-1.0%.

[0015] The preparation method of the above-mentioned suspoemulsion composition for controlling cockroaches comprises the following steps:

[0016] Step 1: fully stirring the main drug A with an organic solvent to obtain a pre-dissolved main drug A;

[0017] Step 2, deionized water, dispersant, and thickener are subjected to high-speed shearing of the dispersant for 1 hour to obtain a dispersion;

[0018] Step 3: Add a thixotropic agent, a defoaming agent, a preservative, a cockroach pheromone, and an antifreeze agent to the dispersion in sequence, then slowly add the ground solid main drug B and solid main drug C to the obtained dispersion, and high-speed shear for 2 hours to obtain a dispersed and stable suspoemulsion;

[0019] Step 4: Slowly add the pre-dissolved main drug A to the obtained suspoemulsion while maintaining high-speed shearing, and continue high-speed shearing for 1 hour to obtain a stable suspoemulsion.

[0020] As an improvement, the mass fraction of the organic solvent in step 1 is 10-25%, and the organic solvent is a mixture of one or more of xylene, cyclohexanone, ethyl acetate, propylene glycol methyl ether, isopropanol, dichloromethane, ethylene glycol or toluene.

[0021] As an improvement, the shear speed of the high-speed shear is 1000-8000 r / min, the grinding medium is 95% zirconia beads of 0.8-1.0 mm, and after grinding, it is detected by a laser particle size distribution analyzer until the particle size D90 is less than 4 μm.

[0022] Beneficial effects:

[0023] Compared with the prior art, the cockroach control suspoemulsion composition and preparation method thereof of the present invention have the following advantages:

[0024] 1. Multi-phase synergistic effect

[0025] The present invention uses a unique suspoemulsion dispersion system to evenly distribute the main drugs with different solubility characteristics, allowing for the synchronous release of drugs in both the solid and liquid phases. The multi-target mechanism of action and the cumulative effect of drug efficacy are significantly superior to those of a single dosage form, controlling cockroach resistance to cockroach drugs. Specifically, the three main drug components simultaneously act on the insect nervous system by combining different biochemical targets, avoiding the drug resistance problem caused by a single mechanism of action. At the same time, the cumulative effect on different targets can significantly enhance the overall insecticidal activity. A provides a strong toxic effect to ensure long-lasting efficacy, B further prolongs the duration of efficacy through enzyme inhibition, supplementing the deficiencies of other drugs, and C has a faster rate of action, which can quickly knock down insects. The combination of the three ingredients: shows a rapid and efficient killing effect on cockroaches under all experimental conditions, and the killing time is shorter and the effect is more lasting.

[0026] 2. Stability and long-term effectiveness

[0027] The present invention uses micron / nanotechnology to optimize the dispersibility of solid-phase components, which not only increases the contact area of ​​the drug effect, but also avoids sedimentation through viscosity control, and improves storage stability by more than 50%. At the same time, the preparation has a simple processing technology and low production cost. Oil phase dissolution: The oil-solubility property of A causes it to be distributed in the oil phase part of the suspoemulsion, which contributes to slow release and long-lasting toxicity. Solid phase dispersion: The solid phase form of B can form a stable solid particle distribution in the suspoemulsion, slowly release toxicity and maintain the stability of the overall system. Water phase dissolution: As a water-soluble component, C can quickly dissolve in the aqueous phase, forming a uniform distribution, so that its effect is quickly exerted and insects are knocked down. The combination of the three enables the drug effect to achieve the best balance in time and space, avoiding the drug effect disappearing too quickly or uneven release.

[0028] 3. Stronger environmental adaptability

[0029] The anti-settling properties of suspoemulsions can withstand changes in temperature and humidity, and the drug's efficacy is 30% longer than that of emulsifiable concentrates. It is also less susceptible to stratification and failure due to environmental factors.

[0030] 4. Easy to use and environmentally friendly

[0031] The invention can be applied directly through spray equipment, with coverage uniformity increased by 60% compared with powders. The micro-high-efficiency design reduces drug residues, and the dosage is only 1 / 3 of that of traditional dosage forms. DETAILED DESCRIPTION

[0032] Below in conjunction with embodiment, the present invention is further described, and clear purpose, technical scheme and advantage of the present invention are clear.In following embodiment, A, B, C and other auxiliary agents are commercially available prods, and the present invention, by carrying out a large amount of screening work to auxiliary agent system, finally draws the ingredient prescription of part embodiment, and formula table is shown in chart 1 (it is the weight of each medicine in 100g suspoemulsion, and the remaining is supplemented with deionized water).

[0033] Preparation example:

[0034] The present invention is weighed according to the formula in Table 1, and the specific preparation steps are as follows:

[0035] Using a grinder equipped with 0.8 mm 95% zirconium oxide beads, 10 g of ethiprole (Main Agent A), 6 g of carbosulfan (Main Agent B), and 12 g of cycloheximide (Main Agent C) were ground at 6000 rpm. A solid particle size D90 of less than 4 μm was determined by laser particle size analysis. The pre-dissolved ethiprole solution of the main agent A was obtained by thorough mixing with an organic solvent.

[0036] Deionized water, 5 g of dispersant NNO, and 0.7 g of thickener agar were sheared at a speed of 6000 r / min for 1 hour in a high-speed disperser to obtain a dispersion. Thixotropic agent polyamide wax 0.3 g, defoaming agent polydimethylsiloxane 1 g, preservative sodium benzoate 0.3 g, cockroach pheromone 1 g, antifreeze agent ethylene glycol 2 g and other auxiliary agents were then added to the dispersion in sequence. Then, the main drug B carbosulfan and the main drug C cycloheximide were slowly added. The high-speed disperser was sheared at a speed of 6000 r / min for 2 hours to obtain a stable suspension emulsion. The high-speed shear was maintained, and the pre-dissolved main drug A ethiprole solution was slowly added to the obtained suspension emulsion. The high-speed disperser was continued to shear at a speed of 6000 r / min for 1 hour to obtain a stable suspension emulsion.

[0037] Taking Example 1 as a preparation example, the following experimental schemes are used as parallel examples, as shown in Table 1.

[0038] Table 1 Recipe table for each example

[0039]

[0040]

[0041] Performance testing

[0042] The performance of the suspoemulsion obtained in the above embodiment was tested. Various performance standards were tested in accordance with the current standards formulated by the General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China and the Standardization Administration of China. The results are shown in Table 2 below.

[0043] Table 2 Detection performance of each embodiment

[0044]

[0045]

[0046] Drug efficacy testing

[0047] (1) Materials and equipment

[0048] Materials: cockroach drug suspension emulsion, appropriate amount of cockroaches (common experimental cockroaches such as German cockroaches or American cockroaches), bait (conventional cockroach breeding bait), deionized water, standard solution and control solution.

[0049] Equipment: experimental cages or glass bottles (for raising cockroaches), feeding utensils, pipettes and tips, electronic balance, data recording table, video equipment (optional, for recording cockroach behavior), thermometer and hygrometer.

[0050] (2) Experimental steps

[0051] Preparation: Select healthy cockroaches of similar weight and divide them into several groups (e.g., treatment group and control group), with at least 5 cockroaches per group. Keep the cockroaches in experimental cages, provide standard bait and water, and maintain an appropriate temperature and humidity (e.g., 25-28°C, 50-60% humidity). Prepare cockroach drug suspension emulsion solutions of varying concentrations (e.g., 1%, 0.5%, 0.1%, etc.). Use deionized water or a blank solution for the control group.

[0052] Experimental process: Spray the suspoemulsion evenly on the cockroach bait, ensuring that each group of cockroaches ingests the same amount of drug or control solution. Feed the treated bait and record the initial time. Observe and record the survival of the cockroaches at regular intervals (such as every 6 hours or 12 hours). Record the number of cockroach deaths, abnormal behavior, eating conditions, etc. Continue to observe until the end of the experiment (such as 48 hours or 72 hours). Count the mortality rate, half-lethal time (LT50) and other indicators of cockroaches in each group. Compare the mortality rate of different concentration groups with the control group, and analyze the dose-effect relationship of the drug. Use statistical software (such as SPSS, Excel, etc.) to analyze the data and determine the significance of the results.

[0053] (3) Insecticidal performance test

[0054] Table 3 Insecticidal performance test of each embodiment

[0055]

[0056] Currently, there are eight common cockroach repellents on the market, including baits, gel baits, cockroach traps, and aerosols. We selected three brands (PREMISE, Black Tornado, and Duoduomie) and tested them on 160 German cockroaches. We observed and recorded the results for 48 hours. The results are as follows:

[0057] Table 4 Insecticidal performance test of each comparative example

[0058]

[0059] In summary, the present invention utilizes a multi-target synergistic effect of a chloride channel inhibitor, an acetylcholine receptor agonist, and an acetylcholinesterase inhibitor to significantly enhance insecticide efficacy and reduce pest resistance. Comparative tests show that the knockdown and mortality rates of this suspoemulsion against cockroaches are comparable to those of mainstream commercial products, but it offers advantages in terms of resistance resistance and long-lasting efficacy, making it particularly suitable for controlling highly resistant pest populations.

Claims

1. A suspoemulsion composition for controlling cockroaches, characterized in that: The suspoemulsion composition comprises a pre-dissolved main drug A, a solid main drug B, a solid main drug C, a dispersant, a thickener, a thixotropic agent, a defoaming agent, a preservative, an antifreeze agent, and a cockroach pheromone. The main drug A is a chloride ion channel inhibitor, the solid main drug B is an acetylcholine receptor agonist, and the solid main drug C is an acetylcholine enzyme inhibitor. The mass fraction of the main drug A in the suspoemulsion composition is 5-20%; the mass fraction of the solid main drug B in the composition is 5-20%; and the mass fraction of the solid main drug C in the composition is 5-20%. The mass ratio of the main drug A and the solid main drug C is 1:1:-1:5:

5.

2. The suspoemulsion composition for controlling cockroaches according to claim 1, wherein The chloride channel inhibitor is any one of fipronil, ethiprole, fipronil and acetamiprid; the acetylcholinesterase inhibitor is any one of propoxur, beniocarb, carbaryl, carbosulfan, methiocarb and methylaminocarb; the acetylcholine receptor agonist is any one of acetamiprid, clothianidin, cyclohexidine, dinotefuran, imidacloprid, nitramoxadone, thiacloprid and thiamethoxam.

3. The suspoemulsion composition for controlling cockroaches according to claim 1, wherein The mass fraction of the dispersant is 1.0-15.0%, and the dispersant includes one or more of polymer polycarboxylate, dispersant NNO, dispersant MF, sodium lignin sulfonate, sodium lauryl sulfate, castor oil polyoxyethylene ether, and polyoxyethylene ether carboxylate.

4. The suspoemulsion composition for controlling cockroaches according to claim 1, characterized in that The mass fraction of the thickener is 0.5-1.0%, and the thickener includes one or more of starch, gum arabic, pectin, agar, gelatin, sodium alginate, carrageenan, xanthan gum, methyl cellulose, carboxymethyl cellulose, hydroxyethyl cellulose, polyacrylamide, polyvinyl alcohol or sodium polyacrylate.

5. The suspoemulsion composition for controlling cockroaches according to claim 1, characterized in that: The mass fraction of the thixotropic agent is 0.1-0.5%, and the thixotropic agent is one or more of fumed silica, organic bentonite, hydrogenated castor oil, and polyamide wax; the mass fraction of the defoaming agent is 1.0-1.5%, and the defoaming agent is one or more of polydimethylsiloxane, polyoxypropylene glycerol ether, palmitic acid, isopropyl ester, octanoate, and polyether-modified polysiloxane; the mass fraction of the preservative is 0.1-0.5%, and the preservative includes one or two of benzoic acid, sodium benzoate, and sodium phenylpropionate; the mass fraction of the antifreeze is 1.0-5.0%, and the antifreeze includes one or two of propylene glycol and ethylene glycol; the mass fraction of the cockroach pheromone is 0.5-1.0%.

6. The method for preparing the suspoemulsion composition for controlling cockroaches according to claim 1, characterized in that: The following steps are involved: Step 1: fully stirring the main drug A with an organic solvent to obtain a pre-dissolved main drug A; Step 2, deionized water, dispersant, and thickener are subjected to high-speed shearing of the dispersant for 1 hour to obtain a dispersion; Step 3: Continue to add a thixotropic agent, a defoaming agent, a preservative, a cockroach pheromone, and an antifreeze agent to the dispersion in sequence, then slowly add the ground solid main drug B and solid main drug C to the obtained dispersion, and high-speed shear for 2 hours to obtain a dispersed and stable suspoemulsion; Step 4: Slowly add the pre-dissolved main drug A to the obtained suspoemulsion while maintaining high-speed shearing, and continue high-speed shearing for 1 hour to obtain a stable suspoemulsion.

7. The preparation method according to claim 6, characterized in that: The mass fraction of the organic solvent in step 1 is 10-25%, and the organic solvent is a mixture of one or more of xylene, cyclohexanone, ethyl acetate, propylene glycol methyl ether, isopropanol, dichloromethane, ethylene glycol or toluene.

8. The preparation method according to claim 6, characterized in that: The shearing speed of the high-speed shearing is 1000-8000 r / min, the grinding medium is 95% zirconium oxide beads with a diameter of 0.8-1.0 mm, and after grinding, the particles are tested with a laser particle size distribution instrument until the particle size D90 is less than 4 μm.

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