A natural botanical extract biotype insecticide and methods of making and using same

Abstract

This invention discloses a natural plant-extracted biological insecticide and its preparation and application methods, belonging to the field of agricultural biotechnology. The insecticide uses cypress leaves, stemona root, clematis root, pinellia root, and ailanthus leaves as raw materials, prepared through boiling, cooling, filtration, sealed maturation, double-barrel water bath temperature gradient concentration, and pasteurization. This insecticide kills pests by sealing their spiracles and rapidly penetrating their bodies, causing suffocation. It primarily works through contact, exhibiting good residual effect, low resistance development, no chemical residues, and is environmentally friendly. The preparation process is mild, maximizing the retention of heat-sensitive active ingredients. The product is highly stable and low-cost, particularly suitable for controlling Diptera, Coleoptera, Orthoptera, Hemiptera, and / or Lepidoptera pests.

Description

[0001] This invention belongs to the field of agricultural biotechnology, especially pest and disease control technology, and specifically relates to a biological insecticide extracted from natural plants and its preparation and application methods. Background Technology

[0002] In agricultural production and landscaping, pest and disease control directly determines crop yield and product quality. In the past, production relied heavily on large-scale spraying of chemical pesticides for pest control. These agents are fast-acting and provide significant short-term control. However, long-term excessive use of chemical agents leads to a series of problems: it promotes pesticide resistance in pests, requiring increasingly higher dosages; pesticides have long degradation cycles, easily leaving residues in soil, water, and agricultural products, threatening food safety and damaging crop quality and flavor; furthermore, chemical agents indiscriminately kill organisms, harming beneficial predators such as bees and ladybugs while eliminating pests, thus disrupting the regional ecological balance.

[0003] To address the aforementioned drawbacks of chemical pesticides, the preparation of bio-pesticides using natural plant extracts—which are easily degradable, have low residues, are environmentally friendly, and are less likely to induce pesticide resistance in pests—is attracting increasing attention. However, existing plant-derived insecticides and their preparation processes still have many shortcomings.

[0004] First, most commercially available products such as neem, pyrethrum, and sophora flavescens utilize organic solvent reflux extraction, steam distillation, or simple ethanol soaking processes. These processes easily introduce solvent residues, and high temperatures can damage heat-sensitive insecticidal active substances, resulting in significant loss of effective components and overall low extraction efficiency. Second, some traditional Chinese medicine insecticides are prepared using simple methods such as water decoction or room-temperature soaking, leading to insufficient purification depth, high impurity content, and the resulting extracts are prone to oxidation, precipitation, and even mold growth during storage, resulting in insufficient product stability and a short shelf life. Third, some existing methods employ a two-step acid-base extraction process. Extreme acidic or alkaline environments can damage the plant's active components, reducing extraction efficiency and negatively impacting the stability of the finished product's efficacy.

[0005] Furthermore, conventional chemical or biological pesticides work by ingesting the toxic sap from leaves or stems after spraying. This toxic substance is absorbed through the stomach and enters the bloodstream, reaching the pest's nervous system and causing temporary paralysis, sedation, or a state of temporary death. However, once exposed to wind, dew, or rain, the pesticide is diluted, and the pest recovers. At this point, the pest has developed resistance to the pesticide, requiring a higher dosage to kill it upon subsequent spraying. Crustaceans and underground pests, even if exposed to chemical pesticides, do not actively ingest the toxic sap, and the pesticide does not quickly penetrate their bodies. Because they cannot be quickly killed, these pests will flee the areas where chemical pesticides are present, resulting in ineffective pest control. Imported plant-derived insecticides are more effective but expensive, making them unaffordable for farmers. Domestically produced biological pesticides, on the other hand, have unstable effects and short-lasting effects, failing to meet actual production needs. Summary of the Invention

[0006] In view of the above-mentioned problems of existing plant-derived biological pesticides and the shortcomings of existing chemical pesticides in terms of their mechanism of action, which are not conducive to killing insects, this invention provides a natural plant-extracted biological insecticide that can seal the stomata of pests, allow the pesticide solution to quickly penetrate into the insect body, and cause the pests to suffocate and die, as well as its preparation method and application method.

[0007] To achieve the above objectives, the technical solution adopted by the present invention is as follows: A biological insecticide extracted from natural plants is characterized by being prepared from cypress leaves, stemona root, clematis root, pinellia root, and ailanthus leaves through a process of boiling, cooling and filtering, sealed maturation, water bath concentration, and sterilization. This insecticide relies on the synergistic effect of its components to block the stomata on the insect's surface, promoting rapid penetration of the insecticide into the insect's body, ultimately killing the pest.

[0008] The cypress leaves mentioned in this invention refer to the scaly needles of all varieties of cypress trees, which may include tender twigs. Preferred are the leaves of the Chinese arborvitae (Platycladus orientalis).

[0009] Furthermore, based on the mass fractions, the proportions of each group are as follows: 50-60 parts of cypress leaves, 20-25 parts of stemona root, 10-15 parts of clematis root, 1-5 parts of pinellia tuber, and 1-5 parts of ailanthus leaves.

[0010] The preparation method of the above-mentioned biological insecticide extracted from natural plants includes the following steps: S1: Crush the cypress leaves, add water and heat to boil, let stand to cool, and filter to obtain cypress leaf liquid. S2: Add Stemona japonica, Clematis chinensis, Pinellia ternata and Ailanthus altissima leaves to the cypress leaf solution. After soaking, boiling, cooling and filtering, the crude insecticide solution is obtained. The crude solution is sealed and left to stand at room temperature for 20-25 days. S3: The crude insecticide solution is concentrated by water bath heating. The water bath temperature is controlled to be higher than the solution temperature to form a temperature gradient. During the concentration process, the water in the crude solution is evaporated to remove water while retaining the effective insecticidal components, and finally the purified insecticide stock solution is obtained. S4: Sterilize the undiluted insecticide to achieve preservation and produce a biological insecticide that can be stored for a long time.

[0011] Furthermore, the cooking in steps S1 and S2 is heated to 80℃~100℃ and maintained at a constant temperature for 2-4 hours to allow the insecticidal active ingredients to fully dissolve.

[0012] Furthermore, in step S3, the water bath heating adopts a double-barrel structure: the crude insecticide liquid is placed in the inner barrel, and then the inner barrel is placed in the outer barrel containing the heating medium. The outer barrel is heated so that its temperature is higher than that of the inner barrel, thus forming the temperature gradient. Under this temperature gradient, the water in the crude liquid is preferentially evaporated and removed, while the heat-sensitive effective insecticide components are retained.

[0013] Furthermore, the outer tub temperature is 80℃-100℃ (preferably 80℃-95℃), and the inner tub temperature is 60℃-80℃.

[0014] Furthermore, the sterilization process described in step S4 is pasteurization, with a sterilization temperature of 75–95°C.

[0015] The biological insecticide of this invention is used to control agricultural and garden pests, especially for controlling Diptera, Coleoptera, Orthoptera, Hemiptera and / or Lepidoptera pests.

[0016] Furthermore, the method of use is as follows: dilute the insecticide concentrate 200-1000 times and spray it evenly on the plant surface or apply it to the field with water for root irrigation. It can be applied throughout the entire growth period of the plant.

[0017] Furthermore, the preferred dilution ratio is 300 times, and the dosage per acre is 100 mL of the insecticide concentrate.

[0018] The optimal storage conditions for the biological insecticide of this invention are: low temperature (5-25℃), protection from light, coolness, and relative humidity (60-70%). Under normal temperature conditions, it can generally be stored for 2 years. Before use, the bottled concentrate can be gently shaken; if uniform foam appears, it indicates that the system is stable and ready for use.

[0019] The advantages of this invention will be explained below based on its mechanism of action: 1. This invention uses five plants as raw materials: cypress leaves, stemona root, clematis root, pinellia rhizome, and ailanthus leaves. These raw materials exhibit synergistic effects. Cypress leaves (especially arborvitae leaves) and ailanthus leaves are rich in terpenoid volatile oils. These oils not only enhance the penetration of the pesticide solution but also repel pests through their volatile components. Clematis root contains lignans A and other active ingredients that can interfere with the transmission of nerve signals in pests. Stemona root alkaloids act on the nervous system of pests, synergistically enhancing the insecticidal effect with clematis root. Pinellia rhizome contains lectins and other components that exert a stomach poison effect, interfering with the intestinal function of pests. The various raw materials work together to improve the overall insecticidal effect. After the pesticide solution is sprayed onto the surface of pests, it can penetrate the insect's skin barrier and enter the body, penetrating the nervous system and digestive tract, forming a synergistic effect of penetration, behavioral interference, and ultimate poisoning. This not only accelerates the insecticidal speed and improves the insecticidal effect but also delays the development of pesticide resistance in pests.

[0020] 2. In extracting the effective insecticidal components, this invention relies on the natural components such as volatile oils contained in the plants themselves. After being boiled to a certain degree and sealed and left to stand for a period of time, it produces a viscosity similar to a microemulsion, resulting in good adhesion. When sprayed onto plant leaves, it is not easily washed away by rain or dew; it also has good dispersibility. Furthermore, the insecticidal liquid of this invention contains *Clematis chinensis* extract, which is rich in natural penetrating components. When mixed with water, it has good solubility, is water-compatible, and easily dissolves in water.

[0021] 3. The biological insecticide of this invention has all components derived from natural plants, containing no chemically synthesized ingredients. It employs a low-temperature extraction and a two-tank dual-temperature purification process, unlike the high-temperature extraction commonly used in existing patents (which easily damages heat-sensitive plant components). During extraction, the main raw materials are mixed in proportion and soaked in water at room temperature, then the temperature is gradually increased and maintained, avoiding damage to the effective insecticidal components. The purification process uses a water bath stepped temperature control mode to further ensure that the effective insecticidal components are not destroyed. Calculations show that the cost of producing 1 ton of biological insecticide concentrate using this invention is approximately 5,000 yuan for raw materials (cypress leaves, Stemona japonica, Clematis chinensis, Pinellia ternata, and Ailanthus altissima leaves), and approximately 15,000 yuan for packaging materials, transportation, labor, water, electricity, and other expenses, totaling approximately 20,000 yuan, or 20 yuan / kg. In contrast, similar biological insecticides sold abroad cost approximately 100 yuan / kg, meaning the cost of this invention is only one-fifth of foreign products. Detailed Implementation

[0022] The technical solution of the present invention will be further illustrated below through several embodiments and detailed preparation methods. Example 1

[0023] The preparation method of the present invention is as follows: Step 1: Weigh out the following ingredients according to the proportions: 55 parts arborvitae leaves, 23 parts stemona root, 12 parts clematis root, 3 parts pinellia tuber, and 3 parts ailanthus leaves. Chop the arborvitae leaves into 1-3 cm lengths and grind them into a paste-like powder with a moisture content of about 20%. The moisture content of the stemona root, clematis root, pinellia tuber, and ailanthus leaves should be about 10%.

[0024] Step 2: Add purified water to the paste-like arborvitae leaves, stir well, put it into a reaction vessel, and slowly heat it to 100℃. After 2 hours, filter it through a cloth bag to obtain the juice made from the arborvitae leaves.

[0025] Step 3: Add Stemona japonica, Clematis chinensis, Pinellia ternata, and Ailanthus altissima leaves to the reaction vessel and soak at room temperature for 24 hours. Then heat the reaction vessel to 100°C and maintain the temperature for 2 hours before rapidly cooling it to room temperature. Use a cloth bag to separate the liquid and residue to obtain a crude insecticide solution. Seal the crude insecticide solution at room temperature and let it stand for about 20 days to promote the stable dissolution of the active ingredients and allow the solution to mature naturally, forming a stable and well-adhesive system.

[0026] Step 4: Purify the crude insecticide solution using a double-barrel water bath method. The specific steps are as follows: A circular stainless steel drum with a diameter of 1.8m and a height of 2m is used as the outer drum, and filled with tap water to a height of 1.5m. A stainless steel drum with a diameter of 1m and a height of 1.5m is placed inside the outer drum as the inner drum, and the crude biological insecticide obtained in step three is poured into the inner drum. The tap water in the outer drum is slowly heated, with the temperature controlled at 80-100℃ (preferably 85-95℃), allowing the water to evaporate without vigorous boiling. The hot water in the outer drum is used to heat the crude insecticide in the inner drum in a water bath, maintaining the temperature of the crude liquid in the inner drum at 60-80℃. Under these conditions, the water in both the outer and inner drums evaporates simultaneously, and the liquid levels drop simultaneously, achieving gentle dehydration and purification of the crude liquid. Because the boiling points of effective insecticidal components such as benzoyl peroxide are much higher than water, they will not volatilize with water vapor under the above purification temperature conditions, nor will they be lost due to water vapor entrainment. The retention rate of effective components can reach over 95%, and the purified product is the original insecticide solution of this invention. Throughout the purification process, the water temperature in the outer tank is controlled below the boiling point. This temperature range allows for slow evaporation of water without violent boiling, thus ensuring a stable purification process.

[0027] Step 5: Use pasteurization to kill mold at a temperature of 75-95℃ for 30-40 minutes to facilitate the preservation of the finished biological insecticide solution. Example 2

[0028] The difference from Example 1 is that a standard laboratory-grade constant-temperature water bath is used in the fourth step. Specifically, an open container holding the crude insecticide solution is placed in the constant-temperature water bath, achieving the same gentle dehydration and purification effect as the 'two-barrel' method. This method also utilizes the principle that the boiling point of water is much lower than that of the effective insecticide component, and the retention rate of the effective component can reach over 95%. Example 3

[0029] The biological insecticide stock solution prepared in Example 1 was diluted with water at a ratio of 1:300 (e.g., 10 kg of insecticide stock solution was diluted with 3000 kg of water) to prepare a diluted pesticide solution, which can be used for pest control in a field of 66,667 square meters (equivalent to 100 mu). This pesticide solution can control underground pests (leek maggots, white grubs) and lepidopteran larvae (fall armyworm, cabbage caterpillar, peach fruit moth). Field trials conducted in Daiyue District, Tai'an City, Shandong Province in 2024 and 2025 verified that this insecticide solution achieved a corrected mortality rate of 98.6% against adult *Pseudomonas reticulatus*, 95.1% against *Pseudomonas reticulatus*, and 91.7% against *Cabbage Caterpillar* (trial location: within the factory area of ​​Shandong Zhongke Shengnong Fertilizer Co., Ltd., Daolang Town, Daiyue District, Tai'an City, Shandong Province).

[0030] To further verify the advantages of the insecticide of the present invention, insecticidal tests were conducted indoors and outdoors using the insecticide prepared in Example 1, the commercially available chemical pesticide cyhalothrin, and water. Application Example 1: Indoor Insecticide Test Experimental conditions: The target pest was the adult *Pseudobulbus terrestrialus*, which was collected from farmland in Chengzizhai, Daolang Town, Daiyue District, Tai'an City, Shandong Province.

[0031] Experimental Method: The collected pests were divided into three groups of 20 each. Each group was sprayed with diluted insecticide of this invention, the chemical pesticide cyhalothrin, and water, respectively. The time to 50% and 100% mortality of the pests was recorded. The experimental results are shown in Table 1.

[0032] In Table 1, both the insecticide solution of this invention and the chemical pesticide cyhalothrin were used according to their respective recommended dosages. The "dosage" in the table represents the actual volume of the stock solution used to treat 20 pests, diluted with water to the same volume before application. The water control group was operated on using an equal volume of water instead of the pesticide solution.

[0033] As shown in Table 1, for the same number of pests, the insecticide of this invention can achieve rapid pest control with a small dosage. Additionally, one pest died in the water group during the experiment, presumably due to individual stress or fluctuations in environmental conditions, which does not affect the conclusion regarding the comparison of pesticide efficacy.

[0034] Application Example 2: Outdoor Test Experimental conditions: The target pest was the adult of the mitten beetle, which was sourced from Chengzizhai (Spring Land) in Daolang Town, Daiyue District, Tai'an City, Shandong Province.

[0035] The experimental method was as follows: A plot of land with uniform soil was selected in the field and divided into three 2m² plots as experimental fields. The plots were isolated from each other and not connected. The plots were then flooded with the insecticide solution of this invention diluted 1:300, the chemical pesticide cyhalothrin, and water. The number of pests killed in each plot was counted after 24 hours and 48 hours of flooding. The experimental results are shown in Table 2.

[0036] As shown in Table 2, under the premise of using less insecticide solution, the number of insects killed in 24h and 48h is better than that of the chemical pesticide control group, indicating that the present invention has the characteristics of low dosage and high efficiency.

[0037] Application Example 3: Outdoor Test Experimental conditions: The pond area was 10m², separated by cement walls. Each treatment was replicated three times, meaning each group had three ponds. The soil in each pond came from the same plot of land, was uniformly mixed, and then filled into each pond to ensure consistent experimental conditions. The filling depth was 130cm, with 0-30cm being the topsoil layer and below 30cm being the plow pan, simulating field conditions.

[0038] Experimental Method: 125 ml of the insecticide concentrate of this invention was diluted with 50 kg of water (equivalent to a 400-fold dilution) and applied via irrigation. Chemical pesticides (cyhalothrin) were treated with the same dilution ratio, with water serving as a control. At 24 h, 48 h, 72 h, and 96 h after application, each pond was dug to a depth of 30 cm (below this depth is the plow pan, where pests generally cannot distribute). All excavated soil was sieved, and the number of dead insects was counted. The experimental results are shown in Table 3 below:

[0039] As shown in Table 3, under the same conditions, the insecticide of the present invention has better insecticidal effect than the chemical pesticide cyhalothrin within 24h, 48h, 72h and 96h. It can also be seen that the insecticide of the present invention can achieve good insecticidal effect within 24h.

[0040] To further investigate the mechanism of action of the insecticide of this invention, in March 2026, experiments were conducted at the State Key Laboratory of Crop Biology, Shandong Agricultural University. Fifth-instar larvae of white grubs and adult *Pseudobulbus terrestris* were selected as experimental pests. The insecticide of this invention (1500-fold dilution), a chemical pesticide (1500-fold dilution), and water were sprayed on the pests, respectively. The results showed that after spraying the insecticide of this invention, the pests exhibited a violent rolling reaction, their spiracles closed, followed by suffocation and body spasms, becoming completely immobile within 3-8 minutes. The pests sprayed with the chemical pesticide showed significantly reduced activity but did not roll, dying 8-12 hours later. The water control group showed no mortality. Simultaneously, continuous observation under a microscope of the pests sprayed with the insecticide of this invention revealed that the spiracles closed 2-3 minutes after spraying. Dissection 3-5 minutes after spraying showed that the pesticide had penetrated the pests' bodies, at which point the pests exhibited spasms and suffocation symptoms, their heartbeats gradually stopped, and they ultimately lost their ability to move and died.

[0041] This invention's biological insecticide exerts its insecticidal effect through contact. Indoor toxicity testing at Shandong Agricultural University revealed the following: the solution was diluted to 1:300, 1:500, 1:700, 1:900, 1:1100, 1:1300, and 1:1500, with three replicates per group. Each treatment used at least 10 grubs. Experimental conditions included a temperature of 25±1℃ and a relative humidity of 60–80%. Pest mortality was recorded at 24, 48, 72, and 96 hours, with a control mortality rate <10%. Using the logarithm of concentration (x) and the mortality probability unit (y), a regression equation Y=a+bx was fitted to determine the median lethal concentration (LC). 50 The solution was diluted 1000 times, which is the main reason why this invention recommends a dilution factor of no more than 1000. The measured mortality rates were: 1:300 (96.8%), 1:500 (80.55%), 1:700 (65.4%), 1:900 (55.3%), 1:1100 (45.2%), 1:1300 (40.1%), and 1:1500 (19.4%). Field trials showed significant insecticidal effect 24 hours after application.

[0042] It should be noted that the content of the active ingredient, Stemona alkaloid, in the insecticide concentrate of this invention is 11.6%. After being prepared at three concentration gradients of 1:300, 1:500, and 1:1000, the content of the active ingredient Stemona alkaloid, calculated according to the formula w = concentrate concentration ÷ (1 + dilution factor), is 385 ppm, 232 ppm, and 116 ppm respectively; converted to mg / kg (1% = 1 × 10⁻⁶ mg / kg). 4The corresponding concentrations were 385 mg / kg, 232 mg / kg, and 116 mg / kg, respectively. This result indicates that the higher the dilution ratio, the lower the effective concentration of the pesticide. This invention recommends a dilution ratio of 200-1000. Therefore, in practical application of this invention, the dilution ratio should be determined according to different application scenarios. Even in the same field, the dilution ratio should be adjusted according to different crop cycles to achieve the best control effect. Furthermore, the above embodiments are merely limited examples to demonstrate the technical solution and positive effects of this invention, and are not intended to limit the technical solution of this invention. Any modifications and refinements made to the technical solution of this invention without creative effort should fall within the protection scope of this invention, and the claims shall ultimately prevail.

Claims

1. A biological insecticide extracted from natural plants, characterized in that, It is prepared from cypress leaves, stemona, clematis, pinellia and ailanthus leaves through boiling, cooling and filtering, sealed maturation, water bath concentration and sterilization processes.

2. The biological insecticide extracted from natural plants as described in claim 1, characterized in that, Based on the mass fractions, the proportions of each group are as follows: 50-60 parts of cypress leaves, 20-25 parts of stemona root, 10-15 parts of clematis root, 1-5 parts of pinellia tuber, and 1-5 parts of ailanthus leaves.

3. The biological insecticide extracted from natural plants as described in claim 1, characterized in that, The cypress leaves mentioned are those of the Chinese arborvitae.

4. A method for preparing a biological insecticide extracted from natural plants as described in any one of claims 1-3, characterized in that, Includes the following steps: S1: Crush the cypress leaves, add water and heat to boil, let stand to cool, and filter to obtain cypress leaf liquid. S2: Add Stemona japonica, Clematis chinensis, Pinellia ternata and Ailanthus altissima leaves to the cypress leaf solution. After soaking, boiling, cooling and filtering, the crude insecticide solution is obtained. The crude solution is sealed and left to stand at room temperature for 20-25 days. S3: The crude insecticide solution is concentrated by water bath heating. The water bath temperature is controlled to be higher than the solution temperature to form a temperature gradient. During the concentration process, the water in the crude solution is evaporated to remove water while retaining the effective insecticidal components, and finally the purified insecticide stock solution is obtained. S4: Sterilize the undiluted insecticide to achieve preservation and produce a biological insecticide that can be stored for a long time.

5. The method for preparing the biological insecticide extracted from natural plants as described in claim 4, characterized in that, In both steps S1 and S2, the cooking temperature is raised to 80°C to 100°C and maintained at a constant temperature for 2-4 hours.

6. The method for preparing the biological insecticide extracted from natural plants as described in claim 4, characterized in that, In step S3, the water bath heating adopts a double-barrel structure: the crude insecticide liquid is placed in the inner barrel, and then the inner barrel is placed in the outer barrel containing the heating medium. The outer barrel is heated so that the temperature of the outer barrel is higher than that of the inner barrel, thus forming the temperature gradient. Under this temperature gradient, the water in the crude liquid is preferentially evaporated and removed, while the heat-sensitive effective insecticide components are retained.

7. The method for preparing the biological insecticide extracted from natural plants as described in claim 6, characterized in that, The outer drum temperature is 80℃-100℃, and the inner drum temperature is 60℃-80℃.

8. The use of a biological insecticide extracted from natural plants as described in any one of claims 1-3 in the control of Diptera, Coleoptera, Orthoptera, Hemiptera and / or Lepidoptera pests.

9. The method of using the biological insecticide extracted from natural plants as described in claim 8, characterized in that, When using, dilute the insecticide concentrate 200-1000 times and spray it evenly on the plant surface or apply it to the field by watering the roots. It can be used throughout the entire growth period of the plant.

10. The method of using the biological insecticide extracted from natural plants as described in claim 9, characterized in that, The dilution ratio is 300 times, and the dosage per acre is 100 mL of the undiluted insecticide.

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