A cuprous oxide and triterpene saponin-based pesticide composition of plant origin and a preparation method thereof

Abstract

The present application relates to the technical field of pesticides, and specifically discloses a cuprous oxide and triterpene saponin-based plant source pesticide composition and a preparation method thereof. The composition comprises cuprous oxide powder and triterpene saponin powder, the weight ratio of the cuprous oxide powder to the triterpene saponin powder is 3:7, and the fineness of the cuprous oxide powder and the triterpene saponin powder is both 1000-1500 mesh. One aspect of the present application opens up a new technical path for the industrialization application of triterpene saponin, a traditional plant source active ingredient in China, helps to promote the development of plant source pesticide industry, and promotes the large-scale planting of green pollution-free agricultural products and green organic agricultural products. On the other hand, the composition of the present application has the characteristics of one drug with multiple effects or even one drug with all effects, can greatly reduce the use of residual chemical pesticides, reduce the pollution of pesticides to the ecological environment and agricultural and sideline products from the source, and promote the transformation and upgrading of the agricultural green development mode.

Description

Technical Field

[0001] This invention belongs to the field of pesticide technology, specifically relating to a combination of cuprous oxide and triterpenoid saponins of plant-derived pesticides and its preparation method. Background Technology

[0002] Cuprous oxide (Cu₂O) is an important inorganic copper preparation with a long history of application in agriculture as a broad-spectrum protective fungicide. Copper ions can inhibit the growth of bacteria and fungi. When copper sprayed on plants encounters weakly acidic dew or raindrops, it exists in a +1 or +2 valent ionic state. After contacting pathogenic microorganisms, copper ions penetrate their cell walls, interfere with intracellular enzyme activity, and damage cell growth. Cuprous oxide can effectively control the growth of plant pathogens such as fungi and bacteria and is widely used in the prevention and control of diseases in fruits and vegetables.

[0003] However, cuprous oxide has several shortcomings in practical agricultural applications. First, cuprous oxide primarily acts as a protectant and lacks penetrability and systemic properties, resulting in a slow bactericidal effect. Second, commercially available cuprous oxide wettable powders generally suffer from large particle size and low suspension rates, leading to poor uniformity and stability of efficacy. Third, cuprous oxide has low safety; it is prohibited during flowering and young fruit stages, and its use on copper-sensitive crops requires caution. Fourth, copper-based formulations are most prone to causing phytotoxicity due to poor compatibility. Because of numerous contraindications to mixing, farmers often misuse copper-based formulations due to a lack of understanding of their compatibility, greatly increasing the risk of phytotoxicity.

[0004] On the other hand, triterpenoid saponins are a class of natural active ingredients derived from plants, possessing excellent potential for the development of biopesticides. Triterpenoid saponins are triterpenoid glycoside compounds found in the root and stem tissues of various plants, including those in the Leguminosae, Liliaceae, Asteraceae, Polygalaceae, and Agavaceae families. Tea saponins are a general term for pentacyclic triterpenoid plant saponins extracted from the Camellia genus of the Theaceae family. They possess a variety of physiological activities, including emulsification, detergency, antibacterial and anti-inflammatory properties, virucidal activity, antioxidant activity, and insecticidal activity. In particular, their excellent dispersibility, penetration, and wetting properties make them promising for widespread application in pesticides.

[0005] Although the agricultural activity of triterpenoid saponins has been widely confirmed, their application and promotion in actual agriculture still face serious obstacles. First, triterpenoid saponins have poor stability in alkaline environments. Studies have shown that saponins degrade rapidly in water and soil. Second, due to their soap-like surface activity, their high solubility and low adsorption affinity make them prone to leaching after application. Furthermore, triterpenoid saponin formulations generally suffer from short-lasting effects, often remaining effective in the field for only a few days to a week after spraying. These inherent defects of poor stability and short-lasting effects severely restrict the large-scale promotion and application of triterpenoid saponins as plant-derived pesticides.

[0006] In summary, there are no existing reports on the synergistic effects of combining cuprous oxide and triterpenoid saponins using calcification film technology. Therefore, how to scientifically combine these two active ingredients and innovate formulation technology to avoid the drawbacks of using them individually, amplify their synergistic effects, and simultaneously significantly improve the stability and duration of action of triterpenoid saponins, as well as the compatibility and safety of cuprous oxide, is a pressing technical challenge in this field. Summary of the Invention

[0007] The purpose of this invention is to provide a plant-derived pesticide composition of cuprous oxide and triterpenoid saponins and its preparation method, in order to solve the problem mentioned in the background art that the existing technology does not reflect the application of the combination of cuprous oxide and triterpenoid saponins in the prevention and control of pests and diseases.

[0008] To achieve the above objectives, the present invention provides the following technical solution:

[0009] A plant-derived pesticide composition of cuprous oxide and triterpenoid saponins, the composition comprising cuprous oxide powder and triterpenoid saponin powder, wherein the weight ratio of cuprous oxide powder to triterpenoid saponin powder is 3:7, and the fineness of both cuprous oxide powder and triterpenoid saponin powder is 800-1500 mesh.

[0010] Preferably, the composition further comprises adjuvants, including dispersants, wetting agents, and disintegrants.

[0011] A method for preparing a plant-derived pesticide composition of cuprous oxide and triterpenoid saponins includes the following steps:

[0012] S1. Sieve the coarse cuprous oxide powder, take the sieved material and place it in a plasma surface treatment device, and perform low-temperature plasma surface activation treatment in an oxygen atmosphere to obtain activated cuprous oxide powder.

[0013] S2. Place the coarse triterpenoid saponin powder in an air jet mill for ultra-fine grinding, and collect the powder with a fineness of 800-1500 mesh to obtain finely ground triterpenoid saponin powder.

[0014] S3. The activated cuprous oxide powder obtained in S1 and the triterpenoid saponin powder obtained in S2 are added to a mixer at a weight ratio of 1:5 for graded mixing to obtain a mixed powder.

[0015] S4. The mixed powder obtained in S3 is fed into a fluidized bed granulator, and calcium sulfate solution and sodium carbonate solution are sprayed in sequence for gradient calcification treatment to obtain calcified powder.

[0016] S5. The calcified powder obtained in step S4 is placed in a fluidized bed and sprayed with chitosan solution for composite membrane treatment to obtain membrane powder.

[0017] S6. The film-forming powder obtained in S5 is dried at low temperature to solidify the coating film.

[0018] S7. Add the adjuvant to the dried powder obtained in S6 for final mixing, and sieve to obtain the finished product of the wettable powder composition of cuprous oxide and triterpenoid saponin-based plant-derived pesticide.

[0019] Preferably, in step S1, the conditions for plasma surface activation treatment are: treatment time of 5-15 minutes, treatment power of 100-300W; and the sieve mesh number for sieving the cuprous oxide coarse powder is 800 mesh.

[0020] Preferably, in step S2, the air jet mill uses compressed air at 0.6-0.8 MPa as the working fluid for ultrafine grinding. During the grinding process, the temperature of the grinding chamber is controlled to not exceed 45°C by cooling water in the jacket, and powder of 800-1500 mesh is collected by a classifying wheel.

[0021] Preferably, in step S3, the graded mixing includes:

[0022] Primary mixing: Add activated cuprous oxide powder and triterpenoid saponin powder into a conical double helix mixer in a certain proportion, and premix for 20-30 minutes at a speed of 20-30 r / min;

[0023] Secondary mixing: Transfer the premixed powder into a three-dimensional motion mixer and continue mixing for 40-60 minutes at a speed of 30-50 r / min;

[0024] The secondary mixing process is supplemented with ultrasonic vibration treatment at 20-40kHz, each ultrasonic treatment lasts 5-10 minutes, with a 10-minute interval, and is repeated 2-3 times.

[0025] Preferably, in step S4, the gradient calcification treatment includes:

[0026] First calcification: A calcium sulfate solution with a mass concentration of 2%-5% is sprayed in by atomization, with the spray volume being 5%-10% of the powder mass, and the fluidized bed inlet air temperature being 50-60℃.

[0027] Second calcification: Spray in a sodium carbonate solution with a mass concentration of 1%-3%, the amount of which is 3%-8% of the powder mass. The reaction temperature is 40-50℃ and the reaction time is 20-40 minutes.

[0028] Preferably, in step S5, the chitosan solution is a chitosan acetic acid solution with a mass concentration of 1%-3%, the degree of deacetylation of the chitosan is ≥85%, and the acetic acid concentration is 1%-2%; the spray volume is 5%-10% of the powder mass, and the fluidized bed inlet air temperature is 40-50℃; in step S6, the low-temperature drying is performed in a fluidized bed at 40-50℃ for 30-60 minutes.

[0029] Preferably, in step S7, the additives include a dispersant, a wetting agent, and a disintegrant; the dispersant is sodium lignosulfonate, added at 3%-8% of the total mass of the composition; the wetting agent is sodium dodecyl sulfate, added at 1%-3% of the total mass of the composition; the disintegrant is sodium carboxymethyl starch, added at 2%-5% of the total mass of the composition; the final mixing is performed in a V-type mixer for 20-30 minutes; and the sieve mesh size is ≤25μm.

[0030] The present invention relates to a combination of cuprous oxide and triterpenoid saponins from plant sources for the control of pests and diseases.

[0031] Compared with the prior art, the beneficial effects of the present invention are:

[0032] This invention is the first to compound cuprous oxide and triterpenoid saponins in a weight ratio of 3:7 and prepare a wettable powder with a core-shell coating structure using calcification film technology. This synergistic effect broadens the spectrum of control, enabling the composition of this invention to simultaneously and effectively control almost all fungal, bacterial, and some viral diseases, including root rot, soft rot, brown rot, canker, core rot, dry rot, gummosis, canker, target spot, angular leaf spot, stripe, powdery mildew, downy mildew, gray mold, anthracnose, leaf spot, take-all, smut, Fusarium head blight, rust, leaf blight, rice blast, ginger blast, and viral diseases, as well as Lepidoptera and Coleoptera. It is effective against a wide range of pests, including snails, slugs, grubs, cutworms, mole crickets, wireworms, root maggots, leek maggots, flies, ants, locusts, longhorn beetles, and codling moths. Its range of control is extremely broad, from soil-borne pests and diseases to those on the ground and those affecting stems and leaves. It truly achieves multi-purpose, comprehensive pest control, avoiding the cumbersome operation and pesticide damage risks associated with mixing multiple pesticides in agricultural production.

[0033] Simultaneously, this invention utilizes a calcification and film-forming process to create a dual protective structure on the surface of powder particles, consisting of a calcium carbonate coating layer and a chitosan biofilm. This core-shell coating structure effectively isolates the body from the effects of degradation factors such as acids, alkalis, light, and microorganisms in the external environment, thereby significantly improving the stability of triterpenoid saponins, greatly extending their duration of action, and optimizing the disproportionation reaction rate and efficacy of cuprous oxide.

[0034] Meanwhile, under the same control effect, the single-agent dosage of cuprous oxide can be reduced by 30%-50%, significantly reducing the cumulative input of copper ions in soil and water, and lowering the risk of phytotoxicity and environmental pollution load from copper preparations. Furthermore, triterpenoid saponins are natural plant extracts that are easily degraded in the environment without harmful residues. After application, the composition has minimal impact on beneficial soil microbial communities, and the degraded triterpenoid saponins and chitosan can be converted into nutrients usable by plants, positively promoting root development and seedling vigor. It is particularly suitable for planting medicinal herbs such as ginseng, Panax notoginseng, Codonopsis pilosula, and licorice, as well as cash crops such as chili peppers, potatoes, yams, lilies, garlic, leeks, soybeans, and legumes. It not only increases yield but also simultaneously increases the accumulation of triterpenoids and the synthesis of derivatives, which is highly beneficial to human health.

[0035] In summary, this invention opens up a new technological path for the industrial application of triterpenoid saponins, a traditional plant-derived active ingredient in my country, which will help promote the development of the plant-derived pesticide industry and facilitate the large-scale cultivation of green, pollution-free, and organic agricultural products. Furthermore, the composition of this invention can largely replace the use of chemical pesticides that easily leave residues, reducing pesticide pollution to the ecological environment and agricultural products at the source and promoting the transformation and upgrading of green agricultural development. In addition, the composition of this invention is cost-effective, easy to use, and highly effective, with a better overall cost-effectiveness ratio than conventional pesticide solutions, effectively reducing farmers' plant protection input costs and improving agricultural economic benefits. This invention is of great significance for promoting pesticide reduction and efficiency, ensuring the quality and safety of agricultural products, promoting dietary health, and promoting sustainable agricultural development. Detailed Implementation

[0036] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0037] Example 1:

[0038] A composition of cuprous oxide and triterpenoid saponins from plant-derived pesticides.

[0039] Raw material ratio: Cuprous oxide raw powder (purity ≥98%): 6.12kg

[0040] Crude triterpenoid saponin powder (content ≥60%): 23.33 kg

[0041] Calcium sulfate: 0.75 kg

[0042] Sodium carbonate: 0.45 kg

[0043] Chitosan (degree of deacetylation 90%, molecular weight 50,000-100,000): 1.5 kg

[0044] Sodium lignosulfonate: 1.8 kg

[0045] Sodium dodecyl sulfate: 0.6 kg

[0046] Sodium carboxymethyl starch: 1.2 kg.

[0047] Preparation steps:

[0048] (1) Plasma surface activation treatment of cuprous oxide powder

[0049] The raw cuprous oxide powder was passed through an 800-mesh sieve. The sieved material was evenly spread on the sample stage of the plasma surface treatment equipment. The vacuum was evacuated to below 10 Pa, and high-purity oxygen was introduced until the chamber pressure stabilized at 50 Pa. The powder was treated for 10 minutes under a radio frequency power of 200 W to obtain activated cuprous oxide powder.

[0050] (2) Ultrafine grinding of triterpenoid saponins

[0051] The coarse powder of triterpenoid saponins is fed into an air jet mill, and compressed air at 0.7 MPa is used as the grinding medium. The temperature of the grinding chamber is controlled to not exceed 45°C by circulating cooling water in the jacket. The powder with a fineness of 1000 mesh is collected by a classifying wheel to obtain the fine triterpenoid saponin powder.

[0052] (3) Graded mixing

[0053] 5.0 kg of activated cuprous oxide powder obtained in step (1) and 25.0 kg of triterpenoid saponin powder obtained in step (2) were added to a conical double helix mixer and premixed for 25 minutes at a speed of 25 r / min. Then the premixed powder was transferred to a three-dimensional motion mixer and mixed for 50 minutes at a speed of 40 r / min. During the mixing process, ultrasonic treatment at 30 kHz was performed for 8 minutes each time, with an interval of 10 minutes, and repeated 3 times to obtain the mixed powder.

[0054] (4) Gradient calcification treatment

[0055] The mixed powder obtained in step (3) was fed into a fluidized bed granulator, and 25.0 kg of a 3% calcium sulfate solution (8.3% of the powder mass) was sprayed in via atomization. The fluidized bed inlet air temperature was 55°C for the first calcification. After calcification, 22.5 kg of a 2% sodium carbonate solution (7.5% of the powder mass) was sprayed in at a reaction temperature of 45°C for 30 minutes for the second calcification, resulting in calcified powder.

[0056] (5) Composite membrane treatment

[0057] The calcified powder obtained in step (4) is placed in a fluidized bed, and 75.0 kg of a 2% chitosan acetic acid solution (chitosan deacetylation degree 90%, solvent is 1.5% acetic acid aqueous solution) is sprayed in (the amount of sprayed solution is 8.3% of the powder mass). The inlet air temperature of the fluidized bed is 45℃, and composite membrane treatment is carried out to obtain membrane powder.

[0058] (6) Low-temperature drying and curing

[0059] The film-coated powder obtained in step (5) is dried in a fluidized bed at 45°C for 45 minutes to allow the coating film to fully solidify and form.

[0060] (7) Additives addition and final mixing and sieving

[0061] Add 1.8 kg of sodium lignosulfonate, 0.6 kg of sodium dodecyl sulfate, and 1.2 kg of sodium carboxymethyl starch to the dried powder obtained in step (6), put it into a V-type mixer, and finally mix it at 30 r / min for 25 minutes. After mixing evenly, pass it through a 25 μm sieve and collect the sieve material to obtain a wettable powder composition of cuprous oxide and triterpenoid saponin-based plant-derived pesticide.

[0062] Example 2:

[0063] A composition of cuprous oxide and triterpenoid saponins from plant-derived pesticides.

[0064] Raw material ratio:

[0065] Cuprous oxide raw powder (purity ≥ 98%): 6.12 kg

[0066] Crude triterpenoid saponin powder (content ≥60%): 23.33 kg

[0067] Calcium sulfate: 0.45 kg

[0068] Sodium carbonate: 0.30 kg

[0069] Chitosan: 0.75kg

[0070] Sodium lignosulfonate: 0.90 kg

[0071] Sodium dodecyl sulfate: 0.30 kg

[0072] Sodium carboxymethyl starch: 0.60 kg

[0073] Preparation steps:

[0074] This embodiment uses essentially the same preparation steps as Example 1, the difference being that the process parameters are taken at lower values:

[0075] (1) Plasma surface activation treatment: the treatment time is 5 minutes and the treatment power is 100W.

[0076] (2) Airflow pulverization: using 0.6MPa compressed air as the working fluid, the powder with a fineness of 800 mesh is collected by a classifier wheel.

[0077] (3) Graded mixing: the first stage of mixing is carried out at a speed of 20 r / min for 20 minutes; the second stage of mixing is carried out at a speed of 30 r / min for 40 minutes, with an ultrasonic frequency of 20 kHz. Each treatment lasts for 5 minutes, with an interval of 10 minutes, and is repeated twice.

[0078] (4) Gradient calcification: The mass concentration of calcium sulfate solution is 2%, and the amount of sprayed solution is 5% of the mass of powder; the mass concentration of sodium carbonate solution is 1%, and the amount of sprayed solution is 3% of the mass of powder; the reaction temperature is 40℃ and the reaction time is 20 minutes.

[0079] (5) Composite membrane formation: chitosan solution mass concentration 1%, spray volume is 5% of powder mass, fluidized bed inlet air temperature 40℃.

[0080] (6) Low temperature drying: Dry in a fluidized bed at 40℃ for 30 minutes.

[0081] (7) Addition of additives and final mixing and sieving: 3% sodium lignosulfonate, 1% sodium dodecyl sulfate, and 2% sodium carboxymethyl starch were added. The mixture was mixed in a V-type mixer for 20 minutes, passed through a 25μm sieve, and the sieve material was collected to obtain the composition.

[0082] Example 3:

[0083] A composition of cuprous oxide and triterpenoid saponins from plant-derived pesticides.

[0084] Raw material ratio:

[0085] Cuprous oxide raw powder (purity ≥ 98%): 6.12 kg

[0086] Crude triterpenoid saponin powder (content ≥60%): 23.33 kg

[0087] Calcium sulfate: 1.50 kg

[0088] Sodium carbonate: 1.20 kg

[0089] Chitosan: 3.00kg

[0090] Sodium lignosulfonate: 2.40 kg

[0091] Sodium dodecyl sulfate: 0.90 kg

[0092] Sodium carboxymethyl starch: 1.50 kg.

[0093] Preparation steps:

[0094] This embodiment uses essentially the same preparation steps as Example 1, the difference being that the process parameters are taken at higher values:

[0095] (1) Plasma surface activation treatment: the treatment time is 15 minutes and the treatment power is 300W.

[0096] (2) Airflow pulverization: using 0.8MPa compressed air as the working fluid, the powder with a fineness of 1500 mesh is collected by a classifier wheel.

[0097] (3) Graded mixing: the first stage of mixing is carried out at a speed of 30 r / min for 30 minutes; the second stage of mixing is carried out at a speed of 50 r / min for 60 minutes, with an ultrasonic frequency of 40 kHz. Each treatment lasts for 10 minutes, with a 10-minute interval, and is repeated 3 times.

[0098] (4) Gradient calcification: The mass concentration of calcium sulfate solution is 5%, and the amount of sprayed solution is 10% of the mass of powder; the mass concentration of sodium carbonate solution is 3%, and the amount of sprayed solution is 8% of the mass of powder; the reaction temperature is 50℃ and the reaction time is 40 minutes.

[0099] (5) Composite membrane formation: chitosan solution mass concentration 3%, spray volume is 10% of powder mass, fluidized bed inlet air temperature 50℃.

[0100] (6) Low temperature drying: Dry in a fluidized bed at 50℃ for 60 minutes.

[0101] (7) Addition of additives and final mixing and sieving: 8% sodium lignosulfonate, 3% sodium dodecyl sulfate, and 5% sodium carboxymethyl starch were added. The mixture was mixed in a V-type mixer for 30 minutes, passed through a 25μm sieve, and the sieve residue was collected to obtain the composition.

[0102] The specific experimental results of this invention are as follows:

[0103] Experimental Example 1: The control effect of the composition on soil-borne diseases and underground pests

[0104] Experimental Design:

[0105] A cucumber field that had been continuously cultivated in a greenhouse for three years was used as the experimental field. This field suffered from severe soil-borne diseases such as root rot and wilt, and had high population densities of root-knot nematodes and snails. The experiment included the following treatment groups:

[0106] Treatment Group 1: The composition prepared in Example 1 was applied evenly to the soil surface at a rate of 2.5 kg per acre 7 days before cucumber transplanting, and then lightly tilled into the soil (10-15 cm deep).

[0107] Treatment Group 2: The composition prepared in Example 2, used in the same manner and dosage as Treatment Group 1.

[0108] Treatment Group 3: The composition prepared in Example 3, used in the same manner and dosage as Treatment Group 1.

[0109] Control group 1: 86.2% cuprous oxide wettable powder (commercially available control), applied at a rate of 1.0 kg per mu (the content of active ingredient is equivalent to that of the treatment group) in the same manner.

[0110] Control group 2: Triterpenoid saponin single-agent wettable powder (self-made, fineness 1000 mesh), applied at a rate of 2.5 kg per mu in the same manner.

[0111] Blank control group: No treatment was given, and routine watering management was performed.

[0112] Each treatment had three replicate plots, each 30 m², arranged in a randomized block design. Root rot control efficacy, nematode reduction rate, and snail reduction rate were assessed at 30, 45, and 60 days post-transplanting.

[0113] Disease investigation method: Five points were randomly selected from each plot, and 10 plants were investigated at each point. The number of plants with root rot and the disease index were recorded. Disease grading standards: Grade 0 - No lesions; Grade 1 - Root lesions cover 1%-10% of the total root area; Grade 2 - 11%-30%; Grade 3 - 31%-50%; Grade 4 - ≥51%.

[0114] Pest survey method: Five points were randomly selected from each plot, and a 20cm×20cm×20cm soil sample was taken from each point. The number of female root-knot nematodes and snails was manually separated and counted.

[0115] Experimental results:

[0116] Root rot prevention efficacy (%) Nematode reduction rate (%) Snail regression rate (%) Processing Group 1 88.6 74.8 91.3 Processing Group 2 87.3 73.1 90.2 Processing Group 3 90.7 79.3 96.7 Control group 1 75.5 — 81.1 Control group 2 80.3 61.1 38.9 Blank control — — —

[0117] Note: "—" indicates that the treatment has no control effect on the target or the control effect is less than 10%; the control effect and reduction rate are calculated values ​​relative to the blank control.

[0118] Results analysis:

[0119] Verification showed that the composition of this invention (treatment groups 1-3) achieved a control efficacy of over 85% against cucumber root rot 30 days after transplanting, stabilized at 82%-87% 45 days after transplanting, and maintained a relatively high level of 78%-83% 60 days after transplanting, demonstrating excellent control effect and persistence. In contrast, the triterpenoid saponin single-agent control group 2 showed acceptable control efficacy (80.3%) 30 days after transplanting, but the efficacy significantly decreased to 48.6% by 60 days, indicating insufficient persistence. The cuprous oxide single-agent control group 1 showed a 30-day control efficacy against root rot that was more than 10% lower than the treatment groups of this invention; after 60 days, the efficacy against root rot decreased to 69.8%, almost indicating that the disease was out of control.

[0120] Regarding the control of root-knot nematodes, the nematode reduction rate of the treatment group treated with the composition of this invention reached 73-79% 45 days after transplanting, which was significantly better than the single-agent control of triterpenoid saponins (61.1%), indicating that the combination of the two has a significant synergistic effect on nematodes.

[0121] Statistics on the 60-day reduction rate of snails: the combined effect exceeded 90%; more than 10% higher than the control group cuprous oxide single agent; the effect of triterpenoid saponin single agent was 81.9% after 30 days, but decreased to 38.9% after 60 days, with a significant decrease in effect and insufficient duration of effect.

[0122] The above results indicate that the composition of the present invention, through the synergistic effect of cuprous oxide and triterpenoid saponins, has a broad-spectrum and highly effective control effect on root rot and underground pests, and its duration of action is significantly better than that of any single agent.

[0123] Experimental Example 2: The Control Effect of the Composition on Tree Trunk Diseases and Pests

[0124] Experimental Design:

[0125] Red Fuji apple trees aged 8-12 years were selected from a major apple-producing area in Shaanxi Province as the experimental subjects. Apple tree rot, longhorn beetles, and trunk borers were prevalent in this orchard. The experiment included the following treatment groups:

[0126] Treatment Group 1: The composition obtained in Example 1 was diluted with water at a ratio of 1:5 (by mass) and then evenly applied to the base of the trunk up to the branch of the first main branch using a brush, with a coating thickness of about 0.05 mm.

[0127] Treatment group 2: The composition obtained in Example 2 was applied by the same method.

[0128] Treatment group 3: The composition obtained in Example 3 was applied by the same method.

[0129] Control group 1: 86.2% cuprous oxide wettable powder (commercially available), applied by brushing with the same dilution ratio and method.

[0130] Control group 2: Triterpenoid saponin single-agent wettable powder (self-made), applied by brushing with the same dilution ratio and method.

[0131] Blank control group: coated with water.

[0132] For each treatment, 30 apple trees with similar vigor were selected. Before application, existing canker lesions on each tree were marked and the area of ​​the lesions was measured. The number of frass holes drilled by borers was also recorded. After the application, the expansion of canker lesions and the number of newly added borer holes were investigated at 1 month, 3 months, and 6 months.

[0133] The effectiveness of rot control: The lesion area expansion rate (lesion area after treatment / lesion area before treatment × 100%) is used as the evaluation index. The lower the area expansion rate, the better the control effect.

[0134] Control efficacy against borers: The number of newly formed borer holes is used as the evaluation index; the fewer the number of newly formed borer holes, the better the control effect. The integrity of the coating layer and its resistance to rain erosion are also observed.

[0135] Experimental results:

[0136] 1 month 3 months 6 months Processing Group 1 3.2 1.2 5.3 Processing Group 2 4.1 1.5 6.1 Processing Group 3 2.8 0.8 4.2 Control group 1 4.5 10.9 9.9 Control group 2 2.6 5.6 29.6 Blank control 17.9 11.2 35.5

[0137] As shown in Table 2, ① after the composition of the present invention was applied to the apple tree trunk, the area expansion rate of canker lesions was only 4.2%-6.1% within 6 months, which was much lower than that of cuprous oxide single agent control (9.9%) and triterpenoid saponin single agent control (29.6%), indicating that the composition of the present invention has excellent inhibitory effect on canker.

[0138] Meanwhile, verification showed that triterpenoid saponins had a significant short-term control effect on dry rot disease, with a concentration of less than 2.6%, but the duration of effectiveness was severely insufficient, with the effect becoming negligible after 3 months.

[0139] ② It is also effective in controlling longhorn beetles and stem borers. The number of new borer holes per plant in 3 months is only 0.8-1.5 per plant, while the number of new borer holes per plant in the control group is as high as 6-10 per plant.

[0140] ③ It is worth noting that the film formed after application of the composition of the present invention remains essentially intact after 6 months, exhibiting excellent resistance to rain erosion and long-lasting physical protection. The continued presence of the film ensures the slow release of the active ingredients and long-lasting protection. In contrast, the cuprous oxide single-agent coating, lacking the protection of film-forming aids, becomes very thin after one month due to leaching; the triterpenoid saponin single-agent coating, due to its strong water solubility, almost completely dissolves and disappears after two weeks.

[0141] The above results show that the composition of the present invention, through the protection of calcification film technology, gives the coating film excellent water resistance and long-lasting adhesion. A single application can effectively control tree trunk diseases and pests for up to 3-6 months, significantly reducing the labor costs of repeated application.

[0142] Experimental Example 3: The effect of the composition on the control of diseases and pests of leaves and fruits on the above-ground parts (application in orchard sanitation)

[0143] Experimental Design:

[0144] A strawberry greenhouse in Shandong Province was selected as the experimental subject. The previous crop in the greenhouse was tomato, which suffered from severe gray mold, powdery mildew, aphids, and thrips. Spring sanitation treatment was carried out before strawberry transplanting, and the following treatment groups were established:

[0145] Treatment Group 1: The composition prepared in Example 1 was diluted 400 times with water at a dosage of 1.5 kg per acre, and then evenly sprayed or misted onto the ground, pillars, inner surface of the greenhouse film, and strawberry seedlings.

[0146] Treatment group 2: The composition obtained in Example 2 was applied in the same manner.

[0147] Treatment group 3: The composition prepared in Example 3 was applied in the same manner.

[0148] Control group 1: 86.2% cuprous oxide wettable powder (commercially available), applied at a rate of 0.5 kg per acre using the same method.

[0149] Control group 2: Triterpenoid saponin single-agent wettable powder (self-made), applied at a rate of 1.5 kg per mu in the same manner.

[0150] Blank control group: sprayed with an equal amount of water.

[0151] Seven days after the garden was cleaned, strawberry seedlings were transplanted. After transplanting, the occurrence of gray mold and powdery mildew, as well as the population density of aphids and thrips, were observed and recorded regularly. Thirty plants were randomly selected from each plot, and two leaves from the top, middle, and bottom of each plant were collected for the survey.

[0152] Experimental results (30 days: 60 days): Gray mold, powdery mildew; aphids, thrips

[0153] 30d 60d 30d 60d Processing Group 1 86.5 72.3 84.2 63.1 Processing Group 2 83.8 70.6 81.5 61.3 Processing Group 3 88.2 76.1 85.8 65.6 Control group 1 81.3 66.6 — — Control group 2 78.6 36.9 80.8 43.2

[0154] Results analysis:

[0155] As shown in Table 3, the composition of this invention, when applied during spring garden sanitation, exhibited a control efficacy of 84%-88% against gray mold and powdery mildew in strawberries 30 days after transplanting, and maintained at 70%-76% 60 days after transplanting, with a residual effect exceeding 60 days. The reduction rate against pests initially exceeded 80%, decreasing to around 63% after 60 days. Compared to the effects of currently available pesticides, this residual effect is considered quite ideal. In contrast, the triterpenoid saponin single agent showed a disease control efficacy exceeding 78% 30 days after transplanting, but significantly decreased to 36.9% by 60 days; the pest control efficacy also decreased from 80.8% to 43.2%, indicating a significantly insufficient residual effect. Cuprous oxide single agent showed good disease control efficacy, but not as good as the compound formulation, because it lacks penetrating activity; and it had almost no control effect against aphids and thrips.

[0156] In terms of the control of aphids and thrips, the composition of the present invention also has a remarkable control effect. It is worth noting that the composition of the present invention has a significantly extended period of effectiveness against aphids and thrips, and still maintains a reduction rate of more than 60% 60 days after transplanting, which reflects the significant enhancement effect of calcification and film formation technology on the long-term effectiveness of triterpenoid saponins.

[0157] The above results indicate that the composition of the present invention can form a protective film layer covering all surfaces within the covering facility when used for orchard sanitation. This film layer has an inward permeability and can continuously release active ingredients, achieving highly efficient control of various aboveground pests and diseases with "one spray for multiple preventions," and its effective period exceeds 30 days.

[0158] Experiment Example 4: Safety and growth-promoting effect of the composition at different crop seedling stages

[0159] Experimental Design:

[0160] Pepper seedlings (4-leaf-1-heart stage) and cucumber seedlings (3-leaf-1-heart stage) grown in greenhouses were selected as experimental subjects. A 1500-fold dilution of the composition prepared in Example 1 was sprayed on each seedling. An equal volume of water was sprayed as a blank control, and a 1500-fold dilution of commercially available 86.2% cuprous oxide wettable powder was used as a copper-based control. Each treatment was applied to 30 seedlings, with three replicates. Phytotoxicity symptoms (leaf yellowing, scorching spots, dwarfing, etc.) were investigated 7 and 14 days after spraying, and growth indicators such as plant height, stem diameter, above-ground fresh weight, and root fresh weight were measured.

[0161] Experimental results:

[0162] Composition A of the present invention Cuprous oxide control Water comparison Plant height growth rate (%) 28.6 16.5 21.3 Stem diameter growth rate (%) 15.2 8.6 11.8 Fresh weight of above-ground parts (g / plant) 8.76 7.12 7.65 Fresh root weight (g / plant) 2.13 1.56 1.78 Symptoms of pesticide damage none Some are slightly yellow none

[0163] Results analysis:

[0164] As shown in Table 4, no phytotoxicity symptoms appeared after the composition of the present invention was sprayed on chili seedlings and cucumber seedlings, while the cuprous oxide single-agent control showed mild phytotoxicity (mild yellowing of young leaves). All growth indicators of the composition-treated group were superior to those of the water control and the cuprous oxide single-agent control. Specifically, the plant height growth rate and root fresh weight of chili seedlings increased by 34.3% and 19.7% respectively compared to the water control, while the corresponding indicators for cucumber seedlings increased by 31.0% and 24.9% respectively.

[0165] The growth-promoting effect exhibited by the composition of this invention stems from the following aspects: First, triterpenoid saponins, as active organic matter, have a certain promoting effect on crop growth and development, while also regulating the internal structure of soil aggregates, facilitating nutrient transport, and promoting root development; second, the chitosan oligosaccharides produced after chitosan degradation have plant immune-inducing activity, which can promote plant growth; third, copper is supplied in a slow-release manner, avoiding the inhibition of root development caused by excessively high concentrations of copper ions at one time, and instead promoting normal plant metabolism as a trace element. These results indicate that the composition of this invention is safe for crop seedlings and also has an auxiliary effect in promoting root development and seedling vigor.

[0166] Experimental Example 5: Experimental Protocol for Soil Drip Irrigation Control of Onion / Garlic Root Rot and Underground Pests Using Cuprous Oxide-Triterpenoid Saponin Combination

[0167] I. Experimental Objective

[0168] The synergistic effect of the composition of the present invention was verified by comparing its control efficacy with that of cuprous oxide and oxamyl alone against root rot of onions / garlic and underground pests (such as grubs, wireworms, and root maggots).

[0169] II. Experimental Design

[0170] T1 Cuprous oxide and triterpenoid saponin composition 1000g 70-80% drip irrigation T2 86.2% Cuprous oxide wettable powder 500g 70-80% drip irrigation T3 30% Mancozeb·Oxyphenidyl Aqueous Solution 1000g 70-80% drip irrigation CK Clear water — 70-80% drip irrigation

[0171] Note: For drip irrigation with 70-80% water, the water usage per acre should be controlled at 5-7 m³, and the pesticide should be injected in the last 20 minutes. In actual production, most growers use excessive water when drip irrigation, resulting in low pesticide concentration and unsatisfactory effects!

[0172] Cell size: 30m², replicated 3 times, randomized block design

[0173] Application time: After onion transplanting / when garlic has 2-3 leaves, apply twice at 10-15 day intervals.

[0174] III. Survey Methods and Time

[0175] Root rot survey (30 days, 45 days, and 75 days after the first application of the pesticide):

[0176] Five sampling points were used, with 10 plants at each point, for a total of 50 plants.

[0177] Grading standards: Grade 0 (no lesions) → Grade 4 (root rot ≥ 51%)

[0178] Calculate the disease severity index and prevention and control effectiveness (%)

[0179] Survey of underground pests (30 days, 45 days, and 75 days after pesticide application):

[0180] Five soil samples (20×20×20cm) were collected from each plot, and the number of larvae was isolated and counted.

[0181] Calculate the insect population reduction rate and corrected control efficacy (%)

[0182] Safety observation: symptoms of pesticide damage, plant height, and growth vigor

[0183] IV. Experimental Results

[0184] The composition's control efficacy against root rot reached 92.6% after 30 days; decreased to 84.3% after 45 days; and decreased to 72.1% after 75 days. The composition's synergistic effect against underground pests showed a reduction rate of 0.9% after 30 days; increased to 2.6% after 45 days; and increased to 5.9% after 75 days.

[0185] The control efficacy of 86.2% cuprous oxide as a single agent against root rot was as follows: 87.1% after 30 days; maintained at 81.5% after 45 days; decreased to 72.9% after 75 days; cuprous oxide had almost no effect on underground pests.

[0186] The control efficacy of 30% methyl thiophanate-methyl aqueous solution against root rot was 92.9% after 30 days; it decreased to 65.3% after 45 days; and to 30.9% after 75 days. methyl thiophanate-methyl had almost no effect on underground pests.

[0187] The statistical table is as follows:

[0188] Control efficacy (%) of different treatments against root rot in onions / garlic

[0189] T1: Cuprous oxide and triterpenoid saponin composition 92.6 84.3 72.1 T2: 86.2% cuprous oxide wettable powder 87.1 81.5 72.9 T3: 30% Mancozeb·Oxyphenidyl aqueous solution 92.9 65.3 30.9 CK: Shimizu — — —

[0190] Population reduction rate (%) of underground pests under different treatments

[0191] T1: Cuprous oxide and triterpenoid saponin composition 0.9 2.6 5.9 T2: 86.2% cuprous oxide wettable powder Almost no effect Almost no effect Almost no effect T3: 30% Mancozeb·Oxyphenidyl aqueous solution Almost no effect Almost no effect Almost no effect CK: Shimizu — — —

[0192] Conclusions: ① The invented composition showed ideal efficacy against root rot, with a residual effect of up to 60 days; the effect of cuprous oxide alone against root rot was about 5% lower than that of the invented composition in the early stage, but slightly higher in the later stage, and the residual effect could also reach 60 days; ② In the early stage, the invented composition was superior to cuprous oxide alone; the later stage effects were comparable, indicating that film formation had a good influence on the residual effect, while the cuprous oxide alone ensured the later stage effect due to the large amount of cuprous oxide used; ③ 30% methyl methacrylate·oxadixyl had excellent early stage effects, but poor residual effect. 30 days after the second application, the effect had decreased by 65.3%, and by 60 days it had decreased to 30.9%. By 75 days after the first application, its effect was actually negligible (soil disease experiment data, due to the influence of early stage effects, does not directly show no effect).

[0193] The composition showed that its efficacy and persistence against root rot were no weaker than those of the two control groups. The composition also showed significant efficacy against underground pests, with a residual effect of up to 30 days. Observation of application showed that the composition was safe for crops, and the growth of the experimental plots was better than that of the control plots, indicating that the invented composition also has a growth-promoting effect.

[0194] Experiment Example 6: Orchard sanitation during the early spring budding stage of fruit trees to control spider mites, aphids, scale insects, fruit borers, leafminer moths, mulberry longhorn beetles, bark beetles, and other pests, as well as diseases such as rot, brown spot, ring rot, anthracnose, pear core rot, leaf spot, dry rot, and gummosis.

[0195] 1. Experimental Objective

[0196] This study compares the control efficacy of the composition of this invention with commonly used orchard sanitation agents such as lime sulfur and mineral oil against red spider mites, aphids, scale insects, fruit borers, canker, leaf spot, core rot, dry rot, and gummosis in apple / pear trees. Experimental Design

[0197] T1 Cuprous oxide and triterpenoid saponin composition 200 times dilution Spray evenly over the entire plant T2 45% lime-sulfur mixture crystals 50x dilution (recommended dosage) Spray evenly over the entire plant T3 95% mineral oil emulsion 200 times dilution (recommended dosage) Spray evenly over the entire plant CK Clear water — Spray evenly over the entire plant

[0198] Five apple / pear trees with uniform vigor were selected for each treatment.

[0199] Application time: Before bud break in spring (during garden cleanup), spray until the branches and trunks are moist and dripping wet.

[0200] Survey Methods

[0201] Spider mites, aphids, scale insects 15 days, 30 days, 45 days, and 60 days after application Take one-year-old branches from the east, south, west, and north sides of each plant and check the number of live insects on the leaves and branches. Leaf spot disease, moldy core disease After leaf expansion (approximately 30, 45, and 60 days after application) and during harvest. Investigate 200 leaves and 100 fruits per plant, and record the percentage of diseased leaves and fruits.

[0202] Calculation indicators:

[0203] Insect population reduction rate (%), corrected control efficacy (%)

[0204] Diseased leaf rate (%), diseased fruit rate (%), control effect (%)

[0205] Observation conclusion:

[0206] I. Disease Control

[0207] ① The invented composition has a significant effect on the early control of dry rot and gummosis, with an effective period of more than 45 days. After 60 days, if there is rainfall, dry rot and gummosis will be out of control, indicating that the control of dry rot and gummosis at a 200-fold dilution does not exceed 60 days. Analysis suggests that the spray film layer of the invented composition at a 200-fold dilution can withstand 60 days. For subsequent control of gummosis, dry rot, bark beetles, longhorn beetles, and snails, the fruit tree branches and trunks can be sprayed again with a 50-fold dilution of the composition slurry 45 days after spring orchard sanitation for comprehensive protection of the branches and trunks.

[0208] ② Control of anthracnose and leaf spot disease by the invented composition: No disease occurred two months before the application of the medicine. Three months later, in mid-July, the disease incidence on diseased trees was much less than that of the control group, and the onset of disease was delayed by about 25 days. The diseased leaf rate was lower than that of the control group, less than half of that of the control group. Analysis suggests that this is due to the combination of the medicine's control over pathogens and its long-lasting effect. In addition, the triterpenoid component of the medicine itself has nutritional effects and a certain calcium supplementation function, so it can play a certain role in alleviating leaf drop disease (including physiological leaf drop).

[0209] ③ Control of ring rot, canker, and moldy core disease; Compared with the control group, the fruit drop rate of diseased fruit before maturity was only 1.7%, which was 38.6% of the control group's 4.4%, indicating that the control effect of canker, ring rot, etc. was significantly improved compared with the control group; Autumn harvest comparison: The proportion of moldy core, rotten core, and rotten fruit showed that the disease rate of the invented composition was only 1.2%, while that of the control group was 3.1%, a reduction of 61.3%; This indicates that the composition has a good effect on the control of diseases infecting during the flowering period and the overall disease control in the orchard.

[0210] II. Pest Control

[0211] ① Observation and statistics on spider mites, aphids, and scale insects in the early stage of pesticide application: After 30 days of observation, the invented combination showed good killing effect on scale insects, with a mortality rate of over 90%, which was higher than the 81.2% of the control group. Compared with the control group, the effect on aphids and spider mites was comparable to that of lime sulfur and superior to that of mineral oil alone. From the observation of the occurrence time and severity of aphid and spider mite infestations, minerals had the worst killing effect on overwintering eggs and the earliest and most severe outbreak time.

[0212] ② Observations on fruit borers, leaf miners, longhorn beetles, and bark beetles: Observations on leaf grazing, fruit holes, and newly formed borer holes in tree trunks revealed that the invention composition's control ability against the above pests was far superior to the control group within 60 days, with almost no appearance of the above pests and a very low probability of occurrence; after 60 days, the effect declined rapidly, with an increase rate comparable to the control group, indicating that the composition's control effect on the above pests disappeared after two months, and the control group also did not have a control effect.

[0213] Comprehensive analysis and comparison: The invented composition has insecticidal, acaricidal, and bactericidal effects, providing multiple protections with one spray. Its overall effect is superior to spring and autumn orchard sanitation products such as lime sulfur mixture, and it can completely replace many traditional orchard sanitation agents.

[0214] Experiment Example 7: Control of root-knot nematodes in watermelons / eggplants—Comparison with abamectin and thiazophos

[0215] Experimental Objective

[0216] A comparison of the control efficacy of the composition of this invention with abamectin and thiazophos against root-knot nematodes in watermelon / eggplant.

[0217] Experimental Design

[0218] T1 Cuprous oxide and triterpenoid saponin composition 1000g Soil trenching / hole application before transplanting T2 5% abamectin microemulsion 1000mL (as recommended) Apply in the same way T3 30% Thiazolphosphine Microcapsule Suspension 1000g (as recommended) Apply in the same way CK Blank control — No medicine

[0219] The cell area is 30m², repeated 3 times, and arranged in a randomized block design.

[0220] Application time: 7 days before transplanting watermelons / eggplants, mix the pesticide with fine soil and apply it into the planting hole or furrow.

[0221] Survey Methods

[0222] Root knot index 30 days and 60 days after transplanting Five samples were taken from each community, with five plants at each point. The roots were dug up and graded from 0 to 5. Nematode density 60 days after transplanting Five soil samples (500g) were taken from each plot, and the modified Behmann funnel method was used for separation and counting. Plant growth 60 days after transplanting Measure plant height, stem diameter, and above-ground fresh weight.

[0223] Calculation indicators

[0224] Root knot index = ∑(number of diseased plants at each level × level value) / (total number of plants surveyed × highest level value) × 100;

[0225] Control efficacy (%) = (Root knot index of control area - Root knot index of treatment area) / Root knot index of control area × 100%;

[0226] Nematode reduction rate (%)

[0227] Observation conclusions

[0228] The combination's control effect on root-knot nematodes is inferior to 30% thiazophos microcapsule suspension, but close to that of abamectin. Among nematode control agents, this result is already very outstanding. It can be used to control soil-borne diseases such as root rot, while also controlling root-knot nematodes and underground pests, thereby saving on pesticide costs. Alternatively, it can be used in combination with abamectin or thiazophos to enhance the killing effect of the combination.

[0229] Control of mollusks (snails, slugs) – Comparison with cuprous oxide alone and metaldehyde

[0230] Experiment Example 8: Experimental Objective

[0231] The killing effects and duration of the composition of the present invention on snails and slugs were compared with those of cuprous oxide and metaldehyde.

[0232] Experimental Design:

[0233] T1 Cuprous oxide and triterpenoid saponin composition 2000g Apply to the soil surface between plant rows / rhizosphere. T2 86.2% Cuprous oxide wettable powder 1000g Apply in the same way T3 40% metaldehyde suspension 2000g Apply in the same way CK Blank control — No medicine

[0234] The area of ​​the enclosure is 30m² (or a small fenced area is set up according to the density of molluscs occurrence), and no duplicates are allowed.

[0235] Application time: evening (before the peak activity period of snails / slugs), keep the soil moist after application.

[0236] Survey Methods

[0237] Number of live insects 3 days, 7 days, 30 days, and 60 days after application Five samples were taken from each area, each covering 1 square meter. Live snails / slugs were counted on the ground and plants in the evening. Leaf damage rate 14 days after application At each site, 10 plants were surveyed to determine the extent of damage to new leaves.

[0238] Calculation indicators

[0239] Pest population reduction rate (%); corrective control efficacy (%); leaf damage rate (%) and leaf preservation effect (%)

[0240] Evaluation of duration of effectiveness (number of days when the efficacy drops below 50%)

[0241] Observation results

[0242] The composition showed excellent control efficacy against snails and slugs: the efficacy reached 92.5% and 95.6% at 3 and 7 days, respectively; it decreased to 85.3% at 30 days, but still reached 81.8% at 60 days, indicating that the composition had excellent early-stage efficacy and a sustained effect of up to 60 days.

[0243] The control efficacy of 86.2% cuprous oxide against snails / slugs: the efficacy was 80.5% and 89.1% at 3 and 7 days, respectively; it remained at 86.9% at 30 days; and decreased to 82.5% at 60 days.

[0244] The effect of 40% metaldehyde on snails / slugs: the effect reached 88.9% and 83.1% after 3 days and 7 days respectively, but dropped to 50.6% after 30 days and even lower to 6.1% after 60 days, which is almost ineffective;

[0245] Experimental observations showed that: ① The initial effects of the composition were significantly better than those of cuprous oxide alone and metaldehyde; ② At 30 and 60 days, the effects of the composition were comparable to those of cuprous oxide alone, with a longer effective period of 60 days; ③ The effectiveness of metaldehyde began to decline after 7 days, and by 30 days it could only maintain 50.6%; in fact, the effect had basically disappeared (the early killing reduced the insect population density in the experimental plot, affecting the subsequent statistical data), indicating that the effective period of metaldehyde would not exceed 15 days; ④ The growth in the experimental plots with the composition was better than that in the control plots, and there were basically no other pests or diseases, indicating that the composition had a prominent advantage in dual prevention and control, and its economic benefits were also more prominent.

[0246] Experiment Example 9: Comparative Experiment on Snail Control by Applying Plaster to Peach Tree Trunks

[0247] The purpose of this experiment is to compare the efficacy, duration of effect, and cost-effectiveness of the composition of this invention with cuprous oxide (coating combination) and metaldehyde alone in controlling snails (mainly gray snails and homolar snails) on peach tree trunks, and to verify the outstanding advantages of the composition of this invention in trunk protection.

[0248] Experimental Design

[0249] A peach orchard (trees aged 6-8 years, severely infested with snails) was selected as the experimental site. Peach trees with similar vigor were selected and the following treatment groups were established.

[0250] T1 The composition of the present invention (Example 1) Dilute with water at a ratio of 1:3 (by weight). Apply the coating evenly with a brush from the base of the trunk to the branch of the first main branch, to a thickness of approximately 0.15 mm. T2 86.2% Cuprous Oxide Wettable Powder (TuNiu Combination) Same dilution factor as T1 (equivalent copper content) Apply using the same method T3 40% metaldehyde suspension Same dilution factor as T1 (equivalent active ingredient) Apply using the same method CK Clear water — Apply using the same method

[0251] Five peach trees were selected for each treatment, and one tree was selected for the water control (a total of 16 trees were selected due to severe losses). The trees were arranged in a randomized block design. Before application, any existing snails on the tree trunks were removed and the observation areas were marked.

[0252] Survey Methods

[0253] The following indicators were investigated on days 7, 30, 60, 90, and 120 after application:

[0254] Number of snails in the trunk coating area and at the root: Manually count the number of dead or inactive snails in the coating area (width not less than 50cm) and at the root of the trunk, calculate the insect population reduction rate and correct the control effect.

[0255] Number of surviving snails in the upper part of the painted area: The number of surviving snails in the upper part of the painted area is counted manually to calculate the insect population reduction rate.

[0256] Coating integrity: Visually inspect the percentage of peeled area of ​​the coating layer to evaluate its resistance to rain erosion and its long-lasting adhesion.

[0257] Fruit protection effect: Investigate the number of damaged fruits (per tree) in each treatment.

[0258] Test results

[0259] Processing group Snail correction efficacy (%) at different time points Coating integrity rate (120d, %) Number of damaged fruits (per plant) 7d 30d 60d 90d 120d T1 97.1 95.3 91.5 84.2 78.4 78.6 1.2 T2 91.2 90.1 81.3 69.4 42.7 35.4 9.8 T3 88.9 69.2 28.6 12.3 2.1 0.6 109.3 CK — — — — — — —

[0260] Results Analysis

[0261] Immediate effect (7 days after application)

[0262] T1 (the composition of the present invention) has a control efficacy of 97.1%, which is higher than T2 (cuprous oxide coated with bovine oxen) at 91.2%, with a difference of nearly 6%. Both of them show excellent rapid killing effects. T3 (40% metaldehyde) has a control efficacy of only 88.1%, and its rapid effect is relatively poor.

[0263] Duration of effect (30–120 days)

[0264] T1: The efficacy declines most gradually over time. It is 95.3% at 30 days, 91.5% at 60 days, 84.2% at 90 days, and still maintains 78.4% at 120 days. This indicates that the efficacy of the composition of the present invention can last for more than 120 days, and still has high activity in the later 90 days.

[0265] T2: The rate of decline is significantly faster than that of T1. It is 90.1% at 30 days, 81.3% at 60 days, 69.4% at 90 days, and only 42.7% at 120 days, with a duration of effectiveness of approximately 90 days.

[0266] T3: Its effectiveness is extremely short. It drops to 69.2% after 30 days, plummets to 28.6% after 60 days, reaches only 12.3% after 90 days, and is basically ineffective (2.1%) after 120 days. Its effective period is less than 15 days, which is consistent with the characteristics of easy photolysis and water solubility reported in the literature.

[0267] Weather resistance and integrity of coating (after 120 days)

[0268] T1: The coating integrity rate is as high as 78.6%. Due to the dual protection of the calcification film and the chitosan film, the film layer has excellent resistance to rain erosion and long-term adhesion, and it still remains basically intact under 120 days of field weather conditions.

[0269] T2: The coating integrity rate is 35.4%, the film layer has been washed away and thinned, with large areas exposed, and the protective effect is significantly reduced.

[0270] T3: The coating integrity rate is only 0.6%. Due to its strong water solubility, the film layer almost completely dissolves within 15 days and cannot provide long-term physical barrier.

[0271] Fruit protection effect

[0272] Treatment T1 resulted in the fewest damaged fruits, with only 1.2 fruits per plant, significantly lower than T2 (9.8 fruits per plant) and T3 (109.3 fruits per plant). This trend is highly consistent with the efficacy data, indicating that the composition of this invention can effectively prevent snails from climbing trees and eating the fruits in the long term.

[0273] Overall Conclusion

[0274] The composition of this invention (T1) is significantly superior to the cuprous oxide coating combination (T2) and metaldehyde single agent (T3) in all three core indicators. Its triple characteristics of "rapid and efficient action + slow-release and long-lasting effect + physical barrier" make it the preferred solution with the highest overall cost-effectiveness in preventing snails from climbing trees and eating fruits on peach trees and other fruit trees (Note: Applying the composition of this invention at a high concentration for orchard sanitation in the early spring when fruit trees are in bloom can also control snails for more than 60 days).

[0275] In summary, this invention significantly improves the synergistic effect, storage stability, and field efficacy (over 30 days for foliar spraying and 3-6 months for trunk spraying) of the composition by compounding cuprous oxide and triterpenoid saponins in a 3:7 ratio and then subjecting them to calcification and film formation to form a core-shell coating structure. It also provides multiple beneficial effects such as broad-spectrum and highly effective pest and disease control, reducing copper dosage by 30%-50%, environmental friendliness, and promotion of crop rooting and seedling growth. This invention offers a practical and feasible technical solution for multi-purpose application of a single pesticide and green agricultural pest control.

[0276] In summary, the cuprous oxide-triterpenoid saponin composition of this invention has significant advantages in the following aspects: spring and autumn orchard sanitation of fruits and vegetables, control of soil-borne diseases including difficult-to-treat diseases, control of copper-based safe crop diseases, and control of snails, slugs, nematodes, root maggots, and leek maggots. ① In orchard sanitation, it offers comprehensive and broad-spectrum control with a combined effective period exceeding 45 days, providing comprehensive, economical, effective, and environmentally friendly benefits. ② Regarding soil-borne diseases and difficult-to-treat diseases, it possesses advantages such as surface isolation of pathogens on the copper ion membrane, strong penetration into affected areas, and enhanced systemic absorption to improve resistance, making it particularly effective against difficult-to-treat diseases while also controlling various pests. ③ In the control of copper-based safe crop diseases, because copper-based agents have sensitive crops and sensitive periods, although the membrane-coated cuprous oxide is safer, to avoid disputes after use, this case study seriously proposes not to develop foliar application plans for copper-sensitive crops and copper-based sensitive periods. For safe crops, the composition of this invention not only controls the targeted diseases but also prevents other diseases and pests, making it economical and convenient. 1. Comprehensive and rain-resistant, with a lasting effect of over 30 days, making it particularly useful for diseases that easily break out during rainy weather; 2. For snail and slug control, it can be applied to tree trunks, with a lasting effect of over 120 days, or used as a pre-planting treatment in fields, effectively killing snail and slug eggs and adults. With precautions taken to prevent them from crawling into the field, the effect can last for about 90 days, while also preventing other underground pests, nematodes, and various soil-borne diseases; 3. Nematodes, root maggots, and leek... Maggots are a notoriously difficult pest to control. When they are not yet known to exist, the composition of this invention can be used normally to control soil-borne diseases and underground pests, effectively controlling their spread. For areas where they have already become severely infested, this agent can be used in combination with other targeted agents. The triterpenoid saponins can effectively penetrate other agents, enhancing their efficacy. Under the combined pharmacological action, the effect is twice as good with half the effort. At the same time, the composition can also control other pests and diseases, making it economical, effective, and comprehensive.

[0277] The composition of this invention has significant advantages in the above-mentioned aspects. It is of great significance in terms of practicality, economy, society and environmental protection. In particular, the introduction of triterpenoid saponins into soil can improve soil remediation, promote crop growth, increase yield and income, increase the accumulation of triterpenoids and their derivatives in agricultural products such as Chinese medicinal materials, vegetables, fruits and grains, and play a positive role in promoting human dietary health!

[0278] It should be understood that numerous specific implementation decisions can be made during the development of any practical implementation, such as in any engineering or design project. Such development efforts may be complex and time-consuming, but for those skilled in the art who benefit from this disclosure, the development effort will be a routine work of design, manufacturing, and production without requiring much experimentation.

[0279] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all such modifications or substitutions should be covered within the scope of the claims of the present invention.

Claims

1. A composition of cuprous oxide and triterpenoid saponins from plant sources, characterized in that, The composition comprises cuprous oxide powder and triterpenoid saponin powder, wherein the weight ratio of cuprous oxide powder to triterpenoid saponin powder is 3:7, the fineness of both cuprous oxide powder and triterpenoid saponin powder is 1000-1500 mesh, and the total weight of cuprous oxide powder and triterpenoid saponin powder accounts for 2%-98% of the total weight of the composition.

2. The pesticide composition according to claim 1, characterized in that: The composition further comprises adjuvants, including dispersants, wetting agents, and disintegrants.

3. The method for preparing the composition of cuprous oxide and triterpenoid saponin-based plant-derived pesticide according to any one of claims 1 to 2, characterized in that, Includes the following steps: S1. Sieve the coarse cuprous oxide powder, take the sieved material and place it in a plasma surface treatment device, and perform low-temperature plasma surface activation treatment in an oxygen atmosphere to obtain activated cuprous oxide powder. S2. Place the coarse triterpenoid saponin powder in an air jet mill for ultra-fine grinding, and collect the powder with a fineness of 1000-1500 mesh to obtain finely ground triterpenoid saponin powder. S3. The activated cuprous oxide powder obtained in S1 and the triterpenoid saponin powder obtained in S2 are added to a mixer at a weight ratio of 1:5 for graded mixing to obtain a mixed powder. S4. The mixed powder obtained in S3 is fed into a fluidized bed granulator, and calcium sulfate solution and sodium carbonate solution are sprayed in sequence for gradient calcification treatment to obtain calcified powder. S5. The calcified powder obtained in step S4 is placed in a fluidized bed and sprayed with chitosan solution for composite membrane treatment to obtain membrane powder. S6. The film-forming powder obtained in S5 is dried at low temperature to solidify the coating film. S7. Add the adjuvant to the dried powder obtained in S6 for final mixing, and sieve to obtain the finished product of the wettable powder composition of cuprous oxide and triterpenoid saponin-based plant-derived pesticide.

4. The method according to claim 3, characterized in that: In step S1, the conditions for plasma surface activation treatment are: treatment time of 5-15 minutes and treatment power of 100-300W; the sieve mesh number for sieving the cuprous oxide coarse powder is 800 mesh.

5. The method according to claim 3, characterized in that: In S2, the air jet mill uses compressed air at 0.6-0.8 MPa as the working fluid for ultra-fine grinding. During the grinding process, the temperature of the grinding chamber is controlled to not exceed 45°C by cooling water in the jacket, and powder of 800-1500 mesh is collected by a classifying wheel.

6. The method according to claim 3, characterized in that: In S3, the hierarchical mixing includes: Primary mixing: Add activated cuprous oxide powder and triterpenoid saponin powder into a conical double helix mixer in a certain proportion, and premix for 20-30 minutes at a speed of 20-30 r / min; Secondary mixing: Transfer the premixed powder into a three-dimensional motion mixer and continue mixing for 40-60 minutes at a speed of 30-50 r / min; The secondary mixing process is supplemented with ultrasonic vibration treatment at 20-40kHz, each ultrasonic treatment lasts 5-10 minutes, with a 10-minute interval, and is repeated 2-3 times.

7. The method according to claim 3, characterized in that: In step S4, the gradient calcification process includes: First calcification: A calcium sulfate solution with a mass concentration of 2%-5% is sprayed in by atomization, with the spray volume being 5%-10% of the powder mass, and the fluidized bed inlet air temperature being 50-60℃. Second calcification: Spray in a sodium carbonate solution with a mass concentration of 1%-3%, the amount of which is 3%-8% of the powder mass. The reaction temperature is 40-50℃ and the reaction time is 20-40 minutes.

8. The method according to claim 3, characterized in that: In step S5, the chitosan solution is a chitosan acetic acid solution with a mass concentration of 1%-3%, the degree of deacetylation of the chitosan is ≥85%, and the acetic acid concentration is 1%-2%; the spray volume is 5%-10% of the powder mass, and the fluidized bed inlet air temperature is 40-50℃. In step S6, the low-temperature drying is performed in a fluidized bed at 40-50℃ for 30-60 minutes.

9. The method according to claim 3, characterized in that, In step S7, the additives include a dispersant, a wetting agent, and a disintegrant; the dispersant is sodium lignosulfonate, added at 3%-8% of the total mass of the composition; the wetting agent is sodium dodecyl sulfate, added at 1%-3% of the total mass of the composition; the disintegrant is sodium carboxymethyl starch, added at 2%-5% of the total mass of the composition; the final mixing is performed in a V-type mixer for 20-30 minutes; the sieve mesh size is ≤25μm.

10. The cuprous oxide and triterpenoid saponin-based plant-derived pesticide composition according to claim 1 is used in the prevention and control of pests and diseases.