Validamycin and osthole compound pesticide preparation and preparation method thereof

Abstract

The invention relates to the field of pesticide preparations, and particularly discloses a validamycin and osthole compound pesticide preparation and a preparation method thereof. The validamycin and cnidium lactone compound pesticide preparation is prepared from the following raw materials in percentage by weight: 8 to 15.6 percent of validamycin A, 0.1 to 0.3 percent of cnidium lactone, 7 to 10 percent of castor oil polyoxyethylene ether, 0.3 to 0.8 percent of lauryl sodium sulfate, 0.3 to 0.5 percent of dispersing agent, 0.1 to 0.3 percent of phosphate stabilizer, 0.1 to 0.3 percent of preservative, 1 to 3 percent of thickening agent, 0.3 to 0.5 percent of propylene glycol and the balance of water, the validamycin A and the cnidium lactone are compounded, the proper proportion of the validamycin A and the cnidium lactone is adjusted, and the validamycin A and the cnidium lactone are in synergistic interaction with other auxiliary materials, so that the stability and the control effect of the compound

Description

Technical Field

[0001] The present application relates to the field of pesticide preparations, and in particular to a composite pesticide preparation of jinggangmycin and osthole and a preparation method thereof. Background Art

[0002] With the development of agricultural production, pests and diseases are becoming increasingly serious, which has had a serious impact on the yield and quality of crops. Jinggangmycin is a water-soluble antibiotic-glucoside compound produced by Streptomyces aquaticus Jinggang variant. It is non-toxic to humans, livestock and fish, safe for crops, and is a pollution-free pesticide for producing green food. Osthole is mainly used to control aphids, cabbage worms and stored grain pests in cruciferous vegetables. Jinggangmycin and osthole are two biological pesticides with broad-spectrum antibacterial and insecticidal activities and have been widely used in agricultural production.

[0003] However, the single use of Jinggangmycin or osthole is often difficult to achieve the ideal control effect. The long-term and large-scale use of a single pesticide will cause the disease to develop drug resistance, increase the application amount, increase the cost of control, and also cause a series of environmental problems and pose a certain threat to food safety. Summary of the invention

[0004] In order to improve the problems of drug resistance and low insecticidal efficiency caused by a single pesticide preparation, the present application provides a composite pesticide preparation of Jinggangmycin and osthole and a preparation method thereof.

[0005] In the first aspect, the present application provides a composite pesticide preparation of Jinggangmycin and osthole, which adopts the following technical solution: A composite pesticide preparation of validamycin and osthole comprises the following raw materials in weight ratio: 8-15.6% of validamycin A, 0.1-0.3% of osthole, 7-10% of castor oil polyoxyethylene ether, 0.3-0.8% of sodium lauryl sulfate, 0.3-0.5% of dispersant, 0.1-0.3% of phosphate stabilizer, 0.1-0.3% of preservative, 1-3% of thickener, 0.3-0.5% of propylene glycol and the balance of water.

[0006] By adopting the above technical scheme, Jinggangmycin A has a strong systemic effect. When the hyphae of rice sheath blight come into contact with Jinggangmycin, they are quickly absorbed by the bacterial cells and conducted in the bacterial body, interfering with and inhibiting the normal growth and development of the bacterial cells, thereby playing a role in preventing and controlling pests. At the same time, Jinggangmycin A can interfere with the metabolism and growth of the cell membrane of pathogens, causing the leakage of active substances in the cells, preventing the protein synthesis of pathogens, and ultimately causing the rupture and death of pathogen cells, thereby preventing and controlling plant diseases caused by pathogens such as fungi and bacteria, and protecting the healthy growth of crops. Osthole can inhibit the physiological functions of pests, affect the nervous system of pests, cause the growth and development of pests to be hindered, reduce the reproductive capacity of pests, and thus reduce the damage of pests to crops.

[0007] The compounding of Jinggangmycin A and osthole and adjusting the appropriate ratio of the two have a synergistic effect on the prevention and control of pests and diseases, can improve the stability and high efficiency of the composite pesticide preparation, and significantly reduce the use amount of the composite pesticide preparation. Castor oil polyoxyethylene ether has a good emulsifying effect, can keep osthole and Jinggangmycin A uniformly dispersed in water, improve the uniformity and stability of the active ingredients in the pesticide preparation, and enhance the adhesion of the active ingredients in the pesticide preparation to crops. Sodium dodecyl sulfate can synergistically enhance the effect with castor oil polyoxyethylene ether, reduce the surface tension of water, promote the uniform spreading of the pesticide preparation on the surface of crops, increase the coverage area and penetration capacity of the pesticide preparation, and improve the prevention and control effect of the pesticide preparation. Propylene glycol can reduce the freezing point of the pesticide preparation, reduce the freezing of the pesticide preparation under low temperature conditions, maintain the good fluidity and stability of the pesticide preparation, reduce the precipitation or decomposition of the active ingredients, and extend the shelf life of the pesticide preparation.

[0008] Preferably, the dispersant is lignin sulfonate.

[0009] Preferably, the preservative is one of sodium benzoate and kason.

[0010] By adopting the above technical solution, sodium benzoate and kason can effectively inhibit the growth of microorganisms such as bacteria and fungi in pesticide preparations, prevent microbial contamination of pesticide preparations during storage and use, and maintain the purity and stability of pesticide preparations. Sodium benzoate and kason can reduce the failure of pesticides caused by microbial contamination and prolong the biological activity and control effect of pesticide preparations.

[0011] Preferably, the phosphate stabilizer is at least one of sodium tripolyphosphate and sodium hexametaphosphate.

[0012] By adopting the above technical scheme, sodium tripolyphosphate and sodium hexametaphosphate as stabilizers can reduce the aggregation and precipitation of active ingredients in pesticide preparations in aqueous solutions, promote the uniform dispersion of Jinggangmycin A and osthole in the pesticide preparation system, and improve the uniformity and stability of the pesticide preparation. Sodium tripolyphosphate and sodium hexametaphosphate can form soluble complexes with metal ions such as calcium and magnesium in water to reduce the hardness of water. At the same time, they can also synergize with castor oil polyoxyethylene ether to form a stable emulsion of the active ingredients of the pesticide in the water phase and the oil phase, improve the emulsification stability of the pesticide preparation, and then improve the coverage area and adhesion of the pesticide preparation.

[0013] Preferably, the validamycin A and osthole are prepared in advance into validamycin-osthole composite sustained-release microspheres, and the preparation method of the sustained-release microspheres comprises the following specific steps: Sodium alginate is dissolved in water, and then validamycin A and osthole are added and stirred evenly to form a mixed solution, and then the mixed solution is dropped into a cross-linking agent for mixing reaction, and microspheres are separated after suction filtration to form microsphere semi-finished products, and then the microsphere semi-finished products are added to chitosan for mixing reaction, and then the microspheres are separated by suction filtration, washed and dried to obtain validamycin-osthole composite sustained-release microspheres.

[0014] By adopting the above technical scheme, the sodium alginate-crosslinker-chitosan is used to form a film on the cinnamycin A and osthole, and the gradual decomposition of the sodium alginate and chitosan is utilized to slowly release the active ingredients, thereby achieving the sustained-release effect of the pesticide preparation, prolonging the control effect of the pesticide, and reducing the frequency and amount of pesticide use.

[0015] Sodium alginate, as a carrier, can form a stable colloidal solution after being dissolved in water, undergo a cross-linking reaction with a cross-linking agent, form the skeleton structure of the microspheres, and then form a film to coat the virgin mycin A and osthole, achieving a sustained release effect. At the same time, sodium alginate has a strong adhesion force, which can promote virgin mycin A and osthole to firmly adhere to the surface of crops, improving the sustained release and adhesion properties of pesticide preparations. The carboxyl group of sodium alginate can have an intermolecular force with the amino group of chitosan, which can enhance the density of the sustained release microspheres, reduce the penetration of external impurities into the interior of the sustained release microspheres, and improve the strength and stability of the sustained release microspheres.

[0016] Preferably, the cross-linking agent is one of calcium chloride and glutaraldehyde.

[0017] In the second aspect, the present application provides a method for preparing a composite pesticide preparation of Jinggangmycin and osthole, using the following technical solution: A preparation method of a composite pesticide preparation of validamycin and osthole comprises the following specific steps: mixing validamycin, osthole, a dispersant, a phosphate stabilizer, a preservative, a thickener, propylene glycol and water, then adding castor oil polyoxyethylene ether and sodium lauryl sulfate and mixing evenly, standing, inspecting, packaging, testing and accepting, so as to prepare the composite pesticide preparation of validamycin and osthole.

[0018] By adopting the above technical scheme, the prepared composite pesticide preparation has a significant improvement in the scope and effect of crop prevention and control. Through the synergistic enhancement of Jinggangmycin A and osthole, the dosage of the pesticide preparation can be reduced, the occurrence of drug resistance can be reduced, and the durability of the prevention and control effect can be improved.

[0019] Preferably, the composite sustained-release microspheres of Jinggangmycin-osthole, a dispersant, a phosphate stabilizer, a preservative, a thickener, propylene glycol and water are mixed, and then castor oil polyoxyethylene ether and sodium lauryl sulfate are added and mixed, wet-grinded, sheared and dispersed, allowed to stand, inspected, packaged, tested and accepted to obtain a composite pesticide preparation of Jinggangmycin and osthole.

[0020] In summary, this application has the following beneficial effects: 1. Since the present application combines Jinggangmycin A and osthole, and adjusts the appropriate ratio between the two, the control effect of the composite pesticide preparation is improved. It is combined with sodium dodecyl sulfate, castor oil polyoxyethylene ether, and propylene glycol excipients to increase the coverage area and penetration capacity of the pesticide preparation, improve the uniformity and stability of the active ingredients in the pesticide preparation, and thus improve the stability and efficiency of the composite pesticide preparation.

[0021] 2. In the present application, Jinggangmycin A and osthole are prepared into Jinggangmycin-osthole composite sustained-release microspheres in advance, and the Jinggangmycin A and osthole are coated with sodium alginate-crosslinking agent-chitosan to achieve the sustained-release effect of the pesticide preparation, prolong the control effect of the pesticide preparation, and reduce the emergence of pest resistance. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 is the chromatogram of Jinggangmycin A in the sample of Example 1 of the present application; Figure 2 This is the chromatogram of osthole in the sample of Example 1 of the present application. DETAILED DESCRIPTION

[0023] The present application is further described in detail below with reference to the accompanying drawings and embodiments.

[0024] All raw materials in the examples are commercially available.

[0025] Jinggangmycin A was purchased from Tonglu Huifeng Biotechnology Co., Ltd., Zhejiang Province.

[0026] Osthole was purchased from Hubei Tianhui Biotechnology Co., Ltd. Example

[0027] Example 1 This embodiment provides a composite pesticide preparation of Jinggangmycin and osthole, comprising the following raw materials in weight ratio: Jinggangmycin A 11.8%, osthole 0.2%, castor oil polyoxyethylene ether 8.5%, sodium lauryl sulfate 0.5%, dispersant 0.4%, phosphate stabilizer 0.2%, preservative 0.2%, thickener 2%, propylene glycol 0.4%, water to 100%, wherein the dispersant is lignin sulfonate, the lignin sulfonate is sodium lignin sulfonate, the phosphate stabilizer is sodium tripolyphosphate, the preservative is sodium benzoate, and the thickener is magnesium aluminum silicate.

[0028] The preparation method of the composite pesticide preparation of Jinggangmycin and osthole comprises the following specific steps: The composite pesticide preparation of Jinggangmycin and osthole was prepared by mixing the mixture of Jinggangmycin, osthole, dispersant, phosphate stabilizer, preservative, thickener, propylene glycol and water, stirring at a speed of 100 r / min for 20 minutes, then adding castor oil polyoxyethylene ether and sodium lauryl sulfate, mixing, continuing to stir for 10 minutes, standing, inspecting, packaging, testing and accepting.

[0029] The composite pesticide preparation of Jinggangmycin and osthole prepared in this example was used as a sample, and the chromatogram of Jinggangmycin A and the chromatogram of osthole in the sample were determined by high performance liquid chromatography, referring to the standard of GB / T9553-1993 "Jinggangmycin Aqueous Solution".

[0030] Example 2 The difference between Example 2 and Example 1 is that the weight ratio of validamycin A in the raw materials of the validamycin and osthole composite pesticide preparation is 8%, the weight ratio of osthole is 0.3%, the weight ratio of castor oil polyoxyethylene ether is 7%, the weight ratio of sodium lauryl sulfate is 0.8%, the weight ratio of the dispersant is 0.3%, the weight ratio of the phosphate stabilizer is 0.3%, the weight ratio of the preservative is 0.1%, the weight ratio of the thickener is 3%, the weight ratio of propylene glycol is 0.3%, and the water is supplemented to 100%.

[0031] Example 3 The difference between Example 3 and Example 1 is that the weight ratio of validamycin A in the raw materials of the validamycin and osthole composite pesticide preparation is 15.6%, the weight ratio of osthole is 0.1%, the weight ratio of castor oil polyoxyethylene ether is 10%, the weight ratio of sodium lauryl sulfate is 0.3%, the weight ratio of the dispersant is 0.5%, the weight ratio of the phosphate stabilizer is 0.1%, the weight ratio of the preservative is 0.3%, the weight ratio of the thickener is 1%, the weight ratio of propylene glycol is 0.5%, and the water is supplemented to 100%.

[0032] Example 4 The difference between Example 4 and Example 1 is that the preservative in the raw material of the compound pesticide preparation of Jinggangmycin and osthole is kasone.

[0033] Example 5 The difference between Example 5 and Example 1 is that the phosphate stabilizer in the raw material of the composite pesticide preparation of Jinggangmycin and osthole is a mixture of sodium tripolyphosphate and sodium hexametaphosphate, and the mass ratio of sodium tripolyphosphate to sodium hexametaphosphate is 1:1.

[0034] Example 6 The difference between Example 6 and Example 5 is that in the composite pesticide preparation of validamycin and osthole, validamycin A and osthole are prepared in advance into validamycin-osthole composite sustained-release microspheres.

[0035] The preparation method of the composite pesticide preparation of Jinggangmycin and osthole comprises the following specific steps: S1: Sodium alginate is dissolved in hot water, and then validamycin A and osthole are added and stirred to form a mixed solution. The mixed solution is then dropped into a cross-linking agent aqueous solution and mixed for reaction for 2 hours. The cross-linking agent in the cross-linking agent aqueous solution has a mass fraction of 3%, and the cross-linking agent is calcium chloride. The microspheres are separated after filtration to form a microsphere semi-finished product. The microsphere semi-finished product is then added to a chitosan-acetic acid solution and mixed for reaction for 2 hours. The mass fraction of chitosan in the chitosan-acetic acid solution is 0.3%, and the mass ratio of chitosan: cross-linking agent: sodium alginate: validamycin A is 0.3:0.2:0.4:1. The microspheres are then separated by filtration, washed and dried to constant weight to obtain validamycin-osthole composite sustained-release microspheres.

[0036] S2: Mix the composite sustained-release microspheres of jinggangmycin-osthole, dispersant, phosphate stabilizer, preservative, thickener, propylene glycol and water, stir at a speed of 100 r / min for 20 min, then add castor oil polyoxyethylene ether and sodium dodecyl sulfate, mix, wet sand mill for 1 h, shear disperse at a speed of 1000 rpm for 10 min, let stand, inspect, package, test and accept, to obtain a composite pesticide preparation of jinggangmycin and osthole.

[0037] Example 7 The difference between Example 7 and Example 6 is that the cross-linking agent in the raw material for preparing the composite sustained-release microspheres of Jinggangmycin-osthole in the composite pesticide preparation of Jinggangmycin and osthole is glutaraldehyde.

[0038] Example 8 The difference between Example 8 and Example 6 is that chitosan is not used as a raw material for preparing the composite sustained-release microspheres of validamycin-osthole in the composite pesticide preparation of validamycin and osthole.

[0039] The preparation method of the composite pesticide preparation of Jinggangmycin and osthole comprises the following specific steps: S1: Sodium alginate is dissolved in hot water, and then jinggangmycin A and osthole are added, stirred evenly to form a mixed solution, and then the mixed solution is dropped into a cross-linking agent aqueous solution for mixing and reacting for 2 hours. The cross-linking agent in the cross-linking agent aqueous solution has a mass fraction of 3%, and the cross-linking agent is calcium chloride. The microspheres are separated after filtration, washed and dried to constant weight to obtain jinggangmycin-osthole composite sustained-release microspheres.

[0040] S2: Mix the composite sustained-release microspheres of jinggangmycin-osthole, dispersant, phosphate stabilizer, preservative, thickener, propylene glycol and water, stir at a speed of 100 r / min for 20 min, then add castor oil polyoxyethylene ether and sodium dodecyl sulfate, mix, wet sand mill for 1 h, shear disperse at a speed of 1000 rpm for 10 min, let stand, inspect, package, test and accept, to obtain a composite pesticide preparation of jinggangmycin and osthole.

[0041] Comparative Example Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that no phosphate stabilizer is used in the raw materials of the compound pesticide preparation of Jinggangmycin and osthole.

[0042] Comparative Example 2 The difference between Comparative Example 2 and Example 1 is that the weight ratio of osthole in the raw material of the composite pesticide preparation of validamycin and osthole is 3%.

[0043] Performance testing According to the composite pesticide preparation of Jinggangmycin and osthole provided in Examples 1-8 and Comparative Examples 1-2 of the present application, the following performance tests were performed, and the specific test results are shown in Table 1.

[0044] Detection Methods 1. Field trials for the prevention and control of rice false smut The experimental field is a land heavily planted with rice for many years, and the incidence of rice false smut has been serious over the years. The incidence was investigated and field efficacy tests were conducted. The experimental field was divided into 18 plots, each with an area of ​​20m2. The pesticide was applied after closing the rows at the early stage of rice sheath blight, i.e., the peak period of rice tillering. The base of the rice stem should be sprayed wet when the pesticide was applied, and the rice field should be kept with water. 55 grams of the composite pesticide preparation of Jinggangmycin and osthole prepared by this application was used per mu, and water was added and sprayed evenly. Clean water was used in the control area. The second spraying was carried out 7 days after the first spraying. The investigation of the prevention effect was carried out 14 days after the second application of the pesticide. The investigation method was to sample at five points in each plot, investigate 10 clusters at each point, and a total of 50 clusters were investigated. The total number of ears and the number of diseased ears were recorded, and they were graded according to the grading standards to calculate the disease index and the prevention and control effect.

[0045] Rice false smut classification standards: Level 0: no disease; Level 1: There is one diseased kernel per ear; Level 2: 2-4 diseased kernels per ear; Level 3: 5-7 diseased kernels per ear; Level 4: There are 8-10 diseased kernels per ear.

[0046] Level 5: There are more than 10 diseased grains in each ear.

[0047] Disease index (%) = Σ(disease level*number of diseased ears at each level)*100% ÷ (number of investigated ears*highest disease level).

[0048] Control effect (%) = (disease index of control area - disease index of treated area) * 100% ÷ (disease index of control area).

[0049] Table 1: Performance test results data table Example Disease index (%) Control effect (%) Example 1 2.91 81.37 Example 2 3.05 80.95 Example 3 2.95 81.23 Example 4 3.06 80.71 Example 5 2.84 82.05 Example 6 2.51 83.12 Example 7 2.56 83.09 Example 8 2.67 83.01 Comparative Example 1 5.61 75.46 Comparative Example 2 11.2 65.85 Based on the performance test results and Figure 1 , Figure 2 It can be seen that the composite pesticide preparation of Jinggangmycin and osthole prepared in the present application is compounded by Jinggangmycin A and osthole, which improves the stability and efficiency of the composite pesticide preparation and improves the control effect of the pesticide preparation.

[0050] It can be seen from Examples 6-8 that preparing the composite sustained-release microspheres of jinggangmycin A and osthole in advance can help the pesticide formulation to achieve a sustained-release effect, thereby prolonging the control effect of the pesticide. By comparing Example 6 with Example 8, it can be seen that Example 8 does not use chitosan, and the control effect of the pesticide formulation is reduced, further illustrating that the intermolecular force between sodium alginate and chitosan can enhance the compactness of the sustained-release microspheres, improve the strength and stability of the sustained-release microspheres, and thereby improve the durability and stability of the control effect of the pesticide formulation.

[0051] By comparing Comparative Examples 1-2 with Example 1, it can be seen that changing any component of the pesticide preparation of the present application, or changing the dosage ratio of Jinggangmycin A and osthole, will affect the control effect of the pesticide preparation and may also cause pests to develop drug resistance.

[0052] This specific embodiment is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make modifications to the present embodiment without any creative contribution as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.

Claims

1. A composite pesticide preparation of Jinggangmycin and osthole, characterized in that: The invention comprises the following raw materials in weight ratio: 8-15.6% of Jinggangmycin A, 0.1-0.3% of osthole, 7-10% of castor oil polyoxyethylene ether, 0.3-0.8% of sodium lauryl sulfate, 0.3-0.5% of dispersant, 0.1-0.3% of phosphate stabilizer, 0.1-0.3% of preservative, 1-3% of thickener, 0.3-0.5% of propylene glycol and the balance of water.

2. The composite pesticide preparation of Jinggangmycin and osthole according to claim 1, characterized in that: The dispersant is lignin sulfonate.

3. The composite pesticide preparation of Jinggangmycin and osthole according to claim 1, characterized in that: The preservative is one of sodium benzoate and kason.

4. The composite pesticide preparation of Jinggangmycin and osthole according to claim 1, characterized in that: The phosphate stabilizer is at least one of sodium tripolyphosphate and sodium hexametaphosphate.

5. The composite pesticide preparation of Jinggangmycin and osthole according to claim 1, characterized in that: The validamycin A and osthole are prepared in advance into validamycin-osthole composite sustained-release microspheres. The preparation method of the sustained-release microspheres comprises the following specific steps: Sodium alginate is dissolved in water, and then validamycin A and osthole are added and stirred evenly to form a mixed solution, and then the mixed solution is dropped into a cross-linking agent for mixing reaction, and microspheres are separated after suction filtration to form microsphere semi-finished products, and then the microsphere semi-finished products are added to chitosan for mixing reaction, and then the microspheres are separated by suction filtration, washed and dried to obtain validamycin-osthole composite sustained-release microspheres.

6. The composite pesticide preparation of Jinggangmycin and osthole according to claim 5, characterized in that: The mass ratio of chitosan: cross-linking agent: sodium alginate: validamycin A is (0.1-0.5): (0.1-0.3): (0.3-0.5):

1.

7. The composite pesticide preparation of Jinggangmycin and osthole according to claim 5, characterized in that: The cross-linking agent is one of calcium chloride and glutaraldehyde.

8. A method for preparing the composite pesticide preparation of Jinggangmycin and osthole according to any one of claims 1 to 7, characterized in that: The method comprises the following specific steps: mixing validamycin, osthole, dispersant, phosphate stabilizer, preservative, thickener, propylene glycol and water, then adding castor oil polyoxyethylene ether and sodium lauryl sulfate and mixing evenly, standing, inspecting, packaging, testing and accepting, so as to prepare the validamycin and osthole composite pesticide preparation.

9. The method for preparing the composite pesticide preparation of Jinggangmycin and osthole according to claim 8, characterized in that: The composite sustained-release microspheres of Jinggangmycin-osthole, a dispersant, a phosphate stabilizer, a preservative, a thickener, propylene glycol and water are mixed, and then castor oil polyoxyethylene ether and sodium lauryl sulfate are added and mixed, wet-grinded, sheared and dispersed, allowed to stand, inspected, packaged, tested and accepted to obtain a composite pesticide preparation of Jinggangmycin and osthole.

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