Pesticide composition containing trinexapac-ethyl and S-abscisic acid

Abstract

The invention discloses a pesticide composition containing trinexapac-ethyl and S-abscisic acid and a preparation method of the pesticide composition. 4.0%-6.0% of trinexapac-ethyl and 0.1%-0.5% of S-abscisic acid are used as main effective components, and a surfactant and liquid caustic soda are used as auxiliary components to prepare an aqueous solution; and further performing micro-fluidization nano-emulsification to prepare nano-emulsion particles with D90 of 50-150nm, embedding the nano-emulsion particles in a sodium alginate or chitosan matrix, and applying the nano-emulsion particles to foliar spraying or seed coating / root coating dual-mode administration. According to the technology, quick spraying effectiveness and early seed coating seedling protection are both considered, an obvious synergistic effect is achieved according to the proportion of 5: 5, and 90%-98% of the lodging prevention effect can be achieved within the effective component concentration range of 20-50 g / L. Residues can be degraded within 1-3 days, and the advantages of high efficiency, long acting and environmental protection are achieved.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of plant growth regulators and pesticide compositions, in particular to a nano-emulsion pesticide composition based on a mixture of trinexapac-ethyl and S-antimycin (natural plant hormone abscisic acid) and its preparation and application. BACKGROUND

[0002] Lodging is one of the main agronomic obstacles affecting grain quality and yield, especially in high-stalk crops such as wheat and rice, high temperature and rain or wind disturbance can easily cause lodging during the mature period. Existing agronomic measures and gibberellin inhibitors mostly rely on foliar spraying, which has the disadvantages of short persistence, incomplete absorption and insufficient stress resistance. Although abscisic acid and its analogues can enhance stem strength, the application of single component can easily cause growth inhibition or environmental residues.

[0003] Commercially available adjuvant formulations mainly focus on suspension or dispersion systems, and rarely consider seed stage prevention and seedling stage protection, which cannot achieve continuous anti-lodging throughout the whole growth period. At the same time, the particle size of traditional spray preparations is relatively large, and the penetration and adhesion are poor, which is difficult to meet the dual requirements of new type low dose and high efficiency and green degradation. In view of this, a compound preparation with rapid effect and early seedling protection function is urgently needed, which can not only inhibit gibberellin synthesis through foliar spraying, but also play a slow-release protection role in seed coating stage, so as to realize the comprehensive anti-lodging technology of low dose, long persistence and environmental degradation. SUMMARY

[0004] In view of the above problems, the present application provides a nano-emulsion pesticide composition containing trinexapac-ethyl and S-antimycin and its preparation method. The present application has the advantages of low dose, high efficiency, long-acting slow release, rapid degradation and green environmental protection, and is suitable for anti-lodging of crops such as wheat, rice and corn throughout the whole growth period.

[0005] In order to achieve the above purpose, the present application adopts the following technical scheme: A pesticide composition containing trinexapac-ethyl and S-antimycin, the pesticide composition is prepared from the following raw materials by weight: Trinexapac-ethyl 4.0-6.0 parts, S-antimycin 0.1-0.5 parts, surfactant 108 2.0-5.0 parts, liquid alkali 2.0-4.0 parts, natural polysaccharide matrix 0-20 parts, and deionized water to 100 parts; The composition is subjected to microfluidization treatment to form D 90 Nano-emulsion particles with a size of 50-150 nm.

[0006] Alternatively, the pesticide composition containing trinexapac-ethyl and S-antimycin, wherein the natural polysaccharide matrix is selected from one or more of sodium alginate, chitosan, gelatin and sodium carboxymethyl cellulose.

[0007] Optionally, the pesticide composition containing trinexapac-ethyl and S-elicitor, wherein the natural polysaccharide matrix is 0 parts, the composition is in the form of a foliar spray; the natural polysaccharide matrix is 5-20 parts, and the composition is in the form of a seed coating / root coating agent.

[0008] Optionally, the foliar spray of the pesticide composition containing trinexapac-ethyl and S-elicitor, the specific preparation steps are as follows: S1, dissolve trinexapac-ethyl, S-elicitor, surfactant 108 and liquid caustic in deionized water; S2, the obtained solution is treated by microfluidization emulsification to obtain D 90 nanolipid with a particle size of 50-150 nm; Optionally, the seed coating / root coating agent of the pesticide composition containing trinexapac-ethyl and S-elicitor, the specific preparation steps are as follows: S1, mix the nanolipid prepared in claim 3 with 5-20 parts of a natural polysaccharide matrix solution; S2, coat the mixed solution on the surface of the seed or root, and dry to obtain a coating layer with a thickness of 1-5 microns.

[0009] Optionally, the preparation method of the pesticide composition containing trinexapac-ethyl and S-elicitor, wherein the microfluidization treatment adopts a pressure of 100-200 MPa and circulates 2-5 times.

[0010] Optionally, the preparation method of the pesticide composition containing trinexapac-ethyl and S-elicitor, wherein the foliar spray is applied, and when the total effective ingredient concentration is 20-50 g / L, the anti-lodging effect can reach 90%-98%.

[0011] Optionally, the pesticide composition containing trinexapac-ethyl and S-elicitor is applied to prevent and treat lodging of wheat, rice, corn, lawn, tobacco and tomato crops.

[0012] The beneficial effects of the present application are: The nanolipid pesticide composition prepared by the present application has a high anti-lodging rate of 90%-98% when the ratio is 5:5 and the total effective ingredient is 20-50 g / L, realizing low-dose high-efficiency synergy; 90 ultra-fine particles with a particle size of 50-150 nm significantly improve the foliar and rhizosphere absorption rate; the seed coating / root coating agent based on the natural polysaccharide coating has long-acting and slow-release properties, and can continuously protect seedlings; after adding a photocatalytic degradation aid, the spray residue is rapidly degraded within 1-3 days, and has the advantages of green environmental protection and wide application. BRIEF DESCRIPTION OF DRAWINGS

[0013] The accompanying drawings are included to provide a further understanding of the application and are incorporated in and constitute a part of the specification, illustrate embodiments of the application and are used to explain the application, but are not to be considered limiting of the application.

[0014] Figure 1 A bar chart of the anti-lodging rate and yield of each sample in the present application in the field; Figure 2 A bar chart of the anti-lodging rate and yield of each sample in the present application in the field; Figure 3 A bar chart of the anti-lodging rate and yield of each sample in the present application in the field; Figure 4 A bar chart of the anti-lodging rate and yield of each sample in the present application in the field. DETAILED DESCRIPTION

[0015] The technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the embodiments of the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments of the present application. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application. EMBODIMENT

[0016] A pesticide composition containing trinexapac-ethyl and S-elicitor according to the present embodiment 1 is prepared from the following raw materials by weight: Trinexapac-ethyl 5.0 parts, S-elicitor 0.3 parts, surfactant 108 3.0 parts, liquid alkali 3.0 parts, natural polysaccharide matrix 0 parts, and deionized water to 100 parts; The specific preparation method is as follows: S1, dissolve trinexapac-ethyl, S-elicitor, surfactant 108 and liquid alkali in deionized water in sequence, and stir at a speed of 400 rpm for 15 min at room temperature; S2, pass the obtained homogeneous solution through a microfluidizer at a pressure of 100 MPa for 3 times to obtain D 90 of 100 nm; S3, dilute the nanoemulsion to a total effective ingredient of 40 g / L for foliar spraying. EMBODIMENT

[0017] A pesticide composition containing trinexapac-ethyl and S-elicitor according to the present embodiment 2 is prepared from the following raw materials by weight: Trinexapac-ethyl 5.0 parts, S-elicitor 0.3 parts, surfactant 108 3.0 parts, liquid alkali 3.0 parts, natural polysaccharide matrix 10 parts, and deionized water to 100 parts; The specific preparation method is as follows: S1, sequentially dissolve trinexapac-ethyl, S-antimycin, surfactant 108 and liquid alkali in deionized water, stir at room temperature at a speed of 400 rpm for 15 min; S2, the obtained homogeneous solution is treated by microfluidizer at a pressure of 100 MPa for 3 times to obtain D 90 The nanoemulsion particles are 100 nm in size; S3, mix the obtained nanoemulsion with a chitosan solution, stir at room temperature at a speed of 400 rpm for 10 min, and then ultrasonic for 8 min to eliminate bubbles to obtain a uniform solution; S4, coat the mixed solution on the surface of the seed to be coated, and dry to a coating layer thickness of 2 µm. Example

[0018] A pesticide composition containing trinexapac-ethyl and S-antimycin according to this example 3 is prepared from the following raw materials by weight: Trinexapac-ethyl 5.0 parts, S-antimycin 0.3 parts, surfactant 108 3.0 parts, liquid alkali 3.0 parts, natural polysaccharide matrix 20 parts, deionized water to 100 parts; The preparation method of the pesticide composition containing trinexapac-ethyl and S-antimycin in this example 3 is the same as that in example 2.

[0019] To explore the effect of microfluidization on performance, a pesticide composition containing trinexapac-ethyl and S-antimycin according to this comparative example 1 is prepared from the following raw materials by weight: Trinexapac-ethyl 5.0 parts, S-antimycin 0.3 parts, surfactant 108 3.0 parts, liquid alkali 3.0 parts, natural polysaccharide matrix 0 parts, deionized water to 100 parts; The specific preparation method is as follows: S1, sequentially dissolve trinexapac-ethyl, S-antimycin, surfactant 108 and liquid alkali in deionized water, stir at room temperature at a speed of 400 rpm for 15 min; S2, the obtained homogeneous solution is treated by microfluidizer at a pressure of 100 MPa for 3 times to obtain D 90 The nanoemulsion particles are 100 nm in size; S3, dilute the nanoemulsion to a total effective ingredient of 40 g / L for foliar spraying.

[0020] To explore the effect of S-antimycin on performance, a pesticide composition according to this comparative example 2 is prepared from the following raw materials by weight: Trinexapac-ethyl 5.0 parts, S-antimycin 0 parts, surfactant 108 3.0 parts, liquid alkali 3.0 parts, natural polysaccharide matrix 0 parts, deionized water to 100 parts; The specific preparation method is as follows: S1, sequentially dissolve trinexapac-ethyl, surfactant 108 and liquid alkali in deionized water, stir at room temperature at a speed of 400 rpm for 15 min; S2, the obtained homogeneous solution is treated by microfluidizer at a pressure of 100 MPa for 3 times to obtain D 90 nanoparticulate emulsion with a particle size of 120 nm; S3, dilute the nanoemulsion to a total active ingredient of 40 g / L for foliar spraying.

[0021] To explore the effect of trinexapac-ethyl on performance, a pesticide composition of the present comparative example 3 is prepared from the following raw materials by weight: trinexapac-ethyl 0 parts, S-antuxin 0.3 parts, surfactant 108 3.0 parts, liquid alkali 3.0 parts, natural polysaccharide matrix 0 parts, deionized water to 100 parts; The specific preparation method is as follows: S1, sequentially dissolve trinexapac-ethyl, surfactant 108 and liquid alkali in deionized water, stir at room temperature at a speed of 400 rpm for 15 min; S2, the obtained homogeneous solution is treated by microfluidizer at a pressure of 100 MPa for 3 times to obtain D 90 nanoparticulate emulsion with a particle size of 100 nm; S3, dilute the nanoemulsion to a total active ingredient of 40 g / L for foliar spraying.

[0022] 1, field anti-lodging test At the late jointing stage (Zadoks 32-34) of wheat, select crops with uniform growth, and arrange eight treatments in the field according to the randomized block test: example groups 1-3, comparative example groups 1-3, conventional gibberellin control group and untreated group, set three parallel plots for each treatment, with an area of 10 m 2 Dilute the corresponding composition or gibberellin inhibitor to a total active ingredient of 40 g / L, and use a manual backpack sprayer to spray the leaves at a volume of 500 L / ha and a pressure of 100 kPa, spray twice, spray again 7 days after the first application, and spray water for the untreated group. After 30 days of application, randomly select 5 1 m 2 sample areas in each area, count the number of lodging plants and total plants to calculate the anti-lodging rate, and simultaneously measure the average plant height (cm), stem diameter (mm) and yield at maturity (kg / ha); all data are statistically analyzed with P<0.05 as the significant level, and Duncan's multiple comparison method is used for statistical analysis.

[0023] Table 1, field anti-lodging and crop property test results of each sample The nanoemulsion compositions of Examples 1-3 are superior to conventional gibberellin and the untreated group in terms of preventing lodging, plant height, stem diameter, and yield, and the persistence and yield continue to increase with the increase of the amount of polysaccharide coating. The microfluidization and single-dose comparative examples verify that microfluidization and the 5:5 complex of the two active ingredients are the key to preventing lodging and increasing yield. In summary, the nanoemulsion and polysaccharide carrier integration technology of the present application realizes high-efficiency prevention of lodging and yield increase under low-dose conditions.

[0024] 2. Particle size distribution test After the microfluidization-prepared nanoemulsion is diluted with deionized water at a ratio of 1:100 (v / v), it is first ultrasonicated for 2 min to remove air bubbles; then, at an ambient temperature of 25°C, a dynamic light scattering particle size instrument (DLS, measurement angle 90°) is used to measure the sample, with each sample being measured continuously for 5 times, and each measurement lasting for 60 s; if the test result shows that the D 90 In the range of 50 nm-150 nm and with a standard deviation ≤10%, it is determined that the nanoemulsion preparation meets the requirements.

[0025] Table 2 Five D 90 Test data table (nm) Table 2 shows that Examples 1-3 all obtain ultrafine nanoemulsion with an average D 90 of 100 nm under the condition of microfluidization, while Comparative Example 2 and Comparative Example 3 can also achieve an average D 90 of 101 nm and 120 nm, but Comparative Example 1 has a D 90 of 605 nm, which is far beyond 100 nm. It can be seen that microfluidization emulsification is the key technology to realize nano particle size, and the formula composition has limited effect on particle size.

[0026] 3. Leaf surface absorption / transmittance test The microfluidized nanoemulsion is labeled with 0.1 mg of FITC (1 mL of nanoemulsion, room temperature, dark reaction for 2 h), and the free dye is removed by centrifugation at 12000 rpm for 10 min and the original volume is added with water; 6 wheat plants each at the jointing terminal stage (Zadoks 32-34) are selected, and 2 mL / plant (40 g / L) is uniformly sprayed on the 3rd unfolded leaf, and 3 leaf blades are taken at 0.5 h, 1 h, 3 h, 6 h, and 24 h, respectively, and the surface is washed with water for 30 s before cutting 50 µm thick sections; at 25°C, a confocal microscope (FITC excitation 488 nm, 40x water immersion objective, 1024x1024 pixels, 400 Hz scanning) is used to take fluorescence images of the epidermis and mesophyll layers, and the fluorescence intensity (FIU) is measured under the same exposure conditions using ImageJ, and the transmittance (mesophyll / epidermis x 100%) is calculated. If the transmittance at 6 h and 24 h is significantly improved (P<0.05) compared with the conventional suspension agent group, it is proved that the nanoemulsion significantly improves the leaf surface absorption and internal transfer efficiency.

[0027] Table 3 Leaf Penetration Test Results (%) The leaf penetration of Examples 1-3 were significantly higher than the control groups and GA control at all time points, with Example 1 increasing from 20% to 38% at 0.5-1 h, and reaching 80% at 24 h, while Control 1-3 and the untreated group were only 25% or below. Examples 2 and 3 had slightly lower penetration at the initial stage due to the polysaccharide coating, but still maintained 60-75% and 58-70% at 6 h and 24 h, proving that nanoemulsification combined with polysaccharide coating can achieve both rapid absorption and long-term penetration.

[0028] 4. Persistence Test At the late jointing stage (Zadoks 32-34) of wheat, eight treatments (Examples 1-3, Controls 1-3, GA control, and untreated) were arranged in randomized blocks in the field, with 3 plots of 10 m 2 Example 1, Controls 1-3, and the GA control were sprayed once (40 g / L, 500 L / ha, 100 kPa); Examples 2 and 3 were only coated on the seeds (2 or 5 pm coating layer), and no further application was made after sowing; the untreated group was sprayed with an equal amount of water. At 0, 3, 7, 14, and 21 d after application, 5 sample plots of 1 m 2 were randomly selected from each plot, and the number of lodging plants and total plants were counted to calculate the lodging prevention rate, and the stem diameter (mm) was measured. All data were analyzed using Duncan's multiple range test with a significance level of P<0.05 to comprehensively evaluate the sustained lodging prevention performance of different formulations and dosage forms at each time point.

[0029] Table 4 Persistence Test Results (%) The experimental results showed that the lodging prevention rates of Examples 1-3 remained the lowest during the 0-21 d period, while the lodging rates of Control 1 (without microfluidization), Controls 2 and 3 (single dosage forms), and the GA control group rapidly climbed from 15.8-60.2% to 30.1-70.5% during the same period. Therefore, nanoemulsification spraying combined with polysaccharide coating not only significantly outperformed conventional and single-component formulations, but also exhibited a more persistent lodging prevention effect.

[0030] 5. Residue Degradation Test After spraying in the field test area, 10 leaves of about 5 g in the same leaf layer were collected at random in each treatment plot at 1, 3, 5, 7 and 14 days after spraying, and soil samples of about 20 g at a depth of 0-5 cm were collected and placed in aluminum foil bags to be taken back to the laboratory; the leaf samples were extracted with 10 mL of acetonitrile: water (80:20, v / v) in a 200 rpm shaking box for 30 min, and then filtered to obtain the supernatant; the soil samples were first dried, sieved through a 40 mesh sieve, then extracted with 15 mL of acetonitrile: water (80:20, v / v) for 20 min, and then centrifuged at 12000 rpm for 10 min, and the supernatant was filtered through a 0.22 μm filter; The residual concentrations of mephenate and S-antibiotic were determined by high performance liquid chromatography (HPLC) analysis using a C18 column, 4.6x150mm, 5μm; the mobile phase was methanol: water at 70:30; the flow rate was 1.0 mL / min; the column temperature was 30℃; the detection wavelength was 220nm; the injection volume was 10μL, and the residual-time curve was drawn to evaluate the degradation rate and half-life.

[0031] Table 5 Leaf surface residual degradation test results of different samples at different times (mg / kg) The data in the table show that the leaf surface residues of Examples 1-3 are significantly lower than those of the comparative examples and the gibberellin control group at 1d, and decrease to about 1.0-1.2 mg / kg at 14d, while the comparative examples still retain 3.2-5.0 mg / kg. Examples 2 and 3, although the initial residues are slightly higher than the spray type, also show rapid degradation within 14d. It can be seen that the nano-emulsification combined with polysaccharide coating technology significantly improves the degradation rate of the active ingredient on the leaf surface, meeting the requirements of green and rapid degradation.

[0032] The above examples are only used to illustrate the technical solutions of the present application, but not to limit them; although the present application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that the technical solutions recorded in the foregoing examples can be modified, or some technical features can be replaced by equivalents; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. A pesticide composition containing anti-rot ester and S-inducer, characterized in that, The pesticide composition is prepared from the following raw materials in parts by weight: Anti-acid ester 4.0-6.0 parts, S-inducer 0.1-0.5 parts, surfactant 108 2.0-5.0 parts, liquid alkali 2.0-4.0 parts, natural polysaccharide matrix 0-20 parts, deionized water to make up to 100 parts; The composition is microfluidized to form D 90 It consists of nanoemulsion particles ranging from 50 to 150 nm.

2. The pesticide composition containing anti-rot ester and S-inducer according to claim 1, characterized in that, The natural polysaccharide matrix is ​​selected from one or more of sodium alginate, chitosan, gelatin, and sodium carboxymethyl cellulose.

3. The pesticide composition containing anti-rot ester and S-inducer according to claim 1, characterized in that, The natural polysaccharide matrix is ​​0 parts, and the composition is a foliar spray formulation; the natural polysaccharide matrix is ​​5-20 parts, and the composition is used as a seed coating / root coating formulation.

4. A foliar spray formulation of a pesticide composition containing anti-rot ester and S-inducer according to any one of claims 1-2, characterized in that, The specific preparation steps are as follows: S1. Dissolve the anti-rebound ester, S-inducer, surfactant 108 and liquid alkali in deionized water; S2. The obtained solution is subjected to microfluidic emulsification to obtain D. 90 Nanoemulsions of 50-150 nm.

5. A seed coating / root coating formulation of a pesticide composition containing anti-loosening ester and S-inducer according to any one of claims 1-2, characterized in that, The specific preparation steps are as follows: S1. Mix the nanoemulsion prepared according to claim 3 with 5-20 parts of natural polysaccharide matrix solution; S2. Apply the mixed solution to the surface of the seeds or roots, and after drying, the coating layer should be 1-5 µm thick.

6. The method for preparing a pesticide composition containing anti-rot ester and S-inducer according to claim 4, characterized in that, The microfluidization process is carried out at a pressure of 100-200 MPa for 2-5 cycles.

7. The pesticide composition containing anti-rot ester and S-inducer according to claim 3, characterized in that, When the foliar spray formulation is applied at a total effective ingredient concentration of 20-50 g / L, it can achieve a lodging prevention effect of 90%-98%.

8. The pesticide composition containing anti-lodging ester and S-inducer as described in claim 1, for use in controlling lodging in wheat, rice, corn, lawn, tobacco and tomato crops.

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