Insecticide for solanaceous vegetables and preparation method thereof

Abstract

The invention relates to the technical field of insecticides, in particular to an insecticide composition for solanaceous vegetables and a preparation method thereof.The insecticide composition is prepared from, by mass, 92-95 parts of composite emulsion, 3-5 parts of loaded particles and 0.5-1 part of synergist; the composite emulsion is prepared from sodium alginate, flurala sodium, guaiacol, solvent oil, alkyl glycoside and deionized water; the sodium alginate is obtained by mixing ultra-high molecular weight sodium alginate and low molecular weight sodium alginate in a mass ratio of 9: (1-1.5); the loaded particles are prepared from polysuccinimide, D-glutamic acid, fluralan, guaiacol and sodium dodecyl sulfate; the synergist is prepared from esterified starch, esterified chitosan, glycerol and 2-hydroxy-4 '-(2-hydroxyethoxy)-2-methyl propiophenone, and the synergist is prepared from the esterified starch, the esterified chitosan, the glycerol and the 2-hydroxy-4'-(2-hydroxyethoxy) Therefore, the pesticide composition disclosed by the invention has higher pesticide effect stability, longer lasting period and wider application prospect in areas with larger temperature difference in the morning and evening and dry environment.

Description

Technical Field

[0001] The present invention relates to the technical field of pesticides, in particular to a pesticide for solanaceous vegetables and a preparation method thereof. Background Art

[0002] Solanaceous vegetables refer to vegetables with berries as the edible part, mainly including tomatoes, eggplants, peppers, etc. Solanaceous vegetables are not only rich in vitamin C, vitamin E, carotene and other nutrients, and have antioxidant and immune-enhancing effects; they also contain minerals such as potassium and magnesium, which help maintain normal physiological functions of the human body; and they have diverse tastes and strong adaptability. Due to the special geographical environment of the Qinghai-Tibet Plateau, the Solanaceous vegetables grown in this area are not only more flavorful, but also have higher content of nutrients such as vitamins and minerals, and have higher nutritional value; at the same time, its special climate also allows the Solanaceous vegetables grown in this area to be put on the market in different seasons from Solanaceous vegetables grown in other areas.

[0003] However, due to the special geographical environment of the region, the large temperature difference between morning and evening makes the effect of the pesticides used in the planting process unsatisfactory. The pesticides disclosed in the prior art are mostly suitable for other regions, such as the patent technology document CN118476544B discloses a composite pesticide containing plant extracts and its preparation method; the invention discloses a composite pesticide containing plant extracts, and the composite pesticide contains the following raw material components in terms of mass percentage: 10%-15% of holly extract, 10%-15% of garlic extract, 20%-40% of synergist and 40%-50% of solvent. Although the composite pesticides prepared by these invention technologies have good preventive effects on plant mites, whiteflies, aphids and mosquitoes; however, the stability of the efficacy and the duration of the drug effect will be significantly reduced when used in areas with large temperature differences between morning and evening and dry environments.

[0004] Therefore, according to the above-mentioned related technologies, it is urgent to develop an insecticide for Solanaceae vegetables and a preparation method thereof. Summary of the invention

[0005] In view of this, the purpose of the present invention is to provide an insecticide for Solanaceae vegetables and a preparation method thereof, so as to solve the problem that the insecticide prepared by the prior art has poor efficacy stability and duration when used in areas with large temperature differences between morning and evening and dry environments.

[0006] Based on the above purpose, the present invention provides an insecticide for Solanaceae vegetables and a preparation method thereof.

[0007] An insecticide composition for solanaceous vegetables, comprising the following raw materials in parts by weight: 92-95 parts of a composite emulsion, 3-5 parts of loaded microparticles, and 0.5-1 part of a synergist;

[0008] The composite emulsion is prepared from sodium alginate, flurellana, guaiacol, solvent oil, alkyl glycoside and deionized water;

[0009] The sodium alginate is obtained by mixing ultra-high molecular weight sodium alginate and low molecular weight sodium alginate in a mass ratio of 9:1-1.5;

[0010] The number average molecular weight of the ultra-high molecular weight sodium alginate is 470641-511205;

[0011] The number average molecular weight of the low molecular weight sodium alginate is 157263-170620;

[0012] The loaded microparticles are prepared from polysuccinimide, D-glutamic acid, flurellana, guaiacol, and sodium dodecyl sulfate;

[0013] The particle size of the loaded microparticles is 200-350 nm;

[0014] The synergist is prepared from esterified starch, esterified chitosan, glycerol and 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone.

[0015] Preferably, the preparation method of the composite emulsion is as follows:

[0016] Step A1: adjusting the pH of the sodium alginate solution to 3.5-3.6, then adding octylamine, formaldehyde and cyclohexyl isocyanate, stirring for 24-25 hours, dialyzing with distilled water for 72-75 hours, and freeze-drying to obtain a surfactant;

[0017] Step A2: dissolving a surfactant in deionized water to obtain a surface dispersion;

[0018] Step A3: Flurellanine, guaiacol, solvent oil and alkyl glycoside are mixed, and then the surface dispersion liquid is added at a rotation speed of 20000-22000 rpm to obtain a composite emulsion.

[0019] Preferably, the dosage ratio of the sodium alginate solution, octylamine, formaldehyde and cyclohexyl isocyanate in step A1 is 100-200 mL: 0.36-0.72 g: 0.31-0.63 g: 0.43-0.87 g;

[0020] The surfactant and deionized water in step A2 are used in a ratio of 1.5-3 g: 500-1000 mL;

[0021] The usage ratio of flurellana, guaiacol, solvent oil, alkyl glycoside and surface dispersion in step A3 is 1-2 g: 0.05-0.1 g: 7-14 g: 2-4 g: 500-1000 mL.

[0022] Preferably, the concentration of the sodium alginate solution in step A1 is 2.5wt%-3wt%.

[0023] Preferably, the preparation method of the loaded microparticles is as follows:

[0024] Step B1: dissolving polysuccinimide in dimethyl sulfoxide to obtain an organic solution;

[0025] Step B2: Dissolve D-glutamic acid and sodium hydroxide in water, slowly add the organic solution while stirring, and react for 1-2 hours to obtain a mixed solution;

[0026] Step B3: adding the mixed solution dropwise into a citric acid buffer solution with a pH of 2.5-3, centrifuging at 11090-12000 rpm for 10-15 min, filtering, washing, and freeze-drying to obtain the nanocarrier;

[0027] Step B4: Flurellana, guaiacol and nanocarriers are dissolved in dimethyl sulfoxide, then added dropwise to an aqueous solution of sodium dodecyl sulfate, stirred for 90-100 minutes, and centrifuged at 11090-12000 rpm for 10-15 minutes, and then washed, freeze-dried and sieved to obtain loaded microparticles.

[0028] Preferably, the usage ratio of polysuccinimide and dimethyl sulfoxide in step B1 is 5.82-6 g: 40-45 mL;

[0029] The mass ratio of D-glutamic acid, sodium hydroxide, water and organic solution in step B2 is 0.88-1g: 0.48-0.54g: 60-70ml: 40-45mL;

[0030] The ratio of the mixed solution to the citric acid buffer in step B3 is 100-115 mL: 500-550 mL;

[0031] The usage ratio of flurellana, guaiacol, nanocarrier, dimethyl sulfoxide and sodium dodecyl sulfate aqueous solution in step B4 is 0.05-0.1 g: 0.01-0.03 g: 5 g: 30 mL: 50 mL.

[0032] Preferably, the concentration of the sodium dodecyl sulfate aqueous solution in step B4 is 0.25wt%-0.25wt%.

[0033] Preferably, the preparation method of the synergist is as follows:

[0034] Step C1: adding starch to distilled water and adjusting the pH to 8.8-9.1, then adding methacrylic anhydride and adjusting the pH to 8.0-9.0, continuing stirring until the pH drops to 6.7-7, removing the supernatant, dialyzing, drying, and passing through a 100-200 mesh sieve to obtain esterified starch;

[0035] Step C2: dissolving chitosan in a 55-60° C. glacial acetic acid solution, then adding a methacrylic anhydride solution, stirring for 6-7 hours, and then dialyzing, freeze-drying, and sieving to obtain esterified chitosan;

[0036] Step C3: adding esterified starch to deionized water, and gelatinizing at 85-90° C. for 30-40 min to obtain esterified starch paste;

[0037] Step C4: dissolving the esterified chitosan in a 55-60° C. glacial acetic acid solution, then adding the esterified starch paste and stirring for 30-40 minutes, then adding glycerol and 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone and continuing stirring for 30-40 minutes to obtain a synergist.

[0038] Preferably, the usage ratio of starch, distilled water and methacrylic anhydride in step C1 is 40-50 g: 100-150 mL: 4-5 g;

[0039] The starch is any one of corn starch, potato starch and wheat starch;

[0040] In step C2, the ratio of chitosan, glacial acetic acid solution and methacrylic anhydride solution is 2-3 g: 100-150 mL: 5.8-8.7 g;

[0041] In step C3, the ratio of deionized water to esterified starch is 20-30 mL: 25-30 g;

[0042] In step C4, the usage ratio of esterified chitosan, glacial acetic acid solution, esterified starch paste, glycerol, and 2-hydroxy-4'-(2-hydroxyethoxy)methylpropiophenone is 2.5-3 g: 20-30 mL: 40-55 g: 8.5-11.5 g: 0.85-1.15 g;

[0043] The concentration of the glacial acetic acid solution is 1%-1.5%.

[0044] A method for preparing an insecticide composition for Solanaceae vegetables, characterized in that the preparation method of the insecticide for Solanaceae vegetables is as follows:

[0045] The loaded microparticles and the synergist are added to the composite emulsion and mixed evenly to obtain the insecticide composition for solanaceous vegetables.

[0046] Beneficial effects of the present invention:

[0047] The invention provides an insecticide for solanaceous vegetables and a preparation method thereof. The invention effectively increases the thickness of the interface layer of the insecticide droplets by adjusting the concentration of the surfactant in the insecticide composition, thereby further significantly improving the stability of the insecticide solution; the surfactant and alkyl glycoside in a specific ratio are compounded to improve the wettability, adhesion and stability of the insecticide on the leaf surface; the loaded microparticles can transport flurellanine and guaiacol to plant tissues, thereby enhancing the insecticidal rate; the synergist in the invention can enable the insecticide composition to remain on the leaf surface for a long time after the water evaporates, thereby increasing the persistence and stability.

[0048] Therefore, compared with the prior art, the insecticide composition for Solanaceae vegetables prepared by the present invention has higher efficacy stability, lasting effect and broader application prospects in areas with large temperature difference between morning and evening and dry environment. DETAILED DESCRIPTION

[0049] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments.

[0050] The sources and properties of some of the raw materials used in the present invention are as follows:

[0051] Sodium alginate was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.; flurellanine was purchased from Shanghai Yuanye Biotechnology Co., Ltd.; guaiacol was purchased from Shanghai Yuanye Biotechnology Co., Ltd.; S-200 solvent oil was purchased from Jiangsu China Resources Chemical Co., Ltd., and alkyl glycoside was purchased from Wuhan Jiyesheng Chemical Co., Ltd.; polysuccinimide was purchased from Wuhan Huajiu Pharmaceutical Technology Co., Ltd.; D-glutamic acid was purchased from Shanghai Yuanye Biotechnology Co., Ltd.; sodium dodecyl sulfate was purchased from Shanghai Yuanye Biotechnology Co., Ltd.; corn starch was purchased from Shanghai Yuanye Biotechnology Co., Ltd.; potato starch was purchased from Shanghai Yuanye Biotechnology Co., Ltd.; wheat starch was purchased from Shanghai Yuanye Biotechnology Co., Ltd.; chitosan was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.; 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone was purchased from Shanghai Yuanye Biotechnology Co., Ltd.

[0052] Example 1: A method for preparing an insecticide composition for Solanaceae vegetables is as follows:

[0053] S1: 9 g of ultra-high molecular weight sodium alginate with a number average molecular weight of 470641 and 1 g of low molecular weight sodium alginate with a number average molecular weight of 157263 are mixed evenly to obtain sodium alginate;

[0054] S2: The pH of 100 mL of 2.5 wt% sodium alginate solution was adjusted to 3.5 with 0.5 mol / L HCl, and then 0.36 g of octylamine, 0.31 g of formaldehyde, and 0.43 g of cyclohexyl isocyanate were added, stirred for 24 h, dialyzed with distilled water for 72 h, and freeze-dried to obtain a surfactant;

[0055] S3: Dissolve 1.5 g of surfactant in 500 mL of deionized water to obtain a surface dispersion;

[0056] S4: 1 g of flurellana, 0.05 g of guaiacol, 7 g of solvent oil and 2 g of alkyl glycoside were mixed, and then 500 mL of the surface dispersion liquid was added at a rotation speed of 20,000 rpm to obtain a composite emulsion;

[0057] S5: dissolving 5.82 g of polysuccinimide in 40 mL of dimethyl sulfoxide to obtain an organic solution;

[0058] S6: Dissolve 0.88 g of D-glutamic acid and 0.48 g of sodium hydroxide in 60 ml of water, slowly add 40 mL of organic solution while stirring, and react for 1 h to obtain a mixed solution;

[0059] S7: 100 mL of the mixed solution was added dropwise into 500 mL of citric acid buffer at pH 2.5, and then centrifuged at 11090 rpm for 10 min, and then filtered, washed, and freeze-dried to obtain nanocarriers;

[0060] S8: 0.05 g of flurellana, 0.01 g of guaiacol and 5 g of nanocarrier were dissolved in 30 mL of dimethyl sulfoxide, and then added dropwise to 50 mL of 0.2 sodium dodecyl sulfate aqueous solution, stirred for 90 min, centrifuged at 11090 rpm for 10 min, and then washed, freeze-dried and sieved to obtain loaded microparticles with a particle size of 200-350 nm;

[0061] S9: 40 g corn starch was added to 100 mL distilled water, stirred at 20 rpm at room temperature, and a 3% NaOH solution was added dropwise to adjust the pH value to 8.8, then 4 g methacrylic anhydride was added and a 3% NaOH solution was added dropwise to adjust the pH value to 8.0, and stirring was continued until the pH value dropped to 6.7 to obtain an esterified starch suspension;

[0062] S10: The esterified starch suspension was allowed to stand for stratification, the upper clear liquid was removed, distilled water was added and the above operation was repeated twice, then 2 volumes of distilled water were added, the suspension was placed in a dialysis bag with a molecular weight of 12,000 and dialyzed in distilled water at 35° C. for 45 h, and after dialysis, excess water was removed, and the remaining water was then dried in an oven at 65° C. and passed through a 100-mesh sieve to obtain esterified starch;

[0063] S11: 2 g of chitosan was dissolved in 100 mL of 1% glacial acetic acid solution at 55°C, and then 5.8 g of methacrylic anhydride solution was slowly added and stirred for 6 h to obtain an esterified chitosan solution;

[0064] S12: The esterified chitosan solution is placed in a dialysis bag with a molecular weight of 12,000 and dialyzed at room temperature for 72 hours, during which the water is changed every 5 hours, and then freeze-dried and sieved to obtain esterified chitosan;

[0065] S13: adding 25 g of esterified starch into 20 mL of deionized water, and gelatinizing at 85° C. for 30 min to obtain esterified starch paste;

[0066] S14: 2.5 g of esterified chitosan powder was dissolved in 20 mL of 1% glacial acetic acid solution at 55° C., then 40 g of esterified starch paste was added and stirred for 30 min, and then 8.5 g of glycerol and 0.85 g of 2-hydroxy-4′-(2-hydroxyethoxy)-2-methylpropiophenone were added and stirred for 30 min to obtain a synergist;

[0067] S15: adding 3 g of loaded microparticles and 0.5 g of synergist to 92 g of the composite emulsion, and mixing them evenly to obtain an insecticide composition for solanaceous vegetables;

[0068] Example 2: A method for preparing an insecticide composition for Solanaceae vegetables is as follows:

[0069] S1: 9 g of ultra-high molecular weight sodium alginate with a number average molecular weight of 501007 and 1.25 g of low molecular weight sodium alginate with a number average molecular weight of 161633 are mixed evenly to obtain sodium alginate;

[0070] S2: The pH of 150 mL of 2.8 wt% sodium alginate solution was adjusted to 3.6 with 0.5 mol / L HCl, and then 0.52 g of octylamine, 0.53 g of formaldehyde, and 0.67 g of cyclohexyl isocyanate were added, stirred for 24.5 h, dialyzed with distilled water for 74 h, and freeze-dried to obtain a surfactant;

[0071] S3: Dissolve 2 g of surfactant in 700 mL of deionized water to obtain a surface dispersion;

[0072] S4: 1.5 g of flurellana, 0.08 g of guaiacol, 10 g of solvent oil and 3 g of alkyl glycoside were mixed, and then 8000 mL of the surface dispersion liquid was added at a rotation speed of 21000 rpm to obtain a composite emulsion;

[0073] S5: dissolving 5.9 g of polysuccinimide in 43 mL of dimethyl sulfoxide to obtain an organic solution;

[0074] S6: Dissolve 0.95 g of D-glutamic acid and 0.51 g of sodium hydroxide in 65 ml of water, slowly add 43 mL of organic solution while stirring, and react for 1.5 h to obtain a mixed solution;

[0075] S7: 110 mL of the mixed solution was added dropwise to 530 mL of citric acid buffer at pH 3, and then centrifuged at 11500 rpm for 13 min, and then filtered, washed, and freeze-dried to obtain the nanocarrier;

[0076] S8: 0.08 g of flurellana, 0.02 g of guaiacol and 5 g of nanocarrier were dissolved in 30 mL of dimethyl sulfoxide, and then added dropwise to 50 mL of 0.23 wt% sodium dodecyl sulfate aqueous solution, stirred for 95 min, centrifuged at 11500 rpm for 13 min, and then washed, freeze-dried and sieved to obtain loaded microparticles with a particle size of 200-350 nm;

[0077] S9: 45 g of potato starch was added to 125 mL of distilled water, stirred at 40 rpm at room temperature, and a 3% NaOH solution was added dropwise to adjust the pH value to 9, then 4.5 g of methacrylic anhydride was added and a 3% NaOH solution was added dropwise to adjust the pH value to 8.5, and stirring was continued until the pH value dropped to 6.9 to obtain an esterified starch suspension;

[0078] S10: The esterified starch suspension was allowed to stand for stratification, the upper clear liquid was removed, distilled water was added and the above operation was repeated twice, then 2 volumes of distilled water were added, the suspension was placed in a dialysis bag with a molecular weight of 12,000 and dialyzed in distilled water at 38° C. for 47 h, and after dialysis, excess water was removed, and the remaining water was then dried in an oven at 67° C. and passed through a 150-mesh sieve to obtain esterified starch;

[0079] S11: 2.5 g of chitosan was dissolved in 130 mL of 1.3% glacial acetic acid solution at 58° C., and then 7.5 g of methacrylic anhydride solution was slowly added and stirred for 6.5 h to obtain an esterified chitosan solution;

[0080] S12: The esterified chitosan solution is placed in a dialysis bag with a molecular weight of 12,000 and dialyzed at room temperature for 74 hours, during which the water is changed every 5.5 hours, and then freeze-dried and sieved to obtain esterified chitosan;

[0081] S13: adding 28 g of esterified starch into 25 mL of deionized water, and gelatinizing at 88° C. for 35 min to obtain esterified starch paste;

[0082] S14: 2.8 g of esterified chitosan powder was dissolved in 25 mL of 1.3% glacial acetic acid solution at 58° C., and then 50 g of esterified starch paste was added and stirred for 35 min, and then 10 g of glycerol and 1 g of 2-hydroxy-4′-(2-hydroxyethoxy)-2-methylpropiophenone were added and stirred for 35 min to obtain a synergist;

[0083] S15: adding 4 g of loaded microparticles and 0.8 g of synergist to 93 g of the composite emulsion, and mixing them evenly to obtain an insecticide composition for solanaceous vegetables;

[0084] Example 3: A method for preparing an insecticide composition for Solanaceae vegetables is as follows:

[0085] S1: 9 g of ultra-high molecular weight sodium alginate with a number average molecular weight of 511205 and 1.5 g of low molecular weight sodium alginate with a number average molecular weight of 170620 are mixed evenly to obtain sodium alginate;

[0086] S2: The pH of 200 mL of 3 wt% sodium alginate solution was adjusted to 3.6 with 0.5 mol / L HCl, and then 0.72 g of octylamine, 0.63 g of formaldehyde, and 0.87 g of cyclohexyl isocyanate were added, stirred for 25 h, dialyzed with distilled water for 75 h, and freeze-dried to obtain a surfactant;

[0087] S3: Dissolve 3 g of surfactant in 1000 mL of deionized water to obtain a surface dispersion;

[0088] S4: 2 g of flurellana, 0.1 g of guaiacol, 14 g of solvent oil and 4 g of alkyl glycoside were mixed, and then 1000 mL of the surface dispersion liquid was added at a rotation speed of 22000 rpm to obtain a composite emulsion;

[0089] S5: dissolving 6 g of polysuccinimide in 45 mL of dimethyl sulfoxide to obtain an organic solution;

[0090] S6: Dissolve 1 g of D-glutamic acid and 0.54 g of sodium hydroxide in 70 ml of water, slowly add 45 ml of organic solution while stirring, and react for 2 h to obtain a mixed solution;

[0091] S7: 115 mL of the mixed solution was added dropwise to 550 mL of citric acid buffer at pH 3, and then centrifuged at 12000 rpm for 15 min, and then filtered, washed, and freeze-dried to obtain the nanocarrier;

[0092] S8: 0.1 g of flurellana, 0.03 g of guaiacol and 5 g of nanocarrier were dissolved in 30 mL of dimethyl sulfoxide, and then added dropwise to 50 mL of 0.25 wt% sodium dodecyl sulfate aqueous solution, stirred for 100 min, centrifuged at 12000 rpm for 15 min, and then washed, freeze-dried and sieved to obtain loaded microparticles with a particle size of 200-350 nm;

[0093] S9: 50 g of wheat starch was added to 150 mL of distilled water, stirred at 50 rpm at room temperature, and a 3% NaOH solution was added dropwise to adjust the pH value to 9.1, then 5 g of methacrylic anhydride was added and a 3% NaOH solution was added dropwise to adjust the pH value to 9.0, and stirring was continued until the pH value dropped to 7 to obtain an esterified starch suspension;

[0094] S10: The esterified starch suspension was allowed to stand for stratification, the upper clear liquid was removed, distilled water was added and the above operation was repeated twice, then 2 volumes of distilled water were added, the suspension was placed in a dialysis bag with a molecular weight of 12,000 and dialyzed in distilled water at 40° C. for 48 h, and after dialysis, excess water was removed, and the remaining water was then dried in an oven at 70° C. and passed through a 200-mesh sieve to obtain esterified starch;

[0095] S11: 3 g of chitosan was dissolved in 150 mL of 1.5% glacial acetic acid solution at 60°C, and then 8.7 g of methacrylic anhydride solution was slowly added and stirred for 7 h to obtain an esterified chitosan solution;

[0096] S12: The esterified chitosan solution is placed in a dialysis bag with a molecular weight of 12,000 and dialyzed at room temperature for 75 hours, during which the water is changed every 6 hours, and then freeze-dried and sieved to obtain esterified chitosan;

[0097] S13: adding 30 g of esterified starch into 30 mL of deionized water, and gelatinizing at 90° C. for 40 min to obtain esterified starch paste;

[0098] S14: 3 g of esterified chitosan powder was dissolved in 30 mL of 1.5% glacial acetic acid solution at 60° C., then 55 g of esterified starch paste was added and stirred for 40 min, and then 11.5 g of glycerol and 1.15 g of 2-hydroxy-4′-(2-hydroxyethoxy)-2-methylpropiophenone were added and stirred for 40 min to obtain a synergist;

[0099] S15: adding 5 g of loaded microparticles and 1 g of synergist to 95 g of the composite emulsion, and mixing them evenly to obtain an insecticide composition for solanaceous vegetables;

[0100] Comparative Example 1:

[0101] Compared with Example 1, this comparative example only replaces the "1g low molecular weight sodium alginate" added in the sodium alginate mixing process with "1g ultra-high molecular weight sodium alginate", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally obtains an insecticide composition for solanaceous vegetables;

[0102] Comparative Example 2:

[0103] Compared with Example 1, this comparative example only replaces the "9g ultra-high molecular weight sodium alginate" added in the sodium alginate mixing process with "9g low molecular weight sodium alginate", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally obtains an insecticide composition for Solanaceae vegetables;

[0104] Comparative Example 3:

[0105] Compared with Example 1, this comparative example only replaces the "9g ultra-high molecular weight sodium alginate and 1g low molecular weight sodium alginate" added during the sodium alginate mixing process with "5g ultra-high molecular weight sodium alginate and 5g low molecular weight sodium alginate", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally obtains an insecticide composition for Solanaceae vegetables;

[0106] Comparative Example 4:

[0107] Compared with Example 1, this comparative example only replaces the "1.5 g surfactant" added in the preparation process of the surface dispersion with "1.5 g sodium alginate", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally obtains an insecticide composition for Solanaceae vegetables;

[0108] Comparative Example 5:

[0109] Compared with Example 1, this comparative example only replaces the "guaiacol" added in the preparation process of the composite emulsion with "flurana", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally obtains an insecticide composition for Solanaceae vegetables;

[0110] Comparative Example 6:

[0111] Compared with Example 1, this comparative example only replaces the "guaiacol" added in the preparation process of the loaded microparticles with "flurana", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally obtains an insecticide composition for Solanaceae vegetables;

[0112] Comparative Example 7:

[0113] Compared with Example 1, this comparative example does not add loaded microparticles during the preparation of the insecticide composition for Solanaceae vegetables, and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally obtains an insecticide composition for Solanaceae vegetables;

[0114] Comparative Example 8:

[0115] Compared with Example 1, this comparative example only replaces the "esterified starch paste" added in the preparation process of the synergist with "esterified chitosan", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally obtains an insecticide composition for solanaceous vegetables;

[0116] Comparative Example 9:

[0117] Compared with Example 1, this comparative example only replaces the "esterified chitosan" added in the preparation process of the synergist with "esterified starch paste", and the remaining steps and parameters are the same, which will not be repeated in this comparative example, and finally obtains an insecticide composition for Solanaceae vegetables;

[0118] Comparative Example 10:

[0119] Compared with Example 1, this comparative example does not add a synergist during the preparation of the insecticide composition for Solanaceous vegetables, and the remaining steps and parameters are the same, which will not be repeated in this comparative example. Finally, an insecticide composition for Solanaceous vegetables is obtained.

[0120] Performance Testing:

[0121] 100 mL of the insecticide composition for Solanaceous vegetables prepared in Examples 1 to 3 and Comparative Examples 1 to 10 were stirred evenly to obtain insecticide, and the performance of the obtained insecticide was tested:

[0122] Insecticidal stability test:

[0123] Refer to the test standard of NY / T1154.1-2006 "Guidelines for Indoor Bioassay Tests of Pesticides. Insecticides. Part 1: Contact Activity Test. Spot Method". When the room temperature is 25℃ and the air humidity is about 50%, use a brush to select a group of test insects between the ages of 3-4 and place them in a culture dish for use. The test insects in the culture dish are treated with drops one by one. For lepidopteran larvae, drop them on the pronotum of the insect body, and drop 0.5μL-1.0μL of insecticide per head; for aphids, whiteflies, etc., drop them on the abdomen of the insect body, and drop 0.02μL-0.1μL of insecticide per head. The test insects after the drop are transferred to normal conditions for breeding. And set 100mL of water without the agent as a control. Investigate the death of the test insects 24 hours after treatment, and record the total number of insects and the number of dead insects. The group of test insects includes 20 armyworms, 20 striped stem borers, 20 cotton bollworms, 20 aphids and 70 whiteflies. The insecticide rates (%) of the insecticide compositions for solanaceous vegetables of Examples 1 to 3 and Comparative Examples 1 to 10 after 1 day of placement and the insecticide rates (%) after 30 days of placement are measured according to this method; the test results are shown in Table 1;

[0124] Insecticide rate calculation formula:

[0125] Test of insecticidal activity at different temperatures:

[0126] Referring to the test standard of NY / T1154.1-2006 "Guidelines for Indoor Bioassay Tests of Pesticides. Insecticides. Part 1: Contact Activity Test. Spot Method", when the air humidity is about 50%, a group of test insects between the ages of 3-4 are selected with a brush and placed in a culture dish for use. The test insects in the culture dish are treated with drops one by one. Lepidoptera larvae are dripped on the pronotum of the insect body, and 0.5μL-1.0μL of insecticide is dripped on each head; aphids, whiteflies, etc. are dripped on the abdomen of the insect body, and 0.02μL-0.1μL of insecticide is dripped on each head. The test insects after dripping are transferred to normal conditions for breeding. A group of 100mL water without the agent is set as a control. The death of the test insects is investigated 24 hours after treatment, and the total number of insects and the number of dead insects are recorded. The group of test insects includes 20 armyworms, 20 striped stem borers, 20 cotton bollworms, 20 aphids and 70 whiteflies. According to this method, the insecticide compositions for Solanaceae vegetables prepared in Examples 1 to 3 and Comparative Examples 1 to 10 were respectively measured for insecticidal rates (%) at temperatures of 5°C and 50°C; the test results are shown in Table 1;

[0127] Insecticide rate calculation formula:

[0128] Test of insecticidal activity at different humidity:

[0129] Referring to the test standard of NY / T1154.1-2006 "Guidelines for Indoor Bioassay Tests of Pesticides. Insecticides. Part 1: Contact Activity Test. Spot Method", at room temperature of about 25°C, a group of test insects between the ages of 3-4 were selected with a brush and placed in a culture dish for use. The test insects in the culture dish were treated with drops one by one. Lepidoptera larvae were dropped on the pronotum of the insect body, and 0.5μL-1.0μL of insecticide was dropped on each head; aphids, whiteflies, etc. were dropped on the abdomen of the insect body, and 0.02μL-0.1μL of insecticide was dropped on each head. The test insects after the drops were transferred to normal conditions for breeding. A group of 100mL water without the agent was set as a control. The death of the test insects was investigated 24h after the treatment, and the total number of insects and the number of dead insects were recorded. The group of test insects included 20 sticky insects, 20 striped stem borers, 20 cotton bollworms, 20 aphids and 70 whiteflies. According to this method, the insecticide compositions for Solanaceae vegetables prepared in Examples 1 to 3 and Comparative Examples 1 to 10 were respectively measured for insecticidal rates (%) at humidity of 20% and 95%; the test results are shown in Table 1;

[0130] Insecticide rate calculation formula:

[0131] Determination of leaf retention:

[0132] Tomato leaves were cut into 1.5 cm x 1.5 cm small pieces, and the mass of the leaves was weighed and recorded as M1. The leaves were then immersed in the insecticide composition for Solanaceous vegetables prepared in Examples 1 to 3 and Comparative Examples 1 to 10 of the present invention for 15 seconds. The leaves were then taken out and hung vertically. When the solution no longer dripped, the mass of the leaves was weighed and recorded as M2; after continuing to hang for 30 days, the mass of the leaves was weighed and recorded as M3. The final average mass data was determined by three measurements. Finally, the retention amount of the insecticide composition on the surface of tomato leaves can be calculated according to the following formula. All tests were carried out at least 10 times. In the formula, M1 is the fresh weight of tomato leaves, M2 is the weight of tomato leaves after being soaked in the insecticide composition, and M3 is the weight of tomato leaves after being soaked in the insecticide composition and left to stand for 30 days. S represents the surface area of ​​tomato leaves, and Q represents the retention amount of the insecticide composition on the surface of tomato leaves; the measurement results are shown in Table 1;

[0133] The calculation formula of leaf retention is:

[0134] The calculation formula of leaf retention after 30 days is:

[0135] Table 1

[0136]

[0137]

[0138] Data Analysis:

[0139] As can be seen from Table 1, the insecticide composition for Solanaceae vegetables prepared by the present invention has more excellent insecticidal stability, high and low temperature resistance, dryness resistance, moisture resistance and leaf retention capacity, that is, the insecticide composition prepared by the present invention has strong environmental adaptability, strong insecticidal stability and strong insecticidal persistence;

[0140] This may be because, in the present invention, sodium alginate with a specific molecular weight is selected and compounded in a specific ratio, wherein ultra-high molecular weight sodium alginate can interact with the loaded particles after treatment, adsorb the loaded particles to increase the dispersibility of the loaded particles; low molecular weight sodium alginate can adjust the overall stability and fluidity of the composite emulsion after treatment, thereby maximizing the wetting ability and leaf adhesion ability of the insecticide composition on the leaf surface of Solanaceae vegetables; and adjusting the concentration of the surfactant in the insecticide composition effectively increases the thickness of the interface layer of the insecticide droplets, thereby further significantly improving the stability of the insecticide solution; the compounding of the surfactant and the alkyl glycoside in a specific ratio of the present invention effectively improves the wettability and adhesion of the insecticide on the leaf surface. The invention provides a novel method for preparing a novel compound of flurella and guaiacol, which can improve the effect and stability of the compound. The compound use of flurella and guaiacol can not only prevent the influence of whiteflies on plants, but also improve the antiviral ability of plants themselves. Compared with the use of the two alone, the compound use of a specific ratio can maximize the effects of various aspects. The invention uses amino acid-modified polysuccinimide to prepare loaded microparticles with a specific particle size to load flurella and guaiacol, which can effectively transport flurella and guaiacol to plant tissues, thereby enhancing the utilization rate of flurella and guaiacol. The synergist in the invention can gradually cross-link with the plant leaf surface and the insecticide in the composition under the irradiation of high altitude strong light, and can still stay on the leaf surface for a long time even after the water of the insecticide composition evaporates, thereby increasing the persistence and stability.

[0141] Those skilled in the art should understand that the discussion of any of the above embodiments is merely illustrative and is not intended to imply that the scope of the present invention is limited to these examples. Under the concept of the present invention, the technical features in the above embodiments or different embodiments may be combined, the steps may be implemented in any order, and there are many other variations of the different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity.

[0142] The present invention is intended to cover all such substitutions, modifications and variations that fall within the broad scope of the appended claims. Therefore, any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. An insecticide composition for Solanaceae vegetables, characterized in that: The method comprises the following raw materials in parts by weight: 92-95 parts of composite emulsion, 3-5 parts of loaded microparticles, and 0.5-1 parts of synergist; The composite emulsion is prepared from sodium alginate, flurellana, guaiacol, solvent oil, alkyl glycoside and deionized water; The sodium alginate is obtained by mixing ultra-high molecular weight sodium alginate and low molecular weight sodium alginate in a mass ratio of 9:1-1.5; The number average molecular weight of the ultra-high molecular weight sodium alginate is 470641-511205; The number average molecular weight of the low molecular weight sodium alginate is 157263-170620; The loaded microparticles are prepared from polysuccinimide, D-glutamic acid, flurellana, guaiacol, and sodium dodecyl sulfate; The particle size of the loaded microparticles is 200-350 nm; The synergist is prepared from esterified starch, esterified chitosan, glycerol and 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone.

2. The insecticide composition for Solanaceae vegetables according to claim 1, characterized in that: The preparation method of the composite emulsion is as follows: Step A1: adjusting the pH of the sodium alginate solution to 3.5-3.6, then adding octylamine, formaldehyde and cyclohexyl isocyanate, stirring for 24-25 hours, dialyzing with distilled water for 72-75 hours, and freeze-drying to obtain a surfactant; Step A2: dissolving a surfactant in deionized water to obtain a surface dispersion; Step A3: Flurellanine, guaiacol, solvent oil and alkyl glycoside are mixed, and then the surface dispersion liquid is added at a rotation speed of 20000-22000 rpm to obtain a composite emulsion.

3. The insecticide composition for Solanaceae vegetables according to claim 2, characterized in that: The usage ratio of the sodium alginate solution, octylamine, formaldehyde and cyclohexyl isocyanate in step A1 is 100-200 mL: 0.36-0.72 g: 0.31-0.63 g: 0.43-0.87 g; The surfactant and deionized water in step A2 are used in a ratio of 1.5-3 g: 500-1000 mL; The usage ratio of flurellana, guaiacol, solvent oil, alkyl glycoside and surface dispersion in step A3 is 1-2 g: 0.05-0.1 g: 7-14 g: 2-4 g: 500-1000 mL.

4. The insecticide composition for Solanaceae vegetables according to claim 2, characterized in that: The concentration of the sodium alginate solution in step A1 is 2.5wt%-3wt%.

5. The insecticide composition for Solanaceae vegetables according to claim 1, characterized in that: The preparation method of the loaded microparticles is as follows: Step B1: dissolving polysuccinimide in dimethyl sulfoxide to obtain an organic solution; Step B2: Dissolve D-glutamic acid and sodium hydroxide in water, slowly add the organic solution while stirring, and react for 1-2 hours to obtain a mixed solution; Step B3: adding the mixed solution dropwise to a citric acid buffer solution with a pH of 2.5-3, centrifuging at 11090-12000 rpm for 10-15 min, filtering, washing, and freeze-drying to obtain a nanocarrier; Step B4: Flurellana, guaiacol and nanocarriers are dissolved in dimethyl sulfoxide, then added dropwise to an aqueous solution of sodium dodecyl sulfate, stirred for 90-100 minutes, and centrifuged at 11090-12000 rpm for 10-15 minutes, and then washed, freeze-dried and sieved to obtain loaded microparticles.

6. The insecticide composition for Solanaceae vegetables according to claim 1, characterized in that: The usage ratio of polysuccinimide and dimethyl sulfoxide in step B1 is 5.82-6 g: 40-45 mL; The mass ratio of D-glutamic acid, sodium hydroxide, water and organic solution in step B2 is 0.88-1g: 0.48-0.54g: 60-70ml: 40-45mL; The ratio of the mixed solution to the citric acid buffer in step B3 is 100-115 mL: 500-550 mL; The usage ratio of flurellana, guaiacol, nanocarrier, dimethyl sulfoxide and sodium dodecyl sulfate aqueous solution in step B4 is 0.05-0.1 g: 0.01-0.03 g: 5 g: 30 mL: 50 mL.

7. The insecticide composition for Solanaceae vegetables according to claim 1, characterized in that: The concentration of the sodium dodecyl sulfate aqueous solution in step B4 is 0.25wt%-0.25wt%.

8. The insecticide composition for Solanaceae vegetables according to claim 1, characterized in that: The preparation method of the synergist is as follows: Step C1: adding starch to distilled water and adjusting the pH to 8.8-9.1, then adding methacrylic anhydride and adjusting the pH to 8.0-9.0, continuing stirring until the pH drops to 6.7-7, removing the supernatant, dialyzing, drying, and passing through a 100-200 mesh sieve to obtain esterified starch; Step C2: dissolving chitosan in a 55-60° C. glacial acetic acid solution, then adding a methacrylic anhydride solution, stirring for 6-7 hours, and then dialyzing, freeze-drying, and sieving to obtain esterified chitosan; Step C3: adding esterified starch to deionized water, and gelatinizing at 85-90° C. for 30-40 min to obtain esterified starch paste; Step C4: dissolving the esterified chitosan in a 55-60° C. glacial acetic acid solution, then adding the esterified starch paste and stirring for 30-40 minutes, then adding glycerol and 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone and continuing stirring for 30-40 minutes to obtain a synergist.

9. The insecticide composition for Solanaceae vegetables according to claim 1, characterized in that: The usage ratio of starch, distilled water and methacrylic anhydride in step C1 is 40-50 g: 100-150 mL: 4-5 g; The starch is any one of corn starch, potato starch and wheat starch; In step C2, the amount ratio of chitosan, glacial acetic acid solution and methacrylic anhydride solution is 2-3 g: 100-150 mL: 5.8-8.7 g; In step C3, the ratio of deionized water to esterified starch is 20-30 mL: 25-30 g; In step C4, the usage ratio of esterified chitosan, glacial acetic acid solution, esterified starch paste, glycerol, and 2-hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone is 2.5-3 g: 20-30 mL: 40-55 g: 8.5-11.5 g: 0.85-1.15 g; The concentration of the glacial acetic acid solution is 1%-1.5%.

10. A method for preparing the insecticide composition for Solanaceae vegetables according to any one of claims 1 to 9, characterized in that: The preparation method of the insecticide for solanaceous vegetables is as follows: The loaded microparticles and the synergist are added to the composite emulsion and mixed evenly to obtain the insecticide composition for solanaceous vegetables.

Images