CN113498782B - Emamectin benzoate nano preparation based on zein and preparation method thereof - Google Patents
Emamectin benzoate nano preparation based on zein and preparation method thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/22—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients stabilising the active ingredients
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- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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Abstract
The application provides a zein-based emamectin benzoate nano preparation and a preparation method thereof. The emamectin benzoate nano preparation based on zein comprises the following components in percentage by mass: 1-5 parts of emamectin benzoate; 1-5 parts of zein; 1-5 parts of phosphoric acid compounds; 40-50 parts of a solvent; 30-50 parts of water. The emamectin benzoate nano preparation based on the zein has small influence on the environment and high drug effect and utilization rate.
Description
Technical Field
The invention relates to the technical field of pesticides, and particularly relates to a zein-based emamectin benzoate nano preparation and a preparation method thereof.
Background
The methylamino abamectin benzoate has the advantages of good biological activity, easy degradation and no pollution, is currently used for controlling vegetable and grain pests, and can effectively control \40023, pests of the orders of homoptera, coleoptera and various vegetable root-knot nematodes. However, the emamectin benzoate is a novel high-efficiency semisynthetic antibiotic synthesized from a fermentation product, namely, abamectin B1, the melting point of the emamectin benzoate is 141-146 ℃, the solubility of the emamectin benzoate in water at 20 ℃ is 0.024g/L, the emamectin benzoate is insoluble in hexane, the emamectin benzoate is soluble in organic solvents such as methanol and dichloromethane, the emamectin benzoate is easy to decompose under ultraviolet light, and if the emamectin benzoate is exposed in the environment, the emamectin benzoate is influenced by environmental factors such as illumination, air and rainwater, so that the problems of poor drug effect, short drug effect and low utilization rate generally exist.
However, the use amount of organic solvents in the preparation process of general nano-preparations is large, the influence on the environment is large, and the preparation steps are complex and the cost is high.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the emamectin benzoate nano preparation based on the zein with small influence on the environment and the preparation method of the emamectin benzoate nano preparation based on the zein, which has simple preparation steps and low cost.
The purpose of the invention is realized by the following technical scheme:
a zein-based emamectin benzoate nano preparation comprises the following components in percentage by mass:
in one embodiment, the zein-based emamectin benzoate nano preparation further comprises 2-4 parts by mass of a dispersing agent.
In one embodiment, the dispersant is at least one of a phosphate dispersant, a polycarboxylate dispersant, an organophosphate dispersant, and a non-ionic surfactant dispersant.
In one embodiment, the solvent is at least one of an alcohol solvent, a ketone solvent, an amide solvent, an aromatic solvent and an environment-friendly solvent.
In one embodiment, the environmentally friendly solvent is at least one of SV-92, GREEN 21, and FMPC.
In one embodiment, the phosphoric acid-based compound is at least one of potassium tripolyphosphate, sodium tripolyphosphate, and phosphorus oxychloride.
A method for preparing a zein-based emamectin benzoate nano-preparation, which is used for preparing the zein-based emamectin benzoate nano-preparation in any one of the embodiments, wherein the method for preparing the zein-based emamectin benzoate nano-preparation comprises the following steps:
preparing a solvent and water to obtain a binary solution;
respectively placing zein, a phosphoric acid compound and emamectin benzoate into the binary solution for dissolving;
and (3) putting water into the binary solution after the dissolution treatment for nanocrystallization treatment to obtain the emamectin benzoate nano preparation based on the zein.
In one embodiment, the dissolving treatment of zein, the phosphoric acid compound and emamectin benzoate in the binary solution respectively comprises the following steps:
placing the zein in the binary solution for first dissolution treatment;
and (3) placing the phosphoric acid compound and the emamectin benzoate into the binary solution for second dissolving treatment.
In one embodiment, the phosphoric acid compound and the emamectin benzoate are placed in the binary solution for second dissolution treatment under the condition that the rotating speed is 200 r/min-250 r/min.
In one embodiment, the binary solution contains 60 to 70 mass percent of solvent.
Compared with the prior art, the invention has at least the following advantages:
in the emamectin benzoate nano preparation based on zein, the zein is subjected to hydrophilic modification by adopting a phosphoric acid compound, so that the use amount of an organic solvent is reduced, the influence of the emamectin benzoate nano preparation on the environment is further reduced, the hydrophilicity and the electronegativity of the zein are improved, the stability and the biocompatibility of the emamectin benzoate are further improved when the modified emamectin benzoate is coated by adopting the modified zein, the emamectin benzoate is enabled to have stable bioactivity, crops are enabled to have better systemic property on the emamectin benzoate, the emamectin benzoate has better conductivity in the crops, and the pesticide effect and the utilization rate of the emamectin benzoate are further improved.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a reaction formula of the present invention using a phosphoric acid compound to modify zein;
fig. 2 is a flowchart of a method for preparing a zein-based emamectin benzoate nano-formulation in accordance with an embodiment of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only and do not represent the only embodiments.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The application provides a zein-based emamectin benzoate nano preparation. The emamectin benzoate nano preparation based on zein comprises the following components in percentage by mass: 1-5 parts of emamectin benzoate; 1-5 parts of zein; 1-5 parts of phosphoric acid compounds; 40-50 parts of a solvent; 30-50 parts of water.
In the emamectin benzoate nano preparation based on zein, the zein is subjected to hydrophilic modification by adopting a phosphoric acid compound, the use amount of an organic solvent is reduced, the influence of the emamectin benzoate nano preparation on the environment is further reduced, the hydrophilicity and the electronegativity of the zein are improved, the stability and the biocompatibility of the emamectin benzoate are further improved when the modified zein is adopted to coat the emamectin benzoate, the emamectin benzoate is enabled to have more stable bioactivity, the crops are enabled to have better systemic property on the emamectin benzoate, the emamectin benzoate has better conductivity in the crops, and the pesticide effect and the utilization rate of the emamectin benzoate are further improved.
It should be noted that, zein contains about 225 amino acid residues, wherein more than 50% of zein is hydrophobic amino acid residues, specifically including leucine, proline and alanine with higher content, so the zein has stronger hydrophobicity, therefore, if zein is directly used for preparing the nano preparation of emamectin benzoate, zein is easy to agglomerate and is difficult to be uniformly coated on the periphery of the emamectin benzoate, and further the effect of improving the utilization rate and the drug effect of the emamectin benzoate is achieved, therefore, in order to improve the hydrophilicity and the electronegativity of the zein, the zein is modified by using the phosphate compound, because the phosphate compound is an inorganic compound, the use of an organic solvent in the emamectin benzoate nano preparation is reduced, the influence of the emamectin benzoate nano preparation on the environment is reduced, and the phosphate compound can be decomposed into a micro-organism to be beneficial to the growth of plants along with the emamectin benzoate entering into the plants or soil to be beneficial to the growth of the plants, and is further beneficial to the phosphate fertilizer modification of the zein by combining with the positive and negative charge of the zein, and the zein can be further improved by the property of the zein that the phosphate compound is more soluble in water, the nano preparation prepared by coating the emamectin benzoate with the zein modified by the phosphoric acid compound has better biocompatibility and higher stability, so that the emamectin benzoate has more stable bioactivity, the crops have better systemic property on the emamectin benzoate and better conductivity in the crops, and the drug effect and the utilization rate of the emamectin benzoate are effectively improved.
Please note that, please refer to fig. 1: according to the reaction formula of modifying the zein by using the phosphoric acid compound, the molecular weight of the phosphoric acid compound is smaller, so that when the phosphoric acid compound is used for carrying out hydrophilic modification on the zein, the combination resistance of the phosphoric acid compound and the zein is smaller, the combination of the zein and the phosphoric acid compound is facilitated, the combination rate of the phosphoric acid compound and the zein is improved, the hydrophilicity of the zein is further effectively improved, when the zein is coated by zein high protein, the encapsulation rate of the zein to the emamectin benzoate is higher, the particle size of the prepared emamectin benzoate nano preparation is smaller, and the prepared emamectin benzoate nano preparation is more stable.
In one embodiment, the zein-based emamectin benzoate nano preparation further comprises 2-4 parts by mass of a dispersing agent. It can be understood that, because zein has poor hydrophilicity and strong lipophilicity, in the process of dissolving zein, an organic solvent and water need to be used for compounding to form a mixed solution to dissolve the zein, and in the process of preparing the emamectin benzoate nano preparation, water needs to be further added into the mixed solution, so that in the process of adding water, the modified zein is coated on the periphery of the emamectin benzoate to form emamectin benzoate nano particles, but in the process of adding water, the emamectin benzoate nano particles are easily separated out, so that in order to reduce the separation of the emamectin benzoate nano particles based on zein, the use of water needs to be reduced, so that the content of the organic solvent in the emamectin benzoate nano preparation is increased, the influence of the emamectin benzoate nano preparation on the environment is large, therefore, in the emamectin benzoate nano preparation based on the zein, a dispersing agent is added to play a role in the zein benzoate nano preparation, the effect of the zein is increased, the influence of the emamectin benzoate nano preparation based on the content of the emamectin benzoate is reduced, and the emamectin benzoate nano preparation based on the content of the emamectin benzoate in the environment is increased, and the emamectin benzoate nano preparation based on the content of the emamectin benzoate nano preparation is reduced. Furthermore, the dispersant is added in an amount of 2-4 parts by mass, so that the effect of increasing the volume of the emamectin benzoate nanoparticles based on zein is effectively achieved, and if the usage amount of the dispersant is too small, the usage amount of an organic solvent cannot be reduced well; if the usage amount of the dispersing agent is too high, the content of organic matters in the emamectin benzoate nano preparation based on the zein is increased, and the effect of reducing the influence of the emamectin benzoate nano preparation based on the zein on the environment is difficult to achieve.
In one embodiment, the dispersant is at least one of a phosphate-based dispersant, a polycarboxylate-based dispersant, an organophosphate-based dispersant, and a nonionic surfactant-based dispersant. It can be understood that the phosphate dispersant, the polycarboxylate dispersant, the organic phosphate dispersant and the nonionic surfactant dispersant all have a good compatibilization effect on the emamectin benzoate nanoparticles, and can effectively improve the dispersion stability of the emamectin benzoate nanoparticles, thereby reducing the polymerization of the emamectin benzoate nanoparticles, reducing the particle size of the emamectin benzoate nanoparticles, and being beneficial to the absorption and utilization of the emamectin benzoate nanoparticles.
In one embodiment, the solvent is at least one of an alcohol solvent, a ketone solvent, an amide solvent, an aromatic solvent, and an environmentally friendly solvent. It can be understood that the zein has good solubility in an aqueous solution of at least one of alcohols, ketones, amides, aromatic hydrocarbons and environment-friendly solvents, the encapsulation rate of the zein is effectively improved, the content of the emamectin benzoate in the emamectin benzoate nano preparation based on the zein is further improved, the usage amount of the organic solvent is reduced, and the influence of the emamectin benzoate nano preparation based on the zein on the environment is further reduced.
In one embodiment, the alcoholic solvent is at least one of ethanol, isopropanol, ethylene glycol, and n-butanol. It can be understood that the solubility of zein in the aqueous solution of alcohol solvents ethanol, isopropanol, ethylene glycol and n-butanol is high, and the solubility of emamectin benzoate in the mixture of alcohol solvents ethanol, isopropanol, ethylene glycol and n-butanol is high, so that the solubility of zein and the content of emamectin benzoate are effectively ensured.
In one embodiment, the ketone solvent is at least one of acetone and cyclohexanone. It can be understood that the solubility of zein in the aqueous solution of the ketone solvents acetone and cyclohexanone is high, and the solubility of emamectin benzoate in the mixture of the ketone solvents acetone and cyclohexanone is high, so that the solubility of zein and the content of emamectin benzoate are effectively ensured.
In one embodiment, the amide solvent is dimethylformamide. It can be understood that the solubility of the zein in the aqueous solution of the amide solvent dimethylformamide is high, and the solubility of the emamectin benzoate in the mixture of the aqueous solution of the amide solvent dimethylformamide is high, so that the solubility of the zein and the content of the emamectin benzoate are effectively ensured.
In one embodiment, the aromatic hydrocarbon solvent is at least one of benzene, toluene, and xylene. It can be understood that the solubility of the zein in the aromatic solvent benzene, toluene and xylene aqueous solution is high, and the solubility of the emamectin benzoate in the mixture of the aromatic solvent benzene, toluene and xylene aqueous solution is high, so that the solubility of the zein and the content of the emamectin benzoate are effectively ensured.
In one embodiment, the environmentally friendly solvent is at least one of SV-92, GREEN 21, and FMPC. In addition, the SV-92 molecule composition comprises ether bonds and hydroxyl groups, has better solubility on zein and emamectin benzoate, and effectively ensures the solubility of the zein and the content of the emamectin benzoate. GREEN 21 is a mixture of an amide dispersant and an amide ester dispersant, the molecular composition of GREEN 21 comprises amide and ester groups, and the compound has good solubility for zein and emamectin benzoate, so that the solubility of the zein and the content of the emamectin benzoate are effectively ensured. FMPC is a mixture of morpholine derivatives and carbonic acid ester, has good miscibility with water, has good solubility to zein and emamectin benzoate, and effectively ensures the solubility of zein and the content of emamectin benzoate.
In one embodiment, the solvent is a mixed solvent of SV-92 and GREEN 21, so that the solubility of the zein is better improved, the solubility of the emamectin benzoate is better improved, the use amount of an organic solvent is reduced, and the encapsulation rate of the emamectin benzoate by the zein and the content of the emamectin benzoate are ensured.
In one embodiment, the mass ratio of SV-92 to GREEN 21 is 3 to 7. It is understood that SV-92: GREEN 21= 3-7, further reduces the use amount of organic solvent, and ensures the encapsulation rate of zein to emamectin benzoate and the content of the emamectin benzoate.
In one embodiment, the phosphoric acid-based compound is at least one of potassium tripolyphosphate, sodium tripolyphosphate, and phosphorus oxychloride. It can be understood that potassium tripolyphosphate, sodium tripolyphosphate and phosphorus oxychloride are all easily soluble in water, and can form electronegative phosphate radicals after being dissolved in water, and have positive and negative charge attraction with electropositive groups formed by zein dissolved in a solvent and water, so that the combination of zein and a phosphoric acid compound is effectively improved, the hydrophilic modification of zein is facilitated, and after the zein is modified by adopting a phosphoric acid compound, the zein contains phosphate radicals, so that the property of the zein is closer to that of a cell membrane, the biocompatibility of the zein is further improved, and the biocompatibility of the emamectin benzoate nano preparation is further improved.
In one embodiment, the phosphoric acid based compound is potassium tripolyphosphate. It can be understood that potassium tripolyphosphate forms potassium ions and phosphate ions after being dissolved in water, wherein phosphate is used for modifying zein, potassium ions are absorbed and utilized by plants to facilitate the growth of the potassium tripolyphosphate, the deposition of chemical substances in soil is reduced, and emamectin benzoate nano-preparations have a growth promoting effect on the plants.
It should be noted that, if the modifier is an organic substance, when the zein is modified by using the organic modifier, an excessive amount of the organic modifier needs to be provided to dissolve the zein, even if an organic solvent is additionally selected to dissolve the organic modifier and the zein, if the pesticide is coated by directly using the modified zein containing a large amount of the organic solvent to form the nano preparation, the content of the organic solvent in the zein-based pesticide nano preparation is greatly increased, the influence of the zein-based pesticide nano preparation on the environment is improved, if the modified zein containing a large amount of the organic solvent is used after removing the organic solvent, even if the pesticide is coated by using the modified zein containing no or a small amount of the organic solvent to form the nano preparation, the organic solvent in the zein-based pesticide nano preparation does not have a great influence on the environment, but the preparation difficulty of the zein-based pesticide nano preparation is increased, and the possibility that the utilization rate of the zein is reduced exists, thereby increasing the preparation steps of the zein-based pesticide nano preparation, and increasing the preparation cost of the zein-based pesticide nano preparation. Therefore, in the emamectin benzoate nano preparation based on zein, the zein is modified by adopting the phosphoric acid compound, the use problem of a solvent used for dissolving an organic modifier and the zein in the early stage is solved, a solvent system which is favorable for dissolving the modified zein and the emamectin benzoate is selected, the optimization of the use amount of the organic solvent is ensured, the use amount of the organic solvent is further controlled, and the preparation difficulty of the emamectin benzoate nano preparation based on the zein is reduced.
The application also provides a preparation method of the zein-based emamectin benzoate nano preparation, and the preparation method of the zein-based emamectin benzoate nano preparation is used for preparing the zein-based emamectin benzoate nano preparation in any embodiment. The preparation method of the emamectin benzoate nano preparation based on the zein comprises the following steps: preparing a solvent and water to obtain a binary solution; respectively placing zein, a phosphoric acid compound and emamectin benzoate into a binary solution for dissolving; and (3) putting water into the binary solution after the dissolution treatment for nanocrystallization treatment to obtain the emamectin benzoate nano preparation based on the zein.
In the preparation method of the emamectin benzoate nano preparation based on the zein, the solvent and water are prepared to obtain the binary solution, the zein is dissolved, the phosphoric acid compound and the emamectin benzoate are added into the binary solution at the same time after the zein is dissolved, the zein is modified, the whole stirring process is stirring and mixing the modified zein and the emamectin benzoate, the modified zein and the emamectin benzoate are quickly and uniformly mixed, the preparation efficiency of the emamectin benzoate nano preparation is improved, in addition, the zein, the phosphoric acid compound and the emamectin benzoate are placed into the binary solution for dissolving and modifying, the using amount of the organic solvent is reduced, the influence of the emamectin benzoate nano preparation on the environment is reduced, the preparation steps of the emamectin benzoate nano preparation are simplified, the preparation efficiency of the emamectin benzoate nano preparation is further improved, and the preparation cost of the emamectin benzoate nano preparation is reduced.
Referring to fig. 2, in order to better understand the preparation method of the zein-based emamectin benzoate nano-formulation of the present application, the following further explains the preparation method of the zein-based emamectin benzoate nano-formulation of the present application, and the preparation method of the zein-based emamectin benzoate nano-formulation of an embodiment includes the following steps:
s100, preparing the solvent and water to obtain a binary solution. It can be understood that the zein contains about 225 amino acid residues, wherein more than 50% of the zein is hydrophobic amino acid residues, and specifically includes leucine, proline and alanine with higher content, so the zein has stronger hydrophobicity and weaker hydrophilicity, and if the zein is to be dissolved, a solvent and water need to be mixed, so that the solubility of the zein is ensured.
S200, respectively placing the zein, the phosphoric acid compound and the emamectin benzoate into a binary solution for dissolving treatment. The preparation method can be understood that after the zein is dissolved, the phosphoric acid compound and the emamectin benzoate are added into the binary solution at the same time, so that the zein is favorably modified, the whole stirring process is stirring and mixing the modified zein and the emamectin benzoate, the modified zein and the emamectin benzoate are favorably and uniformly mixed, the preparation efficiency of the emamectin benzoate nano preparation is improved, in addition, the zein, the phosphoric acid compound and the emamectin benzoate are all placed into the binary solution for dissolving and modifying, the problem that the zein and the phosphoric acid compound are dissolved by adopting an organic solvent, the preparation method of the emamectin benzoate nano preparation is complicated due to the fact that the emamectin benzoate is dissolved by adopting the organic solvent, the preparation difficulty of the emamectin benzoate nano preparation is increased, the preparation efficiency of the emamectin benzoate nano preparation is reduced, the use amount of the organic solvent is increased, the influence of the emamectin benzoate nano preparation on the environment is increased, and the problem that the cost of the emamectin benzoate nano preparation is reduced is solved.
S300, placing water in the dissolved binary solution for nanocrystallization to obtain the emamectin benzoate nano preparation based on the zein. It can be understood that both the modified zein and the emamectin benzoate can be uniformly dissolved in the binary solution, and therefore, the modified zein is difficult to coat the periphery of the emamectin benzoate, and therefore, the solubility of the emamectin benzoate in the binary solution is reduced by adding water into the binary solution, so that the modified zein is coated on the periphery of the emamectin benzoate, and the preparation of the emamectin benzoate nano preparation is effectively realized.
In the preparation method of the emamectin benzoate nano preparation based on the zein, the solvent and water are prepared to obtain the binary solution, the zein is dissolved, after the zein is dissolved, the phosphoric acid compound and the emamectin benzoate are added into the binary solution at the same time, the zein is favorably modified, the whole stirring process is stirring and mixing the modified zein and the emamectin benzoate, the modified zein and the emamectin benzoate are favorably and uniformly mixed, the preparation efficiency of the emamectin benzoate nano preparation is improved, in addition, the zein, the phosphoric acid compound and the emamectin benzoate are placed into the binary solution for dissolving and modifying, the using amount of the organic solvent is reduced, the influence of the emamectin benzoate nano preparation on the environment is reduced, the preparation steps of the emamectin benzoate nano preparation are simplified, the preparation efficiency of the emamectin benzoate nano preparation is further improved, and the preparation cost of the emamectin benzoate nano preparation is reduced.
In one embodiment, the zein, the phosphoric acid compound and the emamectin benzoate are respectively placed in a binary solution for dissolving treatment, and the method comprises the following steps:
zein is placed in a binary solution for a first dissolution treatment. It can be understood that the zein has stronger hydrophobicity and weaker hydrophilicity, and if the phosphoric acid compound and the emamectin benzoate are added before the zein is not completely dissolved, the polarity of the binary solution can be changed, so that the solubility of the zein in the binary solution is reduced, further the zein cannot be effectively dissolved in the binary solution and is agglomerated, and further the encapsulation rate of the emamectin benzoate is influenced.
Further, placing the phosphoric acid compound and the emamectin benzoate into a binary solution for second dissolving treatment. The method has the advantages that after the zein is placed in the binary solution for first dissolving treatment, the phosphoric acid compound and the emamectin benzoate are placed in the binary solution for second dissolving treatment, so that the problem that the preparation method of the emamectin benzoate nano preparation is complicated due to the fact that an organic solvent is additionally needed to dissolve the emamectin benzoate is avoided, the preparation difficulty of the emamectin benzoate nano preparation is increased, the preparation efficiency of the emamectin benzoate nano preparation is reduced, the usage amount of the organic solvent is increased, the problem of influence of the emamectin benzoate nano preparation on the environment is increased, the whole stirring process is stirring and mixing of the modified zein and the emamectin benzoate, the modified zein and the emamectin benzoate are favorably and uniformly mixed quickly, and the preparation efficiency of the emamectin benzoate nano preparation is further improved.
In one embodiment, the phosphoric acid compound and the emamectin benzoate are placed in a binary solution for second dissolution treatment under the condition that the rotating speed is 200 r/min-250 r/min, so that the hydrophilicity modification sufficiency of the zein is ensured, and the mixing uniformity of the zein and the emamectin benzoate is ensured.
In one embodiment, the solvent in the binary solution accounts for 60-70% by mass, so that the solubility of the zein and the content of the emamectin benzoate are effectively ensured.
In one embodiment, water and a dispersing agent are placed in a binary solution after dissolution treatment for nanocrystallization treatment, so that the emamectin benzoate nano preparation based on zein is obtained. It can be understood that, in the process of performing nanocrystallization treatment on water in a binary solution after dissolution treatment, in order to reduce precipitation of emamectin benzoate nanoparticles based on zein, water usage needs to be reduced, so that the content of an organic solvent in the emamectin benzoate nanoparticle preparation is increased, and the effect of the emamectin benzoate nanoparticle preparation on the environment is large, therefore, in the emamectin benzoate nanoparticle preparation based on zein, a dispersing agent is added to play a role in compatibilization on the zein, the content of water in the emamectin benzoate nanoparticle preparation based on the zein is increased, the content of the organic solvent in the emamectin benzoate nanoparticle preparation based on the zein is further reduced, and the effect of the emamectin benzoate nanoparticle preparation based on the zein on the environment is reduced.
Compared with the prior art, the invention has at least the following advantages:
in the emamectin benzoate nano preparation based on zein, the zein is subjected to hydrophilic modification by adopting a phosphoric acid compound, so that the use amount of an organic solvent is reduced, the influence of the emamectin benzoate nano preparation on the environment is further reduced, the hydrophilicity and the electronegativity of the zein are improved, the stability and the biocompatibility of the emamectin benzoate are further improved when the modified emamectin benzoate is coated by adopting the modified zein, the emamectin benzoate is enabled to have stable bioactivity, crops are enabled to have better systemic property on the emamectin benzoate, the emamectin benzoate has better conductivity in the crops, and the pesticide effect and the utilization rate of the emamectin benzoate are further improved.
Some specific examples are listed below, all of which are expressed in weight percent if any. It should be noted that the following examples are not intended to be exhaustive of all possible cases, and that the materials used in the following examples are commercially available without specific recitation.
Example 1
Preparing 50kg of SV-92 and 35kg of water to obtain a binary solution;
putting 1kg of zein into a binary solution for full dissolution;
under the condition that the rotating speed is 210r/min, 1kg of potassium tripolyphosphate and 1kg of emamectin benzoate are placed in a binary solution to be fully stirred and dissolved.
Putting 2kg of TRST (the main component is phosphate dispersant) into the binary solution, and adding the rest water (complementing to 100 kg) into the binary solvent to obtain the emamectin benzoate nano preparation based on the zein.
Example 2
40kg green 21 and 22.4kg water are prepared to obtain binary solution;
2kg of zein is put into a binary solution for full dissolution;
under the condition that the rotating speed is 220r/min, 1kg of sodium tripolyphosphate and 4kg of emamectin benzoate are placed in a binary solution to be fully stirred and dissolved.
Putting 2kg 100-LQ-TH (the main component is phosphate substances) into the binary solution, and adding the residual water (complementing to 100 kg) into the binary solution to obtain the zein-based emamectin benzoate nano preparation.
Example 3
Preparing 40kg of FMPC and 17kg of water to obtain a binary solution;
putting 3kg of zein into a binary solution for full dissolution;
under the condition that the rotating speed is 230r/min, 1kg of phosphorus oxychloride and 3kg of emamectin benzoate are placed in a binary solution to be fully stirred and dissolved.
Putting 4kg 601 (the main component is phenol derivative polyoxyethylene/polyoxypropylene ether) into the binary solution, and adding the rest water (complementing to 100 kg) into the binary solution to obtain the zein-based emamectin benzoate nano preparation.
Example 4
Preparing 40kg of acetone and 35kg of water to obtain a binary solution;
4kg of zein is placed in a binary solution for full dissolution;
under the condition that the rotating speed is 240r/min, 2.5kg of potassium tripolyphosphate and 1kg of emamectin benzoate are placed in a binary solution to be fully stirred and dissolved.
Placing 3kg 1601 (the main component is phenol derivative polyoxyethylene/polyoxypropylene ether) into the binary solution, and adding the residual water (to make up to 100 kg) into the binary solution to obtain the zein-based emamectin benzoate nano preparation.
Example 5
Preparing 37.5kg of SV-92, 12.5kg of green 21 and 35kg of water to obtain a binary solution;
placing 5kg of zein in a binary solution for full dissolution;
under the condition that the rotating speed is 250r/min, 2.5kg of potassium tripolyphosphate and 1kg of emamectin benzoate are placed in a binary solution to be fully stirred and dissolved.
Putting 2kg SG-LQ-MH (the main component is cetyl alcohol ether phosphate) into a binary solution, and adding the rest water (complementing to 100 kg) into the binary solution to obtain the emamectin benzoate nano preparation based on the zein.
Example 6
Preparing 41.5kg of SV-92, 8.5kg of green 21 and 35kg of water to obtain a binary solution;
placing 5kg of zein in a binary solution for full dissolution;
under the condition of the rotation speed of 200r/min, 2.5kg of potassium tripolyphosphate and 1kg of emamectin benzoate are placed in a binary solution to be fully stirred and dissolved.
Putting 2kg SG-LQ-MH (the main component is cetyl alcohol ether phosphate) into a binary solution, and adding the rest water (complementing to 100 kg) into the binary solution to obtain the emamectin benzoate nano preparation based on the zein.
Example 7
Preparing 44kg of SV-92, 6kg of green 21 and 35kg of water to obtain a binary solution;
placing 5kg of zein in a binary solution for full dissolution;
under the condition of the rotation speed of 200r/min, 2.5kg of potassium tripolyphosphate and 1kg of emamectin benzoate are placed in a binary solution to be fully stirred and dissolved.
Putting 2kg SG-LQ-MH (the main component is cetyl alcohol ether phosphate) into a binary solution, and adding the rest water (complementing to 100 kg) into the binary solution to obtain the emamectin benzoate nano preparation based on the zein.
Example 8
Preparing 45kg of SV-92 and 20kg of water to obtain a binary solution;
3kg of zein is placed in a binary solution for full dissolution;
under the condition that the rotating speed is 250r/min, 5kg of phosphorus oxychloride and 5kg of emamectin benzoate are placed in a binary solution to be fully stirred and dissolved.
2kg of SDS (the main component is sodium dodecyl benzene sulfonate) is placed into the binary solution, and the residual water (which is complemented to 100 kg) is added into the binary solution to obtain the emamectin benzoate nano preparation based on the zein.
Example 9
Preparing 50kg of SV-92 and 35kg of water to obtain a binary solution;
4kg of zein is placed in a binary solution for full dissolution;
and under the condition that the rotating speed is 200r/min, 5kg of potassium tripolyphosphate and 5kg of emamectin benzoate are placed in the binary solution to be fully stirred and dissolved.
2kg of SP-3645 (the main component is polycarboxylate substances) is put into the binary solution, and the residual water (the complement is 100 kg) is added into the binary solvent to obtain the zein-based emamectin benzoate nano preparation.
The performance tests of the emamectin benzoate nano-formulations of examples 1 to 9 prepared by the preparation method of the emamectin benzoate nano-formulation of the present application were performed as follows:
examples 1 to 9 are amounts of each substance added in an actual production process, and the data of examples 1 to 9 are converted into amounts of each substance added in a laboratory test, and specifically, examples 1 to 6 correspond to examples 10 to 18 one by one.
The amounts of the substances added in examples 10 to 18 are shown in Table 1:
table 1: the amounts of the respective substances of examples 10 to 18 added
The test results are shown in table 2:
table 2: various performances of methylamino abamectin benzoate nano preparation
As can be seen from tables 1 and 2, the emamectin benzoate nano-formulations prepared in examples 10 to 18 all have higher dispersion stability, smaller particle size and higher drug-loading rate, and especially the emamectin benzoate nano-formulations of examples 14 to 16 have smaller particle size and higher drug-loading rate; and it can be seen from tables 1 and 2 that the heat storage stability of the emamectin benzoate nano preparation is qualified, which indicates that the emamectin benzoate of the emamectin benzoate nano preparation obtained by the preparation method of the emamectin benzoate nano preparation has higher stability.
The conductivity of the emamectin benzoate nano-formulations prepared in examples 10 to 18 was tested as follows:
the detection method comprises the following steps: diluting the emamectin benzoate prepared in the examples 10 to 18 by using purified water respectively to obtain 100ppm emamectin benzoate samples prepared in the examples 10 to 18, carrying out water culture on pepper seedlings, and detecting the content of the emamectin benzoate in the leaf parts, the root parts and the stem parts of the pepper seedlings after 48 hours.
The results of the conductivity test of the emamectin benzoate nano-formulation are shown in table 3:
table 3: conductivity of methylamino abamectin benzoate nano preparation
From tables 1 and 3, it can be seen that all of examples 10 to 18 have better systemic properties, and especially, the emamectin benzoate nano-formulations prepared in examples 14 to 16 have better systemic properties, can better enter and conduct in plants, improve the drug effect of the emamectin benzoate nano-formulations, and are beneficial to the prevention and treatment of plant diseases and insect pests by the emamectin benzoate nano-formulations.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (5)
1. The emamectin benzoate nano preparation based on zein is characterized by comprising the following components in percentage by mass:
wherein, the solvent and water are prepared to obtain a binary solution for dissolving the zein, and the mass percentage of the solvent in the binary solution is 60-70%;
the solvent is a mixed solvent of SV-92 and GREEN 21, and the mass ratio of SV-92 to GREEN 21 is 3-7;
the dispersing agent is SG-LQ-MH;
the phosphoric acid compounds are potassium tripolyphosphate and phosphorus oxychloride;
the mass ratio of the zein, the phosphoric acid compound, the emamectin benzoate, the solvent, the dispersant and the water is 5:2.5:1:50:2:49.5.
2. a method for preparing a zein-based emamectin benzoate nano-formulation, which is used for preparing the zein-based emamectin benzoate nano-formulation of claim 1, wherein the method for preparing the zein-based emamectin benzoate nano-formulation comprises the following steps:
preparing a solvent and water to obtain a binary solution;
respectively placing zein, a phosphoric acid compound and emamectin benzoate into the binary solution for dissolving treatment;
and (3) putting water into the binary solution after the dissolution treatment for nanocrystallization treatment to obtain the emamectin benzoate nano preparation based on the zein.
3. The method for preparing a zein-based emamectin benzoate nano-formulation according to claim 2, wherein the zein, the phosphoric acid compound and the emamectin benzoate are respectively placed in the binary solution for dissolution treatment, comprising the following steps:
placing the zein in the binary solution for first dissolving treatment;
and (3) placing the phosphoric acid compound and the emamectin benzoate into the binary solution for second dissolving treatment.
4. The method for preparing a zein-based emamectin benzoate nano-formulation according to claim 2, characterized in that under the condition of a rotation speed of 200r/min to 250r/min, a phosphoric acid compound and emamectin benzoate are placed in the binary solution for a second dissolution treatment.
5. The method for preparing a zein-based emamectin benzoate nano formulation as claimed in any of claims 2 to 4, wherein the solvent content in said binary solution is 60-70% by weight.
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