CN111616142A - Pesticide nano preparation and preparation method thereof - Google Patents
Pesticide nano preparation and preparation method thereof Download PDFInfo
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- CN111616142A CN111616142A CN202010524484.5A CN202010524484A CN111616142A CN 111616142 A CN111616142 A CN 111616142A CN 202010524484 A CN202010524484 A CN 202010524484A CN 111616142 A CN111616142 A CN 111616142A
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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
- A01N25/26—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 in coated particulate form
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- 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
- A01N25/08—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 solids as carriers or diluents
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- 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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- A—HUMAN NECESSITIES
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- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having no bond to a nitrogen atom
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- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/0666—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms
- C08G73/0672—Polycondensates containing five-membered rings, condensed with other rings, with nitrogen atoms as the only ring hetero atoms with only one nitrogen atom in the ring
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Abstract
The invention provides a pesticide nano preparation and a preparation method thereof, belonging to the technical field of pesticide preparations. The preparation method of the pesticide nano preparation provided by the invention comprises the following steps: dissolving a pesticide in an organic solvent, adding the obtained pesticide solution into water, and performing ultrasonic treatment to obtain a pesticide nanoparticle dispersion liquid; mixing the pesticide nanoparticle dispersion liquid, dopamine hydrochloride aqueous solution and Tris-HCl buffer solution to enable the pH value of the obtained mixed feed liquid to be 7.5-9.5, and then carrying out polymerization reaction to obtain a polymerization product system; and (3) dialyzing and drying the polymerization product system in sequence to obtain the pesticide nano preparation. According to the invention, dopamine hydrochloride in-situ polymerization is utilized to form a polydopamine shell on the surface of the pesticide nanoparticles, and the polydopamine shell can absorb light well, so that the polydopamine shell has a protection effect on the pesticide and avoids photolysis of the pesticide. Meanwhile, the method provided by the invention is simple and convenient to operate, low in cost, good in repeatability and environment-friendly.
Description
Technical Field
The invention relates to the technical field of pesticide preparations, in particular to a pesticide nano preparation and a preparation method thereof.
Background
Many pesticides are susceptible to photolysis, and lose activity due to photolysis in the use process, thereby causing waste and pollution. In the prior art, the preparation of the photolysis-resistant pesticide nano preparation usually comprises the steps of firstly preparing a nano carrier with a photolysis-resistant function and then loading a pesticide, so that the preparation process is complex, the cost is high, and pollution and waste are easily caused.
Disclosure of Invention
The invention aims to provide a pesticide nano preparation and a preparation method thereof, wherein dopamine hydrochloride in-situ polymerization is utilized to form a polydopamine shell on the surface of pesticide nano particles, and the polydopamine shell can absorb light well, has a protection effect on pesticides and avoids photolysis; meanwhile, the method provided by the invention is simple and convenient to operate and low in cost.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a pesticide nano preparation, which comprises the following steps:
dissolving a pesticide in an organic solvent, adding the obtained pesticide solution into water, and performing ultrasonic treatment to obtain a pesticide nanoparticle dispersion liquid;
mixing the pesticide nanoparticle dispersion liquid, dopamine hydrochloride aqueous solution and Tris-HCl buffer solution to enable the pH value of the obtained mixed feed liquid to be 7.5-9.5, and then carrying out polymerization reaction to obtain a polymerization product system;
and (3) dialyzing and drying the polymerization product system in sequence to obtain the pesticide nano preparation.
Preferably, the pesticide comprises at least one of abamectin, fipronil, prochloraz and phoxim, and the organic solvent is ethanol or methanol; the volume ratio of the organic solvent to the water in the pesticide nanoparticle dispersion liquid is (1-10): (90-99).
Preferably, the frequency of the ultrasound is 35-45 kHz, and the time is 15-25 s.
Preferably, the concentration of the pesticide in the pesticide nanoparticle dispersion liquid is 0.01-100 mg/mL; the concentration of the dopamine hydrochloride in the dopamine hydrochloride aqueous solution is 5-20 mg/mL; the volume ratio of the pesticide nanoparticle dispersion liquid to the dopamine hydrochloride aqueous solution is 100: (5-1).
Preferably, the polymerization reaction is carried out under the conditions of light shielding and room temperature, and the time of the polymerization reaction is 10-30 h.
Preferably, the method of dialysis comprises the steps of:
the polymerization product system is filled into a dialysis bag, and then the dialysis bag filled with the polymerization product system is placed in a saturated aqueous solution of the pesticide for dialysis.
Preferably, the molecular weight cut-off of the dialysis bag is 3500, and the dialysis time is 45-55 h.
Preferably, the drying is freeze drying, and the freeze drying time is 20-30 h.
The invention provides a pesticide nano preparation prepared by the preparation method of the technical scheme, which comprises pesticide nano particles and a polydopamine shell coated on the surfaces of the pesticide nano particles.
Preferably, the particle size of the pesticide nano preparation is 50-300 nm, and the thickness of the polydopamine shell is 10-80 nm.
The invention provides a preparation method of a pesticide nano preparation, which comprises the following steps: dissolving a pesticide in an organic solvent, adding the obtained pesticide solution into water, and performing ultrasonic treatment to obtain a pesticide nanoparticle dispersion liquid; mixing the pesticide nanoparticle dispersion liquid, dopamine hydrochloride aqueous solution and Tris-HCl buffer solution to enable the pH value of the obtained mixed feed liquid to be 7.5-9.5, and then carrying out polymerization reaction to obtain a polymerization product system; and (3) dialyzing and drying the polymerization product system in sequence to obtain the pesticide nano preparation. According to the invention, dopamine hydrochloride in-situ polymerization is utilized to form a polydopamine shell on the surface of pesticide nanoparticles, the polydopamine shell can absorb light well, the pesticide is protected and prevented from photolysis, and the pesticide can be slowly released through the polydopamine shell, so that the effect of slow release is achieved; and the surface of the pesticide is only provided with a polydopamine shell, so that the pesticide has good water dispersibility, good biocompatibility, no toxicity and no harm. Meanwhile, the method provided by the invention is simple and convenient to operate, low in cost, good in repeatability and environment-friendly.
Drawings
FIG. 1 is the particle size distribution of the nano-preparation of avermectin in water in example 1;
fig. 2 is a cumulative release curve of the avermectin nano-solution and the avermectin nano-formulation dispersion in example 1.
Detailed Description
The invention relates to a preparation method of a pesticide nano preparation, which comprises the following steps:
dissolving a pesticide in an organic solvent, adding the obtained pesticide solution into water, and performing ultrasonic treatment to obtain a pesticide nanoparticle dispersion liquid;
mixing the pesticide nanoparticle dispersion liquid, dopamine hydrochloride aqueous solution and Tris-HCl buffer solution to enable the pH value of the obtained mixed feed liquid to be 7.5-9.5, and then carrying out polymerization reaction to obtain a polymerization product system;
and (3) dialyzing and drying the polymerization product system in sequence to obtain the pesticide nano preparation.
The pesticide is dissolved in an organic solvent, and the obtained pesticide solution is added into water for ultrasonic treatment to obtain the pesticide nanoparticle dispersion liquid. In the present invention, the pesticide preferably includes at least one of abamectin, fipronil, prochloraz and phoxim, more preferably abamectin, fipronil, prochloraz or phoxim; the pesticides are easily decomposed by light, the polydopamine shell formed by dopamine hydrochloride in-situ polymerization is coated on the surface of the pesticide by adopting the method provided by the invention, the pesticide is protected and prevented from photolysis, and the pesticide can be slowly released through the polydopamine shell to achieve the effect of slow release. In the present invention, the organic solvent is preferably ethanol or methanol; in the embodiment of the present invention, anhydrous methanol or anhydrous ethanol is specifically used as an organic solvent to dissolve the pesticide.
In the invention, the volume ratio of the organic solvent to the water in the pesticide nanoparticle dispersion liquid is preferably (1-10): (90-99), more preferably (1-5): (95-99), and more preferably 2: 98. in the invention, the concentration of the pesticide in the pesticide nanoparticle dispersion liquid is preferably 0.01-100 mg/mL, more preferably 0.01-20 mg/mL, and further preferably 0.05-5 mg/mL; the concentration of the pesticide in the pesticide nanoparticle dispersion liquid is too high, and after subsequent polymerization reaction, nanoparticles in the system are easy to agglomerate and precipitate, so that the stability of the finally obtained pesticide nano preparation is poor.
The pesticide is dissolved in the organic solvent, preferably, the obtained pesticide solution is rapidly added into water for ultrasonic treatment, and the pesticide nanoparticles are molded through sudden change of the solvent environment to obtain the pesticide nanoparticle dispersion liquid; specifically, the ultrasonic treatment can be performed immediately after the pesticide solution is rapidly added into the water, or the pesticide solution can be directly and rapidly added into the water in an ultrasonic state. In the invention, the frequency of the ultrasonic wave is preferably 35-45 kHz, and more preferably 40 kHz; the time of the ultrasonic treatment is preferably 15-25 s, and more preferably 20 s. The invention preferably carries out ultrasonic treatment under the conditions, which is beneficial to ensuring that the pesticide nanoparticle dispersion liquid with uniform granularity and uniform dispersion is obtained.
After the pesticide nanoparticle dispersion liquid is obtained, the pesticide nanoparticle dispersion liquid, dopamine hydrochloride aqueous solution and Tris-HCl buffer solution are mixed to enable the pH value of the obtained mixed feed liquid to be 7.5-9.5, and then polymerization reaction is carried out to obtain a polymerization product system. In the invention, the concentration of the dopamine hydrochloride in the dopamine hydrochloride aqueous solution is preferably 5-20 mg/mL, and more preferably 5-10 mg/mL; the concentration of dopamine hydrochloride in the dopamine hydrochloride aqueous solution is too high, and after subsequent polymerization reaction, nano particles in the system are easy to agglomerate and precipitate, so that the stability of the finally obtained pesticide nano preparation is poor.
In the invention, the concentration of the Tris-HCl buffer solution is preferably 5-20 mg/mL, and more preferably 5-10 mg/mL. The polymerization reaction is carried out under the condition that the pH value is 7.5-9.5 (preferably 8.5), so that the full polymerization of dopamine is facilitated, and a stable polydopamine wrapping layer is further formed.
In the present invention, the volume ratio of the pesticide nanoparticle dispersion liquid to the dopamine hydrochloride aqueous solution is preferably 100: (5-1), more preferably 100: 1; the addition amount of the Tris-HCl buffer solution meets the requirement that the pH value of the system is higher than the above requirement, and preferably, the volume ratio of the Tris-HCl buffer solution to the dopamine hydrochloride aqueous solution is 1: 1.
in the present invention, the polymerization reaction is preferably carried out under ambient temperature conditions protected from light; the room temperature does not need to be heated or cooled additionally, and in the embodiment of the invention, the polymerization reaction is carried out at 25 ℃; the time of the polymerization reaction is preferably 10-30 h, and more preferably 24 h. The polymerization reaction is carried out under the condition of keeping out of the sun, which is favorable for preventing dopamine hydrochloride from being oxidized and ensuring the smooth proceeding of the polymerization reaction. In the invention, in the polymerization reaction process, dopamine hydrochloride is subjected to in-situ polymerization to form a polydopamine shell on the surface of the pesticide nanoparticles, the polydopamine shell can absorb light well, the pesticide is protected and prevented from photolysis, and the pesticide can be slowly released through the polydopamine shell to achieve the effect of slow and controlled release.
After the polymerization reaction is finished, the obtained polymerization product system is dialyzed and dried in sequence to obtain the pesticide nano preparation. In the present invention, the method of dialysis preferably comprises the steps of: the polymerization product system is filled into a dialysis bag, and then the dialysis bag filled with the polymerization product system is placed in a saturated aqueous solution of the pesticide for dialysis. In the present invention, the dialysis bag preferably has a molecular weight cut-off of 3500; the dialysis is preferably performed at room temperature, and the dialysis time is preferably 45-55 h, and more preferably 48 h.
After the dialysis is finished, the invention preferably dries the feed liquid in the dialysis bag to obtain the pesticide nano preparation; the drying is preferably freeze drying, and the freeze drying time is preferably 20-30 hours, and more preferably 24 hours.
The invention provides a pesticide nano preparation prepared by the preparation method in the scheme, which comprises pesticide nano particles and a polydopamine shell coated on the surfaces of the pesticide nano particles, wherein the particle size of the pesticide nano preparation is preferably 50-300 nm, and more preferably 50-100 nm; the thickness of the polydopamine shell is preferably 10-80 nm, and more preferably 10-40 nm.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Dissolving 5mg of abamectin in 2mL of absolute ethyl alcohol, quickly adding the obtained abamectin solution into 98mL of water, and carrying out ultrasonic treatment for 20s under the condition of 40kHz to obtain an abamectin nanoparticle dispersion liquid;
mixing 100mL of abamectin nanoparticle dispersion liquid, 1mL of dopamine hydrochloride aqueous solution (with the concentration of 10mg/mL) and 1mL of Tris-HCl buffer solution (with the concentration of 10mg/mL) to ensure that the pH value of the obtained system is 8.5, standing and reacting for 24 hours under the conditions of light shielding and room temperature (25 ℃), wherein the color of the system is changed into light grey black due to the wrapping of a polydopamine shell after the reaction; and (3) putting the system obtained after the reaction into a dialysis bag with the molecular weight cutoff of 3500, dialyzing in saturated aqueous solution of the abamectin for 2 days, and then freeze-drying the feed liquid in the dialysis bag for 24 hours to obtain the abamectin nano preparation.
The avermectin nanometer preparation prepared in the embodiment is dispersed in water, and the particle size distribution is measured, and the result is shown in fig. 1, and as can be seen from fig. 1, the average particle size of the avermectin nanometer preparation is 68 nm. Moreover, the abamectin nano preparation can be stably dispersed in water for 15 days (the abamectin concentration is 0.05mg/mL), and the abamectin nano particle dispersion liquid has obvious aggregation and precipitation after 15 days, which shows that the obtained abamectin nano preparation has good stability after the surface of the abamectin nano particle is coated with the poly dopamine shell.
And (3) testing the slow release effect: respectively filling 5mL of abamectin nano preparation aqueous dispersion (the concentration of abamectin is 0.05mg/mL, and the abamectin nano preparation is the abamectin nano preparation prepared in example 1) and 5mL of the abamectin nano particle dispersion into dialysis bags with the molecular weight cutoff of 3500, then putting the dialysis bags into beakers filled with 5000mL of dialysate (specifically water), stirring and dialyzing, taking 1mL of the dialysate from the beakers every 4 hours, and detecting the content of abamectin by using liquid chromatography to obtain cumulative release curves of the abamectin nano particle dispersion and the abamectin nano preparation aqueous dispersion, as shown in fig. 2. As can be seen from fig. 2, the accumulated release amount of abamectin not coated with the poly-dopamine shell reaches 78.2% of the initial total amount after dialysis for 24 hours, but the accumulated release amount of the abamectin nano preparation coated with the poly-dopamine shell is only 20.6% of the initial total amount after dialysis for 24 hours. This shows that the avermectin nano preparation provided by the invention has the effect of sustained and controlled release.
Example 2
The pesticide nano preparation is prepared according to the method of the example 1, except that the pesticide avermectin is replaced by fipronil, and the organic solvent for dissolving the fipronil is anhydrous methanol, so that the fipronil nano preparation is finally obtained.
Example 3
The pesticide nano preparation is prepared according to the method of the embodiment 1, except that the pesticide avermectin is replaced by the prochloraz, and the organic solvent for dissolving the prochloraz is the anhydrous methanol, so that the prochloraz nano preparation is finally obtained.
Example 4
The pesticide nano preparation is prepared according to the method of the embodiment 1, and the difference is that the pesticide avermectin is replaced by phoxim, and finally the phoxim nano preparation is obtained.
And (3) testing photolysis resistance: respectively weighing 30mg of the abamectin nano preparation prepared in the example 1 and 30mg of an abamectin original drug, respectively placing the abamectin nano preparation and the abamectin original drug under a 24W ultraviolet lamp for irradiating for 24 hours, and then sampling and analyzing the degradation rate of abamectin by liquid chromatography. The result shows that the degradation rate of the abamectin nano preparation is 6 percent, and the degradation rate of the abamectin original drug is 62 percent.
The concentrated solution nano-preparation prepared in examples 2 to 4 was subjected to photolysis resistance test according to the above method, and compared with the corresponding original pesticide, and the results show that after 24 hours of irradiation with a 24W ultraviolet lamp, the degradation rate of the fipronil nano-preparation prepared in example 2 was 7%, and the degradation rate of the fipronil original pesticide was 67%; the degradation rate of the prochloraz nanometer preparation prepared in the embodiment 3 is 8%, and the degradation rate of prochloraz technical is 58%; the degradation rate of the phoxim nano preparation prepared in example 4 was 9%, and the degradation rate of the phoxim technical was 53%.
According to the result of the photolysis resistance test, the pesticide nano preparation prepared by the method provided by the invention can obviously reduce the degradation rate of the pesticide.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The preparation method of the pesticide nano preparation is characterized by comprising the following steps:
dissolving a pesticide in an organic solvent, adding the obtained pesticide solution into water, and performing ultrasonic treatment to obtain a pesticide nanoparticle dispersion liquid;
mixing the pesticide nanoparticle dispersion liquid, dopamine hydrochloride aqueous solution and Tris-HCl buffer solution to enable the pH value of the obtained mixed feed liquid to be 7.5-9.5, and then carrying out polymerization reaction to obtain a polymerization product system;
and (3) dialyzing and drying the polymerization product system in sequence to obtain the pesticide nano preparation.
2. The preparation method according to claim 1, wherein the pesticide comprises at least one of abamectin, fipronil, prochloraz and phoxim, and the organic solvent is ethanol or methanol; the volume ratio of the organic solvent to the water in the pesticide nanoparticle dispersion liquid is (1-10): (90-99).
3. The method according to claim 2, wherein the ultrasonic wave has a frequency of 35 to 45kHz and a time of 15 to 25 seconds.
4. The preparation method according to any one of claims 1 to 3, wherein the concentration of the pesticide in the pesticide nanoparticle dispersion liquid is 0.01 to 100 mg/mL; the concentration of the dopamine hydrochloride in the dopamine hydrochloride aqueous solution is 5-20 mg/mL; the volume ratio of the pesticide nanoparticle dispersion liquid to the dopamine hydrochloride aqueous solution is 100: (5-1).
5. The preparation method according to claim 1, wherein the polymerization reaction is carried out under the conditions of light shielding and room temperature, and the polymerization reaction time is 10-30 h.
6. The method of preparation according to claim 1, characterized in that said method of dialysis comprises the following steps:
the polymerization product system is filled into a dialysis bag, and then the dialysis bag filled with the polymerization product system is placed in a saturated aqueous solution of the pesticide for dialysis.
7. The preparation method of claim 1, wherein the molecular weight cut-off of the dialysis bag is 3500, and the dialysis time is 45-55 h.
8. The preparation method according to claim 1, wherein the drying is freeze-drying, and the freeze-drying time is 20-30 hours.
9. The pesticide nano-preparation prepared by the preparation method of any one of claims 1 to 8, which is characterized by comprising pesticide nanoparticles and a polydopamine shell coated on the surfaces of the pesticide nanoparticles.
10. The nano pesticide preparation according to claim 9, wherein the nano pesticide preparation has a particle size of 50-300 nm, and the outer polydopamine shell has a thickness of 10-80 nm.
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CN114271267A (en) * | 2021-12-06 | 2022-04-05 | 盐城工学院 | Pesticide delivery system and preparation method thereof |
CN115517251A (en) * | 2022-09-13 | 2022-12-27 | 西南大学 | Chitosan encapsulated hexa-methyl mite acid nano acaricide and preparation method thereof |
CN115735938A (en) * | 2022-11-21 | 2023-03-07 | 广东省科学院微生物研究所(广东省微生物分析检测中心) | Dopamine-modified prochloraz polycaprolactone nanosphere and preparation method and application thereof |
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Address after: 510316, 10 pomegranate Road, Guangzhou, Guangdong Applicant after: Institute of bioengineering, Guangdong Academy of Sciences Address before: 510316, 10, pomegranate Road, Guangzhou, Guangdong, Haizhuqu District Applicant before: GUANGDONG PROVINCIAL BIOENGINEERING INSTITUTE (GUANGZHOU SUGARCANE INDUSTRY Research Institute) |
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