CN114342930A - Pesticide nanocapsule and preparation method thereof - Google Patents
Pesticide nanocapsule and preparation method thereof Download PDFInfo
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Abstract
The invention provides a pesticide nanocapsule and a preparation method thereof, and belongs to the technical field of nano materials. The invention adopts the polylactic acid-glycolic acid copolymer as the capsule wall material, so that the prepared pesticide nanocapsule is nontoxic and has excellent biocompatibility; the preparation method comprises the steps of mixing a capsule wall material, an original pesticide and a hydrophobic organic solvent to obtain an oil phase, mixing the oil phase with a PVA aqueous solution, firstly stirring to preliminarily mix the oil phase with the PVA aqueous solution to form an oil-in-water system with large particle size, then inputting a large amount of energy through ultrasound, and further dispersing the oil phase into a water phase to form a uniform O/W emulsion; then diluting the mixed emulsion, preventing oil drops in the oil phase from colliding with each other in the ultrasonic process to polymerize so as to force the particle size of the pesticide nanocapsule to be increased, and further enabling the prepared pesticide nanocapsule to have a smaller particle size; in addition, the dilution process also promotes the stability of the emulsion, so that the pesticide nanocapsule has good encapsulation and film-forming properties.
Description
Technical Field
The invention relates to the technical field of nano materials, in particular to a pesticide nano capsule and a preparation method thereof.
Background
The pesticide plays an important role in preventing and controlling diseases and insect disasters and keeping grain yield, however, the excessive use of the pesticide not only influences the quality safety of agricultural products and the safety of ecological environment, but also increases the investment of agricultural production and the manual pesticide application cost. Therefore, the agricultural chemical reduction action is developed in each country in the world, and the principle and the way for improving the effective utilization rate of the agricultural chemical are researched. At present, commonly used pesticides such as tebuconazole, thifluzamide, azoxystrobin and the like are often processed into suspending agents for use. However, the particle size of the suspending agent particles is more than 1-30 microns, so the suspending agent particles are easy to fall off from plant leaves and run off in the using process, have poor penetrability and are not easy to be absorbed and run by plant bodies. The pesticide has the functions of targeted transmission and controlled release by using the novel pesticide formulation developed by using nano materials and technology, so that the effective utilization rate of the pesticide is improved.
The research of the nanotechnology in the aspects of research and development and application of pesticide formulations is rapidly advanced, and a new research field of 'nano pesticides' is formed. The dispersion size of the 'nano pesticide' is dozens to hundreds of times smaller than that of the traditional micron-sized pesticide particles, and the properties of absorption, transportation and the like of the 'nano pesticide' are greatly changed by surface modification. The pesticide in a nano-scale dispersion state has higher chemical activity and biological activity due to the large specific surface area of the nano-particles, more interface atoms and unsaturated atom coordination. Compared with the traditional pesticide formulation, the nanometer pesticide can improve the dispersibility of the pesticide, improve the deposition rate of the pesticide on the blades, avoid the off-target or loss of the pesticide caused by overlarge particles, and simultaneously improve the penetrability of the pesticide, thereby improving the absorption and transport performance of the pesticide in plants. However, the existing 'nano pesticide' technology has the technical problems of poor biocompatibility, toxicity, poor encapsulation and film-forming properties and the like. Therefore, a preparation method of pesticide nanocapsules with excellent biocompatibility, no toxicity, good encapsulation and film forming properties is needed.
Disclosure of Invention
The invention aims to provide a preparation method of a pesticide nanocapsule which has excellent biocompatibility, no toxicity and good encapsulation and film formation.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a pesticide nanocapsule, which comprises the following steps:
(1) mixing the capsule wall material, the original pesticide and the hydrophobic organic solvent to obtain an oil phase; the capsule wall material is polylactic acid-glycolic acid copolymer;
(2) mixing the oil phase obtained in the step (1) with a PVA (polyvinyl alcohol) aqueous solution, and then sequentially stirring and ultrasonically treating to obtain a mixed emulsion;
(3) diluting the mixed emulsion obtained in the step (2) to obtain a dispersed emulsion;
(4) and (4) carrying out solid-liquid separation on the dispersed emulsion obtained in the step (3) to obtain the pesticide nanocapsule.
Preferably, the hydrophobic organic solvent in step (1) is dichloromethane or ethyl acetate.
Preferably, the pesticide raw material in the step (1) comprises tebuconazole, thifluzamide or azoxystrobin.
Preferably, the mass ratio of the capsule wall material to the pesticide raw material in the step (1) is (10-40): 2-50.
Preferably, the volume concentration of the PVA aqueous solution in the step (2) is 0.1-5%.
Preferably, the mixing in the step (2) is dropwise adding the oil phase to the aqueous PVA solution.
Preferably, the dilution in the step (3) is 1-5 times.
Preferably, the reagent used for dilution in the step (3) is a PVA aqueous solution with the volume concentration of 0.005-0.02%.
Preferably, the solid-liquid separation in step (4) comprises removing the hydrophobic organic solvent and then removing water.
The invention also provides a pesticide nanocapsule prepared by the preparation method of the technical scheme, which comprises a capsule and a pesticide wrapped in the capsule, wherein the capsule is made of the polylactic-co-glycolic acid.
The invention provides a preparation method of a pesticide nanocapsule, which comprises the following steps: mixing a capsule wall material, a pesticide raw material and a hydrophobic organic solvent to obtain an oil phase, wherein the capsule wall material is a polylactic-co-glycolic acid; mixing the obtained oil phase with a PVA aqueous solution, and then sequentially stirring and ultrasonically treating to obtain a mixed emulsion; diluting the obtained mixed emulsion to obtain dispersed emulsion; and carrying out solid-liquid separation on the obtained dispersion emulsion to obtain the pesticide nanocapsule. The invention adopts the polylactic acid-glycolic acid copolymer as the capsule wall material, is nontoxic and has excellent biocompatibility, so that the prepared pesticide nanocapsule is nontoxic and has excellent biocompatibility; the preparation method comprises the steps of mixing a capsule wall material, an original pesticide and a hydrophobic organic solvent to obtain an oil phase, mixing the oil phase with a PVA aqueous solution, firstly stirring to preliminarily mix the oil phase with the PVA aqueous solution to form an oil-in-water system with large particle size, then inputting a large amount of energy through ultrasound, further dispersing the oil phase into a water phase to form a uniform O/W emulsion, namely a mixed emulsion; then diluting the mixed emulsion, preventing oil drops in the oil phase from colliding with each other in the ultrasonic process to polymerize so as to force the particle size of the pesticide nanocapsule to be increased, and further enabling the prepared pesticide nanocapsule to have a smaller particle size; in addition, the dilution process also promotes the stability of the emulsion, so that the pesticide nanocapsule has good encapsulation and film-forming properties. The data of the examples show that the pesticide nanocapsule prepared by the invention is nontoxic, has good capsule formation and film formation, the encapsulation rate can reach 70.58%, and the particle size can be as low as 358.34 nm.
Drawings
Fig. 1 is an SEM image of the pesticide nanocapsule prepared in example 1 of the present invention.
Detailed Description
The invention provides a preparation method of a pesticide nanocapsule, which comprises the following steps:
(1) mixing the capsule wall material, the original pesticide and the hydrophobic organic solvent to obtain an oil phase; the capsule wall material is polylactic acid-glycolic acid copolymer;
(2) mixing the oil phase obtained in the step (1) with a PVA (polyvinyl alcohol) aqueous solution, and then sequentially stirring and ultrasonically treating to obtain a mixed emulsion;
(3) diluting the mixed emulsion obtained in the step (2) to obtain a dispersed emulsion;
(4) and (4) carrying out solid-liquid separation on the dispersed emulsion obtained in the step (3) to obtain the pesticide nanocapsule.
The invention mixes the capsule wall material, the original pesticide and the hydrophobic organic solvent to obtain the oil phase. In the invention, the capsule wall material is polylactic-co-glycolic acid. In the present invention, unless otherwise specified, the reagents used in the present invention may be commercially available products well known to those skilled in the art.
In the invention, the polylactic-co-glycolic acid is nontoxic and has excellent biocompatibility, and the obtained pesticide nanocapsule is nontoxic and has excellent biocompatibility by using the polylactic-co-glycolic acid as a capsule wall material.
In the invention, the pesticide raw material preferably comprises tebuconazole, thifluzamide or azoxystrobin. In the invention, when the pesticide raw material is of the type, the pesticide nanocapsule prepared by the preparation method has high-efficiency bactericidal action.
In the invention, the mass ratio of the capsule wall material to the pesticide raw material is preferably (10-40): 2-50, and more preferably (20-30): 10-40. In the invention, when the mass ratio of the capsule wall material to the pesticide raw materials is in the range, the capsule wall material can fully wrap the pesticide raw materials, so that the pesticide nanocapsule has higher encapsulation efficiency.
In the present invention, the hydrophobic organic solvent is preferably dichloromethane or ethyl acetate, more preferably dichloromethane. In the present invention, when the hydrophobic organic solvent is of the above type, it has excellent solubility in the crude drug and the capsule wall material, and can sufficiently dissolve the crude drug and the capsule wall material.
The method for mixing the capsule wall material, the pesticide raw material and the hydrophobic organic solvent is not particularly limited, and the components can be uniformly mixed by adopting a mixing method well known by the technical personnel in the field. In the present invention, the method for mixing the capsule wall material, the technical pesticide and the hydrophobic organic solvent is preferably: firstly, mixing a capsule wall material with a hydrophobic organic solvent to obtain a capsule wall material solution, then mixing a pesticide raw drug with the hydrophobic organic solvent to obtain a pesticide raw drug solution, and then mixing the capsule wall material solution with the pesticide raw drug solution to obtain an oil phase.
In the invention, the concentration of the capsule wall material solution is preferably 10-40 mg/mL, and more preferably 20-30 mg/mL; the concentration of the original pesticide solution is preferably 2-50 mg/mL, and more preferably 10-40 mg/mL. In the present invention, when the method for mixing the capsule wall material, the technical pesticide and the hydrophobic organic solvent is within the above range, the above components can be sufficiently and uniformly mixed.
After the oil phase is obtained, the obtained oil phase is mixed with the PVA aqueous solution, and then stirring and ultrasonic treatment are carried out in sequence to obtain the mixed emulsion.
In the present invention, the volume concentration of the PVA aqueous solution is preferably 0.1 to 5%, more preferably 1 to 4%. In the present invention, the aqueous PVA solution is used as a dispersant and a stabilizer, and is used as a dispersant for dispersing an oil phase containing a wall material and a raw pesticide into an aqueous phase, and is used as an aqueous phase, and is capable of forming an O/W emulsion when mixed with the oil phase. In the present invention, when the volume concentration of the PVA aqueous solution is in the above range, it is more advantageous to obtain a uniformly dispersed mixed emulsion.
In the invention, when the concentration of the capsule wall material solution is 10-40 mg/mL, the concentration of the pesticide raw drug solution is 2-50 mg/mL, the volume ratio of the capsule wall material solution to the pesticide raw drug solution is 1:1, and the volume concentration of the PVA aqueous solution is 0.1-5%, the volume ratio of the oil phase to the PVA aqueous solution is preferably (2-16): 1, and more preferably (5-10): 1. In the present invention, when the volume ratio of the oil phase to the aqueous PVA solution is in the above range, it is more advantageous to form a mixed emulsion having a uniform distribution.
In the present invention, the oil phase is mixed with the aqueous PVA solution, preferably directly or by adding the oil phase dropwise to the aqueous PVA solution. In the present invention, the rate of the dropwise addition is preferably 0.03 to 0.05 mL/s. In the invention, the dropping addition can influence the particle size and the encapsulation rate of a final product, and when the dropping addition rate is in the range, the pesticide nanocapsule with uniform particle size and high encapsulation rate can be obtained. In the present invention, the mixing is preferably performed under mechanical stirring when the addition is dropwise. In the present invention, the mechanical stirring can prevent the dropwise added oil phase from agglomerating in the aqueous PVA solution, and can further facilitate the mixing of the dropwise added oil phase with the aqueous PVA solution. The mechanical stirring mode and speed are not specially limited, and the mechanical stirring speed can be adjusted according to experimental requirements.
In the present invention, the stirring can be performed by preliminarily mixing the system obtained by mixing the oil phase with the PVA aqueous solution to form a large-particle-size oil-in-water system. In the present invention, the stirring is preferably magnetic stirring. The speed of the magnetic stirring is not specially limited, and the speed can be adjusted according to the experimental requirements. In the invention, the time of the magnetic stirring is preferably 3-10 min.
In the present invention, the ultrasound can input a large amount of energy to further disperse the oil phase into the water phase to form a uniform O/W emulsion, i.e., a mixed emulsion. In the invention, the power of the ultrasonic wave is preferably 50-150W, and more preferably 100-120W; the time of the ultrasonic treatment is preferably 0.5-2 min.
After the mixed emulsion is obtained, the mixed emulsion is diluted to obtain the dispersed emulsion.
In the present invention, the dilution factor is preferably 1 to 5 times, and more preferably 2 to 4 times. In the invention, as the preparation of the mixed emulsion is carried out under ultrasound, oil drops in an oil phase collide with each other during ultrasound, the probability of polymerization is very high, the particle size is forced to be increased, and the emulsion stability is poor when the concentration of the polymerized emulsion and the concentration of the polylactic-co-glycolic acid copolymer are high under the condition of same volume of dichloromethane; moreover, the surface activity of PVA can promote the effective components to diffuse to the water phase, and the concentration is too high, which can cause the reduction of the encapsulation efficiency; therefore, the stability of the dispersion emulsion can be improved by diluting the mixed emulsion.
In the present invention, the reagent used for the dilution is a PVA aqueous solution having a volume concentration of preferably 0.005 to 0.02%, more preferably 0.01 to 0.015%. In the present invention, the above-mentioned type of the diluting agent is more favorable for the dispersion emulsion obtained after dilution to be distributed more uniformly.
After the dispersed emulsion is obtained, the invention carries out solid-liquid separation on the dispersed emulsion to obtain the pesticide nanocapsule.
In the present invention, the solid-liquid separation preferably comprises removing the hydrophobic organic solvent and then removing water. In the invention, when the solid-liquid separation mode is the type, the damage to the pesticide nanocapsules in the dispersed emulsion in the solid-liquid separation process can be prevented, and the encapsulation rate of the pesticide nanocapsules can be improved.
In the present invention, the method for removing the hydrophobic organic solvent is preferably to stir the dispersion emulsion in a magnetic stirrer. In the present invention, when the hydrophobic organic solvent is dichloromethane or ethyl acetate, it is more volatile, and when the dispersion emulsion is stirred in a magnetic stirrer, it can be removed by volatilization. The stirring temperature and time are not particularly limited, and the hydrophobic solvent in the dispersion solution can be removed by adjusting the stirring temperature and time according to the selected hydrophobic organic solvent.
In the present invention, the method for removing water is preferably centrifugal separation. The method of operation of the centrifugal separation in the present invention is not particularly limited, and a method known to those skilled in the art may be used. In the invention, the centrifugal separation method is preferably to centrifuge for 15min at 5000-12000 r/min.
After solid-liquid separation, the invention preferably washes and dries the solid obtained by the solid-liquid separation in sequence to obtain the pesticide nanocapsule. In the invention, the washing reagent is preferably ultrapure water, and the number of washing is preferably 1-5, more preferably 2-4. In the present invention, the washing can remove impurities on the solid surface. In the present invention, the drying is preferably freeze-drying, the temperature of the freeze-drying is preferably-40 to-60 ℃, more preferably-51 to-53 ℃; the freeze drying time is preferably 2-6 hours, and more preferably 3-5 hours. In the present invention, the freeze-drying can prevent the destruction of the pesticide nanocapsule.
The preparation method provided by the invention adopts the polylactic-co-glycolic acid as the capsule wall material, is nontoxic and has excellent biocompatibility, so that the prepared pesticide nanocapsule is nontoxic and has excellent biocompatibility; according to the invention, the oil phase and the PVA aqueous solution can be primarily mixed by stirring to form an oil-in-water system with large particle size, and then a large amount of energy is input through ultrasound to further disperse the oil phase into the water phase to form a uniform O/W emulsion; then diluting the mixed emulsion, preventing oil drops in the oil phase from colliding with each other in the ultrasonic process to polymerize so as to force the particle size of the pesticide nanocapsule to be increased, and further enabling the prepared pesticide nanocapsule to have a smaller particle size; and the dilution process also promotes the stability of the emulsion, so that the pesticide nanocapsule has good encapsulation and film-forming properties.
The invention also provides a pesticide nanocapsule prepared by the preparation method of the technical scheme, which comprises a capsule and a pesticide wrapped in the capsule.
The particle size of the pesticide nanocapsule provided by the invention is preferably 358.34-603 nm, and more preferably 358.34-414.29 nm; the encapsulation efficiency is preferably 58.21-73.59%, more preferably 70.58-73.59%. The pesticide nanocapsule provided by the invention has uniform particle size distribution, is nano-scale, and has higher chemical activity and biological activity.
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
(1) Dissolving 1.0g of polylactic-co-glycolic acid (PLGA) in dichloromethane to prepare a solution of 20mg/mL to obtain a solution of the capsule wall material; weighing a certain amount of tebuconazole raw drug, dissolving the tebuconazole raw drug in dichloromethane to prepare a solution of 10mg/mL to obtain a pesticide raw drug solution; mixing the obtained capsule wall material solution and the original pesticide solution according to the volume ratio of 1:1 to obtain an oil phase; the mass ratio of the capsule wall material to the pesticide raw material is 2: 1;
(2) under magnetic stirring, 4mL of oil phase liquid is dropwise added into 16mL of PVA aqueous solution with the volume concentration of 2%, and stirring is carried out for 5 min; carrying out ultrasonic disruption on the mixed solution for 2min at the ultrasonic cell disruption instrument with the ultrasonic power of 65W for 3s and the interval of 7s to obtain mixed emulsion;
(3) adding 32mL of PVA aqueous solution with the volume concentration of 0.01% into the obtained mixed emulsion, stably dispersing the mixed emulsion for 20min, and then stirring the mixed emulsion on a magnetic stirrer for 24h to remove dichloromethane in the mixed emulsion; and then centrifuging the mixed solution on a centrifuge at 10000r/min for 15min, washing the precipitate with ultrapure water for 3 times, and freeze-drying at-52 ℃ for 4h to obtain the pesticide nanocapsule.
Scanning electron microscopy was used to test the pesticide nanocapsules prepared in example 1, and the SEM image of the pesticide nanocapsules prepared in example 1 is shown in fig. 1. As can be seen from FIG. 1, the pesticide nanocapsule prepared by the invention has smooth surface, uniform particle size distribution and less breakage.
Example 2
The difference from example 1 was that the concentration of the aqueous PVA solution in step (2) was 0.5%, and the other steps were the same as in example 1.
Example 3
The difference from example 1 was that the concentration of the aqueous PVA solution in step (2) was 1%, and the other steps were the same as in example 1.
The drug loading capacity of the pesticide nanocapsules prepared in examples 1 to 3 was measured by an instrument or method, and the results are shown in table 1;
the encapsulation efficiency of the pesticide nanocapsules prepared in examples 1 to 3 was tested by using (an instrument or a method), and the results are shown in table 1;
the particle size of the pesticide nanocapsules prepared in examples 1 to 3 was measured by an instrument or method, and the results are shown in table 1;
TABLE 1 Effect of PVA concentration on pesticide nanocapsules prepared in examples 1-3
| PVA concentration (%) | Drug loading (%) | Encapsulation efficiency (%) | Particle size (d.nm) |
| 0.5 | 13.96 | 65.25 | 592.68 |
| 1 | 13.58 | 64.83 | 542.16 |
| 2 | 12.69 | 58.21 | 472.34 |
As can be seen from table 1: the drug loading capacity, the encapsulation efficiency and the particle size of the tebuconazole nano capsule are all reduced along with the increase of the PVA concentration, and the particle size of the obtained pesticide nano capsule is nano grade, which shows that the preparation method provided by the invention can obtain the nano grade pesticide nano capsule and the encapsulation efficiency is higher.
Example 4
The difference from example 1 was that the concentration of the cell wall material solution in step (1) was 10%, and the other steps were the same as in example 1.
Example 5
The difference from example 1 was that the concentration of the cell wall material solution in step (1) was 40%, and the other steps were the same as in example 1.
The pesticide nanocapsules prepared in examples 1, 4 and 5 were tested for drug loading, encapsulation efficiency and particle size and the results are shown in table 2:
TABLE 2 Effect of the concentration of the solution of wall material on the pesticide nanocapsules prepared in examples 1, 4 and 5
| PLGA concentration% | Drug loading (%) | Encapsulation efficiency (%) | Particle size (d.nm) |
| 10 | 17.58 | 55.67 | 461.19 |
| 20 | 12.69 | 58.21 | 472.34 |
| 40 | 16.82 | 52.73 | 515.28 |
As can be seen from table 2: the drug loading capacity, the encapsulation efficiency and the particle size of the tebuconazole nano capsule are changed along with the increase of the concentration of the capsule wall material solution, and the particle size of the obtained pesticide nano capsule is nano-scale, which shows that the preparation method provided by the invention can obtain the nano-scale pesticide nano capsule and has higher encapsulation efficiency.
Example 6
The difference from example 1 was that the volume of the 2% aqueous PVA solution in step (2) was 8mL, and the other steps were the same as in example 1.
Example 7
The difference from example 1 was that the volume of the 2% aqueous PVA solution in step (2) was 32mL, and the other steps were the same as in example 1.
The pesticide nanocapsules prepared in examples 1, 6 and 7 were tested for drug loading, encapsulation efficiency and particle size and the results are shown in table 3:
TABLE 3 Effect of the volume of PVA solution on the pesticide nanocapsules prepared in examples 1, 6 and 7
| PLGA volume (mL) | Drug loading (%) | Encapsulation efficiency (%) | Particle size (d.nm) |
| 8 | 15.37 | 70.58 | 593.16 |
| 16 | 12.85 | 58.21 | 472.34 |
| 32 | 10.46 | 47.39 | 601.34 |
As can be seen from table 3: the drug loading capacity, the encapsulation efficiency and the particle size of the tebuconazole nano capsule are changed along with the increase of the concentration of the capsule wall material solution, and the particle size of the obtained pesticide nano capsule is nano-scale, which shows that the preparation method provided by the invention can obtain the nano-scale pesticide nano capsule and has higher encapsulation efficiency.
Example 8
The difference from the example 1 is that the ultrasonic power in the step (2) is 104W, and the other steps are the same as the example 1.
Example 9
The difference from the example 1 is that the ultrasonic power in the step (2) is 130W, and other steps are the same as the example 1.
The pesticide nanocapsules prepared in examples 1, 8 and 9 were tested for drug loading, encapsulation efficiency and particle size and the results are shown in table 4:
TABLE 4 Effect of ultrasound power on pesticide nanocapsules prepared in examples 1, 8 and 9
| Ultrasonic power (w) | Drug loading (%) | Encapsulation efficiency (%) | Particle size (d.nm) |
| 65 | 12.85 | 58.21 | 472.34 |
| 104 | 17.32 | 73.59 | 414.29 |
| 130 | 18.05 | 70.28 | 358.34 |
As can be seen from table 4: the drug loading capacity, the encapsulation efficiency and the particle size of the tebuconazole nano capsule are changed along with the increase of the concentration of the capsule wall material solution, and the particle size of the obtained pesticide nano capsule is nano-scale, which shows that the preparation method provided by the invention can obtain the nano-scale pesticide nano capsule and has higher encapsulation efficiency.
Example 10
The difference from the example 1 is that the technical pesticide in the step (1) is thifluzamide, the ultrasonic power in the step (2) is 130W, and the other steps are the same as the example 1.
Example 11
The difference from the example 10 is that the original pesticide in the step (1) is azoxystrobin, and other steps are the same as the example 10.
The pesticide nanocapsules prepared in examples 1, 10 and 11 were tested for drug loading, encapsulation efficiency and particle size and the results are shown in table 5:
TABLE 5 Effect of different types of pesticides on pesticide nanocapsules prepared in examples 1, 10 and 11
| Pesticide | Drug loading (%) | Encapsulation efficiency (%) | Particle size (d.nm) |
| Tebuconazole | 18.05 | 70.28 | 358.34 |
| Thifluzamide | 25.52 | 84.92 | 482.16 |
| Azoxystrobin | 15.33 | 74.27 | 387.21 |
As can be seen from table 5: the preparation method is utilized to evaluate different drug loading rates, encapsulation rates and particle sizes of three different types of pesticide nanocapsules. Wherein the tebuconazole nano capsule has the smallest average particle size; the thifluzamide nano-capsule has the highest drug loading rate and encapsulation rate, but has larger average particle size; the azoxystrobin nanocapsule has the lowest drug loading. The preparation method provided by the invention can obtain the nano-scale pesticide nanocapsule, the encapsulation efficiency is higher, and the pesticide nanocapsule with the smallest particle size can be obtained when the original pesticide is tebuconazole.
The data of the embodiment show that the method provided by the invention can obtain the nano-scale pesticide nanocapsule, and the encapsulation efficiency is higher; and because the adopted capsule wall material is PLGA, the capsule wall material has excellent compatibility, and the prepared pesticide nanocapsule has the advantages of no toxicity and good biocompatibility.
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. A preparation method of a pesticide nanocapsule comprises the following steps:
(1) mixing the capsule wall material, the original pesticide and the hydrophobic organic solvent to obtain an oil phase; the capsule wall material is polylactic acid-glycolic acid copolymer;
(2) mixing the oil phase obtained in the step (1) with a PVA (polyvinyl alcohol) aqueous solution, and then sequentially stirring and ultrasonically treating to obtain a mixed emulsion;
(3) diluting the mixed emulsion obtained in the step (2) to obtain a dispersed emulsion;
(4) and (4) carrying out solid-liquid separation on the dispersed emulsion obtained in the step (3) to obtain the pesticide nanocapsule.
2. The method for preparing pesticide nanocapsules according to claim 1, wherein the hydrophobic organic solvent in step (1) is dichloromethane or ethyl acetate.
3. The method for preparing pesticide nanocapsules according to claim 1, wherein the raw pesticide in the step (1) comprises tebuconazole, thifluzamide or azoxystrobin.
4. The preparation method of the pesticide nanocapsule of claim 1, wherein the mass ratio of the capsule wall material to the pesticide raw material in the step (1) is (10-40) to (2-50).
5. The method for preparing pesticide nanocapsules according to claim 1, wherein the volume concentration of the PVA aqueous solution in the step (2) is 0.1-5%.
6. The method for preparing a pesticidal nanocapsule according to claim 1, wherein the mixing in the step (2) is dropwise addition of the oil phase to the aqueous PVA solution.
7. The method for preparing pesticide nanocapsules according to claim 1, wherein the dilution in step (3) is 1 to 5 times.
8. The method for preparing pesticide nanocapsules according to claim 1, wherein the reagent used for dilution in step (3) is an aqueous PVA solution having a volume concentration of 0.005-0.02%.
9. The method for preparing a pesticidal nanocapsule according to claim 1, wherein the solid-liquid separation in step (4) comprises removing the hydrophobic organic solvent and then removing water.
10. The pesticide nanocapsule prepared by the preparation method of any one of claims 1 to 9, which comprises a capsule and a pesticide wrapped in the capsule, wherein the capsule is made of polylactic-co-glycolic acid.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1561987A (en) * | 2004-03-19 | 2005-01-12 | 中国科学院长春应用化学研究所 | Nano micro ball with taxol capable of biologically degradating high molecule and its preparing method |
| CN1676121A (en) * | 2004-03-29 | 2005-10-05 | 中国人民解放军军事医学科学院毒物药物研究所 | Slow-release micro-ball formulation for tissue, organ local therapy, and its preparing method and use |
| CN103599073A (en) * | 2013-11-15 | 2014-02-26 | 无锡中科光远生物材料有限公司 | Method for preparing targeted anti-cancer medicament supported PLGA (poly(lactic-co-glycolic) acid) microparticles |
| CN103599074A (en) * | 2013-11-26 | 2014-02-26 | 重庆医药工业研究院有限责任公司 | Iloperidone sustained release microsphere and preparation method thereof |
| CN104206399A (en) * | 2014-09-01 | 2014-12-17 | 中国农业科学院植物保护研究所 | Pyraclostrobin nanoparticle and preparation method of pyraclostrobin nanoparticle |
| CN105001673A (en) * | 2015-07-21 | 2015-10-28 | 上海科涤环保科技有限公司 | Aqueous composite nanometer coloring agent preparation method |
| CN105310997A (en) * | 2014-06-16 | 2016-02-10 | 重庆医药工业研究院有限责任公司 | Aripiprazole sustained-release microspheres and preparation method thereof |
| CN107157957A (en) * | 2017-05-25 | 2017-09-15 | 长春金赛药业股份有限公司 | Progesterone sustained-release micro-spheres and nanoparticle, its preparation method and progesterone are slow-release injected |
| CN107258778A (en) * | 2017-06-23 | 2017-10-20 | 中国农业科学院农业环境与可持续发展研究所 | The preparation method of pesticide nano capsules |
| CN109679055A (en) * | 2018-12-12 | 2019-04-26 | 中国农业科学院农业质量标准与检测技术研究所 | A kind of degradable microencapsulation material and the preparation method and application thereof that uvioresistant is modified |
| CN114028339A (en) * | 2021-09-15 | 2022-02-11 | 济南大学 | Rivastigmine bitartrate-PLGA long-acting slow-release microsphere for injection and process |
-
2022
- 2022-03-01 CN CN202210192359.8A patent/CN114342930A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1561987A (en) * | 2004-03-19 | 2005-01-12 | 中国科学院长春应用化学研究所 | Nano micro ball with taxol capable of biologically degradating high molecule and its preparing method |
| CN1676121A (en) * | 2004-03-29 | 2005-10-05 | 中国人民解放军军事医学科学院毒物药物研究所 | Slow-release micro-ball formulation for tissue, organ local therapy, and its preparing method and use |
| CN103599073A (en) * | 2013-11-15 | 2014-02-26 | 无锡中科光远生物材料有限公司 | Method for preparing targeted anti-cancer medicament supported PLGA (poly(lactic-co-glycolic) acid) microparticles |
| CN103599074A (en) * | 2013-11-26 | 2014-02-26 | 重庆医药工业研究院有限责任公司 | Iloperidone sustained release microsphere and preparation method thereof |
| CN105310997A (en) * | 2014-06-16 | 2016-02-10 | 重庆医药工业研究院有限责任公司 | Aripiprazole sustained-release microspheres and preparation method thereof |
| CN104206399A (en) * | 2014-09-01 | 2014-12-17 | 中国农业科学院植物保护研究所 | Pyraclostrobin nanoparticle and preparation method of pyraclostrobin nanoparticle |
| CN105001673A (en) * | 2015-07-21 | 2015-10-28 | 上海科涤环保科技有限公司 | Aqueous composite nanometer coloring agent preparation method |
| CN107157957A (en) * | 2017-05-25 | 2017-09-15 | 长春金赛药业股份有限公司 | Progesterone sustained-release micro-spheres and nanoparticle, its preparation method and progesterone are slow-release injected |
| CN107258778A (en) * | 2017-06-23 | 2017-10-20 | 中国农业科学院农业环境与可持续发展研究所 | The preparation method of pesticide nano capsules |
| CN109679055A (en) * | 2018-12-12 | 2019-04-26 | 中国农业科学院农业质量标准与检测技术研究所 | A kind of degradable microencapsulation material and the preparation method and application thereof that uvioresistant is modified |
| CN114028339A (en) * | 2021-09-15 | 2022-02-11 | 济南大学 | Rivastigmine bitartrate-PLGA long-acting slow-release microsphere for injection and process |
Non-Patent Citations (6)
| Title |
|---|
| JIAKUN ZHANG等: "Size-Dependent Effect of Prochloraz-Loaded mPEG-PLGA Micro- and Nanoparticles", 《JOURNAL OF NANOSCIENCE AND NANOTECHNOLOGY》, vol. 16, no. 6, 31 December 2016 (2016-12-31), pages 6231 - 6237, XP009525201, DOI: 10.1166/jnn.2016.10894 * |
| MING ZHANG等: "One-step microencapsulation and spraying of pesticide formulations for improved adhesion and sustained release", 《JOURNAL OF MICROENCAPSULATION》, 18 September 2019 (2019-09-18), pages 649 - 658 * |
| 李晶晶等: "基于细乳液聚合的纳米颗粒制备与应用研究进展", 《应用化学》, no. 09, 24 August 2018 (2018-08-24), pages 1026 - 1036 * |
| 杨蕾等: "阿立哌唑缓释微球的工艺优化及体内药动学研究", 《中国新药杂志》, vol. 21, no. 2, 31 December 2012 (2012-12-31), pages 188 - 194 * |
| 林丽等: "伊潘立酮长效缓释微球的制备及体外释药特性研究", 《第三军医大学学报》, vol. 36, no. 3, 15 February 2014 (2014-02-15), pages 274 - 277 * |
| 赵晓等: "基于细乳化/溶剂蒸发法制备复合纳米色素", 《化工学报》, no. 03, 21 November 2013 (2013-11-21), pages 1118 - 1125 * |
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