CN107624769B - Matrine microcapsule gel composite system sustained release preparation and preparation method and application thereof - Google Patents
Matrine microcapsule gel composite system sustained release preparation and preparation method and application thereof Download PDFInfo
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- CN107624769B CN107624769B CN201710854776.3A CN201710854776A CN107624769B CN 107624769 B CN107624769 B CN 107624769B CN 201710854776 A CN201710854776 A CN 201710854776A CN 107624769 B CN107624769 B CN 107624769B
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- matrine
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- ZSBXGIUJOOQZMP-JLNYLFASSA-N Matrine Chemical compound C1CC[C@H]2CN3C(=O)CCC[C@@H]3[C@@H]3[C@H]2N1CCC3 ZSBXGIUJOOQZMP-JLNYLFASSA-N 0.000 title claims abstract description 54
- 229930014456 matrine Natural products 0.000 title claims abstract description 54
- 239000003094 microcapsule Substances 0.000 title claims abstract description 45
- 239000003405 delayed action preparation Substances 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
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- VEHPJKVTJQSSKL-UHFFFAOYSA-N azadirachtin Natural products O1C2(C)C(C3(C=COC3O3)O)CC3C21C1(C)C(O)C(OCC2(OC(C)=O)C(CC3OC(=O)C(C)=CC)OC(C)=O)C2C32COC(C(=O)OC)(O)C12 VEHPJKVTJQSSKL-UHFFFAOYSA-N 0.000 description 2
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Abstract
The invention belongs to the technical field of pesticides, and particularly relates to a botanical pesticide matrine microcapsule gel composite system sustained-release preparation and a preparation method thereof. The preparation comprises gel and microcapsule particles dispersed in the gel, wherein the microcapsule particles take egg white as a capsule material and matrine as an effective component. The preparation method comprises mixing egg white and deionized water uniformly to obtain egg white solution; dissolving matrine in ethanol to obtain matrine ethanol solution; dropwise adding matrine ethanol solution into egg white solution to form uniform mixture, centrifuging, removing supernatant, taking the lower layer precipitate, and freeze-drying to obtain microcapsule particles; dispersing the microcapsule granules into the gel by an equivalent addition method to obtain the plant source pesticide matrine microcapsule gel composite system sustained-release preparation. The medicinal components of the preparation have obvious release rule, the effective period basically covers one leek harvesting period, and the preparation method is simple.
Description
Technical Field
The invention belongs to the technical field of pesticides, and particularly relates to a botanical pesticide matrine microcapsule gel composite system sustained-release preparation and a preparation method thereof.
Background
The Chinese chive maggot is an agricultural and forestry pest which seriously harms the growth and the yield of the Chinese chives, and the harmfulness is the first of the Chinese chive pests. The common radical cure method is to use phoxim to mix seeds to kill pests, but the accumulation of pesticide on roots is caused, and the toxic leek events happen frequently, and the root cause is that phoxim is easy to enter leek roots along with the moisture in soil, and poisoning occurs after people eat the phoxim. Meanwhile, the use of chemical pesticides also causes environmental pollution, and therefore it is important to find a pesticide which can kill the Chinese chive maggots underground in an effective dose without causing pesticide residues and is safe for food. According to the reports of documents, the natural matrine extracted from the roots of the sophora flavescens has the effect of killing pests, and meanwhile, the matrine can be easily decomposed into nontoxic substances by microorganisms in natural water, so that the natural matrine is an ideal pollution-free pesticide.
Disclosure of Invention
The invention aims to solve the problems of poisoning and environmental pollution caused by easy accumulation of the existing pesticide at the root of Chinese chives and provides a microcapsule gel composite system sustained-release preparation which basically covers one Chinese chive harvesting period and releases matrine according to a certain rule and has good safety and a preparation method thereof.
The invention provides a botanical pesticide matrine microcapsule gel composite system sustained-release preparation, which comprises gel and microcapsule particles dispersed in the gel, wherein the microcapsule particles take egg white as a capsule wall material and matrine as an effective component.
Microcapsule sustained-release preparation
As an improvement of the technical scheme, the gel is any one of carbomer 941 hydrogel, carbomer 940 hydrogel, konjac gum, sodium alginate hydrogel and hydroxypropyl methyl cellulose sodium or derivative hydrosol thereof.
The invention also provides a preparation method of the botanical pesticide matrine microcapsule gel composite system sustained-release preparation, which comprises the following process steps:
(1) uniformly mixing egg white with deionized water to obtain an egg white solution;
(2) dissolving matrine in ethanol to obtain matrine ethanol solution;
(3) dropwise adding the matrine ethanol solution obtained in the step (2) into the egg white solution obtained in the step (1) to form a uniform mixture, centrifuging, removing supernatant, taking the lower-layer precipitate, and freeze-drying to obtain microcapsule particles;
(4) the microcapsule particles were dispersed into the gel in equal increments.
As an improvement of the technical scheme, the gel contains 0.5-2% of carbomer 941.
As an improvement of the technical scheme, the concentration of the egg white solution is 75-85%.
As an improvement of the technical scheme, the volume concentration of the ethanol solution is 75-100%.
As an improvement of the above technical scheme, the volume weight ratio of the egg white solution to the matrine is 1: (15-25) (mL/mg).
As an improvement of the technical scheme, the volume ratio of the egg white solution to the ethanol solution is 1: (0.40-0.45) (mL/mL).
As an improvement of the technical scheme, the weight volume ratio of the microcapsule particles to the gel is 1: (5-10) (mg/mL).
The invention also provides a method for preventing and treating Chinese chive maggots by the botanical pesticide matrine microcapsule gel composite system slow-release preparation, wherein 20-30 dosing points are uniformly placed in each mu of land, and the dosing amount is applied according to the principle that the intermediate dosage is high and the peripheral dosage is low.
The compound sustained-release preparation can be used for preventing and treating root knot nematode, grub, cutworm, wireworm and other underground pests, and related shallot, garlic vegetables and the like.
In the invention, carbomer 941 is a retarding material with a skeleton form forming hydrogen bonds, has a slow release effect on the release of water-soluble drugs represented by water as a polar solvent, and also has carbomer 940, konjac glucomannan, sodium alginate, sodium hydroxypropylmethylcellulose and other cellulose derivatives and the like with similar effects, but experiments show that the carbomer 941 has the best effect.
The egg white is a compound with small molecular weight, amino and carboxyl, has certain fluidity, can prepare the particle size of the encapsulated drug particles which is easy to control, has simple and feasible process, is a natural harmless material and has wide source; other egg white materials such as duck egg white and bird egg white have the same effect as the capsule material, but are slightly expensive, have few sources and are not suitable for adoption.
The compound sustained release preparation can be used together with nicotine and azadirachtin insecticides without affecting the effect of nicotine and azadirachtin insecticides.
The invention has the beneficial effects that:
compared with the existing insecticide, the microcapsule gel compound sustained-release preparation prepared by adopting the botanical pesticide matrine has the advantages that the medicine has an obvious release rule, the lasting period covers one leek harvesting period, and the productivity is saved;
the preparation process is simple, can realize industrial production and has obvious economic benefit;
the invention adopts environment-friendly material egg white and natural botanical pesticide matrine, has little environmental pollution and is green and environment-friendly compared with the traditional prevention and treatment method, and more conforms to the sustainable development concept.
The microcapsule sustained-release preparation is usually a human preparation and is regularly dissolved in human body fluid, different drugs have different properties and need different preparation modes for dissolution, and the release environment can also influence the dissolution rule of the preparation. The gel is added to change the release mode of the medicine, and the invention is suitable for being applied to field crops. The invention opens up a precedent that the biological pesticide is released in the soil environment in the form of gel and microcapsule composite system sustained release agent, and provides a powerful theoretical basis for sustainable development of dosage form research and development aiming at underground crop pests.
Drawings
FIG. 1 is a simulated irrigation release curve of matrine microcapsule gel composite system sustained release preparation;
FIG. 2 is the release profile of the matrine microcapsule gel complex sustained release formulation of example 1;
FIG. 3 is a simulation of the field application of example 2.
Detailed Description
The invention provides a botanical pesticide matrine microcapsule gel composite system sustained-release preparation on one hand, which comprises a gel continuous phase and microcapsule particles dispersed in the gel, wherein the microcapsule particles take egg white as a capsule wall material and matrine as an effective component.
In a preferred embodiment of the invention, the gel is a carbomer hydrogel and the shell material is egg white.
In a preferred embodiment of the present invention, the carbomer hydrogel is formed by uniformly mixing carbomer 941 and deionized water.
In a preferred embodiment of the invention, the gel contains 0.5-2% carbomer. In a preferred embodiment of the invention, the gel contains 1% carbomer.
In a preferred embodiment of the present invention, the weight-volume ratio of the microcapsule particles to the gel is 1: (5-10) (mg/mL). In a preferred embodiment of the present invention, the weight-volume ratio of the microcapsule particles to the gel is 1: 7 (mg/mL).
The invention also provides a preparation method of the botanical pesticide matrine microcapsule gel composite system sustained-release preparation, which comprises the following process steps:
(1) uniformly mixing egg white with deionized water to obtain an egg white solution;
(2) dissolving matrine in ethanol to obtain matrine ethanol solution;
(3) dropwise adding the matrine ethanol solution obtained in the step (2) into the egg white solution obtained in the step (1) to form a uniform mixture, centrifuging, removing supernatant, taking the lower-layer precipitate, and freeze-drying to obtain microcapsule particles;
(4) the microcapsule particles were dispersed into the gel in equal increments.
In a preferred embodiment of the invention, the concentration of the egg white solution is 75-85%. In a preferred embodiment of the invention, the concentration of the egg white solution is 80%.
In a preferred embodiment of the present invention, the concentration of the ethanol solution is 75% to 100%. In a preferred embodiment of the invention, the concentration of ethanol is 80%.
In a preferred embodiment of the present invention, the volume weight ratio of the egg white solution to the matrine is 1: (15-25) (mL/mg). In a preferred embodiment of the present invention, the volume weight ratio of the egg white solution to the matrine is 1: 20 (mL/mg).
In a preferred embodiment of the invention, the volume ratio of the egg white solution to the ethanol solution is 1: (0.40-0.45) (mL/mL). In a preferred embodiment of the invention, the volume ratio of the egg white solution to the ethanol is 1: 0.42 (mL/mL).
In one embodiment of the invention, the botanical pesticide matrine microcapsule gel composite sustained-release preparation is used for preventing and controlling the Chinese chive maggots, and 20-30 pesticide application points are uniformly arranged per mu of land. Preferably, 25 administration points are placed in each acre, and the action range of each administration point is about 25m2Left and right.
The present invention will be described in further detail with reference to the following embodiments and the accompanying drawings.
Example 1
The cumulative release curve of the compound sustained-release preparation according to figure 1 conforms to the first order kinetic equation mode, Q is 94.1502 (1-e)-0.5655n) R is 0.9997, where Q represents the cumulative drug release rate (%), n represents the number of administrations (times), and e is a natural constant. Calculating according to 24 days of the longest period of the harvesting period of the Chinese chives (irrigating for 1 time every 3 days and irrigating for 0.5 hour each time on average) to obtain the minimum release rate accounting for 2.39 percent of the total feeding amount, wherein in a field effect experiment, the acting dose of matrine is 22 g/mu (refer to Wu-pass-ten's article of botanical pesticide matrine control Chinese chive maggot test'), so as to determine the standard prescription of each feeding point as follows:
main drug (matrine) 837mg
42mL of 80% ethanol solution
100mL of 80% egg white solution
1% carbomer 94125 mL
The preparation steps of the gel composite system are as follows:
mixing egg white and deionized water uniformly to prepare 80% egg white solution (ml/ml), and stirring uniformly for later use; weighing a prescribed amount of matrine, dissolving the matrine in an ethanol solution, uniformly stirring to obtain a matrine ethanol solution, dropwise adding the matrine ethanol solution into an egg white solution at room temperature, forming uniform solid particles in the solution after 30 minutes, centrifuging the mixture solution, removing a supernatant, freezing and drying a lower-layer precipitate, and weighing to obtain 4.9235g of microcapsule particles containing 17% (g/g) of matrine.
Weighing the formula amount of carbomer 941, adding the carbomer 941 into the formula amount of deionized water in an equivalent progressive method, uniformly stirring, standing for 24 hours to obtain 25mL of 1% (g/g) carbomer 941 gel, and uniformly stirring for later use; adding the obtained microcapsule granules into the gel by equal addition, stirring uniformly to obtain the microcapsule gel composite sustained-release preparation, and filling the microcapsule gel composite sustained-release preparation into a bottle or a bag.
Three batches of samples are prepared according to the prescription amount of the embodiment, the prepared composite sustained-release preparation is subjected to simulated irrigation and timed flushing by using quantitative water, the release rule graph is shown in the attached figure 2 of the specification, and the obtained matrine release amount is shown in the table 1:
TABLE 1 simulation of matrine release in irrigation filtrates
As can be seen from Table 1, within the range of 8 times of washing, the release amount of matrine in each time of the three batches of compound sustained-release preparations is close to the theoretical value, and the single release amount conforms to the insecticidal effective dose (not less than 20mg), and the maximum release amount is within the toxic dose range (the toxic dose of silkworm is 4 x 106mg is taken as a reference).
Example 2
Time: 2017.5.10-2017.6.4
A place: vegetable greenhouse in Tan Jiafang town of Shandong Qingzhou city
The application method comprises the following steps: according to 667m per mu2(25.83m 25.83m), setting a dosing point about every 5m, wherein the distribution of the dosing points is shown in figure 3, the main dose of each dosing point is 0.837mg, the depth of each dosing point is 3-4 cm underground, the dosing is carried out once every 3 days, and the dosing time is determined as that the dosing starts after the chives are harvested for one crop.
Control group: and (4) dressing the seeds with phoxim. A commercial 40% phoxim emulsifiable concentrate (pesticide registration number: PD85157-2) was applied 1 time per 3 days with 60mL per acre as a control.
Other field management was the same for the example group and the control group.
As a result:
the example groups were applied once, watered every three days, no Chinese chive maggot appeared in one Chinese chive growth cycle, and the control group was applied 8 times, no Chinese chive maggot appeared.
The compound sustained-release preparation provided by the invention can be used for preventing and treating root-knot nematodes, grubs, cutworms, wireworms and other underground pests, related to scallion, garlic vegetables and the like, besides the Chinese chive maggots, and the standard prescription per mu is determined according to the method in the embodiment 1. The matrine dosage of the standard prescription is the lowest effective dosage, and the prevention and treatment effect is better if the dosage is slightly larger than the effective dosage.
The above embodiments are intended to illustrate that the present invention may be implemented or used by those skilled in the art, and therefore the present invention includes, but is not limited to, the above embodiments, any methods, processes, products, etc., which are consistent with the principles and novel and inventive features disclosed herein, and which are within the scope of the present invention.
Claims (8)
1. A botanical pesticide matrine microcapsule gel composite system sustained release preparation is characterized by comprising gel and microcapsule particles dispersed in the gel, wherein the microcapsule particles take egg white as a capsule wall material and matrine as an effective component; the gel is any one of carbomer 941 hydrogel and carbomer 940 hydrogel;
the preparation method of the botanical pesticide matrine microcapsule gel composite system slow-release preparation comprises the following process steps:
(1) uniformly mixing egg white with deionized water to obtain an egg white solution;
(2) dissolving matrine in ethanol solution to obtain matrine ethanol solution;
(3) dropwise adding the matrine ethanol solution obtained in the step (2) into the egg white solution obtained in the step (1) to form a uniform mixture, centrifuging, removing supernatant, taking the lower-layer precipitate, and freeze-drying to obtain microcapsule particles;
(4) the microcapsule particles were dispersed into the gel in equal increments.
2. The sustained release formulation of claim 1, wherein the gel comprises from 0.5% to 2% carbomer 941.
3. The sustained-release preparation of claim 2, wherein the concentration of the egg white solution is 75% to 85%.
4. The sustained-release preparation according to claim 3, wherein the concentration of the ethanol solution is 75% to 100%.
5. The sustained-release preparation according to claim 4, wherein the ratio of the egg white solution to the matrine as the raw material drug is as follows: the proportion of each 1mL of egg white solution is 15-25 mg of raw material matrine.
6. The sustained-release preparation of claim 4, wherein the ratio of the egg white solution to the ethanol solution is: each 1mL of egg white solution is matched with 0.40-0.45 mL of ethanol solution.
7. The sustained-release preparation according to claim 4, wherein the ratio of the microcapsule particles to the gel is: the proportion of each 1mg microcapsule particle is 5-10 mL gel.
8. The method for controlling the Chinese chive maggots by using the compound sustained-release preparation as claimed in claim 1, wherein 20-30 dosing points are uniformly arranged per mu of land, and the dosing amount is based on the principle that the middle dosage is high and the peripheral dosage is low.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1520816A (en) * | 2003-01-27 | 2004-08-18 | 上海海天医药科技开发有限公司 | Sophocarpidine gel preparation and its process |
| CN101514128A (en) * | 2009-04-07 | 2009-08-26 | 玉溪山水生物科技有限责任公司 | Micro-encapsulated broad spectrum pollution-free fertilizer with pesticide, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1520816A (en) * | 2003-01-27 | 2004-08-18 | 上海海天医药科技开发有限公司 | Sophocarpidine gel preparation and its process |
| CN101514128A (en) * | 2009-04-07 | 2009-08-26 | 玉溪山水生物科技有限责任公司 | Micro-encapsulated broad spectrum pollution-free fertilizer with pesticide, preparation method and application thereof |
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