CN104430324B - A kind of medicament of preventing and treating the plague of rats and preparation method thereof - Google Patents

Abstract

The present invention relates to a kind of medicament of preventing and treating the plague of rats and preparation method thereof, this medicament comprises the alkaloid microcapsules of 1～10 weight portion, the auxiliary material of 90～99 weight portions, the capsule heart composition of alkaloid microcapsules comprises one or more alkaloids that extract from the rhizome of Chinese monkshood, Aconitum Szechenyianum Gay, datura, black false hellebore, kuh-seng, vomiting nut, and the cyst wall composition of alkaloid microcapsules comprises polyureas prepared by polyamine and multicomponent isocyanate. Alkaloid is through encapsulation, and palatability is obviously improved, and in environment, the speed of oxidized decomposition decreases. The alkaloid microcapsules of being eaten slowly discharge in muroid body, and the acute toxicity of medicament reduces, and taking chronic toxicity as main, can reduce muroid vigilance, and reduce the harm to people and animals and Natural Enemies of Rats.

Description

Medicament for preventing and controlling rodent damage and preparation method thereof

technical field

The invention relates to the field of rodent damage prevention and control, in particular to a medicament for preventing rodent damage and a preparation method thereof.

Background technique

The large-scale reproduction and frequent activities of rodents will cause serious ecological problems. They steal food, eat grass roots and tree roots, dig holes, and seriously endanger the production of agriculture and forestry. In areas where humans are active, rodents can transmit various diseases to humans and domestic animals through various channels. In human history, plague outbreaks have caused tens of millions of deaths. Therefore, the prevention and control of rodent damage is very necessary. Traditional rodent control mainly uses chemical drugs to eliminate rodents. This method has a fast effect and a large area, and can temporarily reduce the density of rodents. However, these chemical drugs can cause secondary poisoning, resulting in the reduction of rodent natural enemies, and the ecological balance is affected. Destruction and improper use will pollute the environment and endanger the health of domestic animals and humans. Therefore it is necessary to develop a rodenticide that has good rodent control effect, little environmental pollution, and can not cause poisoning of humans, animals and rodent natural enemies.

Contents of the invention

The object of the present invention is to provide a medicament for preventing and controlling rodent damage, which has good rodent control effect, little environmental pollution, and will not cause poisoning of humans, animals and rodent natural enemies.

To achieve the above object, the present invention adopts following scheme to implement:

A medicament for preventing and controlling rodent infestation, comprising 1-10 parts by weight of alkaloid microcapsules and 90-99 parts by weight of auxiliary materials. One or more alkaloids extracted from aloe, Sophora flavescens, and Nuxyche chinensis, and the capsule wall composition of the alkaloid microcapsules includes polyurea prepared from polyamines and polyisocyanates.

Specifically: the polyamine is an aliphatic amine, which may be ethylenediamine, diethylenetriamine, tetraethylenepentamine or hexamethylenediamine. The polyisocyanate is toluene diisocyanate or diphenylmethane diisocyanate. The auxiliary materials include food and attractants. Attractants include peanut powder, sugar, and cyclamate.

A more detailed plan is: the medicament includes 1-10 parts by weight of alkaloid microcapsules, 90-98 parts by weight of grain, and 1-4 parts by weight of attractant.

The present invention also provides a preparation method of the alkaloid microcapsules, which comprises the following steps:

S1: extract alkaloids from plants;

S2: Prepare the water phase solution, the organic phase solution, and the water phase monomer respectively. First, add the organic phase to the water phase solution and mix well, then add the water phase monomer dropwise and stir for reaction. After the reaction, perform cooling, filtration, washing, Alkaloid microcapsules are obtained after drying, the composition of the aqueous phase solution includes a dispersant and an emulsifier, the composition of the organic phase solution includes polyisocyanates and alkaloids, and the composition of the aqueous phase monomers includes polyamines;

S3: The excipients and alkaloid microcapsules are mixed with water according to the specified weight ratio, and then compressed to obtain the rodent control agent.

The specific operation of step S1 is:

After crushing the raw material, put it in the extraction equipment, add the extractant for ultrasonic extraction, filter and recover the extract, distill and concentrate it into a paste, dissolve the obtained paste solid in distilled water, add hydrochloric acid to acidify to pH=2~3, and then Perform primary extraction with dichloromethane, recover the aqueous phase of the primary extraction and adjust to pH=9-10 with ammonia water, perform secondary extraction with dichloromethane again, recover the organic phase of the secondary extraction and distill off the dichloromethane, Produce alkaloids.

The concrete operation of step S2 is:

Dissolve the dispersant in distilled water and heat to dissolve to prepare a 2-5% colloidal solution, then add an emulsifier to the dispersant solution to prepare a 0.5% (mass fraction) solution, stir and mix and cool to 45-60°C Stand-by; dissolving polyisocyanate in an organic solvent, then adding alkaloids and mixing to prepare an organic phase solution for use; dissolving polyamine in distilled water and mixing to prepare a water-phase monomer for use; mixing polyisocyanate and organic solvent The volume ratio of polyamine and distilled water is 1:5-10, and the alkaloid is added according to the amount of 0.01-0.05g of alkaloid per milliliter of polyisocyanate; the volume ratio of polyamine and distilled water is 1-1.5:5-10;

Add the organic phase solution to the water phase solution, stir and mix in a water bath at 45-60°C, then add the water phase monomer dropwise with a needle at a rate of 1 drop/s and stir. After the dropwise addition, react for 2 hours, cool to room temperature and After filtering, the filtered filter cake was washed 3 times with 30% ethanol and then 3 times with distilled water, and the obtained solid was vacuum-dried.

The dispersant is polyvinyl alcohol, the molecular weight is between 60,000 and 80,000; the emulsifier is sodium dodecylsulfonate, Tween-80 or OP-10; the organic solvent is chloroform, methylene chloride, xylene or cyclohexane alkyl. The stirring speed when the needle tube is dripping the aqueous phase monomer is 150-250 rev/min.

The above-mentioned alkaloid microcapsules use film-forming polymer materials to coat solid or liquid into tiny particles (2-1000μm). isolated. The invention extracts effective alkaloids and mixtures thereof in various plants, and synthesizes polyurea-wrapped alkaloid microcapsules by using polyamine and polyisocyanate systems in an interfacial polymerization method.

The alkaloids are encapsulated in microcapsules, the palatability is obviously improved, and the speed of oxidation and decomposition in the environment is reduced. The swallowed alkaloid microcapsules are slowly released in the rodents, the acute toxicity of the agent is reduced, and the chronic toxicity is the main one, which can reduce the vigilance of the rodents and reduce the harm to humans, animals and rodent natural enemies.

detailed description

In order to make the objects and advantages of the present invention clearer, the present invention will be specifically described below in conjunction with examples. It should be understood that the following words are only used to describe one or several specific implementation modes of the present invention, and do not strictly limit the protection scope of the specific claims of the present invention.

The alkaloids used in the following examples 1 to 4 are extracted according to the following method:

After the plant sample was crushed mechanically, weighed appropriate powder, put it in a beaker, added 2 times the volume of 95% ethanol, soaked overnight, extracted at 40°C with ultrasonic waves for 30 minutes, vacuum filtered with a Buchner funnel, and the filtrate was rotary evaporated to remove ethanol. The remaining solid was extracted and concentrated in this way, a total of 3 times;

Suspend the obtained solid in distilled water, add 2% hydrochloric acid solution to acidify to pH = 2-3; extract 3 times with 15% dichloromethane by volume of the water phase, and discard the organic phase of dichloromethane;

The aqueous phase was adjusted to pH = 9-10 with 28% ammonia water, extracted three times with dichloromethane equal to the volume of water, the combined organic phases were collected, and the dichloromethane was removed by rotary evaporation to obtain the total alkaloids for use.

Example 1

1) Preparation of aqueous phase solution: dissolve the dispersant polyvinyl alcohol (molecular weight 70,000-80,000) in distilled water, heat and dissolve, and prepare a 2% colloidal solution, add emulsifier Tween 80 to the dispersant solution, and prepare into a 0.5% solution, stirred and dissolved for 5 minutes, and cooled to 50°C.

2) Preparation of organic phase solution: 1.0 ml of toluene diisocyanate was dissolved in 5 ml of chloroform, and 0.02 g of alkaloid was added.

3) Preparation of aqueous phase monomer: 1.0 ml of diethylenetriamine was dissolved in 5 ml of distilled water, and sucked into a needle for use.

4) Reaction procedure, put the reaction container three-neck glass flask in a 50°C water bath, add the organic phase solution to the water phase solution under mechanical stirring, and stir for 10 minutes. After the solution state is stable, add the water phase monomer dropwise with a needle tube , the dropping speed is 1 drop/s, and is stirred at a speed of 150 revolutions/min. After the dropwise addition, react for 2h and cool to room temperature. The reaction solution was suction-filtered with fast filter paper under reduced pressure, the filter cake was washed 3 times with 30% ethanol, and then washed 3 times with distilled water, and the obtained solid was dried in a vacuum desiccator for 1 day to obtain alkaloid microcapsules.

5) Mix alkaloid microcapsules with grain and attractant peanut powder, add water and mix evenly, press the mixture into a columnar shape, and dry in an oven at 45°C for 6 hours to obtain a finished preparation. for:

3 parts by weight of alkaloid microcapsules

Accessories 93 parts by weight

4 parts by weight peanut powder

Example 2

The preparation of alkaloid microcapsules follows the steps below:

1) Preparation of aqueous phase solution: dissolving polyvinyl alcohol (molecular weight 70,000-80,000) in distilled water, heating and dissolving, and preparing 4% colloidal solution. Add emulsifier sodium dodecylsulfonate to the dispersant solution to prepare a 0.5% solution, stir and dissolve for 5 minutes, then cool to 45°C.

2) Preparation of organic phase solution: 1.0 ml of diphenylmethane diisocyanate was dissolved in 10 ml of dichloromethane, and 0.05 g of alkaloid was added.

3) Preparation of water-phase monomer: Dissolve 1.5ml of ethylenediamine in 5-10ml of distilled water, and inhale into a needle for use.

4) Reaction procedure: put the reaction container three-neck glass flask in a 45°C water bath, add the organic phase solution to the water phase solution under mechanical stirring, and stir for 10 minutes. After the solution is stable, add the water phase monomer dropwise with a needle tube , the dropping speed is 1 drop/s, and is stirred at a speed of 200 revolutions/min. After the dropwise addition, react for 2h and cool to room temperature. The reaction solution was suction-filtered with fast filter paper under reduced pressure, the filter cake was washed 3 times with 30% ethanol, and then washed 3 times with distilled water, and the obtained solid was dried in a vacuum desiccator for 1 day to obtain alkaloid microcapsules.

5) Mix the alkaloid microcapsules with grain and the attractant cyclamate, add water and mix evenly, press the mixture into a column, and dry it in an oven at 45°C for 6 hours to obtain a finished preparation. Wherein the content of the original medicine of alkaloid microcapsule, auxiliary material and attractant is:

5 parts by weight of alkaloid microcapsules

Accessories 94 parts by weight

1 part by weight of cyclamate

Example 3

1) Preparation of aqueous phase solution: dissolve the dispersant polyvinyl alcohol (molecular weight 70,000-80,000) in distilled water, heat to dissolve, and prepare a 5% colloidal solution, add emulsifier dodecylbenzene to the dispersant solution Sodium sulfonate was formulated into a 0.5% solution, stirred and dissolved for 5 minutes, and then cooled to 60°C.

2) Preparation of organic phase solution: 1.0 ml of toluene diisocyanate was dissolved in 5 ml of chloroform, and 0.02 g of alkaloid was added.

3) Preparation of water-phase monomer: 1.0 ml of diethylenetriamine was dissolved in 5 ml of distilled water, and sucked into a needle for use.

4) Reaction procedure, put the reaction container three-neck glass flask in a 50°C water bath, add the organic phase solution to the water phase solution under mechanical stirring, and stir for 10 minutes. After the solution state is stable, add the water phase monomer dropwise with a needle tube , the dropping speed is 1 drop/s, and is stirred at a speed of 250 revolutions/min. After the dropwise addition, react for 2h and cool to room temperature. The reaction solution was suction-filtered with fast filter paper under reduced pressure, the filter cake was washed 3 times with 30% ethanol, and then washed 3 times with distilled water, and the obtained solid was dried in a vacuum desiccator for 1 day to obtain alkaloid microcapsules.

5) Mix alkaloid microcapsules with grain and attractant peanut powder, add water and mix evenly, press the mixture into a columnar shape, and dry in an oven at 45°C for 6 hours to obtain a finished preparation. for:

10 parts by weight of alkaloid microcapsules

Accessories 86 parts by weight

4 parts by weight peanut powder

Example 4

The preparation of alkaloid microcapsules follows the steps below:

1) Preparation of aqueous phase solution: dissolving polyvinyl alcohol (molecular weight: 70,000-80,000) in distilled water, heating and dissolving, and preparing a 3% colloidal solution. Add emulsifier OP-10 to the dispersant solution to prepare a 0.5% solution, stir and dissolve for 5 minutes, then cool to 45°C.

2) Preparation of organic phase solution: 1.0 ml of diphenylmethane diisocyanate was dissolved in 10 ml of dichloromethane, and 0.05 g of alkaloid was added.

3) Preparation of water-phase monomer: Dissolve 1.5ml of ethylenediamine in 5-10ml of distilled water, and inhale into a needle for use.

4) Reaction procedure: put the reaction vessel three-necked glass flask in a 50°C water bath, add the organic phase solution to the aqueous phase solution under mechanical stirring, and stir for 10 minutes. After the solution is stable, add the aqueous phase monomer dropwise with a needle tube , the dropping speed is 1 drop/s, and is stirred at a speed of 200 revolutions/min. After the dropwise addition, react for 2h and cool to room temperature. The reaction solution was suction-filtered with fast filter paper under reduced pressure, the filter cake was washed 3 times with 30% ethanol, and then washed 3 times with distilled water, and the obtained solid was dried in a vacuum desiccator for 1 day to obtain alkaloid microcapsules.

5) Mix the alkaloid microcapsules with grain and the attractant cyclamate, add water and mix evenly, press the mixture into a column, and dry it in an oven at 45°C for 6 hours to obtain a finished preparation. Wherein the content of the original medicine of alkaloid microcapsule, auxiliary material and attractant is:

1 part by weight of alkaloid microcapsules

Accessories 98 parts by weight

1 part by weight of white sugar

Example 5

Take 10 healthy mice (5♀5♂) with a body weight of 18-22 g, and fast 12 hours before the test without water. Set up test groups 1 and 2, and a control group. When the test started, the mice in the test group 1 were fed with the medicament (microcapsule-encapsulated alkaloids) prepared in Examples 1-4, and the mice in the test group 2 were fed with the alkaloids without microcapsules. Poisonous bait, fed non-toxic bait to the mice of the control group, and the test was carried out continuously for 7 days, the results are shown in Table 1:

Table 1 Toxicity test of alkaloid microcapsule rodenticide to mice

It can be seen from the feeding coefficient that the palatability of alkaloids wrapped in microcapsules is significantly improved. The shortest death time of the test mice is 48h, and the longest death time is 120h. It is a non-acute rodenticide, and the death rate of the mice in the test group 1 reaches 100%, the rodent killing effect is ideal.

The above is only a preferred embodiment of the present invention. It should be pointed out that for those of ordinary skill in the art, after knowing the content recorded in the present invention, they can also make changes to it without departing from the principle of the present invention. Several equivalent transformations and substitutions should also be deemed to belong to the protection scope of the present invention.

Claims (1)

1. a preparation method of a medicament for preventing and controlling rodent damage, comprising the steps of: The medicament includes 1-10 parts by weight of alkaloid microcapsules and 90-99 parts by weight of auxiliary materials. One or more alkaloids extracted from seeds, the capsule wall composition of alkaloid microcapsules includes polyurea prepared from polyamines and polyisocyanates; S1: extract alkaloids from plants; S2: Prepare the water phase solution, the organic phase solution, and the water phase monomer respectively. First, add the organic phase to the water phase solution and mix well, then add the water phase monomer dropwise and stir for reaction. After the reaction, perform cooling, filtration, washing, Alkaloid microcapsules are obtained after drying, the composition of the aqueous phase solution includes a dispersant and an emulsifier, the composition of the organic phase solution includes polyisocyanates and alkaloids, and the composition of the aqueous phase monomers includes polyamines; S3: mixing the excipients and the alkaloid microcapsules with water according to the specified weight ratio, and then compressing to obtain the rodent control agent; The specific operation of step S1 is: pulverize the raw material and put it in the extraction equipment, add the extractant for ultrasonic extraction, filter and recover the extract, distill and concentrate it into a paste, dissolve the obtained paste solid in distilled water, and add hydrochloric acid to acidify to pH=2～3, then conduct a primary extraction with dichloromethane, recover the aqueous phase extracted once and adjust it to pH=9～10 with ammonia water, perform secondary extraction with dichloromethane again, recover the organic phase extracted twice and Distilled to remove dichloromethane to obtain alkaloids; The specific operation of step S2 is: dissolve the dispersant in distilled water and heat to dissolve, and prepare a 2-5% colloidal solution, then add an emulsifier to the dispersant solution to prepare a 0.5% solution, stir and mix, and then cool to 45 -60°C for use; dissolve polyisocyanate in an organic solvent, then add alkaloid and mix to prepare an organic phase solution for use; dissolve polyamine in distilled water and mix to prepare a water phase monomer for use; polyisocyanate and The volume ratio of organic solvent mixing is 1:5-10, and the alkaloid is added in an amount of 0.01-0.05g alkaloid per milliliter of polyisocyanate; the volume ratio of polyamine and distilled water is 1-1.5:5-10; Add the organic phase solution to the water phase solution, stir and mix in a water bath at 45-60°C, then add the water phase monomer dropwise with a needle tube at a rate of 1 drop/s and stir, react for 2 hours after the dropwise addition, cool to room temperature and Filtration, the filtered filter cake is washed 3 times with 30% ethanol, and then washed 3 times with distilled water, and the obtained solid is vacuum-dried; the dispersant is polyvinyl alcohol, and the molecular weight is between 60,000 and 80,000; sodium nitrite, Tween-80 or OP-10; organic solvents are chloroform, dichloromethane, xylene or cyclohexane; the stirring speed is 150-250 rev/min when adding the aqueous phase monomer drop by needle.