A new method for producing microencapsulated drugs

 

(57) Abstract:

The invention relates to a method of encapsulation of the pesticide. The method comprises (a) combining in water from about 5 to about 60 wt.% the pesticide particles and from about 5 to 20 wt.% the first agent encapsulation, which represents an amide ammonium salt of a copolymer of styrene and maleic anhydride; (b) adding calcium salt and acid to convert the first agent encapsulation in kapsulirujushchej polymer by changing the pH of the water to precipitate the polymer with getting through this encapsulated particles of the pesticide; (c) interaction kapsulirujushchej polymer to calcium salt when heated to a temperature higher than about 40 ° C; (d) the consolidation of dispersed particles from step (C) with the second agent encapsulation selected from the group consisting of copolymers of formaldehyde, polyisocyanates, polyacrylamides and paroxysmal; and (e) heating the resulting combination to a temperature higher than about 40°C. for curing the second agent encapsulation. The invention relates to a method of encapsulation of the pesticide (option) and compositions (options). The invention provides methods of encapsulation, water based, cost-effective and good for OCD is the refining of such materials. 4 C. and 11 C.p. f-crystals.

The invention relates to the improvement of the solid preparations of the chemical reagents. In particular, this invention relates to encapsulated drugs or drugs in suspension capsules (CS) particle compositions of solid chemicals, such as pesticides, and more specifically, it refers to the deposition of solid particles of the coating of polymer films (films) in the aquatic environment.

It is known that solid materials can be microcapsulating by solvent evaporation, solvent extraction, koatservatsii, polymerization in place and spray drying. However, these methods of microencapsulation tend either to engage the use of organic solvents, which are often toxic or hazardous to the environment or human or complex and difficult to apply on an industrial scale. As a result, there are only a few ways using which you can safely and effectively microcapsulating solid insoluble chemicals.

The present invention provides methods of encapsulation, water based and therefore economical and environmentally friendly. odoi such materials. This method can be carried out on relatively simple equipment, using a relatively simple stage of the process.

An unexpected observation was that the encapsulation can be performed using agent encapsulation, which can be transformed into an insoluble form, and which in this insoluble form can form a coating on a solid. In addition, this method of encapsulation unexpectedly can be performed in aqueous suspension without agglomeration of the particles of a solid substance.

Summary of invention

The present invention relates to encapsulated drugs or drugs in suspension capsules (CS) chemicals, which are coated from the first agent encapsulation and an optional second coating of the second agent encapsulation. Particles encapsulated drug preferably have a size of about 1 to 100 microns; more preferably about 1 to 30 μm. Compositions of the present invention are the type that specialists in this field usually called microencapsulated.

The present invention relates also to methods for chemically reamy stages: (a) providing in an aqueous solvent dispersion or suspension of particles of chemical reagea (such as a biologically active agent), water-soluble or dispersible in water first agent encapsulation, which also has the properties of the wetting agent, and, optionally, antifoaming agent; (b) converting the first agent encapsulation in kapsulirujushchej polymer which coagulates or precipitates from the aqueous solvent on the particle chemical reagent and around them, forming encapsulated particles of the chemical reagent.

In preferred embodiments the embodiment of the encapsulated particles remain in suspension. This method can include the stage (s) of interaction besieged kapsulirujushchej polymer with the first compound. Some options include additional stages: (d) optional mixing of the dispersion by adding to it a pure second agent encapsulation or its aqueous solution or dispersion; and (e) an optional second curing agent encapsulation with increasing temperature. In one embodiment, all of the above stage is performed with the particles suspended in the aqueous solvent.

This method has two particularly preferred variant embodiment. If the first agent encapsulation is a polymer phase transformation (b) includes the dispersible oligomers or dispersible polymers, the phase transformation (b) involves the formation of a polymer precipitate from the first agent encapsulation.

In one specific embodiment, the embodiment where the use of the change in pH at the stage of conversion, the first agent encapsulation is a polymer with functional side groups, derivatives of functional groups, anhydrides of carboxylic acids, for example, ammonium salt carboxamido acid. This embodiment is particularly useful derivatives of copolymers of styrene and maleic anhydride.

In another specific embodiment, incarnation, where the transformation involves the formation of a polymer precipitate, the first agent encapsulation is dispersible in water polyisocyanate or polymerizable oligomer suitable resin, such as oligomers, obtained by partial condensation of formaldehyde, for example, phenol, urea or melamine.

Encapsulated particles, optionally, further processed by heating or by heating in combination with hardener, one example of which is calcium lignosulfonate. In some embodiments, the encapsulated particles are subjected to the procedure of the second encapsulation, in which the agent encapsulation the lead two procedures encapsulation, the transformation in the second procedure occurs mainly in the education kapsulirujushchej polymer of the agent encapsulation.

Definition

- Aqueous solvent is a water or a mixture of water and organic solvent, which is freely miscible with water. Ethanol is an example of the organic solvent which can be mixed with water with the formation of the aqueous solvent. Preferably the water is at least about 50% (vol./vol.), more preferably about 95% (vol./about.) water solvent.

The average size of the particles means that at least about 50% of the particles have a diameter within a specified diameter ± 5%, and the diameter shall be measured by light scattering using a device such as an Analyzer of size distribution of particles using laser scattering", Horiba Instrument Corp., Irvine, CA.

- Biologically active agent is a substance, such as a chemical reagent, which can affect cell, virus, organ or organism, including, but not limited to, drugs (i.e. pharmaceuticals and pesticides, to create changes in the activity of the cell, virus, organ or organism. VM agents, which are organic molecules with a molecular weight of about 500 or less or polymeric species, such as proteins, nucleic acids and the like. "Pesticide" is a molecule or combination of molecules that discourage, delay the development or kill pests, such as harmful or annoying insects, weeds, worms, fungi, bacteria and the like (but not limited to), and which can be used for crop protection, protection of structures, soil protection or security of the person; the term pesticide is used here to denote the growth regulators used to stimulate the growth of desirable plant species or to slow the growth of unwanted pests.

Chemical reagent is an organic or inorganic compound, such as compound intended for use as a reagent in synthetic or preparative method, reagent in analytical method, a dye, a biologically active agent, and the like.

- Effective for capsulation number is the number of agent encapsulation, which when used in the method of the present invention is sufficient for the formation of national coverage amount.

Agent encapsulation represents a Monomeric, oligomeric or polymeric substance soluble or dispersible in an aqueous solvent, at least at a certain set of conditions, and which can be converted into an insoluble form when certain changes in the process conditions or chemical form. After such conversion agent encapsulation forms a coating on the particles or homogeneous solid additive particles dispersed or suspended in the aqueous solvent in which is dissolved agent encapsulation.

Functional quantity is the number of agent encapsulation, which, for example, reduces the release of a prisoner in capsules reagent reduces the toxicity of the reagent for mammals, this stabilizes the shape of a reagent that inhibits the crystallization reagent reduces the volatility of the reagent or gives another advantage of the coating of the chemical reagent with the polymer or polymer additives to the chemical reagent.

Microparticles are particles of a chemical reagent with an average diameter from about 1 μm to about 1000 μm.

- Significant increase in viscosity are considered significant increase wascome considered significant increase in viscosity by Brookfield in the range from about 100 to about 200 CP.

Detailed description of the invention

The encapsulation method of the present invention is carried out in accordance with one of several possible variants of embodiment. The method of encapsulation in any case can include adding one or more additives such as xanthan gum; bactericidal agent, for example, 1,2-benzisothiazolin-3-one (from ICI American Inc., Talleyville, DE); amphoteric surface-active substance, such as lauramidopropyl (Proxel®GXL from Rhone-Poulenc Inc., Louisville, KY); inert dye, for example, Tricon Green 18800 (Tricol Colors, Elmwood Park, NJ) or ionic dispersing agent, such as alkylnaphthalenes.

In a particularly preferred variant of embodiment, the particles of the chemical reagent are microparticles that are dispersed in an aqueous solvent and remain in suspension; this method is carried out in a high speed mill, such as a friction mill fine grinding of the pulsating type, in which the first agent encapsulation also acts as a wetting agent.

A typical recipe of the present invention typically contains from about 5 to about 60, preferably from about 20 to about 50 weight percent chemical Rea is the encapsulation relative mass content to be capsulerebel chemical reagent and, if used, from about 0.05 to about 1, preferably from about 0.1 to about 0.9 weight percent antifoaming agent. Antifoaming agents, if they are used, can include, but are not limited to, polydimethylsiloxane.

The present invention, among other things, useful for encapsulation of chemicals that are solid pesticides. The term pesticides includes, but is not limited to, herbicides, insecticides, acaricides, fungicides, nematicides, ectoparasiticide and growth regulators. Solid pesticides that can be microcapsulating according to the present invention, include, but are not limited to, carbamates, urea, triazine, triazole, orally, organophosphates, morpholines, dinitroanilines, acylalanines, pyrethroids and organochlorine compounds. Examples of solid pesticides that can be used in the present invention include, but are not limited to, carbofuran, azinphos-methyl, sulfentrazone, carfentrazone-ethyl, cypermethrin, cyromazine, beta-cyfluthrin, endosulfan and phosmet. If the solid pesticide is a herbicide, the preparations of the present invention regulate the release of herbicide, reducing the rate of release of the herbicide.

Each preferably have the characteristics of a wetting agent, in one variant must be pH-sensitive, so that at acidic pH, they become insoluble in water and deposited on the hydrophobic surface of the particles, as in the basic pH of the polymer was soluble in aqueous solvent. Possessing the properties of the wetting agent and as a pH-sensitive agent encapsulation serves as a wetting agent, and the coating material. The activity of the wetting agent is manifested in the stability in time of the particle size and viscosity of the particles of the chemical reagent in an aqueous solvent in which is dissolved effective for capsulating the number of agent encapsulation and convert it into a form that, as expected, it can capsulerebel these particles. This indicator is the availability of the properties of the wetting agent is of particular importance if there is a hardener, which, as expected, can sew agent encapsulation. However, the properties of the wetting agent is as important, if not use the hardener.

Polymers or resins useful as the first agent encapsulation in one embodiment of the present invention, where the phase transformation causes a change in pH include polyanhydride, in particular copolymers of maleic anhydride, assetsa copolymer metilfenidato ether and maleic anhydride from the ISP, Wayne NJ under the trade mark Agrimer®VEMA. Examples of polymers, derivatives of copolymers of maleic anhydride, are polymers formed by simultaneous or sequential hydrolysis and neutralization of the copolymers of styrene and maleic anhydride (for example, the disodium salt of a copolymer of styrene and maleic anhydride, amide-ammonium salt of a copolymer of styrene and maleic anhydride and ammonium salt of a copolymer of styrene and maleic anhydride). Particularly preferred in this regard, the agent encapsulation is the ammonium salt of carboxamido acid, a derivative of a copolymer of styrene and maleic anhydride (i.e. amide-ammonium salt of a copolymer of styrene and maleic anhydride), from Solutia, Springfield MA, brand Scripset®720. Other polymers which are useful as agents, encapsulation, if the phase transformation causes a change in pH include polysaccharides; acrylic polymers, including polymers of acrylic acid or acrylamide; hydrophobically modified polyacrylic acid; esters of phosphates, acid and sodium salt; N-methylolacrylamide and a copolymer of vinyl chloride-vinyl acetate-hydroxyacrylates.

In one variant embodiment of the encapsulation OS is uppy, you can lower the pH of the aqueous suspension of particles to a value of from about 4 to about 7, preferably to about 6. After adjusting the pH by adding acid, and optionally adding a first curing agent dispersion, optional, structure, heating to a temperature in the range from about 40 to about 90, preferably from about 50 to about 80 ° C, for example, during the period from about 10 minutes to about five hours, preferably from about 10 minutes to about two hours.

For the subsequent wet grinding is usually used mill with high shear. The time within which produce wet grinding aqueous dispersion of microparticles is not critical, but generally ranges from about 15 to about 50 minutes. Factors affecting particle size, which determines the final size of the microcapsules and the stability of the suspension include the speed and duration of grinding, the type and amount of agent encapsulation, temperature and viscosity, and the presence of xanthan resin and agent dispersion alkylnaphthalene, if any, use. Choosing the appropriate size of the microcapsules for the purposes of this invention requires the highest particle size, decreasing below a certain amount, the particle size will increase, and the coating of the microcapsules may be heterogeneous. The increase in the number of the first agent encapsulation can provide a more uniform coating, but above a certain amount as a result of agglomeration can be particles of larger size. In preferred embodiments of the present invention, these parameters are chosen so that a functional number for encapsulation with minimal agglomeration occurring during encapsulation.

In one variant embodiment of the present invention, the average size of the microcapsules is from about 1 to about 100 microns, preferably from about 1 to about 30 microns. Conditions to obtain microcapsules of the desired size depends on various factors, including, where applicable, the size of the original particles, the equipment used for wet grinding, the amount of agent encapsulation and curing agent, the number of stages of coating and the like. For example, typically receive a smaller particle size, if you use less of the agent encapsulation and longer wet grinding. In the light on odawa conditions for encapsulation in the scope of the present invention.

For example, in some embodiments, embodiments of the amount of added acid, if such is used, may be from about 0.05 to about 5.0 and preferably from about 0.1 to about to 3.0 mass% relative to the total weight of the preparation, although this range can vary depending on the type of agent encapsulation and type of the used acid. In General the mass of the added acid is essential to bring the pH of the aqueous solvent to a value of between about 4 and about 6. Acid, which can be useful in certain embodiments of the embodiment of the present invention, can be either a proton acids or Lewis acids. Examples of protonic acids or Lewis acids that can be used include, but are not limited to, hydrochloric acid, Hydrobromic acid, idiscovered acid, sulfuric acid, acetic acid, perchloric acid, triperoxonane acid and 2,2,2-triptorelin.

Preferred is acetic acid.

For example, the first hardeners which can be used in accordance with certain variants of the embodiment of the present invention, represent a divalent salt: lignosulfates, vinyltriethoxysilane), aldehydes, polyhydroxy, epoxides and water soluble resins. Examples of suitable divalent salts still include, but are not limited to, calcium chloride, calcium carbonate, magnesium chloride, calcium lignosulfonate, Las calcium and calcium stearate. An example of a suitable diamine is 2-methylpentylamine (from DuPont, Willmington, DE, under the trade mark Dytek®A). An example of a suitable water soluble resins is Cymel®1141 from Cytec, W. Paterson NJ. Preferred and economical first curing agent is calcium lignosulfonate. If you use the same hardener, it is usually added amount is from about 0.5 to about 10, preferably from about 1 to about 5 weight percent relative to the total quantity of the drug. The amount used of the first curing agent varies depending on the type of the first curing agent. For example, if the first curing agent is calcium lignosulfonate, then use more of the first hardener than in the case of use as a first curing agent is calcium chloride.

In some embodiments of the incarnation, where the stage of converting includes obtaining ianity or soluble or dispersible in water resin, such as copolymers of formaldehyde, polyacrylamides and proximally. Examples of copolymers of formaldehyde, polyacrylamides and paroxysmal that can be used in the present invention are urea resin, melamineformaldehyde resin, phenol resin, resorcinolformaldehyde resin, bottled urea-formaldehyde resin, glycopyrrolate resin and methylolacrylamide. Among these agents, encapsulation preferred melamineformaldehyde resin, polymethylacrylate and especially dispersible in water polyisocyanates. Particularly preferred dispersible in water polymeric or oligomeric isocyanates are compounds based on alkylenediamine in which Allenova group may optionally include a cyclic structure. Particularly preferred dispersible in water oligomeric or polymeric diisocyanates contain the remains of hexamethylenediisocyanate (for example, Bayhydur XP-7063; Bayer Corporation, Pittsburgh, PA).

In some preferred embodiments the embodiment mentioned kapsulirujushchej polymers used in the second stage, encapsulation, and thus, these agents encapsulation, which form the polymerase is implemented agent encapsulation, if used, is usually from about 0.5 to about 10, preferably from about 1 to about 5 mass percent relative to the total mass capsulerebel material.

When specified in the previous paragraph agents encapsulation used in the second stage of encapsulation, it is preferable to add the agent encapsulation more carefully than I prefer in some embodiments, the first encapsulation. For example, you can apply the mixing. The stirring is preferably continued during the curing agent encapsulation when heated to a temperature of from about 40 to about 80, preferably about 70C during, for example, a period of from 10 minutes to ten hours, preferably from one to four hours.

The quantity after encapsulation of additives is the same for all options, and you should generally choose one or more and a content of from about 0.003 to about 0.5, preferably from about 0.005-0.3 weight percent xanthan resin; from about 0.01 to about 0.1, preferably from about 0.01 to about 0.08 to weight percent of one of bactericidal agents; about 0.05, preferably about to 0.04 mass Ave is, each mass percentage relative to the weight of the drug after making additives.

In some embodiments, embodiments of the suspension of the chemical reagent in an aqueous solvent, hardener or without a filter to remove particles with an average size greater than the selected value, namely about 100 microns. For example, the stage filtering can be applied in order to ensure that at least 90% of microencapsulated particles have a size less than about 30 microns.

The preparations of the present invention receive in accordance with the procedures shown below in the examples. The examples serve only to illustrate this invention and should not be construed as restrictive, although specialists in this field further obvious modifications of the disclosed invention. All such modifications should be considered included in the scope of this invention defined by the claims.

Example 1

Receiving the drug in suspension capsules carbofuran 250 g/l (250 CS)

A mixture of 20.0 g of 25% aqueous solution of amide-ammonium salt of a copolymer of styrene and maleic anhydride (Scripset®720, Solutia, Springfield, MA), 100.0 g of carbofuran (FMC Corporation, Chicago, IL), 0.5 g 100% antifoaming agenda to grind for 30 minutes at high speed in a friction mill fine grinding pulsating type (Union Process Type Attritor Mill, Union Process, Inc., Akron, OH). Thereafter, the aqueous dispersion of microparticles were filtered into a glass stainless steel one liter. To the filtrate was added 4.0 g of calcium chloride and 65.0 g of water. Brought the pH of the mixture to 5.7 by adding 0.8 g (20 drops) of acetic acid. Then the suspension was heated to 50 with stirring at about 200 to about 350./min for one hour, using the upper agitator blade type. After this was added 10.0 g of partially methylated melamineformaldehyde resin (Cymel 385, Cytec Industries Inc., West Paterson, NJ). After adding the drug was heated to 70 C and was stirred for one hour. At the end of this period to the mixture was added to 20.0 g aqueous 1% xanthan gums (Kelzan®'s, Monsanto, St. Louis, MO) and 10.0 g of non-ionic polymeric surfactants (Atlox®4913, ICI Americas Inc., Wilmington, DE, a subsidiary of Imperial Chemical Industries Surfactants). After stirring for thirty minutes, the product had a viscosity 336 SP.

Example 2

Receiving the drug in suspension capsules carbofuran 250 g/l (250 CS)

A mixture of 20.0 g of 25% aqueous solution of amide-ammonium salt of a copolymer of styrene and maleic anhydride (Scripset®720), 100.0 g of carbofuran, 1.0 g 100% antifoaming agent polydimethylsiloxane speed in a friction mill fine grinding pulsating type (Union Process Type Attritor Mill, Union Process, Inc., Akron, OH). Thereafter, the aqueous dispersion of microparticles were filtered into a glass stainless steel one liter. Brought the pH of the filtrate (dispersion) to 5.4 by adding a pre-mixed solution of 8.0 g of calcium lignosulfonate (Norlig®11 DA, Ligno Tech USA, Rothschild, WI), 0.8 g (20 drops) of acetic acid and 65.0 g of distilled water. The suspension was heated to 70 C under stirring for about one hour through the top of the agitator vane type. After this was added 6.0 g of N-methylolacrylamide (Cylink®NMA-LF, Cytec Industries Inc., West Paterson, NJ). After adding the drug was heated to 70 C and was stirred for one hour. At the end of this period to the mixture was added 10.0 g water to 1% xanthan gums (Kelzan®S) and 10.0 g of non-ionic polymeric surfactants (Atlox®4913). After stirring for ten minutes, the product had a viscosity of 82 JV.

Example 3

Receiving the drug in suspension capsules carbofuran 250 g/l (250 CS)

A mixture of 30.0 g of 25% aqueous solution of amide-ammonium salt of a copolymer of styrene and maleic anhydride (Scripset®720), 100.0 g of carbofuran, 1.0 g 100% antifoaming agent polydimethylsiloxane (Dow Corning 1520) and 90.0 g of distilled water rayed youseo type (Union Process Type Attritor Mill, Union Process, Inc., Akron, OH). Thereafter, the aqueous dispersion of microparticles were filtered into a glass stainless steel one liter. Brought the pH of the filtrate (dispersion) to 5.6 by adding a pre-mixed solution of 8.0 g of calcium lignosulfonate (Norlig®11 DA), 1.2 g (30 drops) of acetic acid and 65.0 g of distilled water. The suspension was heated to 70C with stirring at a rate of 200 to 350 rpm for about two hours, using the upper agitator blade type. Then to the mixture was added 10.0 g water to 1% xanthan gums (Kelzan®S) and 10.0 g of non-ionic polymeric surfactants (Atlox®4913).

The preparation was stirred for about another ten minutes.

Example 4

Receiving the drug in suspension capsules carbofuran 250 g/l (250CS)

A mixture of 40.0 g of aqueous 25% solution of amide-ammonium salt of a copolymer of styrene and maleic anhydride (Scripset®720), 96,0 g of carbofuran, 1.0 g 100% antifoaming agent polydimethylsiloxane (Dow Corning®1520) and 90.0 g of distilled water were subjected to wet grinding for 20 minutes at high speed in a friction mill fine grinding pulsating type (Union Process Type Attritor Mill, Union Process, Inc., Akron, OH). After this aqueous dispersion is 9, adding a pre-mixed solution of 8.0 g of calcium lignosulfonate (Norlig®11 DA), 2.0 g (50 drops) of acetic acid and 65.0 g of distilled water. The suspension was stirred for one hour at a temperature of about 25 ° C and the stirring speed 200-350 rpm, using the upper agitator blade type, and then added 10.0 g dispersible in water MDI (Bayhydur®XP-7063, Bayer Corp., Pittsburgh, PA). Upon completion of the addition the mixture was heated to 60C and stirred for about 1.5 hours. After this was added to a mixture of 40.0 g of 1% xanthan gums (Kelzan®S) and all of 25.0 g of salt of sodium lignosulphonate (15.0 g Lignosol®SFX-65L and 10.0 grams of Marasperse®B-22, both from Ligno Tech USA, Rothschild, WI). After stirring for ten minutes, the product had a viscosity according to Brookfield 208 SP.

Despite the fact that this invention is described with emphasis on the preferred options of the incarnation, the experts in this field it is obvious that you can use variations of the preferred devices and methods, and have in mind that this invention may be implemented differently than described here. Thus, this invention includes all modifications encompassed by the spirit and scope of the invention as defined by the following d is about 5 to about 60 wt.% the pesticide particles and from about 5 to 20 wt.% the first agent encapsulation, representing amide-ammonium salt of a copolymer of styrene and maleic anhydride; (b) adding calcium salt and acid to convert the first agent encapsulation in kapsulirujushchej polymer by changing the pH of the water to precipitate the polymer with getting through this encapsulated particles of the pesticide; (c) interaction kapsulirujushchej polymer to calcium salt when heated to a temperature higher than about 40 ° C; (d) the consolidation of dispersed particles from step (C) with the second agent encapsulation selected from the group consisting of copolymers of formaldehyde, polyisocyanates, polyacrylamide, phenoxy-resins; and (e) heating the resulting combination to a temperature higher than about 40°C. for curing the second agent encapsulation.

2. The method according to p. 1, wherein the change in pH means lowering the pH by adding acid to a value lower than about 6.

3. The method according to p. 1, where the second agent encapsulation is a polyisocyanate.

4. The method according to p. 1 wherein the calcium salt is calcium chloride.

5. The method according to p. 1 wherein the calcium salt is calcium lignosulfonate.

6. The method according to p. 2, where acid is added together with a salt of calcium.

7. SPO p. 1, containing a suspension of solid particles of the pesticide in water in which the particles are encapsulated in the first agent encapsulation; and the first agent encapsulation is an amide-ammonium salt of a copolymer of styrene and maleic anhydride; encapsulation of the particles is carried out by changing the pH of the water to about 6 to ensure deposition of the amide-ammonium salt of a copolymer of styrene and maleic anhydride and encapsulated particles are covered with a second agent encapsulation selected from the group consisting of copolymers of formaldehyde, polyisocyanates, polyacrylamide, phenoxy-tar.

9. The method of encapsulation of a pesticide, comprising (a) combining in water from about 5 to about 60 wt.% the pesticide particles and from about 5 to 20 wt.% agent encapsulation, which represents an amide ammonium salt of a copolymer of styrene and maleic anhydride; (b) adding calcium salts and acids for conversion agent encapsulation in kapsulirujushchej polymer by changing the pH of the water to precipitate the polymer with formation through this encapsulated particles of the pesticide and (c) interaction kapsulirujushchej polymer to calcium salt when heated to a temperature higher than about 40C.

10. The method according to p. 9, when koto. The method according to p. 9, where the calcium salt is calcium chloride.

12. The method according to p. 9, where the calcium salt is calcium lignosulfonate.

13. The method according to p. 9, where the acid is added together with a salt of calcium.

14. The method according to p. 9, where the calcium salt is added before adding the acid.

15. The composition obtained by the method according to p. 9, containing a suspension of solid particles of the pesticide in water in which the particles are encapsulated in the amide-ammonium salt of a copolymer of styrene and maleic anhydride; encapsulation of the particles is carried out by changing the pH of the water to about 6 to ensure deposition of the amide-ammonium salt of a copolymer of styrene and maleic anhydride.

 

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43 cl, 16 ex, 4 tbl

FIELD: biotechnologies.

SUBSTANCE: invention relates to microbiological industry, in particular to insecticide agents used to control larvae of flies. Insecticide agent contains bacteria Bacillus thuringiensis var. israelensis immobilised into granules of alginate gel, fungi having entomopathogenic activity to larvae of flies and additives. Insecticide agent preferably contains fungi Tolypocladium cylindrosporum as fungi having entomopathogenic activity to larvae of flies, additives include nutrient substances (starch, gelatine) and substances that impart floatability to granules of insecticide agent (vegetable oils).

EFFECT: invention makes it possible to increase efficiency of fly larvae control.

5 cl, 1 dwg, 19 ex

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