Method of obtaining microcapsules of heterocyclic compounds of triazine series

FIELD: chemistry.

SUBSTANCE: invention relates to field of microcapsulation of heterocyclic compounds of triazine series. Method of obtaining microcapsules of triazine series pesticides is characterised by the fact that 0.1 g of triazine series pesticide and 0.02 g of E472c preparation as emulsifying agent are added to 10 g of 5% water solution of polyvinyl alcohol (PVA) and obtained mixture is subjected to mixing. Reaction mixture components are dissolved until transparent solution is formed after which 5 ml of carbinol as the first precipitating agent and then 10 ml of isopropanol as the second precipitating agent are added slowly drop-by-drop. After that, obtained suspension of microcapsules is kept for 1 minute, filtered on filter, washed with propanol several times, dried, with method being realised at 25C without special equipment.

EFFECT: simplification of the process of obtaining microcapsules and increase output by weight.

3 ex

 

The invention relates to the field of microencapsulation of heterocyclic compounds, triazines, which are used in the pharmaceutical industry and agriculture as pesticides.

Previously known methods for producing microcapsules. Thus, in U.S. Pat. 2092155, IPC A61K 047/02, A61K 009/16 published 10.10.1997, Russian Federation, proposed a method for microencapsulation of drugs, based on the use of special equipment use of irradiation with ultraviolet rays.

The disadvantages of this method are the duration of the process and the use of ultraviolet radiation, which can influence the formation of microcapsules.

In Pat. 2095055, IPC A61K 9/52, A61K 9/16, A61K 9/10, Russian Federation published 10.11.1997, method for obtaining solid non-porous microspheres, which comprises melting pharmaceutically inactive substance carrier, the dispersion of a pharmaceutically active substance in the melt in an inert atmosphere, spraying the resulting dispersion in the form of a mist in the freezing chamber under pressure, in an inert atmosphere at a temperature of from -15 to -50C, and the separation of the obtained microspheres into fractions by size. The suspension is intended for administration by parenteral injection, contains an effective amount of these microspheres. edelenyi in a pharmaceutically acceptable liquid vector, and the pharmaceutically active substance is insoluble microspheres in a specified liquid medium.

Disadvantages of the proposed method: duration of the process, the use of special equipment.

In Pat. 2091071, IPC A61K 35/10, Russian Federation, published 27.09.1997, method for obtaining the drug by dispersion in a ball mill to obtain microcapsules.

Disadvantages of the proposed method is the length of the process and application of ball mill, which can lead to the destruction of the microcapsules.

In Pat. 2076765, IPC B01D 9/02, Russian Federation, published 10.04.1997, method for obtaining dispersed particles of soluble compounds in the microcapsules by crystallization from a solution, wherein the solution is dispersed in an inert matrix, cooled and, by changing the temperature, get dispersed particles.

The disadvantage of this method is the difficulty of execution: obtaining microcapsules by dispersion with subsequent change of temperatures, which slows down the process.

In Pat. 2101010, IPC A61K 9/52, A61K 9/50, A61K 9/22, A61K 9/20, AC/19, the Russian Federation, published 10.01.1998 proposed chewable form of the drug with taste masking, having the properties of a controlled release drug product that contains microcapsules R is Merom 100-800 microns in diameter and consists of pharmaceutical kernel crystalline ibuprofen and polymer coating, including plasticizer, elastic enough to resist chewing. The polymer coating is a copolymer based on methacrylic acid.

The drawbacks of the invention: use of a copolymer based on methacrylic acid, as these polymer coatings can cause cancer; complexity; the duration of the process.

In Pat. 2139046, IPC A61K 9/50, A61K 49/00, A61K 51/00, Russian Federation, published 10.10.1999, method for obtaining microcapsules as follows. Emulsion oil-in-water prepared from organic solution containing dissolved mono-, di-, triglyceride, preferably of tripalmitin or tristearin, and possibly therapeutically active substance, and an aqueous solution containing a surfactant, it is possible to evaporate part of the solvent, add redispersible agent and the mixture is subjected to drying by freezing. Subjected to drying by freezing the mixture is then dispersed in an aqueous medium to separate the particles from organic substances and a hemispherical or spherical microcapsules dried.

Disadvantages of the proposed method are the complexity and duration of the process, the use of drying by freezing, which takes time and slows down the process of production of microcapsules.

In Pat. 2159037,IPC A01N 25/28, A01N 25/30, Russian Federation, published 20.11.2000, proposed a method of producing microcapsules by polymerization reaction at the phase boundary, containing solid agrochemical material 0.1 to 55 wt.%, suspended in peremestivsheesya water organic liquid, from 0.01 to 10 wt.% non-ionic dispersant, active on the phase boundary and is not acting as an emulsifier.

Disadvantages of the proposed method: the complexity, duration, using wysokosciowe mixer.

In the article "Razrabotka microencapsulated and gel products and materials for various industries", Russian chemical journal, 2001, I. XLV, No. 5-6, S. 125-135, describes a method of producing microcapsules of drugs by the method of gas-phase polymerization, since the authors considered unsuitable method of chemical koatservatsii from aqueous media for microencapsulation of drugs due to the fact that most of them are water-soluble. The process of microencapsulation by the method of gas-phase polymerization using n-xylylene includes the following basic stages: evaporation dimer n-xylylene (170C), thermal decomposition of it into the pyrolysis furnace (650C at a residual pressure of 0.5 mm RT.cent.), the transfer of the reaction products in the "cold" chamber of polymerization (20C, the residual pressure of 0.1 mm RT.cent.), aside the s and polymerization at the surface of the protected object. Luggage polymerization is performed in the form of a rotating drum, the optimal speed for powder coating 30 rpm, the Thickness of the shell is governed by the time of coating. This method is suitable for the encapsulation of any solids (except prone to intense sublimation). The resulting poly-n-xylylene - vysokokritichnyh polymer with high orientation and dense packing, provides a conformal coating.

Disadvantages of the proposed method are the complexity and duration of the process, using the method of gas-phase polymerization, which makes the method inapplicable to obtain microcapsules of drugs in polymers protein nature due to the denaturation of proteins at high temperatures.

In the article "Development of micro - and nano drug delivery", Russian chemical journal, 2008, t.LII, No. 1, S. 48-57 presents a method of obtaining microcapsules included with proteins, which does not significantly reduce their biological activity carried out by the process of interfacial crosslinking of soluble starch or hydroxyethylamine and bovine serum albumin (BSA) using terephthaloyl chloride. The proteinase inhibitor is Aprotinin, either native or protected with an active center was microcapsular in his introduction to the composition of the aqueous phase. CPF is on form liofilizovannyh particles indicates obtaining microcapsules or particles tank types. Thus prepared microcapsules were not damaged after lyophilization and easily restored its spherical shape after rehydration in a buffered environment. The pH value of the aqueous phase was crucial in obtaining a solid microcapsules with high output.

The disadvantage of the proposed method of producing microcapsules is the complexity of the process that leads to the reduction of the yield of microcapsules.

In Pat. 2173140, IPC A61K 009/50, A61K 009/127, Russian Federation, published 10.09.2001, method for obtaining kremnijorganicheskih microcapsules using a rotary cavitation plants with high shear effort and powerful acoustic phenomena of sound and ultrasound range for dispersion.

The disadvantage of this method is the use of special equipment - rotary-quotational installation, which has ultrasonic action that affects the formation of microcapsules and can cause adverse reactions due to the fact that ultrasound destructive effect on the polymers of protein nature, therefore the proposed method is applicable when working with polymers of synthetic origin.

In Pat. WO/2010/137743 JP, IPC A01N 25/28; A01N 51/00; A01P 7/04; B01J 13/16 published 02.12.2010, a method for the production of microcapsules containing pesticide compounds in epiretinal acid, that delays the release timing of pesticide compounds in comparison with the conventional microcapsules. In the method of producing microcapsules includes:

1) maintaining a mixture of the pesticide compound with polyisocyanate from 20 to 60C for 3 hours or more;

2) adding to the mixture of water containing polyols or polyamine, and preparations for the formation of liquid droplets in the water;

3) formation of a film of polyurethane or polyurea around the drops.

The disadvantages of these methods are the use of special equipment (rotary homogenizer), a multi-stage, which complicates the method of producing microcapsules and makes it long.

The closest method is the method proposed in U.S. Pat. 2165700, Russian Federation, IPC A01N 25/28, A01N 53/00, A01N 57/00, published 27.04.2001, which describes a method of obtaining a microencapsulated insecticide, which is as follows: the solution mixture in an organic solvent composed of natural lipids and organophosphorus and/or a PYRETHROID insecticide in the weight ratio of 2-4:1, was dispersed in water to obtain the desired product. Using the proposed method allows to significantly simplify the process of encapsulation of insecticides and provides high quality insecticide preparation.

The disadvantage of the method proposed in U.S. Pat. 2165700, the two which is a dispersion in an aqueous medium, what makes the proposed method applicable to the production of microcapsules of water-soluble drugs in water-soluble polymers.

The technical problem is to simplify the process of production of microcapsules of the drug in water-soluble polymers, increasing the yield by weight.

The solution of the technical problem is achieved by a method of producing microcapsules of heterocyclic compounds, triazines, wherein upon receipt of the microcapsules physico-chemical method for the deposition nerastvorim uses two precipitator - carbinol and isopropanol, and as the shell of the microcapsules is polyvinyl alcohol, the retrieval process is carried out without special equipment.

A distinctive feature of the proposed method is the use of two precipitators, carbinol and isopropanol, upon receipt of the microcapsules physico-chemical method for the deposition nerastvorim and polyvinyl alcohol as the shell of the microcapsules.

The result of the proposed method is to obtain microcapsules of pesticides at 25C for 15 minutes.

EXAMPLE 1 Obtaining microcapsules of metribuzin in polyvinyl alcohol (PVA), a ratio of 1:5

To 10 g of 5% aqueous solution of PVA added 0.1 g of metribuzin and 0.02 g of the drug E472c as an emulsifier. The resulting mixture is put on a stirring 1000 R/C. After dissolution of the components is tov the reaction mixture until a clear solution is formed - very slowly dropwise 5 ml of carbinol as the first precipitator, and then 10 ml of isopropanol as the second. The resulting suspension of microcapsules leave on for 1 minute, then sucked on the filter SCHOTT 16 class then washed several times with isopropanol and dried.

Received 0,510 g of powder of microcapsules. The yield was 85%.

EXAMPLE 2 Obtaining microcapsules of propiconazole in polyvinyl alcohol (PVA), a ratio of 1:5

To 10 g of 5% aqueous solution of PVA added 0.1 g of propiconazole and 0.02 g of the drug E472c as an emulsifier. The resulting mixture is put on a stirring 1000 R/C. After dissolution of the components of the reaction mixture until a clear solution is formed very slowly dropwise 5 ml of carbinol as the first precipitator, and then 10 ml of isopropanol as the second. The resulting suspension of microcapsules leave on for 1 minute, then sucked on the filter SCHOTT 16 class then washed several times with isopropanol, dry.

Received 0,498 g of powder of microcapsules. The yield was 83%.

EXAMPLE 3 Obtaining microcapsules of tebuconazole in polyvinyl alcohol (PVA), a ratio of 1:5

To 10 g of 5% aqueous solution of PVA added 0.1 g of tebuconazole and 0.02 g of the drug E472c as an emulsifier. The resulting mixture is put on a stirring 1000 R/C. After dissolution of the components of the reaction mixture to education about the solution for this at all - very slowly dropwise 5 ml of carbinol as the first precipitator, and then 10 ml of isopropanol as the second. The resulting suspension of microcapsules leave on for 1 minute, then sucked on the filter SCHOTT 16 class then washed several times with isopropanol and dried.

Received 0,546 g of powder of microcapsules. The yield was 91%.

Thus, the obtained microcapsules heterocyclic triazines. This technique is characterized by high yields, simple design, requires no special equipment and is applicable to both the examples of substances, and any others that contain triazine cycle. In addition, in the described manner it is possible to obtain microcapsules compounds, triazines, which will only be synthesized by chemists organically in the future. The proposed method is applicable for pharmaceutical and agricultural industries.

The method of producing microcapsules pesticides, triazines, characterized by the fact that 10 g of 5% aqueous solution of polyvinyl alcohol (PVA) add 0.1 g of pesticide triazines and 0.02 g of the drug Is as an emulsifier, the resulting mixture is put on a stirring and after the dissolution of the components of the reaction mixture until a clear solution is formed very slowly added dropwise 5 ml of ka is binol as the first precipitator, and then 10 ml of isopropanol as a co-precipitant, and then the resulting suspension of microcapsules leave on for 1 minute, filtered on a filter, washed several times with isopropanol, dried, and the process is carried out at 25 C without special equipment.



 

Same patents:

FIELD: chemistry.

SUBSTANCE: method of obtaining microcapsules of triazine series pesticides is characterised by the following: 0.1 g of triazine series pesticide and 0.02 g of E472c preparation as emulsifier are added to 10 g of 5% water solution of polyvinyl alcohol (PVA), and obtained mixture is subjected to mixing. After dissolution of reaction mixture components and formation of transparent solution 15 ml of isopropanol are very slowly drop-by-drop poured in, and obtained suspension of microcapsules is stayed for 1 minute, filtered on filter, washed several times with isopropanol and dried. Method is realised at 25C without special equipment.

EFFECT: simplification of the process of obtaining microcapsules and increased output by mass.

3 ex

FIELD: chemistry.

SUBSTANCE: method is characterised by the fact that 100 mg of iron sulphate or zinc sulphate are dissolved in 1 ml of water and obtained mixture is dispersed into carrageenan solution in acetone, which contains 300 mg of carrageenan, in presence of 0.01 g of E472c preparation with mixing. After that, 2 ml of ethanol are added, obtained suspension is filtered and dried at room temperature, with realisation of the method without special equipment.

EFFECT: simplification and acceleration of the process of obtaining microcapsules and increase of output by mass.

2 ex

FIELD: chemistry.

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EFFECT: simplification and acceleration of the process of obtaining microcapsules and increased output by mass.

2 ex

FIELD: chemistry.

SUBSTANCE: invention relates to agriculture. The agrochemical composition contains microcapsules. The active ingredient in the capsules is selected from a group comprising chlorpyrifos, fluroxypyr, diflufenican, sulphonylurea and mixtures of diflufenican with sulphonylureas, fluroxypyr with sulphonylureas, chloropyrifos with sulphonylureas, chlorpyrifos with fluroxypyr, fluroxypyr with diflufenican, or is selected from a group comprising triazole fungicides, and mixtures with fluroxypyr and/or chlorpyrifos. In case of mixtures, at least one of the active ingredients is microencapsulated. The microcapsules have size of 1-30 mcm. The shell of the microcapsules is made from polyurea which is formed during reaction of an aromatic isocynate and mono-, di-, tri- or tetra-alkoxyalkylglycoluril, where alkoxy denotes methoxy, ethoxy or isopropoxy, and alkyl denotes methyl, ethyl or isopropyl. The agrochemical composition contains 1-45 wt % styrene acrylic polymer. The reaction of materials which form the shell takes place in aqueous phase. The agrochemical composition is used against fungi, weeds and/or insects.

EFFECT: invention increases stability of the composition.

23 cl, 2 ex, 1 tbl

FIELD: medicine, pharmaceutics.

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21 cl, 4 dwg, 13 ex

FIELD: food industry.

SUBSTANCE: encapsulated antimicrobial material includes (i) a kernel containing an antimicrobial material and a shell (ii) out of an encapsulated material which is a hydrophobic shell with a melting temperature higher than 45C. It is selected out of a group including animal oils and fats, completely hydrogenated vegetable or animal oils, partially hydrogenated vegetable or animal oils, unsaturated hydrogenated or completely hydrogenated fatty acids, unsaturated hydrogenated or completely hydrogenated monoglycerides and diglycerides of fatty acids, unsaturated hydrogenated or completely hydrogenated etherified monoglycerides and diglycerides of fatty acids, unsaturated partially hydrogenated or completely hydrogenated free fatty acids, other emulsifiers, animal waxes, vegetable waxes, mineral waxes, synthetic waxes, natural and synthetic resins as well as their mixtures. The hydrophobic shell is impermeable for the antimicrobial material and is selected to provide release of the antimicrobial material from the encapsulated antimicrobial material while in contact with food products and the antimicrobial material is bacteriocin selected from the lanthionine-containing bacteriocins, bacteriocins formed by Lactococcus, bacteriocins formed by Streptococcus, bacteriocins formed by Pediococcus, bacteriocins formed by Lactobacillus, bacteriocins formed by Camobacterium, bacteriocins formed by Leuconostoc, bacteriocins formed by Enterococcus and their mixtures. The composition contains the antimicrobial material and a carrier. The food product contains the product and the antibacterial material. The method is implemented by introducing the antimicrobial material into the food product.

EFFECT: invention ensures a long antimicrobial effect.

43 cl, 16 ex, 4 tbl

FIELD: food and pharmaceutical industries.

SUBSTANCE: object of invention is production of freely flowing alcohol-containing encapsulated products. Food fat and/or wax are melted in heated reactor at 55-65°C, after which required food additives or additive complexes are added, resulting mixture is stirred to achieve homogenous mass and alcoholic produce with alcohol content from 5 to 96.6% is added in amount 5 to 60 wt parts per 100 wt parts of the reactor charge. Emulsion obtained is supplied to atomization turbine wherein arising drops are solidified in air and collected in receiving device. Thus obtained powder is screened and tightly packaged. Granule size is controlled by turbine rotation speed and varied within a range of 0.1 to 1 mm.

EFFECT: enabled creation of fundamentally novel formulations and production technologies, improved quality, reduced expenses, and prolonged shelf time of produce.

3 cl, 6 ex

The invention relates to compositions containing at least one microencapsulated additive for rubber

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FIELD: chemistry.

SUBSTANCE: method of obtaining microcapsules of triazine series pesticides is characterised by the following: 0.1 g of triazine series pesticide and 0.02 g of E472c preparation as emulsifier are added to 10 g of 5% water solution of polyvinyl alcohol (PVA), and obtained mixture is subjected to mixing. After dissolution of reaction mixture components and formation of transparent solution 15 ml of isopropanol are very slowly drop-by-drop poured in, and obtained suspension of microcapsules is stayed for 1 minute, filtered on filter, washed several times with isopropanol and dried. Method is realised at 25C without special equipment.

EFFECT: simplification of the process of obtaining microcapsules and increased output by mass.

3 ex

FIELD: chemistry.

SUBSTANCE: method is characterised by the fact that 100 mg of iron sulphate or zinc sulphate are dissolved in 1 ml of water and obtained mixture is dispersed into carrageenan solution in acetone, which contains 300 mg of carrageenan, in presence of 0.01 g of E472c preparation with mixing. After that, 2 ml of ethanol are added, obtained suspension is filtered and dried at room temperature, with realisation of the method without special equipment.

EFFECT: simplification and acceleration of the process of obtaining microcapsules and increase of output by mass.

2 ex

FIELD: chemistry.

SUBSTANCE: method is characterised by the fact that 100 mg of iron sulphate of zinc sulphate are dissolved in 1 ml of water and obtained mixture is dispersed into solution of kappa-karrageenan in dioxane, which contains 300 mg of kappa-karrageenan, in presence of 0.01 g of E472c preparation with mixing. After that, 2 ml of methylcarbinol are poured in, obtained suspension is filtered and dried at room temperature, with realisation of the method without special equipment.

EFFECT: simplification and acceleration of the process of obtaining microcapsules and increased output by mass.

2 ex

FIELD: chemistry.

SUBSTANCE: fenbendazole solution is dispersed in a solution of sodium carboxymethyl cellulose in ethyl acetate containing an E472c preparation, with ratio of fenbendazole to sodium carboxymethyl cellulose of 1:3, followed by addition of butanol and distilled water, filtering the obtained suspension of microcapsules and drying at room temperature.

EFFECT: simple and faster process of producing fenbendazole microcapsules and high mass output.

3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to the encapsulation of a hydrophobic liquid by an enteric matrix without the application of organic solvents. A material of the enteric matrix is selected from the group, consisting of zein, shellac and their mixtures. A method of microencapsulation of an active ingredient by the enteric matrix includes mixing of a combination of water, material of the enteric matrix at pH higher than the solubility of enteric polymers, which is used to support complete dissolution, and an emulsifier. The combination is in fact free of organic solvents. After that, the addition of the hydrophobic liquid and homogenisation with obtaining a fine stable emulsion are carried out. Then, the titration of the emulsion with acid with mixing in an amount, efficient for obtaining sediment in the form of particles, is carried out.

EFFECT: invention makes it possible to obtain the composition, possessing enteric properties.

45 cl, 6 dwg, 11 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention relates to pharmaceutical industry, in particular to method of obtaining microcapsules of medications of cephalosporin group. Method of obtaining microcapsules of medications of cephalosporin group consists in the following: surface-active substance is added to konjac solution in toluene, after that, powder of preparation of cephalosporin group is dissolved in dimethylformamide and transferred into solution of konjac in toluene, after formation by antibiotic of its own solid phase carbinol and distilled water are added in drops, obtained suspension of microcapsules is filtered, washed with acetone and dried, with process of obtaining microcapsules being carried out under specified conditions.

EFFECT: method ensures simplification and acceleration of the process of obtaining microcapsules of water-soluble medications.

8 ex

FIELD: chemistry.

SUBSTANCE: invention relates to encapsulation, particularly a method of producing fenbendazole microcapsules in a sodium carboxymethyl cellulose capsule. The method involves dissolving fenbendazole in dioxane or dimethyl sulphoxide or dimethyl formamide, adding the obtained fenbendazole solution to the solution of sodium carboxymethyl cellulose in dioxane in the presence of surfactant E472s while stirring at a rate of 1000 rps. Fenbendazole and sodium carboxymethyl cellulose are taken in weight ratio of 1:3. Methyl carbinol and distilled water, taken in ratio of 2:1 vol/vol, are then added. The obtained suspension of microcapsules is filtered and dried. The process is carried out at 25C for 20 minutes without special equipment.

EFFECT: invention simplifies and speeds up the process of producing microcapsules, reduces losses during production thereof (high mass output).

3 ex

FIELD: chemistry.

SUBSTANCE: fenbendazole is dissolved in dioxane or dimethyl sulphoxide or dimethyl formamide. The obtained fenbendazole solution is added to a solution of sodium carboxymethyl cellulose in ethyl acetate in the presence of an E472s preparation while stirring at a rate of 1000 rps, wherein the fenbendazole and sodium carboxymethyl cellulose are taken in weight ratio of 1:3. Methyl carbinol and distilled water, taken in volume ratio of 2:1, respectively, are then added. The obtained suspension of microcapsules is filtered and dried. The process of producing fenbendazole microcapsules carried out at 25C for 20 minutes without special equipment.

EFFECT: improved method.

3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to agriculture. Microcapsules of pesticides are obtained by mixing solution of sodium carboxymethylcellulose in cyclohexanol in presence of a surface-active substance with solution of pesticides in dimethylsulfoxide with further addition of ethanol after formation of solid phase.

EFFECT: invention makes it possible to simplify the process of obtaining microcapsules of preparation in water-soluble polymers, and increase weight output.

3 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention relates to method of obtaining microcapsules of medication of cephalosporin group in konjac gum. In accordance with claimed method cephalosporin powder, preliminarily dissolved in dimethylformamide, and surface-active substance are added to konjac gum solution in isopropyl alcohol, with addition of carbinol after formation of independent solid phase by cephalosporin. Obtained suspension of microcapsules is filtered, washed with acetone and dried in dessicator.

EFFECT: invention makes it possible to simplify and accelerate process of obtaining microcapsules of water-soluble medications of cephalosporin groups in konjac gum, as well as to increase their output by weight.

4 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention refers to chemical-pharmaceutical industry and represents a method for preparing drug microcapsules by nonsolvent addition differing by the fact that the drugs represent the preparations of cephalosporin group, and a coating is poludan deposited from an aqueous solution by adding diethyl ester and isopropanol at 25 C as a nonsolvent.

EFFECT: invention provides simplifying and accelerating the process of microcapsules, reducing the microcapsule loss (higher weight yield).

3 ex

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