Method for production of microcapsules of dry girasol extract in pectin

FIELD: food industry.

SUBSTANCE: invention relates to food industry. The method for production of dry girasol extract in pectin envisages usage of a microcapsule shell, represented by low-etherified and high-etherified apple and citrus pectins, and a nucleus, represented by dry girasol extract. The microcapsules are produced by way of the pectin mixture stirring in benzol, with the surfactant represented by preparation E472c, in a magnetic stirrer. Then dry girasol extract is added into the mixture which is deposited with acetonitrile. Then the produced microcapsule suspension is filtered, washed with acetonitrile and dried.

EFFECT: invention allows to simplify and accelerate the microcapsules production process and increase weight yield.

7 ex

 

The invention relates to the field of nanotechnology, in particular the microencapsulation of drugs on the example of a dry extract of artichoke in Apple and citrus pectin (high and nizkotemeraturnom) physico-chemical method.

Previously known methods for producing microcapsules of drugs. So, in us 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 application of ultraviolet radiation, which can influence the formation of microcapsules.

In us Pat. 2095055, IPC A61K 9/52, A61K 9/16, A61K 9/10, Russian Federation, published 10.11.1997, a method of producing a solid non-porous microspheres, including melting pharmaceutically inactive substance carrier, the dispersion of the 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 temperatures from - 15 to - 50°C, and separation of the obtained microspheres into fractions by size. The suspension is intended for administration by parenteral injection, contains an effective�objective number of these microspheres, distributed in a pharmaceutically acceptable liquid vector, and a pharmaceutically active substance insoluble microspheres in a specified liquid medium.

Disadvantages of the proposed method are the complexity and duration of the process, the use of special equipment.

In us Pat. 2091071, IPC A61K 35/10, Russian Federation, published 27.09.1997, a method of producing the drug by dispersing in a ball mill to obtain microcapsules.

The disadvantages of this method are the use of the ball mill and the duration of the process.

In us Pat. 2076765, IPC B01D 9/02, Russian Federation, published 10.04.1997, a method of producing dispersed particles of soluble compounds in the microcapsules by means of crystallization from 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 complexity of: obtaining microcapsules by dispersing followed by a change in temperature, which slows down the process.

In us Pat. 2101010, IPC A61K 9/52, A61K 9/50, A61K 9/22, A61K 9/20, A61K 31/19, 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 razmera-800 microns in diameter and consists of pharmaceutical kernel crystalline ibuprofen and polymeric coatings comprising a plasticizer, elastic enough to resist chewing. Polymer coating is a copolymer based on methacrylic acid.

Disadvantages of the invention: use of a copolymer based on methacrylic acid, as these polymer coatings can cause cancer; obtaining microcapsules by the method of suspension polymerization; the difficulty of execution; the duration of the process.

In us Pat. 2139046. IPC A61K 5/50, A61K 49/00, og 51/00 A61K, Russian Federation, published 10.10.1999, a method of producing microcapsules as follows. Emulsion oil-in-water is prepared from an organic solution containing dissolved mono-, di-, triglyceride, preferably of tripalmitin or tristearin and possibly therapeutically active substance, and an aqueous solution containing a surfactant may evaporate the solvent, add redispersible agent and the mixture is subjected to drying by freezing. Subjected to drying, the mixture is then dispersed in an aqueous medium to separate the microcapsules from the remnants of organic matter and a hemispherical or spherical microcapsules are dried.

The disadvantages of the proposed method are the complexity and duration of the process, the use of drying by freezing, which takes a lot of time�and and slows down the process of obtaining microcapsules.

In us Pat. 2159037, IPC 01N 25/28, A01N 25/30, Russian Federation, published 20.11.2000, a method of producing microcapsules by polymerization reaction at the boundary seeded phases containing solid agrochemical material of 0.1 to 55 wt.%, suspended in a stirred water organic liquid, from 0.01 to 10 wt. % non-ionic dispersant, is active on the interface and not acting as an emulsifier.

Disadvantages of the proposed method are the complexity, duration, use of vysokokalievogo mixer.

In us Pat. 2173140, IPC A61K 009/50, A61K 009/127, Russian Federation, published 10.09.2001, a method of producing kremnijorganicheskih microcapsules using a rotary cavitation equipment with high shear forces and powerful hydroacoustic phenomena sonic and ultrasonic range for dispersion.

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

In us Pat. 2359662, IPC A61K 009/56, A61J 003/07, B01J 013/02, A23L 001/00 posted on other sites.� 27.06.2009, Russian Federation, a method of producing microcapsules using spray cooling in the spray tower Niro under the following conditions: air temperature at the inlet 10°C, the temperature at the outlet 28°C, the speed of rotation of the spray drum 10000 rpm /min Microcapsules according to the invention have improved stability and provide adjustable and/or prolonged release of the active ingredient.

The disadvantages of the proposed method are the duration of the process and the use of special equipment, certain set of conditions (the air temperature at the inlet 10°C, the temperature at the outlet 28°C, the speed of rotation of the spray drum 10000 rpm/min).

In us Pat. WO/2010/076360, ES, IPC B01J 13/00; A61K 9/14; A61K 9/10; A61K 9/12 published 08.07.2010, we propose a new method for obtaining solid micro - and nanoparticles with a homogeneous structure with a particle size less than 10 microns, where the treated solids have a natural crystalline, amorphous, polymorphous, and other conditions associated with the reference compound. The method allows to obtain solid micro - and nanoparticles with substantially spheroidal morphology.

The disadvantage of the proposed method is the complexity of the process that results in capsules with a floating output.

In us Pat. WO/2010/119041, EP, IPC A23L 1/00, published�EN 21.10.2010, a method of producing microspheres comprising an active component encapsulated in the gel matrix whey protein, including denatured protein, the serum and active components. The invention relates to a method of producing microspheres, which contain components such as probiotic bacteria. A method of producing microspheres includes the step of production of microspheres in accordance with the method of the invention, and the subsequent solidification of microspheres in a solution of anionic polysaccharide with a pH of 4.6 and below for at least 10, 30, 60, 90, 120, 180 minutes. Examples of suitable anionic polysaccharides: pectin, alginates, carrageenans. Ideally, whey protein is teplogeneriruyuschim, although other methods of denaturation are also applicable, for example, denaturation induced pressure. In a preferred embodiment, the whey protein denatures at a temperature of from 75°C to 80°C, suitably for from 30 minutes to 50 minutes. Typically, whey protein mixed with thermal denaturation. Accordingly, the concentration of the whey protein is from 5 to 15%, preferably from 7 to 12%, and ideally from 9 to 11% (weight / volume). Typically, the implementation process is carried out by filtration through filters with a gradual reduction of pore size. Ideally, the filter of thin clearing �has submicron pore size, for example, from 0.1 to 0.9 microns. The preferred method of producing microspheres is the way with the application encapsulators corresponding vibration (Inotech, Switzerland) and machines production of NISCO stock Engineering AG. Typically, the nozzles have openings 100 and 600 microns, and ideally about 150 microns.

The disadvantage of this method is the use of special equipment (encapsulators corresponding vibration (Inotech, Switzerland)), obtaining microcapsules by means of protein denaturation, the complexity of the allocation obtained by the method of microcapsules - filtration with the use of multiple filters, which makes the process lengthy.

In us Pat. WO/2011/003805, EP, IPC B01J 13/18; B65D 83/14; C08G 18/00 described a method of producing microcapsules that are suitable for use in the compositions forming sealants, foams, coatings or adhesives.

The disadvantage of the proposed method is the use of centrifugation for separation from the process fluid, the duration of the process, and the application of this method in the pharmaceutical industry.

In us Pat. 20110223314, IPC B05D 7/00; 20060101 B05D 007/00, B05C 3/02; 20060101 B05C 003/02; B05C 11/00; 20060101 B05C 011/00, B05D 1/18; 20060101 B05D 001/18; B05D 3/02; 20060101 B05D 003/02, B05D 3/06; 20060101 B05D 003/06 from 10.03.2011, US, describes a method of producing microcapsules by the method of suspension polymerization, belonging to the group of chemical methods with the use of a new device and UV exposure.

The disadvantage of this method are the complexity and duration of the process, the use of special equipment, the use of UV irradiation.

In us Pat. WO/2011/150138, US, IPC C11D 3/37; B01J 13/08; C11D 17/00, published on 01.12.2011, the method of obtaining microcapsules of a solid water-soluble agents polymerization.

The disadvantages of this method are the complexity and duration of the process.

In us Pat. WO/2011/127030, US, IPC A61K 8/11; B01J 2/00; B01J 13/06; C11D 3/37; C11D 3/39; C11D 17/00, published on 13.10.2011 proposed several methods for producing microcapsules by interfacial polymerization, thermoinduced phase separation spray drying, evaporation of the solvent, etc. the Disadvantages of the proposed methods is the difficulty, duration of processes, and the use of special equipment (filter (Albet, Dassel, Germany), spray dryer for collecting particles (Spray-4M8 Dryer from ProCepT, Belgium)).

The disadvantages of the proposed methods is the difficulty, duration of processes, and the use of special equipment (filter (Albet, Dassel, Germany), spray dryer for collecting particles (Spray-M Dryer from ProCepT, Belgium)).

In us Pat. WO/2011/104526, GB, IPC B01J 13/00; B01J 13/14; C09B 67/00; C09D 11/02, published on 01.09.2011, a method of producing a dispersion of encapsulated solid particles in a liquid medium, comprising: a) grinding to�position, including solid, liquid medium and a polyurethane dispersant with an acid number of from 0.55 to 3.5 mmol per gram of dispersant, said composition includes 5 to 40 parts of the polyurethane dispersant per 100 parts of solid product by weight; and b) crosslinking the polyurethane dispersant in the presence of solid and liquid medium so as to encapsulate the solid particles which the polyurethane dispersant contains less than 10% by weight of recurring items from polymer alcohols.

The disadvantages of the proposed method are the complexity and duration of the process of production of microcapsules, and that the encapsulated particles by the proposed method are useful as colorants in inks, especially ink jet printing, for the pharmaceutical industry this practice is not applicable.

In us Pat. WO/2011/056935, US, IPC C11D 17/00; A61K 8/11; B01J 13/02; C11D 3/50, published on 12.05.2011, a method for producing microcapsules with a size of 15 microns. As the shell material of the proposed polymers of the group consisting of polyethylene, polyamides, polystyrene, polyisoprenes, polycarbonates, polyesters, polyacrylates, polyureas, polyurethanes, polyolefins, polysaccharides, epoxy resins, vinyl polymers and mixtures thereof. Proposed polymeric membranes are relatively impermeable to the core material and materials in the environment�e, in which are encapsulated agents, the benefit will be used to provide benefits that will be received. The core of the encapsulated agents may include perfume, silicone oils, waxes, hydrocarbons, higher fatty acids, essential oils, lipids, cooling the skin fluids, vitamins, sunscreens, antioxidants, glycerine, catalysts, bleach particles, particles of silicon dioxide, etc.

The disadvantages of the proposed method are the complexity, the duration of the process, using as the shells of the microcapsules of polymers of synthetic origin and their mixtures.

The closest method is the method proposed in us Pat. 2134967, IPC A01N 53/00, A01N 25/28, published 27.08.1999, Russian Federation (1999). In water dispersed solution of a mixture of natural lipids and PYRETHROID insecticide in a weight ratio of 2-4:1 in an organic solvent, which leads to simplification of the method of microencapsulation.

The disadvantage is with the doping in the aquatic environment, which makes the proposed method applicable for obtaining microcapsules of water-soluble drugs in water-soluble polymers.

The technical objective is the simplification and acceleration of the process of obtaining microcapsules of dry extract of artichoke in pectin, reducing loss upon receipt of the microcapsules (increase of the yield by weight)./p>

The solution of a technical problem is achieved by a method of obtaining microcapsules of dry extract of artichoke, characterized in that as the shell of the microcapsules used pectins, as well as obtaining microcapsules physico-chemical deposition method by nerastvorim using precipitator - acetonitrile, the process is carried out without special equipment.

A distinctive feature of the proposed method is the use as the shell of the microcapsules of dry extract of artichoke, pectins, as well as obtaining microcapsules physico-chemical deposition method by nerastvorim using precipitator - acetonitrile.

The result of the proposed method are obtaining microcapsules of dry extract of artichoke in the pectin at 25°C for 15 minutes. The output of the microcapsules is 100%.

EXAMPLE 1. Obtaining microcapsules of dry extract of artichoke in low-esterified Apple pectin, a ratio of 1:3

To 3 g of the slurry nizkoenergeticheskogo pectin in benzene 0.01 g of the drug Is as surfactants. The resulting mixture is put on the magnetic stirrer and turn the stirring. 1 g of dry extract of artichoke portions slowly added to a slurry of pectin in benzene. Then add 5 ml of acetonitrile. The resulting suspension microcaps�l was filtered on the filter, washed with acetonitrile and dried.

Received 4 grams of cream powder. The yield was 100%.

EXAMPLE 2. Obtaining microcapsules of dry extract of artichoke in Apple vysokodetalizirovannom pectin, a ratio of 1:3

To 3 g of the slurry vysokotarifitsirovannyh pectin in benzene 0.01 g of the drug Is as surfactants. The resulting mixture is put on the magnetic stirrer and turn the stirring. 1 g of dry extract of artichoke is transferred to a slurry of pectin in benzene. After that, add 5 ml of acetonitrile. The resulting suspension of microcapsules is filtered off on a filter, washed with acetonitrile and dried.

Received 4 g to cream color powder. The yield was 100%.

EXAMPLE 3. Obtaining microcapsules of dry extract of artichoke in low-esterified citrus pectin, a ratio of 1:3

To 3 g of the slurry nizkoenergeticheskogo pectin in benzene 0.01 g of the drug Is as surfactants. The resulting mixture was put on a magnetic metal and include stirring. 1 g of dry extract of artichoke is added to a slurry of pectin in benzene. Then add 5 ml of acetonitrile. The resulting suspension of microcapsules is filtered off, washed with acetonitrile and dried.

Received 4 g of a white powder. The yield was 100%.

EXAMPLE 4. Obtaining microcapsules of dry extract that�of inamura in citrus vysokodetalizirovannom pectin, the ratio of 1:3

To 3 g of the slurry vysokotarifitsirovannyh pectin in benzene 0.01 g of the drug Is as surfactants. The resulting mixture is put on the magnetic stirrer and turn the stirring. 1 g of dry extract of artichoke is transferred to a slurry of pectin in benzene. After that, add 5 ml of acetonitrile. The resulting suspension of microcapsules is filtered off, washed with acetonitrile and dried.

Received 4 g of a white to cream color powder. The output was 96,25%.

EXAMPLE 5. Obtaining microcapsules of dry extract of artichoke in low-esterified Apple pectin, a ratio of 5:1

To 1 g of the slurry nizkoenergeticheskogo pectin in benzene 0.01 g of the drug Is as surfactants. The resulting mixture is put on the magnetic stirrer and turn the stirring. 5 g of dry extract of artichoke portions slowly added to a slurry of pectin in benzene. Then add 6 ml of acetonitrile. The resulting suspension of microcapsules is filtered off on a filter, washed with acetonitrile and dried.

Received 6 grams of cream powder. The yield was 100%.

EXAMPLE 6. Obtaining microcapsules of dry extract of artichoke in Apple vysokodetalizirovannom pectin, a ratio of 5:1

To 1 g of the slurry vysokotarifitsirovannyh pectin in benzene 0.01 g of the drug Is as pove�chestno-active substances. The resulting mixture is put on the magnetic stirrer and turn the stirring. 5 g of dry extract of artichoke is transferred to a slurry of pectin in benzene. After that, add 6 ml of acetonitrile. The resulting suspension of microcapsules is filtered off on a filter, washed with acetonitrile and dried.

Received 6 g to cream color powder. The yield was 100%.

EXAMPLE 7. Obtaining microcapsules of dry extract of artichoke in low-esterified citrus pectin, a ratio of 5:1

To 1 g of the slurry nizkoenergeticheskogo pectin in benzene 0.01 g of the drug Is as surfactants. The resulting mixture is put on the magnetic stirrer and turn the stirring. 5 g of dry extract of artichoke is added to a slurry of pectin in benzene. Then add 6 ml of acetonitrile. The resulting suspension of microcapsules is filtered off, washed with acetonitrile and dried.

Received 6 g of a white powder. The yield was 100%.

EXAMPLE 4. Obtaining microcapsules of dry extract of artichoke in a citrus vysokodetalizirovannom pectin, a ratio of 5:1

To 1 g of the slurry vysokotarifitsirovannyh pectin in benzene 0.01 g of the drug Is as surfactants. The resulting mixture is put on the magnetic stirrer and turn the stirring. 5 g of dry extract of artichoke is transferred to a slurry of pectin in benzo�Le. After that, add 6 ml of acetonitrile. The resulting suspension of microcapsules is filtered off, washed with acetonitrile and dried.

Received 6 g of a white to cream color powder. The yield was 100%.

The obtained microcapsules of dry extract of artichoke in Apple and citrus pectin physico-chemical deposition method by nerastvorim using acetonitrile as nerastvorimaya. The process is simple to perform and lasts for 15 minutes, requires no special equipment.

Pectin (E440) is widely used in manufacture of jelly confectionery and pastel products for stabilization of fermented milk products, in the production of jam, as well as in bakery and pastry products. There are data on the use of pectin as a stabilizer of constituency creams, lotions, shampoos.

The proposed method is suitable for cosmetic and pharmaceutical industry due to the minimal loss of speed, ease of acquisition and allocation of microcapsules of dry extract of artichoke in Apple and citrus pectin.

A method of producing microcapsules of a dry extract of artichoke in pectin, characterized in that as the shell of the microcapsules used low-esterified and vysokotarifitsirovannyh Apple and citrus pectins, as nuclei� - dry extract of artichoke, wherein the microcapsules are obtained by stirring the mixture of pectin in benzene with the drug Is as a surfactant on the magnetic stirrer, add dry extract of artichoke in the mixture, the deposition acetonitril, then the resulting suspension of microcapsules is filtered off, washed with acetonitrile and dried.



 

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19 ex

FIELD: metallurgy.

SUBSTANCE: under the suggested method of the melts granulation including product melt supply to the liquid inert medium in form of jets flowing from the calibrated holes, with installed needles, the inert medium is melt. Melting temperature of the inert medium is below melting temperature of the granulated material. The obtained product granules are cooled in the inert liquid to temperature (20-30)°C. The inert liquid density is higher than the inert medium density and below the product granules density. The product melting temperature is (1.5-1.25) of melting temperature of the granulated material, and inert medium temperature is (1.05-1.15) of its melting temperature.

EFFECT: increased quality of produced granulated product, and capacity of the process of melt granulation due to contact of the product melt droplets with inert medium in form of the melt heated to temperature below the melting temperature of the granulated material.

3 tbl

FIELD: chemistry.

SUBSTANCE: in the disclosed microencapsulation method, which includes feeding a coating melt into a fluidised layer of heated granular material, the melt is fed to particles of the granular material through porous heated surfaces located above the fixed layer of granular material and which vibrate in the vertical plane. Temperature of the porous heated surface is 1.05 to 1.25 times the melting point of the coating substance.

EFFECT: high efficiency of the process of microencapsulation of granular materials and the quality of the obtained product owing to contact between the particles of the granular material and the porous heated surfaces, through which the coating melt enters the apparatus and into the fluidised layer of granular material.

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing metribuzin microcapsules. Said method is characterised by that polyvinyl alcohol solution is mixed with metribuzin and an E472c preparation as an emulsifier; the obtained mixture is stirred until components of the reaction mixture dissolve and after formation of a transparent solution, ethyl acetate is slowly added in droplets as a first precipitant and then isopropanol as a second precipitant; the obtained microcapsule suspension is settled for 1 minute and then filtered, washed with isopropanol and dried.

EFFECT: invention provides a simple process of producing microcapsules with a water-soluble envelope and increases mass output.

3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to field of encapsulation, in particular to method of obtaining microcapsules of vitamins A, C, E or Q10 in coating from highly etherified or low etherified apple or citrus pectin. In accordance with method by invention preparation E472c is added to suspension of highly etherified or low etherified apple or citrus pectin in ethanol and mixed. After that, suspension of vitamin in dimethylsulphoxide is added to suspension of pectin in ethanol, with further addition of benzene and distilled water. Obtained suspension of microcapsules is filtered and dried. Process of obtaining microcapsules is realised at 25°C for 15 min.

EFFECT: invention provides simplification and acceleration of process of obtaining microcapsules, reduction of loss in the process of their obtaining (increase of output by weight).

16 ex

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