Method of obtaining nanocapsules of cytokinins in sodium alginate

FIELD: chemistry.

SUBSTANCE: invention relates to field of nanotechnology, in particular to plant growing, and deals with method of obtaining nanocapsules of 6-aminobenzylpurine. Method is characterised by the fact that 6-aminobenzylpurine is used as core and sodium alginate is used as envelope of nanocapsules, obtained by addition of E472c as surfactant to sodium alginate in butanol, portioned addition of 6-aminobenzylpurine into suspension of sodium alginate in butanol and further drop-by-drop introduction of precipitating agent-petroleum ether after formation of separate solid phase in suspension.

EFFECT: simplification and acceleration of process of obtaining nanoparticles and increased output by weight.

3 ex

 

The invention relates to the field of nanotechnology, in particular to the crop.

Previously known methods for producing microcapsules. 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 comprises 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 amount of microspheres distributed in a pharmaceutically acceptable liquid vector, and a pharmaceutically active substance insoluble microspheres in a decree�the auditors liquid medium.

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

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 with a size of 100-800 microns in diameter and consists of pharmaceutical kernel crystalline ibuprofen and polymeric coating 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 RA�new tumors; the difficulty of execution; the duration of the process.

In us Pat. 2139046, IPC A61K 9/50, 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 is time consuming and slows down the process of obtaining microcapsules.

In us Pat. 2159037, IPC A01N 25/28, A01N 25/30, Russian Federation, published 20.11.2000, a method of producing microcapsules by polymerization reaction at the phase boundary, 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, active on Gran�CE interface and not acting as an emulsifier.

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

In the article "Razrabotka and gel microencapsulated products and materials for various industries", Russian chemical journal, 2001, vol. XLV, No. 5-6, pp. 125-135, a method for producing microcapsules of drugs by the method of gas-phase polymerization, as the authors believe the chemical method of coacervation of aqueous media for the 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: vaporization of the dimer of n-xylylene (170°C), thermal decomposition in the pyrolysis furnace (650°C at a residual pressure of 0.5 mm Hg.St.), transfer of the reaction products in the "cold" chamber of polymerization (20°C and a residual pressure of 0.1 mm Hg.St.), deposition and polymerization on the surface of the protected object. The polymerization chamber is made in the form of a rotating drum, the optimal speed for powder coating 30 Rev/min. shell Thickness is controlled by the coating. This method is suitable for the encapsulation of any solids (except prone to intense sublimation). The resulting poly-pccillin - vysokokritichnyh polymer with high orientation and dense packing, provides a conformal coating.

The 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 denaturation of proteins at high temperatures.

In the article "Development of micro - and nanosystems for drug delivery", Russian chemical journal, 2008, t. LII, No. 1, pp. 48-57, presents a method of producing microcapsules with the included proteins, which is not significantly reduces their biological activity by the process of interfacial crosslinking of soluble starch or hydroxyethyl starch and bovine serum albumin (BSA) using terephthaloyl chloride. A the protease inhibitor Aprotinin, either native or protected active site, was microencapsulated in his introduction to the composition of the aqueous phase. Tapered form lyophilized particles confirm the receipt of microcapsules or particles tank types. The thus prepared microcapsules tear after lyophilization and easily regained their spherical shape after rehydration in buffer environment. The pH of the aqueous phase was defined�known in obtaining robust microcapsules with a high yield.

The disadvantage of the proposed method of obtaining microcapsules is the complexity of the process, which, in turn, reduces the yield of the final capsules.

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 published 27.06.2009, Russian Federation, proposed 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 �Lucchini 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/2009/148058 JP, IPC B01J 13/04, A23L 1/00, A61K 35/20 ETF, A61K 45/00, A61K 47/08), A61K 47/26, A61K 47/32, A61K 47/34, A61K 47/36, A61K 9/50, B01J 2/04, B01J 2/06 published 10.12.2009, described the process of obtaining microcapsules that are applicable to industrial production, in which high content of hydrophilic biologically active substances contained in the envelope. Offer microcapsules can be used in food, pharmaceutical and other industries. In the production process are applied dispersant composition consisting of hydrophilic biologically active substances and surfactants in solid fat. Temperature not lower than the melting point of the solid fat.

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

In us Pat. WO/2010/076360 ES, IPC B01J 3/00; 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, and hence the low yield of the final product.

In us Pat. WO/2010/014011 NL, IPC A61K 9/50; B01J 13/02; A61K 9/50; B01J 13/02, published 4.02.2010, a method for producing microcapsules with a diameter from 0.1 μm to 25 μm, comprising: a core particle with a diameter of 90 nm to 23 μm, containing at least 3% active ingredient by weight of the particles; a coating that completely covers the core particles containing at least 20% by weight of a hydrophobic polymer selected from cellulose esters, of cellulose esters, shellac, gluten, polylactide, hydrophobic starch derivatives, polyvinyl acetate, polymers or copolymers of ester of acrylic acid and/or methacrylic acid ester and combinations thereof. The active ingredient is not released when introduced into aqueous food products, beverages, food or pharmaceutical composition. Once inside, however, the active component is released quickly.

The disadvantages of this method are the complexity, the duration of the process, and the use of ultrasound and special equipment, the use of the shells of the microcapsules of the copolymers of acrylic or methacrylic acid, which can cause cancer.

In �at. WO/2010/119041 EP, IPC A23L 1/00, published 21.10.2010, a method of producing microspheres consisting of the active ingredient 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 denature at temperatures 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). Generally, filtration is performed using a plurality of filters with a gradual reduction of pore size. Ideally, filter the tone�Oh cleaning has a 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 this 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, published on 13.01.2011, the method of obtaining 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, VS 3/02; 20060101, VS 003/02, VS 11/00; 20060101, VS 011/00, B05D 1/18; 20060101, B05D 001/18, B05D 3/02; 20060101, B05D 003/02, B05D 3/06; 20060101, B05D 003/06, 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 ultrasonic�violet radiation.

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 3/06; C11D 3/37; C11D 3/39; C11D 17/00, published on 13.10.2011 proposed several ways of obtaining microcapsules: 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-M Dryer from ProCepT, Belgium)).

In us Pat. WO/2011/104526 GB, IPC B01J 13/00; B01J 13/14; SV 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 composition, 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 TVE�Dykh products 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 in which agents are encapsulated to provide benefits that will be received. The core of the encapsulated agents may include perfume, silicone oils, waxes, hydrocarbons, higher fatty acids, essential oil�, 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.

In us Pat. WO/2011/160733 EP, IPC B01J 13/16, published on 29.12.2011, a method for producing microcapsules which contain a shell and core water-insoluble materials. The aqueous solution of protective colloid and a solution of a mixture of at least two structurally different bifunctional diisocyanates (A) and (B) insoluble in water together before formation of the emulsion, is then added to a mixture of bifunctional amine and heated to a temperature of at least 60°C before the formation of the microcapsules.

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.

In us Pat. WO/2011/161229 EP, IPC A61K 8/11; B01J 13/14; B01J 3/16; C11D 3/50, published on 29.12.2011, a method for producing microcapsules containing a shell made of polyurea and spirits in oil, where the shell is obtained by the reaction of two structurally different diisocyanates in emulsion form. In the process of obtaining microcapsules ISP�lesuuda protective colloids. During the reaction of isocyanates and amines must be present protective colloid. This is preferably polyvinylpyrrolidone (PVP). Protective colloid - polymer system, in which the suspension or dispersion prevents caking (agglomeration, coagulation, flocculation). This method can be used for perfume and all kinds of consumer goods. An exhaustive list of consumer goods cannot be transferred. Illustrative examples of consumer products include all applications, including liquid detergents and powder detergents; all for personal hygiene and hair care, including shampoos, conditioners, creams, conditioners, styling cream, soap, body creams, etc.; deodorants and antiperspirants.

The disadvantages of this method of obtaining microcapsules are the complexity and duration of the process, using as the shell of the microcapsules of diisocyanates which are obtained by reaction of two isocyanate.

In us Pat. WO/2012/007438 EP, IPC A61K 8/11; A61Q 13/00; B01J 3/16; B01J 3/18 published 19.01.2012, a method for producing particles with an average diameter less than 50 microns, comprising at least one membrane, the method of stepwise polymerization with the participation of isocyanate monomer. At least one shell formed by chain reaction polymerization growth (preferably free-happy�radical polymerization), not connected with the isocyanate. The invention also relates to a method for producing such particles in which the shell is formed to chain growth polymerization at a temperature at which the chain reaction of growth is suppressed. The invention also provides a fully formulated products, preferably liquids and gels that contain these particles.

The disadvantages of the proposed method are the complexity and duration of the process, obtaining microcapsules by chemical method stepwise polymerization. Produced by this method, the particles are quite large - 50 microns.

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 the dispersion in an aqueous medium, 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 producing nanocapsules vodorastvorimyh agricultural drugs group of cytokinins in the sodium alginate, reduction of losses during sex�starting nanocapsules (increase of the yield by weight).

The solution of a technical problem is achieved by a method of obtaining nanocapsules 6-BAP (6-aminoantipyrine), characterized in that as the shell of the nanocapsules used sodium alginate, as well as obtaining nanocapsules physico-chemical method of deposition of nerastvorim using precipitator - petroleum ether, the process is carried out without special equipment.

The result of the proposed method are obtaining nanocapsules 6-BAP in the sodium alginate for 15 minutes. The output of the nanocapsules is over 90%.

EXAMPLE 1. Obtaining nanocapsules 6-BAP in the ratio of the core:blalock 1:3

To 1.5 g of sodium alginate in butanol is added 0.01 g of the drug Is (an ester of glycerol with one or two molecules of dietary fatty acids and one or two molecules of citric acid, and citric acid as tribasic can be etherification other glycerides and as oxanilate - other fatty acids; free acid groups can be neutralized with sodium) as a surfactant. The resulting mixture is put on the magnetic stirrer and turn the stirring. 0.5 g of powder of 6-BAP is added in portions to a suspension of sodium alginate in butanol. After the formation of independent solid phase very slowly added dropwise 5 ml of petroleum ether. Received �Uspenskiy nanocapsules was filtered on the filter, washed with petroleum ether and dried.

Received 2 g of a white powder. The yield was 100%.

EXAMPLE 2. Obtaining nanocapsules 6-BAP in the ratio of the core:blalock 1:1

To 0.5 g of sodium alginate in butanol is added 0.01 g of the drug Is as surfactants. The resulting mixture is put on the magnetic stirrer and turn the stirring. 0.5 g of powder of 6-BAP is added in portions to a suspension of sodium alginate in butanol. After the formation of independent solid phase very slowly added dropwise 3 ml of petroleum ether. The resulting suspension of nanocapsules was filtered on a filter, washed with petroleum ether and dried.

Received 1 g of white powder. The yield was 100%.

EXAMPLE 3. Obtaining nanocapsules 6-BAP in the ratio of the core:blalock 5:1

To 0.5 g of sodium alginate in butanol is added 0.01 g of the drug Is as surfactants. The resulting mixture is put on the magnetic stirrer and turn the stirring. 2.5 g of powder of 6-BAP is added in portions to a suspension of sodium alginate in butanol. After the formation of independent solid phase very slowly added dropwise 3 ml of petroleum ether. The resulting suspension of nanocapsules was filtered on a filter, washed with petroleum ether and dried.

Obtained 3 g of a white powder. The yield was 100%.

A method of producing nanocapsules-aminoantipyrine, characterized by the fact that as the core of the nanocapsules used 6-aminoantipyrine and sodium alginate as the shell of the nanocapsules obtained by adding Us as a surfactant to the sodium alginate in butanol, portions of Appendix 6-aminoantipyrine in suspension of sodium alginate in butanol and subsequent pocataligo the slow introduction of the precipitant - petroleum ether after the formation of separate solid phase in suspension.



 

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2 ex

FIELD: medicine.

SUBSTANCE: invention represents method of medication encapsulation by method of precipitation with non-solvent, characterized by the fact that as core of nanocapsules albendazole is applied, as casing - sodium alginate, which is precipitated from suspension in butanol by addition of chloroform as non-solvent at 25°C.

EFFECT: simplification and acceleration of nanocapsules obtaining process, reduction of loss in obtaining nanocapsules.

2 ex

FIELD: chemistry.

SUBSTANCE: core of nanocapsules of chondroitin sulphate and the envelope as carrageenan is used, which is deposited from a suspension in butyl alcohol by adding hexane as a nonsolvent at 25°C.

EFFECT: simpler and faster process of producing nanocapsules and reduced losses when producing nanocapsules.

2 ex

FIELD: chemistry.

SUBSTANCE: invention provides a method of encapsulating a medicinal preparation via non-solvent addition, characterised by that the core of the microcapsules used is fenbendazole, the envelope used is sodium carboxymethyl cellulose which is deposited from a solution in toluene by adding, as the nonsolvent, carbinol and water at 25°C.

EFFECT: simpler and faster process of producing microcapsules and reduced losses when producing microcapsules.

3 ex

FIELD: chemistry.

SUBSTANCE: invention provides a method of encapsulating a medicinal preparation via non-solvent addition, characterised by that the core of the microcapsules used is fenbendazole, the envelope used is sodium carboxymethyl cellulose which is deposited from a solution in cyclohexanol by adding, as the nonsolvent, isopropanol and water at 25°C.

EFFECT: simpler and faster process of producing microcapsules and reduced losses when producing microcapsules.

3 ex

FIELD: chemistry.

SUBSTANCE: invention provides a method of producing microcapsules by non-solvent addition, characterised by that the nucleus of the microcapsules is triazine pesticides and the shell is polyvinyl alcohol, which is deposited from an aqueous solution by adding, as the non-solvent at the beginning, a first precipitant - 5% acetic acid solution in acetone, and then acetone as a second precipitant at 25°C.

EFFECT: simpler and faster process of producing microcapsules of a preparation in water-soluble polymers and higher mass output.

3 ex

FIELD: medicine.

SUBSTANCE: invention describes a method for producing Sel-Plex nanocapsules possessing the supramolecular properties by non-solvent addition, characterised by the fact that Sel-Plex is dissolved in dimethyl sulphoxide; the prepared mixture is dispersed in xanthum gum solution used as a nanocapsule shell, in butanol, in the presence of E472c preparation while stirring at 1000 cycles per second; the mixture is added with the precipitator benzol, filtered and dried at room temperature.

EFFECT: simplifying and accelerating the process of nanoencapsulation and ensuring higher weight yield.

4 ex, 12 dwg

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