Method for producing cephalosporin nanocapsules in xanthum gum

FIELD: medicine.

SUBSTANCE: invention represents a method for drug encapsulation by non-solvent addition, differing by the fact that a nanocapsule nucleus is cephalosporin antibiotics; the coating is xanthum gum deposited from a suspension in butanol by adding chloroform as a non-solvent at 25°C.

EFFECT: simplifying and accelerating the nanoencapsulation process, reducing the production loss.

4 ex

 

The invention relates to the field of nanotechnology and medicine, in particular to a method for producing nanocapsules cephalosporin antibiotics.

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 a temperature of 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 dispersed in pharmaceutically acceptable Giacometti, and the 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. 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 FOSS�Himera on the basis of 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 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 mother�l 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 the article "Razrabotka and gel microencapsulated products and materials for various industries", Russian chemical journal, 2001, vol. XLV, No. 5-6, pp. 125-135, describes a method of 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. the thickness of the shell reg�lirums time of deposition. 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.

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, vol. 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 pic�e lyophilization and easily regained their spherical shape after rehydration in buffer environment. The pH of the aqueous phase is crucial in obtaining robust microcapsules with a high yield.

The disadvantage of the proposed method of obtaining microcapsules is the complexity of the process, and hence the floating output of the target 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 RA�playsega 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, the morphologists.

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

In us Pat. WO/2010/119041 EP, IPC A23L 1/00, published 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 probiotics�ski 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). Usually prodcut has to be filtered through multiple filters with a gradual reduction of pore size. Ideally, the fine filter 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 yavl�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, 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 disadvantages of the proposed method are 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 described 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 disadvantages 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 JW�safety 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 ways of obtaining microcapsules: interfacial polymerization, thermoinduced phase separation, spray drying, evaporation of the solvent, etc.

The disadvantages of the methods are the complexity, the 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 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 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 of 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 is proposed�th way 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 are encapsulated, the agent 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.

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.

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 cephalosporin antibiotics in xanthan gums, reducing loss upon receipt of the microcapsules (increase of the yield by weight).

The solution of a technical problem is achieved by a method of obtaining nanocapsules ceph�leporinum antibiotics, related to β-lactam antibiotics, characterized in that as the shell of the nanocapsules used xanthan gum, as well as obtaining nanocapsules physico-chemical method of deposition of nerastvorim using precipitator - chloroform, the process is carried out without special equipment.

A distinctive feature of the proposed method is the use as the shell of the nanocapsules cephalosporin antibiotics, xanthan gum, as well as obtaining nanocapsules physico-chemical method of deposition of nerastvorim using precipitator - chloroform.

The result of the proposed method are obtaining nanocapsules cephalosporin antibiotics in xanthan gum at 25°C for 15 minutes. The output of the nanocapsules is 100%.

EXAMPLE 1. Obtaining nanocapsules Ceftriaxone in the xanthan gum with the use of chloroform as a precipitant, the ratio of core:shell 1:3

To a suspension of 1.5 g of xanthan gum in butanol and 0.01 g of the drug E472 (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 neutralize�Ana sodium) as a surfactant is added 0.5 g of Ceftriaxone powder in 2 ml of benzene. After the formation of Ceftriaxone independent solid phase very slowly added dropwise 5 ml of chloroform. The resulting suspension of nanocapsules was filtered off and dried.

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

EXAMPLE 2. Obtaining nanocapsules Cefazolin in xanthan gum with the use of chloroform as a precipitant, the ratio of core:shell 1:3

To a suspension of 1.5 g of xanthan gum in butanol and 0.01 g of the drug as a surfactant is added 0.5 g of Cefazolin powder in 2 ml of benzene. After the formation of Cefazolin independent solid phase very slowly added dropwise 5 ml of chloroform. The resulting suspension of nanocapsules was filtered off and dried.

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

EXAMPLE 3. Obtaining nanocapsules of cefepime in xanthan gum with the use of chloroform as a precipitant, the ratio of core:shell 1:3

To a suspension of 1.5 g of xanthan gum in butanol and 0.01 g of the drug E472c as a surfactant is added 0.5 g of cefepime powder in 2 ml of benzene. After the formation of the cefepime independent solid phase very slowly added dropwise 5 ml of chloroform. The resulting suspension of nanocapsules filtered.

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

EXAMPLE 4. Obtaining nanocapsules zapato�in SIMA xanthan gum, using chloroform as the precipitant, the ratio of core:shell 1:3

To a suspension of 1.5 g of xanthan gum in butanol and 0.01 g of the drug E472c as a surfactant is added 0.5 g of powder certosimo in 2 ml of benzene. After the formation of Cefotaxime independent solid phase very slowly added dropwise 5 ml of chloroform. The resulting suspension of nanocapsules filtered.

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

The obtained nanocapsules drugs group of cephalosporins related to β-lactam antibiotics, xanthan gum, physico-chemical deposition method by nerastvorim using chloroform as nerastvorimaya. The process is simple to perform and lasts for 15 minutes, requires no special equipment.

The proposed method is suitable for the pharmaceutical industry due to the minimal loss of speed, ease of obtaining and allocating nanocapsules cephalosporins related to β-lactam antibiotics, xanthan gum.

Method of encapsulation of the drug by the method of deposition by aristotelem, characterized in that as the core nanocapsules are used cephalosporin antibiotics, as the shell is xanthan gum, which is deposited from suspension in butanol by the addition of chloroform as herstories at 2°C.



 

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SUBSTANCE: invention relates to field of chemical-pharmaceutical industry and represents method of obtaining microcapsules, which have supermolecular properties, by method of precipitation with non-solvent, characterised by the fact that as a core of microcapsules flavor "apple", preliminarily dissolved in butanol, is applied, as casing - carrageenan, which is precipitated from solution in isopropanol by addition as non-solvent of butanol and water, with the following drying at room temperature.

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

1 dwg, 2 ex

FIELD: chemistry.

SUBSTANCE: invention provides a method of encapsulating a medicinal preparation via nonsolvent deposition, characterised by that the core of the microcapsules used is fenbendazole, which is pre-dissolved in dioxane or dimethylsulphoxide, the envelope used is sodium carboxymethyl cellulose which is deposited from a solution in carbinol by adding, as the nonsolvent, isopropanol and water at 25°C.

EFFECT: simple and faster process of producing microcapsules, reduced losses when producing microcapsules, high mass output.

3 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention relates to chemical-pharmaceutical industry and represents method of medication encapsulation by precipitation with non-solvent, which is characterised by the fact that as medication used is fenbendazole, and as envelope - sodium carboxymethylcellulose, which is precipitated from solution in acetone by addition as non-solvent of methylcarbinol and water at 25°C.

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

3 ex

FIELD: chemistry.

SUBSTANCE: invention provides a method of encapsulating a medicinal preparation via a nonsolvent deposition method, characterised by that the core of the nanocapsule used is fenbendazole, the envelope used is pectin, which is deposited from a suspension in benzene by adding tetrachloromethane as the nonsolvent at 25°C.

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

6 ex

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