Method of production of the microcapsules

FIELD: industrial biotechnology; methods of production of the microcapsules.

SUBSTANCE: the invention is pertaining to the industrial biotechnology and is intended for production of the micro-capsulated biopreparations of the natural compounds. The purpose of the invention is development of the effective method of production of the microcapsules of the liquid-phase natural substances. The method is exercised by the emulsification of the encapsulated substance in the polymer solution and sedimentation of the polymer on the surface of the emulsion drips. The sedimentation(is conducted three times at the temperature of 75-80°C during 5-10 minutes at the continuous stirring with the subsequent treatment with the acetone In the capacity of the polymer solution use 1-2.5 % solution of methyl cellulose with the content of the metoxyl groups from 27.5 up to 32 %. In the capacity of the emulsifier use the rape oil in amount of 7.5-40 mass % from the amount of the polymer solution.

EFFECT: the invention ensures development of the effective method of production of the microcapsules of the liquid-phase natural substances.

4 cl, 4 ex

 

The invention relates to the biotechnology industry and is designed to produce microencapsulated drugs of natural compounds.

A known method of producing microcapsules (patent US 33699000, 1968), which uses a modified phthalic anhydride gelatin. The disadvantage is the use of some expensive components. A known method of producing microcapsules of measles-containing vaccine (patent RU 2210361, 2003). The disadvantage is the technical complexity of the complete method.

Closest to the proposed to the technical essence and the achieved positive effect is the method of production of microcapsules (patent RU 2107542,1998), in which the emulsification of the core material is carried out in the solution of the modified gelatin with its subsequent deposition on the surface of droplets of the emulsion with the formation of shells. The disadvantages of this method include the use of organic components that are prohibited for use inside.

The purpose of the invention is to develop an effective method of producing microcapsules of natural substances.

For this purpose, the proposed method of producing microcapsules in the formation of the shell was used methylcellulose content metaxylene groups from 27,5%to 32%. With increasing degree of methylation hygroscopicity methylcellulose increases. This is because the h is on the macromolecules of cellulose takes place vzaimoponimanie most of hydroxyl groups with the formation of hydrogen bonds.

When reaching a higher degree of substitution in the area of 26.5-32.5% of content metaxylene groups methylcellulose is dissolved in water. With further increase metaxylene groups of up to 38% and higher, it loses its solubility.

On the basis of the proposed method can be implemented microencapsulation of vitamins, antibiotics, proteins, including enzymes, and other biologically-active substances in the liquid phase.

The method of producing microcapsules is as follows.

Receive 1-2,5% solution of methylcellulose. To do this, methylcellulose bring in warm water with a temperature of 50-60°C. the Mixture was kept for 1.5-2 hours. Temperature due to the following restrictions. At temperatures below 50°and above 60°With the gelation process slows down. In the resulting colloidal gel methylcellulose enter capsuleneo substance and emuleret through mixing. The rotation speed of the agitator is in the range of 250-400 min-1. The choice of mode mixing determines the nature of the final product.

As emulsifier use canola or other oil, adding which causes the dispersion of the aqueous solution of the foaming agent distributed therein capsulerebel substance into small droplets. Making emulsifier in amounts less than the lower limit (5.0 wt.% about the amount of polymer) does not create a stable emulsion, with the introduction of higher upper limit (8.0 wt.% the number of polymer) slows down the process of emulsification.

The next step is the formation of a shell of methyl cellulose. For that, the resulting dispersion is heated at a temperature of 75-80°C for 5-10 minutes, stirring constantly. The formation of a new phase in an aqueous solution of the polymer occurs with increasing temperature.

When heated solution of methylcellulose is worsening solubility until the deposition of the polymer. Due to this phenomenon is the formation of "hydroxonium connection metaxylene groups with water, which when the temperature is destroyed, leading to precipitation of the polymer.

This method of forming the shell based on the following physico-chemical phenomena: phase separation in the system occurs with increasing temperature, if the system has a lower critical temperature of dissolution. The solution of methylcellulose in water has a lower critical temperature of dissolution, which is 59.5°C. consequently, the temperature increases above the specified value leads to the deposition of polymer on the surface of the microcapsules. The next step to a chilled solution of the drug add acetone to remove excess oil phase from the reaction mixture. Microcapsules is filtered off, washed with water and dried sushilka or dehydrating means (ethanol) or kept in suspension in water at 4° C.

This method of producing microcapsules is illustrated by concrete examples.

Example 1. In a reactor equipped with a mixer, make 30 ml of a 1.5% solution of methylcellulose in water, capsuleneo substance and stirred at a rotation speed of the mixer 250 min-1within 10 minutes the resulting solution was injected 5 ml of rapeseed oil. After 30 min the reaction mixture is heated on a water bath at 80°5 minutes, stirring constantly. The heating process was repeated 3 times at intervals of 30 s for complete precipitation of the polymer. Then the reactor is cooled to room temperature, treated with 10 ml of acetone and stirred for 1 hour. Microcapsules is filtered off, washed with water and stored in suspension in water at 4°C.

Example 2. In a reactor equipped with a mixer, make 40 ml of 1% solution of methylcellulose in water, capsuleneo substance and stirred at a rotation speed of the mixer 350 min-1within 15 minutes the resulting solution was injected 3 ml of rapeseed oil. After 30 min the reaction mixture is heated on a water bath at 80°With 8 minutes, stirring constantly. The heating process was repeated 3 times at intervals of 30 s for complete precipitation of the polymer. Then the reactor is cooled to room temperature, treated with 7.5 ml of acetone and stirred for 1.5 hours. Microcapsules is filtered off, washed with water and stored in a view of the suspension in water at 4° C.

Example 3. In a reactor equipped with a mixer, make 30 ml of 2.5% solution of methylcellulose in water, capsuleneo substance and stirred at a rotation speed of the mixer 400 min-1within 8 minutes the resulting solution was injected with 8 ml of rapeseed oil. After 30 min the reaction mixture is heated on a water bath at 75°10 min, stirring constantly. The heating process was repeated 3 times at intervals of 30 s for complete precipitation of the polymer. Then the reactor is cooled to room temperature, treated with 15 ml of acetone and stirred for 0.5 hour. Microcapsules is filtered off, washed with water and kept in suspension in the water.

Example 4. In a reactor equipped with a mixer, make 40 ml of 1% solution of methylcellulose in water, capsuleneo substance and stirred at a rotation speed of the mixer 350 min-1within 15 minutes the resulting solution was injected 3 ml of rapeseed oil. After 30 min the reaction mixture is heated on a water bath at 80°8 min, stirring constantly. The heating process was repeated 3 times at intervals of 30 s for complete precipitation of the polymer. Then the reactor is cooled to room temperature, treated with 7.5 ml of acetone and stirred for 1.5 hours. Microcapsules is filtered off, washed with water and dried in a dryer at 50°C.

1. The method of producing microcapsules of liquid-phase materials by among the simulation capsulerebel substance in the polymer solution and precipitation of the polymer on the surface of droplets of the emulsion, characterized in that the polymer solution used 1-2,5%solution of methylcellulose content metaxylene groups from 27,5%to 32%, as emulsifier use of rapeseed oil in the amount of 7.5 to 40 wt.% the number of polymer solution, and the deposition carried out three times at a temperature of 75-80°C for 5-10 min with continuous stirring followed by treatment with acetone.

2. The method according to claim 1, characterized in that as the polymer constituting the shell is methylcellulose at a concentration of 1.5%.

3. The method according to claim 1, characterized in that as the polymer constituting the shell is methylcellulose at a concentration of 2.5%.

4. The method according to claim 1, characterized in that use methylcellulose content metaxylene groups 28%.



 

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