RU2771686C1 - Method for obtaining reindeer antlers extract - Google Patents

Abstract

FIELD: biologically active substances.

SUBSTANCE: invention relates to the production of biologically active substances. Dried antlers of a male reindeer of the second and third grade are selected, together with a fur cover no more than 15 cm in size from the end of the antlers, as well as trimmings of the antlers. The resulting raw material is subjected to grinding to a particle size of 3.7 to 4.7 microns. The obtained ultradispersed antler powder is subjected to extraction with 50% ethanol at a mass ratio of 3:10 at a temperature of 20-27°C for 15-24 hours with occasional stirring of the suspension. The extraction is carried out three times, the resulting solution is separated from the rest of the powder by centrifugation, the ethanol content is adjusted to 50%, the acidity is in the range from 4.3 to 5.1 units. pH and subjected to freezing at a temperature of -40 to -42°C for 15 to 18 hours. The frozen extract is subjected to centrifugation to separate the clarified solution from the precipitate of the protein-lipid fraction. The clarified solution is separated from ultrafine particles by filtration through a system of membrane filters and standardized in terms of ethanol content in the range from 48 to 52%, dry residue in the range from 0.8 to 1.4% and acidity in the range from 5.4 to 6.0 units pH. The primary crushed ultrafine antler powder before the extraction stage is subjected to mechanochemical activation in a ball mill for 1.0-1.5 min to obtain an ultrafine powder with particle sizes from 1.5 to 2.5 microns.

EFFECT: invention makes it possible to increase the recoverability of biologically active substances from reindeer antlers.

1 cl, 4 ex

Description

The present invention relates to medicine and food additives, medical and food industries.

A known method for obtaining an extract from deer antlers according to patent No. 2363482 (A61K 35/36, 10.08.2009 Bull. No. 22). The method includes preparing the feedstock, grinding it, extracting the crushed mass with an alcohol-containing liquid and subsequent processing of the extract, while grape wine is used as an alcohol-containing liquid, extraction is carried out for 36-48 hours at a temperature of 18-24 ° C, and the resulting extract is subjected to vacuum .

The disadvantage is that the deer antlers are cleaned of the fur cover before extraction, which leads to a decrease in the content of extractive substances, and also that when extracted with grape wine (Cahors), the sugar content is 16%, which makes the intake of the finished extract undesirable for people suffering from diabetes mellitus or at risk for diabetes mellitus.

Closest to the proposed invention is a method for manufacturing an extract for a dietary supplement according to patent No. 2310344 (A23L 1/30, op. 06/20/2007, Bull. No. 17). The method is characterized by the fact that the male reindeer antlers of the second and third grades are selected together with a fur cover 10-12 cm in size from the ends of the antlers. They are cleaned of dirt and washed with a 30% alcohol solution. They are dried at a temperature of 10-12°C for 35 hours to a moisture content of about 30%. The resulting raw material is crushed to a fraction of 3.7-4.69 microns. Then the powder is extracted with 50% ethyl alcohol at a temperature of 17-25°C for 15-27 hours with periodic stirring of the solution. After settling, the precipitate is removed and again subjected to extraction in a new solution of 50% ethanol under the same conditions, repeating this process at least three times, until a semi-finished extract of the first, second, third stages is obtained in terms of the number of extraction stages. Next, the obtained semi-finished products of the extract are mixed, ethanol and acetic acid are added until 50% strength and acidity pH 4.3-5.1 are obtained. Then the semi-finished extract is kept at T=-49°C for 8-9 hours, filtered at a temperature of 0-5°C.

The disadvantage is that due to the coarse grinding of antlers, incomplete extraction of bioactive substances occurs, which is expressed in a low dry residue of the final product (only 0.4-1.0 wt.%).

The objective of the invention is to intensify the method and increase the specific activity of a biologically active food additive - an extract from reindeer antlers.

EFFECT: increased intensity of extraction of bioactive substances (BAS) from reindeer antlers by at least 40-50%.

The specified technical result is achieved by the fact that the method for obtaining an extract from reindeer antlers is that dried antlers of a male reindeer of the second and third grade are selected along with a fur cover no more than 15 cm in size from the end of the antlers, as well as trimming the antlers, the resulting raw material subjected to grinding to a particle size of 3.7-4.7 microns, the resulting ultrafine antler powder is subjected to extraction with 50% ethanol at a mass ratio of 3:10 at a temperature of 20-27 ° C for 15-24 hours with periodic stirring of the suspension, at this extraction is carried out three times, the resulting solution is separated from the rest of the powder by centrifugation, the ethanol content is adjusted to 50%, the acidity is in the range from 4.3 to 5.1 units. pH and subjected to freezing at a temperature of -40 to -42°C for 15 to 18 hours, the frozen extract is subjected to centrifugation to separate the clarified solution from the sediment of the protein-lipid fraction, the clarified solution is separated from ultrafine particles by filtration through a system of membrane filters with a diameter pores are not more than 1.2 μm and are standardized in terms of ethanol content in the range from 48 to 52%, dry residue in the range from 0.8 to 1.4% and acidity in the range from 5.4 to 6.0 units. pH, while the primary crushed ultrafine antler powder before the extraction stage is subjected to mechanochemical activation in a ball mill for 1.0-1.5 min to obtain an ultrafine powder with a particle size of 1.5 - 2.5 μm.

The stage of mechanochemical activation of coarsely ground antler powder makes it possible to increase the extractability of biologically active substances from the antler powder and, accordingly, the biological activity of the resulting final product of the extract by at least 40-50%.

The method is carried out as follows.

Dried antlers of a male reindeer of the second and third grade are selected, together with a fur cover up to 15 cm in size from the end of the antlers, as well as trimming the antlers. The resulting raw material is subjected to grinding to a particle size of 3.7-4.7 microns.

The obtained primary crushed ultrafine powder is subjected to mechanochemical activation in a ball mill for no more than 1.0-1.5 min to obtain an ultrafine powder with a particle size of 1.5 - 2.5 μm.

The ultrafine antler powder is subjected to extraction with 50% ethanol at a mass ratio of 3:10 at a temperature of 20-27°C for 15-24 hours with periodic stirring of the suspension, while the extraction is carried out three times.

The resulting solution is separated from the rest of the powder (meal) by centrifugation, the ethanol content is adjusted to 50%, pH is up to 4.3-5.1 and subjected to freezing at a temperature of -40 - -42°C for 15-18 hours.

The frozen extract (semi-finished product) is subjected to centrifugation in a preparative centrifuge at 3600 rpm for 30 minutes at a temperature of 4°C to separate the clarified solution from the sediment of the protein-lipid fraction.

The clarified solution is finally separated from ultrafine particles by filtration through a system of membrane filters with a pore diameter of not more than 1.2 µm.

The resulting transparent solution of light yellow color with a specific odor characteristic of antler raw materials is standardized (adjusted) according to the main parameters of the technical specifications for "Reindeer antler extract - forte": ethanol content - 48-52%, dry residue - 0.8 -1.4%, acidity - 5.4-6.0 units. pH.

Since the novelty, in comparison with the prototype, is the pre-extraction mechanochemical activation of the reindeer antler powder for 1.0-1.5 min, the share of obtaining an ultrafine antler powder, which contributes to a more complete extraction of biologically active substances, the examples below indicate the optimality of this particular time range.

Example 1

Dried antlers of a male reindeer of the second and third grade were selected along with a fur cover up to 15 cm in size from the end of the antlers, as well as trimmings of the antlers. The resulting raw material was subjected to grinding to a particle size of 3.7 μm. The resulting primary ground ultrafine powder was subjected to mechanochemical activation in a ball mill for 1 min to obtain an ultrafine powder with a particle size of 2.5 μm. The ultrafine powder of antlers was subjected to extraction with 50% ethanol at a mass ratio of 3:10 at a temperature of 20°C for 15 hours with periodic stirring of the suspension, while the extraction was carried out three times. The resulting solution was separated from the rest of the powder (meal) by centrifugation, brought the ethanol content to 50%, pH to 4.3 and subjected to freezing at a temperature of -40°C for 15 hours. The frozen extract (semi-finished product) was subjected to centrifugation in a preparative centrifuge at 3600 rpm for 30 min at a temperature of 40°C to separate the clarified solution from the sediment of the protein-lipid fraction. The clarified solution was finally separated from ultrafine particles by filtration through a system of membrane filters with a pore diameter of 1.2 μm.

The resulting transparent solution of light yellow color with a specific odor characteristic of raw antlers was standardized (adjusted) according to the main parameters of the technical specifications for "Reindeer antler extract - forte": ethanol content - 48-52%, dry residue - 0.8 -1.2%, acidity - 5.4-6.0 units. pH.

Example 2

Dried antlers of a male reindeer of the second and third grade were selected along with a fur cover up to 15 cm in size from the end of the antlers, as well as trimmings of the antlers. The resulting raw material was subjected to grinding to a particle size of 4.7 μm. The obtained primary crushed ultrafine powder was subjected to mechanochemical activation in a ball mill for 1.5 min, and an ultrafine powder with a particle size of 1.5 μm was obtained.

The ultrafine powder of antlers was subjected to extraction with 50% ethanol at a mass ratio of 3:10 at a temperature of 27°C for 24 hours with periodic stirring of the suspension, while the extraction was carried out three times. The resulting solution was separated from the rest of the powder (meal) by centrifugation, brought the ethanol content to 50%, pH to 5.1 and subjected to freezing at a temperature of -42°C for 18 hours. The frozen extract (semi-finished product) was subjected to centrifugation in a preparative centrifuge at 3600 rpm for 30 min at a temperature of 40°C to separate the clarified solution from the sediment of the protein-lipid fraction. The clarified solution was finally separated from ultrafine particles by filtration through a system of membrane filters with a pore diameter of 1.2 μm.

The resulting transparent solution of light yellow color with a specific odor characteristic of antler raw materials was standardized (adjusted) according to the main parameters of the technical specifications for "Reindeer antler extract - forte": ethanol content - 48-52%, acidity - 5.4- 6.0 units pH, dry residue, characterizing the content of bioactive substances in the final product, amounted to 0.8-1.4%.

Example 3

Dried antlers of a male reindeer of the second and third grade were selected along with a fur cover up to 15 cm in size from the end of the antlers, as well as trimmings of the antlers. The resulting raw material was subjected to grinding to a particle size of 3.7-4.7 microns. The obtained primary crushed ultrafine powder was subjected to mechanochemical activation in a ball mill for 40-45 s to obtain an ultrafine powder with a particle size of more than 2.5 μm. The ultrafine powder of antlers was subjected to extraction with 50% ethanol at a mass ratio of 3:10 at a temperature of 20°C for 15 hours with periodic stirring of the suspension, while the extraction was carried out three times. The resulting solution was separated from the rest of the powder (meal) by centrifugation, brought the ethanol content to 50%, pH to 4.3 and subjected to freezing at a temperature of -40°C for 15 hours. The frozen extract (semi-finished product) was subjected to centrifugation in a preparative centrifuge at 3600 rpm for 30 min at a temperature of 4°C to separate the clarified solution from the sediment of the protein-lipid fraction. The clarified solution was finally separated from ultrafine particles by filtration through a system of membrane filters with a pore diameter of 1.2 μm.

The resulting transparent solution of light yellow color with a specific odor characteristic of raw antlers was standardized (adjusted) according to the main parameters of the technical specifications for "Reindeer antler extract - forte": ethanol content - 48-52%, dry residue - 0.6 -1.2%, acidity - 5.4-6.0 units. pH.

Example 4

Dried antlers of a male reindeer of the second and third grade were selected along with a fur cover up to 15 cm in size from the end of the antlers, as well as trimmings of the antlers. The resulting raw material was subjected to grinding to a particle size of 3.7-4.7 microns. The resulting primary crushed ultrafine powder was subjected to mechanochemical activation in a ball mill for 2.0-2.5 min, ultrafine powder with a particle size of more than 5 μm was obtained due to particle sintering, which sharply reduced the efficiency of subsequent extraction.

The cake of the ultrafine powder of antlers was subjected to extraction with 50% ethanol at a mass ratio of 3:10 at a temperature of 27°C for 24 hours with periodic stirring of the suspension, while the extraction was carried out three times. The resulting solution was separated from the rest of the powder (meal) by centrifugation, brought the ethanol content to 50%, pH to 5.1 and subjected to freezing at a temperature of -42°C for 18 hours. The frozen extract (semi-finished product) was subjected to centrifugation in a preparative centrifuge at 3600 rpm for 30 min at a temperature of 4°C to separate the clarified solution from the sediment of the protein-lipid fraction. The clarified solution was finally separated from ultrafine particles by filtration through a system of membrane filters with a pore diameter of 1.2 μm.

The resulting transparent solution of light yellow color with a specific odor characteristic of antler raw materials was standardized (adjusted) according to the main parameters of the technical specifications for "Reindeer antler extract - forte": ethanol content - 48-52%, acidity - 5.4- 6.0 units pH. But the dry residue characterizing the content of bioactive substances in the final product was only 0.3-0.6%.

The examples given illustrate the fact that the optimal mechanochemical activation time of 1.0-1.5 min (examples No. 1 and 2) leads to the minimum particle size (1.5 - 2.5 μm), which contributes to maximum extraction bioactive substances: dry residue is 0.8-1.4% (in the prototype, without mechanochemical activation of 0.4-1.0%), which is 40-50% higher than in the prototype. A decrease (example No. 3) or an increase (example No. 4) in the time of mechanochemical activation leads either to insufficient ultrafining (particle size greater than 2.5 μm, example No. 3), or to sintering of the resulting ultrafine particles (particle size greater than 5 μm, example No. 4), i.e. in both cases, to an increase in their size and, accordingly, to a decrease in the efficiency of extraction: dry residue - the content of bioactive substances is reduced to 0.6-1.2% (example No. 3) or to 0.3-0.6% (example No. 4).

Thus, the best option is the mode of mechanochemical activation for 1.0-1.5 min.

Claims (1)

A method for obtaining an extract from reindeer antlers, which consists in taking dried antlers of a male reindeer of the second and third grade together with a fur cover no more than 15 cm in size from the end of the antlers, as well as trimming the antlers, the resulting raw material is subjected to grinding to a particle size of 3.7 to 4.7 microns, the resulting ultrafine antler powder is subjected to extraction with 50% ethanol at a mass ratio of 3:10 at a temperature of 20-27 ° C for 15-24 hours with periodic stirring of the suspension, while the extraction is carried out three times, the resulting solution is separated from the rest of the powder by centrifugation, the ethanol content is adjusted to 50%, the acidity is in the range from 4.3 to 5.1 units. pH and subjected to freezing at a temperature of -40 to -42°C for 15 to 18 hours, the frozen extract is subjected to centrifugation to separate the clarified solution from the sediment of the protein-lipid fraction, the clarified solution is separated from ultrafine particles by filtration through a system of membrane filters and standardized in terms of ethanol content in the range from 48 to 52%, dry residue in the range from 0.8 to 1.4% and acidity in the range from 5.4 to 6.0 units. pH, while the primary crushed ultrafine antler powder before the extraction stage is subjected to mechanochemical activation in a ball mill for 1.0-1.5 min to obtain an ultrafine powder with a particle size of 1.5 to 2.5 microns.