RU2350342C1 - Method of producing gel based on water extraction from unossified antlers - Google Patents

Abstract

FIELD: beiotechnology.

SUBSTANCE: invention concerns production of items with expressed bioactivity and can be applied as healing and preventive medicine in medical cosmetology, balneology, medicine and veterinary. Method involves extraction of bioactive substances from unossified antlers at 40°C or lower temperature, conservation and gelatinisation agent addition to obtain aqueous solution of conservation agents represented by methylparaben and propylparaben. Extraction of bioactive substances is performed by conservation agent extraction to the solution by ultrasonic method in cavitation mode at weight ration of unossified antlers to aqueous solution of 1:1-10 for time period sufficient to obtain required extract concentration. Carbopol is used as gelatinisation agent and mixed with distilled water preliminarily and aged till imbibition, then neutralising agent is added in amount sufficient to form gel mass, further neutralised by adding citric acid solution to 6-7.5, and aqueous solution of unossified antlers and 1-30 wt % of water retentive component are added to obtained gel mass in portions with stirring.

EFFECT: obtaining high-quality gel based on aqueous solution of unossified antlers by ultrasonic extraction of bioactive substances.

2 cl, 5 ex, 2 tbl

Description

The invention relates to the production of products with pronounced biological activity and can be used as a therapeutic agent in medical cosmetology, balneology, medicine and veterinary medicine.

It is known that in the Russian Pharmacopoeia antler extract is indicated in the “tonic drugs” section and is presented on the market by the Pantocrin preparation, the basis of which is alcohol extract (see Medicines: properties, uses, contraindications: Reference / Edited by M.A. Klyueva. - M.: Russian Book, 1993, p. 324-325).

The disadvantage of this drug is the absence of some important elements of the composition of antlers that do not dissolve during the alcohol processing of the feedstock.

Known drug "Pantogran" and a method for producing its substance. "Pantogran" contains antler flour, icing sugar and vanillin in the following ratio of components, wt.%: Antler flour 45-55; icing sugar 49.94-49.96; vanillin 0.04-0.06. The method of obtaining the substance (antler meal) for the Pantogran drug consists in grinding dry antlers with the skin of deer, red deer or sika deer to particles of 5-10 mm, then in re-grinding to particles of not more than 0.1 mm (see application for invention No. 92003697, IPC А61К 35/32).

However, the method of obtaining the substance (antler meal) used for the manufacture of the Pantogran drug involves the re-grinding of dry antlers. In addition, the drying method is used to preserve antlers, which reduces the biological activity of antler meal.

Known dosage form of pantogematogen on a gel basis for external use, which includes, wt.%: Pantogematogen in the form of a 3% aqueous-alcoholic solution containing 8-14% ethyl alcohol 5-35, a polymer gelling composition based on a rare crosslinked acrylic acid polymer and / or polyvinylpyrrolidone 0.5-15 and water - the rest (see RF patent No. 2200564, IPC AK61/35/14).

However, the biologically active component of the helium-based pantogematogen dosage form, pantogematagen is dry, is obtained from the blood of deer, red deer or sika deer by vacuum drying and is introduced into the dosage form in the form of an aqueous-alcoholic solution containing 8-14% ethyl alcohol. Drying of the feedstock, as well as the use of ethyl alcohol, worsen the beneficial properties of pantohematogen.

Closest to the claimed method is a method of preparing a gel from antlers and wastes of their pharmaceutical processing, in which antlers are crushed or the wastes of their pharmaceutical processing are crushed, mixed with artificial gastric juice in a ratio of 1:10, placed in a thermostat at 37-40 ° C on three days, stirred 1 time per day for 2-3 minutes, filtered, the filtrate was disinfected by boiling, preserved with resorcinol, methyl cellulose was added in a ratio of 3 g per 100 ml and mixed until a uniform gel th consistency (see. RF patent №2248802, IPC: A61K 35/32).

The disadvantage of this method is the adverse effects on the biologically active substances of antlers of hydrochloric acid (the main component of artificial gastric juice), heating, boiling, as well as the duration and multi-stage process of preparing the gel.

The objective of the invention is to obtain a high quality gel based on an aqueous extract of antlers due to ultrasonic extraction of biologically active substances.

The technical result is to maintain and increase the biological activity of the obtained gel based on an aqueous extract of antlers due to the exclusion of the influence of high temperatures and treatment with chemical agents.

The problem is solved in that in the method of manufacturing a gel of antlers, including the extraction of biologically active substances from antlers at a temperature not exceeding 40 ° C, the introduction of preservatives and a gelling agent, according to the invention receive an aqueous solution of preservatives, which use methyl paraben in an amount of 0, 01-0.2 wt.% And propyl paraben in an amount of 0.002-0.01 wt.%, The extraction of biologically active substances is carried out by extraction into the resulting preservative solution by ultrasonic method in the cavitation mode at the ratio of the weight of the antlers to the mass of the aqueous solution 1: 1-10 for the time required to obtain the desired concentration of the extract, carbopol is selected as a gelling agent in an amount of 0.5-2 wt.%, which is pre-mixed with distilled water, kept to swell, add a neutralizing agent in an amount that ensures the formation of a gel-like mass, which is neutralized by the introduction of a solution of citric acid to a pH of 6-7.5, and the aqueous extract is added portionwise with stirring with stirring antlers and 1-30 wt.% a water-retaining component.

Glycerin can be used as a water-retaining component, and sodium hydroxide as a neutralizing agent.

It was experimentally established that the content of the gelling agent less than 0.5 wt.% Does not provide sufficient viscosity of the composition, which does not allow to fix it on the body area. When the content of the gelling agent is more than 2 wt.%, Technological difficulties arise, namely, it is difficult to mix and obtain a homogeneous mass of the gel, as well as packaging of the finished product. The limits of the content of the neutralizing agent NaOH are determined by the content of the gelling agent, since alkali is involved in the neutralization of the acid groups (-COOH) of carbopol. The content of citric acid is determined by the amount necessary to adjust the pH of the gel to a value of 6-7.5. The limits of the content of the humidifier (glycerin) are due to the following reasons. When the content is less than 1 wt.%, The lubricating and moisturizing effect is not preserved due to the loss of the gel's ability to retain moisture. With a content of more than 30 wt.%, The natural water-salt balance of the skin and microflora can be disturbed. The lower limit of the content of the mixture of preservatives (MP + PP) is sufficient to prevent the emergence and reproduction of microorganisms during the shelf life (at least 10 months). The upper limit is due to the amount that does not yet have a painful effect on the human body. In addition, we note that obtaining the extract by the ultrasonic method contributes to the disinfection of the gel.

The method is as follows. First, the method of ultrasonic extraction in the cavitation mode prepare an aqueous antler extract containing biologically active substances and including preservatives.

A polymer gelling composition is prepared consisting of a gelling agent and a neutralizing reagent. The gelling agent is selected from the group of polymers, the Carbopol family (according to the international classification - Carbomer, corresponds to the British Pharmacopoeia BP 516-93). The neutralizing reagent is selected from the group of organic and inorganic bases. The organic base is triethanolamine, inorganic bases are selected from the group of alkali metal hydroxides, aqueous ammonia. The pH value is controlled by the introduction of citric acid. The gelling agent is mixed with distilled water, stirred, kept at rest for 30 minutes, sufficient for swelling, then a neutralizing agent is added in an amount that ensures the formation of a gel-like mass, kept for 30 minutes, neutralized with a solution of citric acid to pH 6-7.5 and portionwise with stirring, an aqueous antler extract is introduced containing preservatives, for example, methyl paraben (MP) and propyl paraben (PP). A water-retaining agent (glycerin, propylene glycol) is introduced portionwise into the resulting system, mixed, and left alone for one day. Then the resulting gel is again mixed and Packed in a sterile container (tubes). The composition of the initial components of the gel may contain, by weight,% carbapol - 0.5-2; sodium hydroxide - 0.5-2; citric acid to a pH of 6-7.5; glycerol - 1-30; preservatives MP - 0.01-0.2 and PP - 0.002-0.01.

The resulting gel as a result of the interaction of the components of citric acid and sodium hydroxide will include sodium citrate, which is used in the pharmaceutical industry as a component of many drugs, in particular as an anticoagulant (Chemical Encyclopedia: 5 vol.: Vol. 2: Duff - Copper X 46 / Redkol; Knunyants I.L. (chap. Ed .;) and others - M .: Sov. Encycl., 1990.- pp. 1179-1180).

The following are examples illustrating the present invention.

The conditions for obtaining a gel based on an aqueous extract of antlers and the composition are presented in tables 1 and 2.

Example 1

First, the wool cover is mechanically removed from canned (steam) antlers of red deer, red deer or sika deer. Quartz is carried out and the antlers are cut in the transverse direction into large fractions of 2-5 cm in size. They are placed in an aqueous solution of preservatives (MP - 0.01 wt.% And PP - 0.002 wt.%) With the ratio of the mass of the antlers to the mass of the solution 1:10 . Then carry out ultrasonic extraction in the cavitation mode at a temperature of 40 ° C for 25 minutes After the extraction process is completed, the antler lobes and the aqueous extract are separated, pouring the latter into a sealed container. The conditions for obtaining and characterization of the aqueous extract of antlers are given in table 1.

For the preparation of the gel, simple equipment is used, equipped with a mixer - a reactor with a stirrer. The gel components are loaded into the mixer according to the recipe (wt.%): ULTREZ 10 carbopol (2%), distilled water, NaOH solution (2%), stirred, incubated for 30 min, titrated with citric acid solution to pH 6-7 and an aqueous antler extract containing preservatives is administered. Glycerin is added to the resulting mixture in an amount of 2 wt.%. The system is stirred for 10 minutes and the pH value is measured. The resulting homogeneous gel is packaged in a container. The characteristics of the gel and the composition are given in table.2.

Example 2

The stages of the method of obtaining an aqueous extract from antlers are similar to example 1. In this case, frozen antlers are used. The ratio of the mass of antlers to the mass of water is 1: 5. Ultrasonic extraction is carried out in an aqueous solution of preservatives (With _MP = 0.19 wt.% And With _PP = 0.01 wt.%) At a temperature of 18 ° C for 15 minutes (table 1). To prepare a gel based on this aqueous extract, the carbapol gelling agent is mixed with distilled water and allowed to swell for 30 minutes. Then, NaOH solution is added in an amount sufficient to form a gel, the system is kept for 30 minutes, titrated with a solution of citric acid to pH-6 and the extract, glycerin (9 wt.%) Are added portionwise with stirring, mixed and left to stand for one day to mature. . Then the gel is mixed and a homogeneous mass is Packed in a container. The characteristics and composition of the gel are given in table.2.

Example 3

All stages of obtaining an aqueous extract from antlers are similar to example 2, except for the extraction time (table 1). All operations to obtain a gel from this extract are also similar to example 2. Physico-chemical characteristics and composition of the gel are shown in table 2.

Example 4

In general, the steps for preparing an aqueous extract from antlers are similar to Example 2, except for the extraction time. In addition, for disinfection, the finished extract is filtered through filters with a pore diameter (d _pore ) = 0.8 and 0.45 μm (Table 1). The gel from this extract is obtained analogously to example 2. The characteristics and composition of the gel are given in table.2.

Example 5. It differs from example 3 in the extraction temperature.

The gel based on an aqueous extract of antlers effectively regenerates tissues damaged by injuries and burns, improves skin elasticity and nutrition, relieves the effects of dryness, inflammation and other adverse environmental effects due to the unique composition of biologically active substances, including macro- and microelements , antioxidants, vitamins and other beneficial ingredients. The resulting gel does not contain aggressive media inherent in other preparations from antlers. Using the method allows to obtain a complex multicomponent composition, including proteins, amino acids, hormones, lipids, minerals, complex compounds that have pronounced biological activity.

Industrial applicability. The proposed gel can be prepared both in the conditions of large cosmetic factories, enterprises, and in the workshops of small companies that have the appropriate equipment.

Table 1
Conditions for obtaining and characterization of an aqueous extract of antlers. Name of indicator and unit of measurement Examples one 2 3 four 5 Appearance and color red liquid of various shades Antler canning method steam treatment freezing The ratio of the mass of antlers to the mass of an aqueous solution of preservatives 1:10 1: 5 1: 5 1: 4,5 1: 4,6 The temperature of extraction, T ° C 40 eighteen eighteen 17 35 The extraction time, min 25 fifteen twenty thirty twenty Filtration through biological filters with d _por = 0.8 and 0.45 microns The content of preservatives (wt.%): methyl paraben 0.01 0.19 0.19 0.2 0.19 propyl paraben 0.002 0.01 0.01 0.003 0.01 Solids content, wt.% 0.33 0.81 1,1 1,1 1D The total protein content, wt.% 0.11 0.67 0.82 0.94 1.12 The hemoglobin content, wt.% 0,081 0.36 0.44 0.50 0.8

table 2
Physico-chemical characteristics and composition of the gel. Name of indicator and unit of measurement GOST R52343-2005 norm Examples one 2 3 four 5 Appearance Homogeneous mass free of impurities Homogeneous mass free of impurities Color Inherent to the color of this cream light brown Dark red Smell Inherent to the smell of this gel Inherent to the smell of this gel Mass fraction of water and volatiles, wt.% 5.0-98.0 94.8 88.5 87.5 90.6 92.4 Colloidal stability Stable Stable Thermal stability Stable Stable Mass fraction of the sum of heavy metals,% (mg / kg), no more 0.0020 (20.0) Conforms to standards of GOST P52343-2005 microbiological indicators Conforms to norms of SanPiN 1.2.681-97 Conforms to norms of SanPiN 1.2.681-97 The content of the aqueous extract, wt.% 70 72 72 64 70 The content of the gelling agent (carbopol), wt.% 1,5 0.9 1,1 1.3 1,2 Sodium Citrate 1,5 0.9 1,0 1.3 1.3 The glycerol content, wt.% 2 9.0 9,4 6.0 four The content of methyl paraben, wt.% 0.007 0.14 0.14 0.13 0.14 The content of propyl paraben, wt.% 0.0014 0.007 0.007 0.002 0.007 PH value 5.0-9.0 6.2 6.0 6.8 6.4 7.0

Claims (2)

1. A method of manufacturing a gel of antlers for external use, comprising extracting biologically active substances from antlers at a temperature not exceeding 40 ° C, introducing preservatives and a gelling agent, characterized in that an aqueous solution of preservatives is obtained, which use methyl paraben in an amount of 0, 01-0.2 wt.% And propyl paraben in an amount of 0.002-0.01 wt.%, The extraction of biologically active substances is carried out by extraction into the resulting preservative solution by ultrasonic method in the cavitation mode at a weight ratio antlers to the mass of an aqueous solution of 1: 1-10 for the time required to obtain the desired concentration of the extract, carbopol is selected as a gelling agent in an amount of 0.5-2 wt.%, which is pre-mixed with distilled water, kept until swelling, neutralizing is added the agent in an amount that ensures the formation of a gel-like mass, which is neutralized by introducing a solution of citric acid to a value of 6-7.5, and an aqueous antler extract and 1-30 wt.% are added portionwise with stirring to the resulting gel-like mass water-retaining component. 2. The method according to claim 1, characterized in that glycerin is selected as the water-retaining component, and sodium hydroxide is used as the neutralizing agent.