RU2568586C1 - Method of producing dry extract of bupleurum aureum - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: method of obtaining a dry extract of Bupleurum aureum from Bupleurum aureum herbs which, after crushing, are sieved to obtain a homogeneous material; extraction is carried out via three-step maceration while dividing the extractant into equal portions; the extractant used is a solution of ethyl alcohol in water; extracts obtained by extraction are combined; the obtained extract is purified by centrifuging, filtered and thickened; the obtained product is dried, followed by crushing, sieving to a homogeneous granular state under defined conditions.

EFFECT: method enables to obtain a dry extract of Bupleurum aureum with high output of active substances.

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Description

The invention relates to the food, pharmaceutical, medical and biotechnological industries and can be used for the preparation of extracts from plant materials, in particular the preparation of a dry extract of Golden Wax.

A known method of producing the extract [RU 2509567 C1, A61K 36/06, B01D 11/02, 03/20/2014], based on the fact that the raw material is frozen, poured with an aqueous solution containing dimethyl sulfoxide and sodium hydroxide, and kept at a solution temperature of 50- 90 ° C for 1-2 hours.

Despite the fact that the known method allows to obtain an extract with a high yield of extractive substances and high antioxidant activity, but its disadvantage is the relatively narrow scope, since it can be used mainly to obtain the extract from chaga meal. An attempt to use it without additional modification for another type of raw material leads to a significantly low yield of pharmacologically active substances.

There is also known a method [RU 2501329 C1, A23L 1/30, A23C 9/142, A23J 3/08, 12/20/2013], according to which the feedstock is poured with water and extracted for 10-16 hours at a temperature of 50-100 ° C, the extract obtained is filtered, whey protein concentrate obtained by ultrafiltration of whey with a solids content of 9-25% in a ratio of 1: 5-15 is added to it, the mixture is heated for 5-10 minutes at a temperature of 50-70 ° C, after wherein the mixture is centrifuged at 1000-3000 rpm for 15-30 minutes and filtered.

The disadvantage of this technical solution is also a relatively narrow scope, since it can be used mainly to obtain an extract from the plant Stevia Rebaudiana Bertoni. An attempt to use it without additional modification for another type of raw material leads to a significantly low yield of pharmacologically active substances.

The closest in technical essence to the proposed is the method [Yu.S. Kanunnikova. Development of parameters for extracting the sum of biological active substances of golden grass of the grass // Questions of biological, medical and pharmaceutical chemistry. - 2013, No. 5, p. 35], which disclosed a method of obtaining a dry extract of goldenwort by triple extraction with a 50% alcohol solution for 45 minutes at an operating temperature of 60 ° C.

The disadvantage of the closest technical solution is the relatively low yield of pharmacologically active substances.

The main reason for this is the insufficient elaboration of the modes of operations, methods with their theoretical and experimental elaboration, aimed at increasing the yield of pharmacologically active substances.

The problem that is solved in the proposed invention is to increase the yield of pharmacologically active substances.

The required technical result achieved by the implementation of the claimed invention is to increase the yield of pharmacologically active substances.

The problem is solved, and the required technical result is achieved by the fact that, in a method based on the fact that the original plant material, which is used as golden grass, is crushed and extracted, according to the invention, after grinding, the plant material is sieved on sieves with a diameter holes 1 mm to obtain a homogeneous material, and the extraction is carried out at a temperature of 55-65 ° C by three-stage fractional maceration with dividing the extractant into equal parts, while as ext the reagent, use a 50% solution of ethyl alcohol in purified water, dividing the extractant into equal parts at the end of each stage, the duration of each of which is set within 45 minutes, and the extracts obtained as a result of raw material extraction at each of the three stages are combined and a primary extract is obtained, which purified by centrifugation at 1000 rpm for 30 minutes, followed by filtration, concentrated to 1/16 of the original volume on a rotary evaporator, to a residual moisture content of 20-25%, and the resulting product is dried in a vacuum dryer to a residual moisture content of not more than 3-5%, followed by grinding by sieving to a homogeneous bulk state.

A method of obtaining a dry extract of golden volodushka is as follows.

The feedstock - the golden crocodile grass is pre-crushed in roll-type mills to a particle size of 1 mm. Since deviations from this size to ± 0.1 mm are actually obtained, to obtain a homogeneous material, they are sieved on sieves with a hole size of 1 mm. Based on experimental data, it was found that particles passing through a sieve with an opening of 1 mm are optimal. finer grinding leads to the formation of a cloudy filtrate, which complicates the analysis and further use in technological processes, and also contributes to the "cementing" of the raw material and, as a result, leads to a decrease in the yield of extractive substances. A larger particle size leads to a decrease in the diffusion process from the feedstock, which also entails a decrease in the recoverability of active substances.

Then the process is continued by conducting a three-stage fractional maceration at a temperature of 55-65 ° С with dividing the extractant into equal parts, while a 50% solution of ethyl alcohol in purified water is used as extractant with dividing the extractant into equal parts at the end of each stage, the duration of each of which are set within 45 minutes, and the extracts obtained as a result of extraction of the raw material at each of the three stages are combined and a primary extraction is obtained.

Temperature 55-65 ° C, i.e. about 60 ° C, corresponds to the experimentally confirmed optimal temperature relative to the efficiency of obtaining active substances. At a lower temperature, the yield of active substances is significantly reduced, and at a higher temperature, undesirable additives appear that worsen the properties of the extract.

The three-stage process is due to the following quantitative data being established in the process of experimental studies. At the first contact of the phases, 55-60% of extractive substances go into extraction, at the second - 20-25%, at the third and subsequent contacts 5-10%. Thus, triple extraction ensures the depletion of raw materials by an average of 85-95%. Therefore, a smaller number of stages leads to an insufficient degree of extraction, and a larger number of stages does not allow to improve the result, because raw materials after the third stage are almost completely depleted.

It was also experimentally established that the duration of the stage should lie in the range of 40-50 minutes, since a shorter duration is insufficient, and a longer one is ineffective. In practice, the duration of the stages was set at 45 minutes.

Extracts obtained as a result of raw material extraction at each of the three stages are combined and a primary extract is obtained, which is purified by centrifugation at 1000 rpm for 30 minutes, followed by filtration, concentrated to 1/16 of the initial volume on a rotary evaporator to a residual moisture content of 20-25 % since according to the standard, the humidity of the thick extract after the maximum evaporation of the extractant should be no more than 25%, and the resulting product is dried in a vacuum dryer to a residual moisture content of no more than 3-5%, since according to the standard there should be no more than 5%. In practice, the humidity of the freshly dried extract was 3.5%, but since the extract is hygroscopic, during storage, the humidity increased to 4.0-4.5%.

Finally, subsequent grinding and sieving is carried out to a homogeneous free-flowing state.

According to the proposed method, a dry extract of biologically active substances of the herb Goldenwort is obtained.

The content of phenolic compounds in terms of rutin in the obtained extract is at least 8.0%. The pharmacological activity of golden sheath grass has been studied and proven, in particular, as a choleretic, capillary and P-vitamin, as well as antioxidant and antioxidant agents. The main biologically active substances of the dry extract, causing the pharmacological effects, are phenolic compounds and saicosaponins.

An example of obtaining a dry extract of golden hairwort.

We took 300 g of dry grass of the plant Bupleurum aureum Fisch. seu longifolium L.) with a fineness of about 1 mm, followed by sieving on sieves with a hole diameter of 1 mm and 3450 g of ethyl alcohol 50% (taking into account the absorption coefficient of 1.5). The raw material was poured with the first portion of the extractant ″ to the mirror ″ and extraction was carried out at a temperature of 55-65 ° C for 40-50 minutes. The resulting extract was drained. The raw material was poured with a new portion of the extractant to the volume of the drained extraction. A second extraction was performed. The resulting extract was drained. Then, a third extraction was performed. The obtained extracts were combined. Purification was carried out by centrifugation at 1000 rpm for 30 minutes, followed by filtration and evaporation on a rotary evaporator. Evaporation was carried out at a reaction mass temperature (60 ± 5) ° С and a pressure of 0.09 MPa to approximately 1/16 of the initial volume to a residual moisture content of 20-30%, and the resulting product was dried in a vacuum dryer to a residual moisture content of not more than 3-5% followed by grinding, sieving to a homogeneous loose state.

Thus, due to the introduction of an additional arsenal of technical methods (method operations), the required technical result is achieved, which consists in expanding the scope of the method, which allows to obtain a dry extract of goldenwort with a high yield of pharmacologically active substances.

Claims (1)

A method of obtaining a dry extract of golden volodushka, based on the fact that the source of plant material is crushed and extraction is performed, characterized in that the plant is used as a plant material of golden volodushka, which after grinding is sieved on sieves with a hole diameter of 1 mm to obtain a homogeneous material, and extraction is carried out at a temperature of 55-65 ° C by three-stage fractional maceration with dividing the extractant into equal parts, while 50% ethyl solution is used as the extractant alcohol in purified water, the duration of each extraction stage is set within 45 minutes, and the extracts obtained as a result of raw material extraction at each of the three stages are combined and a primary extract is obtained, which is purified by centrifugation at 1000 rpm for 30 minutes, followed by filtration, thicken to 1/16 of the original volume on a rotary evaporator, to a residual moisture content of 20-25%, and the resulting product is dried in a vacuum dryer to a residual moisture content of not more than 3-5%, followed by grinding, sieving homogeneous particulate state.