RU2257222C1 - Complex processing medicinal fungus polyporus (fomitopsis officinalis (vill.: fr.) bond. et sing.) - Google Patents

Abstract

FIELD: pharmaceutical technology, natural compounds.

SUBSTANCE: invention relates to the complex processing medicinal raw. Method for the complex processing medicinal fungus Polyporus (Fomitopsis officinalis (Vill.: Fr.) Bond. Et Sing.) involves milling raw followed extraction for four steps. At the first step the raw is extracted with fluidized carbon dioxide under definite conditions and carbonic acid extract comprising essential oil, unsaturated fatty acids, carotinoids, vitamins E, A and sterols is isolated. At the second step residue is extracted with diethyl ether under definite conditions and extract comprising agaricic acid, lipid-carotinoid complex and residue is isolated and the latter residue is extracted at the third step and alcoholic extract comprising carotinoids, bioflavonoids and vitamin K is isolated. At the forth step residue is extracted with water under definite conditions followed by infusing under definite conditions and isolation of an aqueous extract comprising carbohydrates, part of tannic substances, vitamins B₁, B₂, B₆ and P. Variation of technological parameters allows retaining large amount of biologically active substances in extracts.

EFFECT: improved processing method.

2 tbl, 2 ex

Description

The invention relates to the field of complex processing of medicinal and technical raw materials, namely to obtain biologically active products that may find application in the composition of cosmetics and medicines.

A known method of obtaining funds with hypothermic action, which is an aqueous extract of wood-destroying fungi. The aqueous extract is obtained by extracting mushrooms (false birch tinder, false oak tinder or aspen tinder) with boiling water (Pat. SU 1827257 A1, A 61 K 35/78. Substance with hypothermic effect / Pereverzev VA, etc. No. 4802214/14, Declared March 14, 90, Published July 15, 93, Bull. No. 26).

The disadvantage of this method is that it releases only water-soluble components of wood-destroying fungi and the resulting product has a narrow spectrum of action.

A known method of obtaining funds with antiulcer and adaptogenic activity by extraction of birch fungus - chaga with hot water using ultrasound with a frequency of 20-55 KHz, intensity of 0.1-2.3 W / cm ² at 60-65 ° C for 50- 60 min (Pat. SU 1805968 A3, A 61 K 35/78 A method of obtaining funds with antiulcer and adaptogenic activity / Ryzhkova G.L. et al. No. 4896239/14, Declared 25.12.90, Publ. 30.03.93, Bull. No. 12).

This product contains only water-soluble Chaga substances, and biologically active substances, such as terpenes, carotenoids, tocopherols and others, are not extracted from raw materials. In addition, the disadvantage of this method is the low utilization of raw materials, which consists in the extraction of only water-soluble substances, and there is no further processing of raw materials.

A known method of obtaining a bioactive extract from Macleaya microcarpa containing alkaloids and additionally terpenes, fatty acids, tocopherols. Carbon dioxide extract is obtained in a supercritical state at a temperature of 40-70 ° C and a pressure of 250-300 atm. (Pat. 2214261 C1, 6 A 61 K 35/78, A 61 P 21/00. Bioactive extract from Macleaya microcarpa and method for its preparation / Averin K.M. et al. No. 20011130380/14, Application. 09.11.01) .

The disadvantage of this method is the extraction in a supercritical state, which is the cause of the following disadvantages. The first drawback is the use of high temperature leads to the decomposition of unstable biologically active substances. The second drawback is the use of high pressure requires additional costs and safety measures.

A known method of complex processing of aromatic raw materials, including the extraction of crushed raw materials with liquefied gas at a pressure of 6.0-6.6 MPa, a temperature of 18-22 ° C for 5 hours with the release of carbon dioxide extract and residue and subsequent extraction of the residue with ethanol (Pat 2135552 С1, 6 С 11 В 1/10, 9/02, А 23 L 1/226 Complex processing of aromatic raw materials / Repyakh S.M. et al. No. 98111161/13, Declaration 10.06.98, Publ. . August 27, 1999, Bull. No. 24).

The disadvantage of this method is the use of only two-stage extraction, which does not allow to fully extract all components of biologically active substances.

The methods of complex processing of fungus tinder fungus medicinal authors are not known.

The invention solves the problem of obtaining new biologically active products and complex processing of the fungus medicinal fungus, that is, the development of non-waste technology with the maximum number of various biologically active products.

The technical result consists in increasing the utilization of raw materials and expanding the range of biologically active substances and the quality of the target products.

The specified technical result is achieved by the fact that in complex processing of the fungus, the medicinal tinder (Fomitopsis officinalis (VilL: Fr.) Bond. Et Sing) raw materials are crushed to a particle size of 1-3 mm and subjected to four-stage extraction, at the first stage they are extracted with liquefied carbon dioxide under pressure 6.0-7.0 MPa, temperature 22-26 ° С for 10-12 hours with the release of carbon dioxide extract containing essential oil, fatty unsaturated acids, carotenoids, vitamins E, A and sterols, then the residue is extracted with diethyl in the second stage ether at temperature 34-36 ° C for 2-3 hours with the selection of the extract containing agaric acid and lipid-carotenoid complex, and the residue, which in the third stage is extracted with 70-96% ethyl alcohol for 3-6 hours at a temperature of 78-80 ° C with the release of an alcoholic extract containing carotenoids, bioflavonoids and vitamin K, in the fourth step, the residue is extracted with water at a temperature of 98-100 ° C for 3-5 hours, followed by infusion for 10-12 hours at a temperature of 18-22 ° C , with the release of an aqueous extract containing carbohydrates, hour s tannins, vitamins B _1, B _2, B _6, R.

The authors obtained a previously undescribed biologically active product - carbon dioxide extract from the fungus tinder fungus Fomitopsis officinalis (VilL: Fr.) Bond. Et Sing.), Which grows on Siberian larch and is a medicinal raw material. The resulting carbon dioxide extract has physico-chemical characteristics shown in table 1.

Table 1 Physico-chemical characteristics of carbon dioxide extract from medicinal tinder fungus (Fomitopsis officinalis (VilL: Fr.) Bond. Et Sing.) Indicators Extract Appearance, color, texture, smell oily, pasty mass, dark brown in color with a pronounced odor characteristic of the feedstock Density, kg / m ³ , (20 ± 2) ° С 978.3-978.8 Refractive Index, n _D ²⁰ (20 ± 2) ° C 1.4922-1.4925 Acid number, mg KOH / g 68.92-70.36 Ether number, mg KOH / g 28.19-34.24

Upon subsequent extraction of the residue in the second, third and fourth stages, ether, alcohol and water extracts were obtained from the medicinal tinder, the physicochemical parameters of which are presented in table 2.

table 2 Physico-chemical characteristics of the ether, alcohol and water extracts from the residues after carbon dioxide extraction Indicators Extracts ethereal alcohol water Appearance, color, texture, smell transparent, bright yellow, liquid, • without a characteristic odor transparent, dark brown, liquid, mild odor of raw materials transparent, brown, liquid, slightly expressed smell of raw materials Density, kg / m ³ , (20 ± 2) ° С 737.0-742.0 805.0-815.0 997.0-998.0 Refractive Index, n _D ²⁰ (20 ± 2) ° C 1,367-1,373 1,361-1,363 1,334-1,3345 Acid number, mg KOH / g 226.64-228.59 210.56-215.76 0.44-0.48 Ether number, mg KOH / g 86.11-88.67 360.84-364.82 is absent

Extraction with carbon dioxide allows you to remove biologically active substances in the native state from the fungus, since the process parameters give carbon dioxide the properties of a universal solvent for almost all classes of biologically active substances, namely, essential oils, tocopherols, carotenoids and unsaturated fatty acids. The following extraction of the post-extraction residue with diethyl ether makes it possible to additionally extract fat-soluble substances insoluble in liquefied gas under mild conditions from the raw material that are characteristic of the fungus of the medicinal tinder. Extraction with ethyl alcohol of various concentrations promotes the release of the maximum amount of biologically active substances, and further extraction with water allows the extraction of water-soluble biologically active substances.

The difference of the proposed method is that in the first stage, the extraction of liquefied carbon dioxide is carried out at a pressure of 6.0-7.0 MPa, a temperature of 22-26 ° C for 10-12 hours. In the second stage, extraction with diethyl ether is carried out at a temperature of 34-36 ° C for 2-3 hours, in the third stage it is extracted with 70-96% ethyl alcohol at a temperature of 78-80 ° C for 3-6 hours, in the fourth stage, extraction is carried out water at a temperature of 98-100 ° C for 3-5 hours, followed by infusion of 10-12 hours at a temperature of 18-22 ° C, which allows to increase the yield of biologically active substances and the quality of the target products.

As a result of the developed technology for processing biomass of the fungus, the medicinal tinder fungus (Fomitopsis officinalis (VilL: Fr.) Bond. Et Sing.), It is possible to obtain products containing a complex of biologically active substances:

- at the first stage - СО ₂ - an extract containing essential oil, fatty unsaturated acids, carotenoids, vitamins E, A and sterols;

- at the second stage - an ether extract containing carotenoids, fatty unsaturated acids, agaricic acid, vitamin A and sterols;

- at the third stage - alcohol extract containing carotenoids, bioflavonoids and vitamin K;

- at the fourth stage - an aqueous extract containing carbohydrates, part of tannins, vitamins B ₁ , B ₂ , B ₆ , R.

The presence in the resulting products of biologically active substances, such as essential oils, carotenoids, vitamins E, A, K, etc., improves the quality of cosmetics and medicines that can be used as part of ointments, gels, emulsions or solutions for external use. So, essential oils give the product antimicrobial and bactericidal activity, a complex of carotenoids and vitamins E, A acts as an antioxidant and stimulator of reparative processes, promotes rapid epithelization of wound and burn surfaces, accelerates the healing of mucous membranes. Vitamin K has a hemostatic effect, and agaricinic acid has healing properties in the treatment of various forms of tuberculosis (Kazarinova I.V., Tkachenko K.G. Medicinal plants in the treatment of various forms of tuberculosis / Plant resources. - 2000. - T. 36. - issue .1. - 92 - 106 p.).

The complex processing of biomass of the fungus medicinal tinder fungus is carried out as follows: in the first stage, the extraction is carried out with carbon dioxide, in the second with diethyl ether, in the third with 70-96% ethyl alcohol, in the fourth with water. According to the invention, the biomass of the fungus with a moisture content of 7-8% is ground to a particle size of 1-3 mm and extracted, in the first stage, with carbon dioxide at a pressure of 6.0-7.0 MPa, a temperature of 22-26 ° C for 10-12 hours to obtain a carbon dioxide extract containing a biolipid complex. Then, in the second stage, the residue is extracted with diethyl ether at a temperature of 34-36 ° C for 2-3 hours, the obtained extract contains a lipid-carotenoid complex. In the third stage, extraction is carried out with 70-96% ethyl alcohol at a temperature of 76-78 ° C for 3-6 hours. At the fourth stage, water is extracted at a temperature of 98-100 ° C for 3-5 hours, followed by 10-12 hours at a temperature of 18-22 ° C.

Example 1

The fungus tinder fungus biomass in the amount of 5350 g with a moisture content of 7-8% is ground to a particle size of 1-3 mm, extracted in the first stage with carbon dioxide at a pressure of 6.0 MPa and a temperature of 22 ° C for 10 hours. Get 74.63 g of the extract with the content of carotenoids - 3.12 mg%, essential oil - 9.66%, vitamin E - 12.5 mg%, vitamin A - 0.8 mg%, fatty unsaturated acids - 46.37% sterols - 1.68% (of extractive substances). The residue obtained after extraction with carbon dioxide in the second stage is extracted with diethyl ether at a ratio of solid residue-solvent 1:15 and a temperature of 34 ° C for 2 hours. Get a product containing: carotenoids - 3.42%, vitamin A - 1.1 mg%, agaricic acid - 6%, sterols - 1.34%, unsaturated acids - 44.45% (from extractive substances). The fat-free residue is extracted with 70% ethyl alcohol at a temperature of 78 ° C to obtain an alcohol extract containing bioflavonoids - 0.20%, carotenoids - 1.81% and vitamin K - 0.12 mg% (by weight of extractive substances). The residue obtained after alcohol extraction is extracted with water at a temperature of 98 ° C for 3 hours and infused for 10 hours at a temperature of 18 ° C. A product is obtained containing: carbohydrates - 6.58%, vitamins B ₁ - 0.9 mg%, B ₂ - 7.75 mg%, B ₆ - 0.55 mg%, P - 0.068 mg%, tannins - 0 , 26% (of extractive substances).

Example 2

The fungus tinder fungus biomass in the amount of 5350 g with a moisture content of 7-8% is crushed to a particle size of 1-3 mm, extracted in the first stage with carbon dioxide at a pressure of 7.0 MPa and a temperature of 26 ° C for 12 hours. Get 75.26 g of extract with the content of: carotenoids - 3.8 mg%, essential oil - 10.82%, vitamin E - 14.3 mg%, vitamin A - 0.85%, unsaturated acids - 47.41%, sterols - 1.72% (of extractive substances). The residue obtained after extraction with carbon dioxide in the second stage is extracted with diethyl ether at a ratio of solid residue-solvent 1:15 and a temperature of 36 ° C for 3 hours. Get a product containing: carotenoids - 3.56%, vitamin A - 1.23 mg%, agaricic acid 8%, sterols - 1.43%, unsaturated acids - 45.62% (by weight of extractive substances). The fat-free residue is extracted with 96% ethyl alcohol at a temperature of 80 ° C to obtain an alcohol extract containing bioflavonoids - 0.28%, carotenoids - 2.15% and vitamin K - 0.16% (by weight of extractive substances). The residue obtained after alcohol extraction is extracted with water at a temperature of 100 ° C for 5 hours and infused for 12 hours at a temperature of 22 ° C. A product is obtained containing: carbohydrates - 6.84%, vitamins B ₁ - 1.2 mg%, B ₂ - 7.97 mg%, B ₆ - 0.58 mg%, P - 0.072 mg%, tannins - 0 , 28% (of extractive substances).

The proposed method allows for more efficient use of medicinal and technical raw materials in its complex processing with the receipt of additional biologically active components. The use of four-stage extraction using solvents with different dielectric constants, as well as varying technological parameters (pressure, temperature, duration, grinding) allows us to expand the range of biologically active additives. Complex processing of mushroom tinder fungus makes it possible to maximize the extraction of biologically active substances. The proposed method allows you to save in extracts a large number of biologically active substances.

Claims (1)

Complex processing of fungus tinder fungus (Fomitopsis officinalis (Vill .: Fr.) Bond. Et Sing.), Characterized in that the raw materials are crushed to a particle size of 1-3 mm and subjected to four-stage extraction, in the first stage, they are extracted with liquefied carbon dioxide at a pressure of 6 , 0-7.0 MPa, temperature 22-26 ° C for 10-12 h with the release of carbon dioxide extract containing essential oil, fatty unsaturated acids, carotenoids, vitamins E, A and sterols, then the residue is extracted into diethyl ether in the second stage at a temperature of 34-36 ° C for 2 -3 hours with the release of an extract containing agaricic acid and a lipid-carotenoid complex, and the residue, which in the third stage is extracted with 70-96% ethanol for 3-6 hours at a temperature of 78-80 ° C with the release of the alcohol extract, containing carotenoids, bioflavonoids and vitamin K, in the fourth step, the residue is extracted with water at a temperature of 98-100 ° C for 3-5 hours, followed by infusion for 10-12 hours at a temperature of 18-22 ° C with the release of an aqueous extract containing carbohydrates , part of tannins, vitamins B ₁ , B ₂ , B ₆ , R.