RU2238663C2 - Method for obtaining biologically active product out of allium victorialis - Google Patents

Abstract

FIELD: food industry, pharmaceutics.

SUBSTANCE: the present innovation deals with obtaining a product containing biologically active substances, out of plant raw material due to extraction by liquefied gas. Moreover, one should apply either pre-reduced or vegetative part of Allium victorialis. Extraction runs at the pressure of 5.8-6.0 MPa for 4-5 h at 20-22 C by obtaining a target product as carbon dioxide extract of ramson. Obtained extract has the following characteristics: ether number - 47.38 or 86.96 mg KOH/1 g, acid number - 27.83 or 38.77 mg KOH/1 g, the sum of chlorophylls being 60.82 or 88.93 mg %, carotene 2.39 mg % or 3.21 mg %, saponifiable substances 64.57% or 87.7%, unsaponifiable substances 8.946% or 27.46%. The innovation enables to obtain the product with high content of biologically active substances.

EFFECT: higher efficiency.

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Description

The invention relates to food and pharmaceutical industries and relates to a method for producing products containing biologically active substances.

The authors obtained biologically active products not previously described from the vegetative part of Allium victorialis.

A known method of producing a biologically active product based on wild garlic - urozall by extraction of plant bulbs with an organic solvent with diethyl ether (Minaeva VG Medicinal plants of Siberia. - Novosibirsk: Nauka, 1991. - 431 S.).

The disadvantage of this method is the use of only plant bulbs as a feedstock, diethyl ether as a solvent and incomplete extraction of biologically active substances.

A known method of obtaining a biologically active product based on wild garlic by extraction of the vegetative part of Allium victorialis with an organic solvent or water with a liquid module of 1: 7 for 1-24 hours (patent RU No. 2152793, MKI A 61 K 35/78, 20/07/00 Bulletin No. 20).

The disadvantage of this method is the incomplete extraction of biologically active substances.

A known method of extracting plant materials with liquefied gases to obtain drugs from medicinal herbs by grinding and processing the extractant in at least two stages, with pressure relief between stages, and before the pressure is released, miscella is drained (Copyright certificate SU No. 1018639 C1, 26/02 / 81).

The disadvantage of this method is the low yield of extractive substances, and only medicinal plants (chamomile, yarrow, wormwood, St. John's wort, etc.) are used as plant materials.

However, the described technologies do not solve the problem of maximum and complete extraction of biologically active substances from raw materials.

The invention solves the problem of obtaining new products from the vegetative part of wild garlic with a high content of biologically active substances and the possibility of isolating certain groups of chemical compounds from raw materials.

The technical effect that can be obtained by carrying out the invention is to create a new method for producing biologically active substances with an increase in the yield of extractive substances.

The specified result in the implementation of the invention is achieved by the fact that in the method for producing a biologically active product from plant materials by extraction with liquefied gas, according to the invention, a pre-shredded or whole vegetative part of Allium victorialis is used as a raw material, extraction is carried out at a pressure of 5.8-6.0 MPa for 4-5 hours at a temperature of 20-22 ° C to obtain the target product in the form of a carbon dioxide extract of wild garlic with an ether number of 47.38 or 86.96 mg KOH / 1 g, an acid number of 27.83 or 38.77 mg KOH / 1 g, total chloro phyll 60.82 mg or 88.93 mg%, carotene 2.39 mg% or 3.21 mg%, saponifiables 64.57% or 87.7%, unsaponifiables 8.946% or 27.46%.

The authors obtained biologically active products not previously described.

Biologically active products obtained by the extraction of wild garlic are carbon dioxide and alcohol extracts obtained by extraction of the whole or chopped vegetative part of Allium victorials, which differ in their composition.

Carbon dioxide extracts:

- from the whole vegetative part of Allium victorials is an oily yellow-green liquid with a characteristic smell of wild garlic. It contains biologically active substances (chlorophylls, carotene, essential oils). The main physical and chemical characteristics (at 20-22 ° C): density 838 kg / m ³ ; refractive index 1.3691; acid number 27.83 mg KOH / 1 g of feed; ether number 86.96 mg KOH / 1 g;

- from the crushed vegetative part of Allium victorials, it is an oily yellow-green liquid with a characteristic smell of wild garlic. It contains biologically active substances (chlorophylls, carotene, essential oils). The main physical and chemical characteristics (at 20-22 ° C): density 827 kg / m ³ ; refractive index 1.3671; acid number 38.77 mg KOH / 1 g of feed; ether number 47.38 mg KOH / 1 g

Alcohol extracts:

- from the whole vegetative part of Allium victorials it is a dark green liquid with a specific smell of wild garlic. It contains biologically active substances (chlorophylls, carotene). The main physical and chemical characteristics (at 20-22 ° C): density 877 kg / m ³ ; refractive index 1.3621; acid number 8.63 mg KOH / 1 g of feed; an ether number of 33.98 mg KOH / 1 g;

- from the crushed vegetative part of Allium victorials is a green liquid with a specific smell of wild garlic. It contains biologically active substances (chlorophylls, carotene). The main physical and chemical characteristics (at 20-22 ° C): density 873 kg / m ³ ; refractive index 1.3641; acid number 10.05 mg KOH / 1 g of feed; ether number 28.43 mg KOH / 1 g.

Processing of medicinal and essential oil plant materials with liquefied gases in order to extract individual components in an unchanged (native) form is one of the highly efficient processes that reduce labor costs, improve product quality, and promote the integrated use of raw materials and materials.

Liquid carbon dioxide has specific properties that determine the effectiveness of its use as an organic extractant for the extraction of biologically active and aromatic substances from plant materials. Extraction and distillation of the solvent at low temperatures (up to 30 ° C) make it possible to extract essential oils that preserve the aroma of the feedstock and biologically active components in their native state. Liquid carbon dioxide does not support the life of microorganisms and molds, which makes it possible to obtain sterile extracts even when using it for raw materials seeded with microorganisms.

Liquefied CO ₂ gas is a colorless, easily mobile liquid, the viscosity of which is 14 times lower than the viscosity of water, 5 times that of ethyl alcohol, such properties of liquefied CO ₂ distinguish it as an extractant with the best diffusion properties. Liquid carbon dioxide is thermally stable at ordinary temperatures, chemically inert, which also allows you to maintain the native properties of the products it extracts. The optimum temperature for extraction with liquid carbon dioxide lies in the range 0-25 ° C. A characteristic feature of carbon dioxide is a low critical temperature of 31.05 ° C. This property determines the upper limit of the temperature range in which extraction can occur.

Liquefied carbon dioxide extracts fatty oils, free organic acids, fat-soluble vitamins, carotenoids, flavonoids, some alkaloids, glycosides, vegetable resins, waxes and some other compounds are extracted worse (Molchanov G.I. Intensive processing of medicinal raw materials. - M .: Medicine, 1981 , - p. 208).

A variety of components of plant materials, dramatically different in their solubility, requires a wide range of extractants for their complete extraction.

Ethyl alcohol 70-94% is used to extract alcohol-soluble substances, for example vitamins C, P.

A method of obtaining biologically active products is as follows.

Vegetative part of wild garlic (whole or chopped) is loaded into the extractor. After closing the hatches, gaseous CO _{2 is} supplied into the system; upon reaching a working pressure of 6 MPa, liquid carbon dioxide is fed through the valve and flow extraction begins.

After the process, the flow of solvent stops. The remaining miscella is poured into the evaporator, where the solvent is distilled off, then the extract is discharged from the evaporator. The solid residue is dried and then extracted with a solution of ethyl alcohol.

The method is illustrated by the following examples.

Example 1

The whole vegetative part of wild garlic is extracted with liquefied carbon dioxide at a pressure of 6.0 MPa, a temperature of 20-22 ° C for 4 hours.

Carbon dioxide extract is obtained in the form of an oily liquid, yellow-green in color with dark shades, with a specific smell of wild garlic. The product yield is 3.45% by weight of absolutely dry raw materials. The main physical and chemical characteristics (at 20-22 ° C): density 838 kg / m ³ ; refractive index 1.3691; acid number 27.83 mg KOH / 1 g of feed; ether number 86.96 mg KOH / 1 g; saponification number, 114.79 mg KOH / 1 g of raw material. Content: saponified substances 64.57%; unsaponifiable substances 27.46%; the sum of chlorophylls 88.93 mg%; carotene 2.39 mg%.

The dried solid residue of whole wild garlic after carbon dioxide extraction is extracted with a 94% solution of ethyl alcohol at atmospheric pressure, a temperature of 20 ° C for 3 hours, with a ratio of solid phase: extractant 1: 3.

An alcoholic extract is obtained in the form of a dark green liquid with a specific smell of wild garlic.

The product yield is 24.87% by weight of absolutely dry raw materials. The main physical and chemical characteristics (at 20-22 ° C): density 877 kg / m ³ ; refractive index 1.3621; acid number 8.63 mg KOH / 1 g of feed; an ether number of 33.98 mg KOH / 1 g; saponification number 42.61 mg KOH / 1 g of raw material; the amount of chlorophyll 28.55 mg%; carotene 0.21 mg%. Mass fraction of alcohol 22.28.

Example 2

The vegetative part of wild garlic (12.5 kg) is crushed, the juice is removed, and then extracted with liquefied carbon dioxide in the same way as in Example 1. The carbon dioxide extract is obtained in the form of an oily liquid, yellow-green in color with dark shades, with a specific smell of wild garlic. The product yield is 2.94% by weight of absolutely dry raw materials. The main physical and chemical characteristics (at 20-22 ° C): density 827 kg / m ³ ; refractive index 1.3671; acid number 38.77 mg KOH / 1 g of feed; an ether number of 47.38 mg KOH / 1 g; saponification number 86.15 mg KOH / 1 g of raw material. Content: saponified substances 87.87%; unsaponifiable substances 8.946%; the sum of chlorophylls 60.82 mg%; carotene 3.21 mg%.

The dried solid residue of chopped wild garlic after carbon dioxide extraction is extracted in the same way as in example 1.

An alcoholic extract is obtained in the form of a green liquid with a specific smell of wild garlic.

The product yield is 22.36% by weight of absolutely dry raw materials. The main physical and chemical characteristics (at 20-22 ° C): density 873 kg / m ³ ; refractive index 1.3641; acid number 10.05 mg KOH / 1 g of feed; an ether number of 28.43 mg KOH / 1 g; saponification number 38.47 mg KOH / 1 g of raw material; the sum of chlorophylls 15.84 mg%; carotene 0.64 mg%. Mass fraction of alcohol 21.52.

Using the proposed method makes it possible to extract certain groups of chemical compounds from raw materials with solvents of different polarity. This property of liquefied gases allows introducing into the technological process a phase of selective extraction with a solvent capable of forming a given amount of extract, extracting individual chemicals, complexes, classes of compounds as needed, without affecting the amount of extractive substances remaining in the solid residue.

The use of organic solvents in the present method, which using modern equipment can be completely removed from the product in a short period of time, the possibility of solvent regeneration makes the present method cheap, simple and affordable for industry.

For the inventive method in the form as described in the independent paragraph of the claims, the possibility of its implementation using the means described in the application is confirmed.

Claims (1)

A method of obtaining a biologically active product from plant material by extraction with liquefied gas, characterized in that the raw material used is a pre-shredded or whole vegetative part of Allium victorialis, the extraction is carried out at a pressure of 5.8-6.0 MPa for 4-5 hours at a temperature 20-22 ° C to obtain the target product in the form of a carbon dioxide extract of wild garlic with an ether number of 47.38 or 86.96 mg KOH / 1g, an acid number of 27.83 or 38.77 mg KOH / 1g, the sum of chlorophylls 60.82 mg or 88.93 mg%, carotene 2.39 or 3.21 mg%, saponified substances 64.57 or 87.7%, neo soluble substances 8.946 or 27.46%.