RU2530656C1 - Method of processing wood green of fir to produce chlorophyll-carotin paste, fir oil and aqueous extract of fir - Google Patents

Abstract

FIELD: biotechnology.

SUBSTANCE: method of processing wood green of fir to obtain fir oil, chlorophyll-carotene paste, aqueous extract of fir, comprising the sequential extraction of wood green with aqueous isopropanol, extraction with water, concentration of the isopropanol extract, hydro-distillation of the volatile components from the concentrate of the isopropanol extract to obtain fir oil, washing with water of hot bottom products for extraction of hydrophilic components and their separation from the lipophilic part, combining of hydrophilic components with an aqueous extract of wood green and concentration in vacuum to obtain the total aqueous fir extract, saponification of lipophilic part with aqueous solution of sodium hydroxide to obtain chlorophyll-carotene paste, under certain conditions.

EFFECT: method enables to extract efficiently fir oil, chlorophyll-carotene paste, aqueous fir extract of wood green of fir.

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Description

The invention relates to the integrated processing of plant materials in the chemical industry and the production of biologically active substances for medicine, cosmetology, agriculture.

The woody greens of Siberian fir contain a large amount of essential oil (2-5%, the content of bornyl acetate in oil is up to 40%). To obtain fir oil, hydrodistillation is used [Kolesnikova RI Essential oils of coniferous plants in Russia. Abstract of diss. Doctors biol. Sciences, Vladivostok, 1998, 58 S.]. After removal of the volatile components, the fir foot contains a large number of valuable extractive components: triterpene and diterpene fatty acids, sterols, diterpene alcohols, chlorophyll derivatives, which can be used to produce chlorophyll-carotene paste. Chlorophyll-carotene paste is used to treat burns, boils, as an additive to hygiene products, as a feed additive for agricultural animals. It is advisable to comprehensively process woody greens to produce a number of products, including fir oil and chlorophyll-carotene paste, as well as an aqueous (hydrophilic) extract, which is used as a biologically active additive in farm animal feed.

A known method of producing products from coniferous woody greens [RU 2041646], including grinding the feedstock and extraction, characterized in that the extraction is carried out with a liquid propane-butane mixture at 20-26 ° C and a pressure of 1.0-0.8 MPa for 3-5 hours, and then the propane-butane extract is re-extracted with 50-60% ethanol at 40-80 ° C for 3-5 hours, after which the mixture is filtered, cooled, left to separate into two layers and each layer is evaporated separately to obtain a coniferous extract and chlorophyll-carotene paste.

The disadvantage of this method is that in the process do not receive fir oil. Volatile components are extracted with a propane-butane mixture together with other non-volatile lipophilic substances and are not separated from the latter. The disadvantage of this method is the extraction of a part of lipophilic substances, in particular carotenoids and chlorophyll derivatives, which do not get into the water-alcohol extract, which affects the yield and quality of the chlorophyll-carotene paste obtained by this method, together with the essential oil with a propane-butane mixture. The disadvantage is the use of a polar extractant of 55% alcohol, which extracts polar fir metabolites relatively well and weakly extracts valuable components for chlorophyll-carotene paste, which also leads to a decrease in the content of chlorophyll derivatives in chlorophyll-carotene paste with an increased content of polar extractives.

A known method of producing products from woody fir green [RU 1375226], in which essential oils are distilled from ground woody fir firs (get fir oil), after which the rest of woody greenery is poured with a 55-65% solution of isopropyl alcohol and the mixture is infused with 30-60 ° C for 8-24 hours. Then the mixture is filtered, the extract is cooled and defended, the upper layer is separated from the lower one and each is evaporated separately. An aqueous coniferous extract is obtained from the upper layer, the lower is used to produce chlorophyll-carotene paste. This method is a prototype of the claimed invention.

The disadvantages of the prototype method are as follows:

- Steam treatment of fir green wood with steam (100 ° C or higher) to separate essential substances (extract of fir oil), which leads to partial saponification of bornyl acetate and a decrease in the quality of the obtained fir oil, destruction of labile lipophilic components extracted by isopropanol, and a decrease in the quality of extractives, in particular, a decrease in the chlorophyll content in the chlorophyll-carotene paste.

- Using a polar extractant of 65% isopropanol, which extracts polar fir metabolites well and weakly extracts valuable components for chlorophyll-carotene paste, in particular chlorophyll derivatives. In this regard, the chlorophyll-carotene paste is enriched with hydrophilic compounds involved in the extraction from wet needles with an irrigated solvent and not removed during separation of the lipophilic and hydrophilic layers, which leads to a decrease in the paste, in particular, the content of chlorophyll derivatives.

An object of the present invention is to provide a process for processing woody green fir to produce improved quality chlorophyll-carotene paste (high in chlorophyll), total hydrophilic coniferous extract, and fir oil with a high content of bornyl acetate.

The problem is solved by a method in which chopped fresh wood fir green is extracted with aqueous isopropanol (80-90%), the extract is concentrated at atmospheric pressure and a temperature of 80 ° C. Water was added to the concentrate and fir oil was distilled off by hydrodistillation in a vacuum ring-pump. Wash the hot bottoms with hot water, removing water-soluble impurities that reduce the quality of the chlorophyll-carotene paste, and separate part of the aqueous extract.

The washed lipophilic extract is treated at 60-65 ° C with an aqueous NaOH solution to pH-8.0-9.0, and a chlorophyll-carotene paste with a moisture content of not higher than 40% is obtained. Fir wood greens after isopropanol extraction is extracted with hot water. Combine the aqueous extract of green wood fir with water washing the isopropanol extract and concentrate it in vacuo (0.5-0.1 bar) at 60-80 ° C to obtain the total aqueous fir extract.

The proposed method has the following advantages.

The use of 80-90% aqueous isopropanol makes it possible to more efficiently extract lipophilic components from a fir foot relative to hydrophilic components compared to the use of less concentrated 65% isopropanol according to the prototype method, which allows to obtain improved quality chlorophyll-carotene paste, in particular with a higher content of derivatives chlorophyll.

Steam distillation of the essential oil from the extract is carried out under mild conditions (low temperature, vacuum), which allows you to save the labile components of the chlorophyll-carotene paste (chlorophyll derivatives), as well as to maintain a high content of bornyl acetate in the distilled oil, while the prototype method sharp steam is used to treat green wood, which partially hydrolyzes boronyl acetate and reduces the chlorophyll content in the chlorophyll-carotene paste.

The distillation of fir oil from the extract is combined with water washing of the lipophilic part from water-soluble impurities, which allows you to effectively remove unwanted impurities of sugars and oligosaccharides from chlorophyll-carotene paste. Water extraction of green wood, carried out after isopropanol extraction, allows you to extract additional hydrophilic extractives (sugars and oligosaccharides) compared with the prototype method.

Example 1

Obtaining chlorophyll-carotene paste according to the conditions of the prototype method. Under the conditions of the prototype method, 2 kg of milled woody green fir is treated with steam and the essential oil is distilled off, after which the residue is extracted with 65% aqueous isopropanol (hydromodule 6, T = 30 ° C), the extract is filtered, settled and the lower organic layer is separated, which is concentrated. A hydrophilic fir extract is obtained from the top layer. To the residue, the sum of lipophilic substances, add 15 ml of 30% NaOH and heat to 60-65 ° C with stirring for 30 minutes, then add water (100 ml). Chlorophyll-carotene paste is obtained, yield 298 g (humidity 40% wt.) pH = 8.7. In the resulting chlorophyll-carotene paste from the extract isolated by the prototype method, the chlorophyll content is 800 mg / 100 g, the wax content is not more than 1%, volatile substances less than 1%. The content of bornyl acetate in essential oil is 27%.

Example 2

Fir wood green (80 kg) is poured with 85% isopropyl alcohol solution (hydromodule is 4) and infused at 40-50 ° C for 4 hours. The extract is filtered, drained, the extraction is repeated one more time. The combined extract is concentrated by heating under reduced pressure of 0.3-0.5 bar (using a vacuum ring pump). Water (100 L) is added to 100 kg of the concentrate (combined extract from several extraction operations) and the essential oil is distilled off with water with stirring (t = 60-80 ° C, P = 0.5-0.1 bar). The upper layer containing the aqueous extract is decanted to obtain an aqueous solution of hydrophilic substances. To the residue (bottom layer - the sum of lipophilic substances) add sodium hydroxide solution (10 l of a 30% NaOH solution) and heat to 60-65 ° C with stirring for 1 h, and a chlorophyll-carotene paste is obtained (moisture content 40%, pH = 8.7). In the resulting chlorophyll-carotene paste (humidity 40% by weight), the chlorophyll content is 1200 mg / 100 g, wax is not more than 3%, and the mass fraction of volatile substances is not more than 1%. The content of boron acetate in distilled essential oil is 34%. After draining the isopropanol extract, water (300 L) is added to the extracted green wood of fir and extracted at 70-80 ° C. The aqueous extract is drained, combined with the hydrophilic extract obtained by washing the lipophilic substances, and concentrated in vacuo (0.5-0.1 bar) at 60-80 ° C, a total aqueous fir extract is obtained (solids content of at least 20%, the mass fraction of hydrolyzable sugars in terms of sucrose is not less than 5%, the mass fraction of oligosaccharides is not less than 10%). The yield data and characteristics of products from green wood fir are presented in the table.

Thus, the inventive method of processing woody green fir to produce chlorophyll-carotene paste, fir oil and an aqueous extract using distillation of fir oil from the extract under mild conditions, allows to obtain fir oil with a higher content of bornyl acetate, as well as chlorophyll-carotene paste with more high chlorophyll content compared to the prototype method. The use of water extraction of green woody fir after isopropanol extraction allows to increase the yield of hydrophilic extract used for animal feed.

Table Product Yields,% weight. per fir green wood, indicators According to example 1 (prototype) According to example 2 Fir oil Yield 2.8%, bornyl acetate content - 25% Yield 2.6%, content of bornyl acetate - 34% Chlorophyll-Carotene Paste Moisture Content 40% Yield 15%, chlorophyll content - 800 mg / 100 g Yield 14%, chlorophyll content - 1200 mg / 100 g Hydrophilic fir extract (in terms of dry matter) Yield 19% Yield 22%

Claims (1)

A method of processing wood green fir to produce fir oil, chlorophyll carotene paste, aqueous fir extract, comprising sequential extraction of wood green with 80-90% aqueous isopropanol at 40 ° -50 ° C, water extraction at 70-80 ° C, isopropanol extract concentration hydrodistillation of volatile components from an isopropanol extract concentrate under reduced pressure of 0.5-0.1 bar at 60-80 ° C to obtain fir oil; washing with water of a hot bottoms to extract hydrophilic components and their dividing from the lipophilic part, combining the hydrophilic components with an aqueous extract of green wood and concentrating in vacuum 0.5-0.1 bar at 60-80 ° C to obtain the total aqueous fir extract, saponification of the lipophilic part with an aqueous solution of caustic soda to pH-8, 0-9.0 at 60-65 ° C to obtain chlorophyll-carotene paste.