A method of obtaining a concentrate of ecdysone and ecdysone from vegetable raw materials

 

(57) Abstract:

The invention relates to medicine and agriculture, in particular to a method of extraction of biologically active compounds from plant material. From freshly harvested leaves of plants of the genus Serratula squeeze out the juice, and then extracted with water, the resulting juice and aqueous extract of unite, filtered, concentrated and extracted with ethyl acetate, the obtained extract was partially evaporated the solvent, the concentrated extract is cooled and filtered off the precipitated crystals of ecdysone. The invention allows to simplify the way to increase output, increase productivity and reduce reagent consumption and energy costs.

The invention relates to a method of extraction of biologically active compounds from plant material, in particular emphases of phytoecdysteroids, namely ecdysone (-ecdysone). Ecdysterone is the insect molting hormone, used in medicine and agriculture.

A method of obtaining ecdysteroids from plants of the genus Rhaponticum [the Patent of Russian Federation N 2063763, A 61 K 35/78, 1996], which consists in extracting raw materials 70% ethanol, remove from the primary extract related substances is ecografia aluminum oxide and its subsequent crystallization. The disadvantages of this method are the use of large amounts of ethanol in the first stage of extraction of large volumes of organic solvents in subsequent multiple liquid-liquid extraction, multi-stage and duration of the process.

Known also three ways to obtain the ecdysone from plants of the genus Serratula. According to one of them [Kholodova Y. D., Baltaev U., Volovenko C. O. and other Phytoecdysteroids Serratula xerathomoides. - "Chemistry of natural compounds", 1979, S. 171.] the secretion of ecdysone from inflorescences Serratula xerathomoides produced by crushing the air-dried leaves with subsequent extraction of them with methanol. The obtained extract was evaporated, diluted with water and repeatedly extracted with hexane, conduct additional distillation of methanol, extraction with butanol, its evaporation, elution with a mixture of chloroform-methanol on a column of alumina. The disadvantage of this method is the low output of ecdysone (0.26% of air-dry weight of raw materials), as well as the multistage and the long duration of the process (ten operations 115 hours).

According to another method [USSR Author's certificate N 1146050, A 61 K 35/78, 1985], the primary extraction of raw materials is carried out with methanol ODN substances liquid extraction and purification of the product liquid-adsorption column chromatography on aluminium oxide. The method includes nine consecutive operations: three extraction, three residues, one filtering operation, one operation of dissolution and column adsorption chromatography. Time, the method 66 - 70 hours. The disadvantages of this method are the use of operations liquid-liquid extraction, which require multiple repetition and at least three times the volume of the extractant to extractable volume for each extraction surgery, duration, complexity and multi-stage process, as well as high energy way as a result of three operations residue and the length of time vacuum-circulating installation.

According to the way [the Patent of Russian Federation N 2063763, A 61 K 35/78, 1996] , to obtain the ecdysone aerial parts of plants of the genus Serratula crushed and extracted with water at a temperature not exceeding 100oC for 1 hour. The extract obtained is passed through a layer of solid hydrophobic sorbent, such as activated carbon, diasorb, Polisorb, while concurrently the Department related substances and purification of the final product. Then the final product is extracted from the sorbent with an organic solvent. The disadvantage of this way is her as well as distilled water. In a typical example of the description of the invention to obtain 1 g of ecdysone consumes 8 liters of distilled water, 4 l of 20% ethanol (which is not regenerated), 8 l of a mixture (1:1) ethyl acetate-ethanol, 200 g of activated charcoal.

The task of the invention is to simplify the method with a simultaneous increase in product yield, increased productivity, and reduced specific consumption of organic solvents and energy consumption.

A distinctive feature of the proposed method, which allows to solve tasks, is squeezing juice followed by extraction with water, which allows to get the concentrate amounts of ecdysteroids. This technique greatly simplifies the process for the isolation of ecdysteroids. Eliminates the long process of drying plant materials. This greatly simplifies the way, increases the release of ecdysone, increases the efficiency of the process, reduces energy consumption, reduces the consumption of organic solvents and the complexity of the method and, consequently, significantly reduces the whole process. The process from point of collection to final product takes only thirty minutes.

Examples of the method.

Example 1. 3 kg above-ground parts of plants of the genus Serratula coronata and on the day of collection squeezed juice (1.5 l). From the residue is extracted with 1.5 liters of water at a temperature of 45-100oC for 15 minutes. Squeezed juice and the resulting aqueous extract, combine, filtered and the resulting filtrate (transparent yellow) concentrate to 1 l of partial freezing and separation of the formed ice. From the thus obtained concentrate is extracted with ethyl acetate (1.5 l 3), the extracts combined evaporated ethyl acetate, 200 ml, cooled and filtered the precipitated crystals of ecdysone. The product yield 4.68 g, which is 0.16% of the wet leaves, or 1.3% in terms of air dried leaves (3 kg of fresh leaves after drying the obtained 0.350 kg of dry leaves).

Example 2. 3 kg above-ground parts of plants of the genus Serratula coronata on the day of collection squeezed juice (1.5 l). From the residue extracted (1.5 is altroot and the obtained filtrate (transparent yellow) concentrate to 1 l by the process of evaporation of water on a rotary evaporator. The combined concentrate is extracted with ethyl acetate (1.5 l 3), the extracts combined evaporated ethyl acetate, 200 ml, cooled and filtered the precipitated crystals of ecdysone. The yield of 5.19 g, which is 0.17% of the wet leaves, or 1.5% in terms of air dried leaves.

A method of obtaining a concentrate of ecdysone and ecdysone from vegetable raw materials, including extraction solvent, wherein from freshly harvested leaves of plants of the genus Serratula squeeze out the juice, the residue after extraction of the juice is extracted with water, squeezed juice and the resulting aqueous extract, combine, filtered, concentrated and extracted with silaceata, the obtained extract was concentrated, the concentrate is cooled and filtered off the precipitated crystals of ecdysone.

 

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