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

 

(57) Abstract:

The invention relates to a method of extraction of biologically active compounds from plant material. From freshly picked leaves of plants of the genus Serratula squeeze out juice, filtered and the filtrate concentrated. To the obtained concentrate is added ethyl acetate, stirred, separating the extract, it evaporated, cooled and filtered the precipitated crystals of ecdysterone. The invention improves the efficiency of the process, to increase output, 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 next sequential liquid-phase extraction, purification of the obtained product column adsorption chromatography oxide Aluminijuma ethanol in the first stage of extraction, large amounts 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 spend methanol with simultaneous evaporation in the extractor vacuum-circulating installation and subsequent removal of related Vesselina. 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 target product. Then the final product is extracted from the sorbent with an organic solvent. The disadvantage of this method is th, 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 regeneriratia), 8 l of a mixture (1:1) ethyl acetate-ethanol, 200 g of activated charcoal.

The aim of the invention is to simplify the way 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 the lack of primary extraction of the target product from plant material using organic solvents or water. Instead of extraction applied squeezing juice with subsequent filtering, that 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 way in which and takes only thirty minutes. This allows you to apply this method to large-scale production.

The method is as follows.

From the aerial parts of plants of the genus Serratula day collection or next day pressed juice (use a juicer, press or other devices), which is filtered, and the filtrate (transparent yellow) concentrate to 0.5 of the original volume by evaporation, freezing water with separation of ice or other techniques. From the obtained concentrate the target product is extracted with ethyl acetate, the extract evaporated (at a temperature of 40-65oC) up to 0.25 of the original volume of the extract is cooled, and the precipitated crystals of ecdysone filtered.

Examples of the method.

Example 1. 3 kg above-ground parts of plants of the genus Serratula on the day of collection squeeze out juice. Received 1.5 l juice is filtered and the resulting clear yellow filtrate is concentrated to 0.7 liters Of concentrate target product is extracted with ethyl acetate (1 l 3), the extracts combined evaporated ethyl acetate, 250 ml, cooled and filtered the precipitated crystals of ecdysone. Yield 4.5 g, which is 0.15% of the wet leaves, or 1.17%, calculated on the air-dried leaves (3 kg fresh tula coronata on the day of collection squeeze out the juice with a volume of 1.5 l, which is filtered and the resulting clear yellow filtrate is concentrated to 0.7 l partial freezing and separation of the formed ice. Concentrate the target product is extracted with ethyl acetate (1 l 3), the extracts combined evaporated ethyl acetate, 250 ml, cooled and (filtered the precipitated crystals of ecdysone. The yield of 4.03 g, which is 0.13% of wet leaves, or 1.15%, calculated on the air dried leaves.

A method of obtaining a concentrate of ecdysone and ecdysone from vegetable raw materials, including extraction with an organic solvent, characterized in that is used as raw material juice, squeezed from freshly harvested leaves of plants of the genus Serratula, which is filtered, concentrated and the concentrate is 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.

 

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