SU595320A1 - Method of extracting esculetin from vegetable raw material - Google Patents

Description

one

This invention relates to an improved method for separating a hydroxycoumarin derivative esculetin from plant raw materials.

Oxycoumarins are of great importance for medicine, on the basis of oxycoumarins and their derivatives, a number of effective drugs have been created for the treatment of various diseases (Eskuzan, Digofton, Flavoliofil-S, etc.).

Many oxycoumarins are used in other areas, such as photography.

However, the methods for isolating them from plant materials are very complicated and do not make it possible to completely get rid of the related substances (phenol carbonic and organic acids, flavonoids and their derivatives).

A known method for the isolation of oxycumarium from plant raw material, according to which the raw material is extracted with aqueous alcohol (50+ ± 5 ° C), the extract is concentrated to 1 / 36-1388 of the initial volume, then treated with a mixture of n-butiol-chloroform (2: 3), organic the phase is evaporated, the residue is dissolved in aqueous alcohol, the solution is treated with carbon tetrachloride and crystallized 1.

However, when isolating esculetin in this way, the resulting preparation contains in

other oxycoumarins are: impurities: fraxin, scopoletin, and umbelliferon, and cannot be used as a standard for the determination of esculetin in plant raw materials and esculetin preparations produced by industry.

In order to increase the purity of the target product, a method is proposed for isolating esculetin from vegetable raw materials, in which vegetable raw materials are extracted with aqueous ethanol, the extract is concentrated to 1 / 36-1 / 38 of the initial volume, the concentrate is treated with n-butanol-chloroform (2: 3), the organic phase is evaporated and the precipitate is additionally dissolved in water at 40-60 ° C, chromatographed on a polyamide sorbent, eluted with water, chromatographed and re-eluted with aqueous ethanol. Preferably use 20-25%

aqueous ethanol.

Example. 1 kg of chicory grass (Cichorium intybus L.) crushed on rollers is loaded into a percolator and extracted with stirring 3 times over

Claims (2)

45 min., Bay every time about 12 l of 50% ethanol. The extracts are combined, evaporated to 1 l and treated 6 times by 2 l with n-butanol-chloroform (2: 3), the organic phase is separated, evaporated under vacuum, and the resulting resin is dissolved at 40-60 ° C in 250 ml water and applied to a chromatographic column filled with polyamide sorbent powder (d 5 cm / g 50 cm). Distilled water is used as an eluting solvent, taking 250 ml fractions. The separation of the mixture of oxycoumarins on the column is observed in filtered UV light (L 360 nm). Fractions 1 - 15 contain esculin, dikhorin, scopoletin, umbelliferon. Fractions 16-26, containing esculetin as the main component, are concentrated in vacuo to a dry residue, which is dissolved in a small amount (100-150 ml) of 20% ethanol and re-chromatographed on a polyamide sorbent column (d 5 cm, / i 30 cm). 20-25% ethanol is used as an eluting solvent, and 200 ml fractions are selected. Fractions 4-15 containing chromatographic pure esculetin are evaporated in vacuo to dryness and crystallized from 30-35% ethanol. Eculetine yield 1 g (75-80% content in raw materials). The composition of the product after elution is known after elution with a 20-25% ethanol method or with water. Separated esculin. Obtained by the proposed method, esculetin is devoid of all impurities of oxycoumarins present in it when isolated by a known method, and can be used as a standard. To control the quality of esculetin samples obtained by the proposed and known methods, paper chromatography and TLC analysis was performed. The results are shown in the table. The proposed method allows to obtain esculetin of improved quality, which can serve as a standard in determining it in raw materials and in esculetin-containing preparations. Claims 1. A method for separating esculetin from plant material by extraction with aqueous ethanol, concentrating the extract to 1 / 36-138 parts of the initial volume, followed by treatment with n-butanol-chloroform and evaporating the organic phase, characterized in that in order to increase the purity after evaporation of the organic phase, the residue is dissolved in water at 40-60 ° C, chromatographed on a polyamide sorbent, eluted with water, chromatographed and re-eluted with aqueous ethanol, followed by evaporation equalizer. 2. A method according to claim 1, characterized in that aqueous ethanol is used with an alcohol content of 20-25%. Sources of information taken into account in the examination 1. Application No. 2198409, cl. From 07D 311/08, 09/29/75, which made the decision to issue an author's certificate.