Method for preparing saponin from beet pulp
SUBSTANCE: invention relates to methods for isolation and purification of triterpene glucosides from vegetable raw, in particular, saponins from beet and waste in sugar manufacturing, in particular, from beet pulp. Method involves alkaline extraction of raw at temperature 80°C for 8 h followed by settling. Granulated anion-exchange resin AV-17-2P in OH-form is used as a sorbent, and desorption process of sorbent is carried out with 70% ethanol. Invention can be used in food, pharmaceutical and cosmetic industry.
EFFECT: improved preparing method.
2 cl, 1 ex
The invention relates to methods of isolation and purification triterpene glucosides from plant material, in particular saponins from sugar beet and waste of sugar manufacture, and can be applied in food, pharmaceutical and cosmetic industries.
A known method of extraction of saponin from sugar beet waste of sugar manufacture (Japan's bid No. 63-93794, About Takahiro, Tanaka, Teruo "extraction and purification of sugar beet saponin, publ. 25.04.88), according to which the crushed feedstock is treated successively with water when heated to 60°C for 30 min (in the case of pulp) with a solution of an alkaline reagent for 1-2 hours at room temperature, the alkaline extract is separated and saponin adsorb on the polymer sorbent, such as hydrophobic macrosector copolymer of styrene and divinylbenzene brands "Amberlite HAAD or Dayan". From sorbent saponin is desorbed with methanol, which is then removed from the eluate. This method requires a sufficiently large consumption of reagents, including toxic (methanol), long and multistage obtained target product characterized by a low content of saponin, which entails the need to develop additional technological schemes of treatment.
In the method proposed in the patent of Russian Federation №2069665, 07 N 1/08, along with Viseu asanami operations to reduce consumption of reagents and removal from the alkaline extract of organic substances, significantly reduces the sorption of saponin, the alkaline extract is further treated non-polar organic solvents, mix, defend and further carry out the selection of saponin from a portion of the eluate enriched by him. The resulting product contains 21-26% saponin, which will also require further purification before use. This method is even more time consuming and requires the development of recycling schemes used nonpolar solvents.
The objective of the invention is to simplify the process by reducing the number of its stages, and obtaining the target product of the beet with a significantly higher content of saponin.
The problem is solved in that in the known method of producing saponin from beet pulp, including the processing of raw materials with an alkaline reagent with stirring, settling and separation of the solid phase, sorption of saponin adsorbent, desorption of polar solvent and isolation of saponin obtained from the eluate, according to the invention the treatment with an alkaline reagent is carried out at a temperature of 80°C for 2 hours followed by 8-hour sedimentation, as a sorbent use granular anion exchange resin AV-17-2P in the form, and desorption from the sorbent are passing 70% ethanol.
It is established that the conduct of alkaline extraction with increasing temperature up to 80°With the over 2 hours of stirring followed by 8-time defending allows not only to improve the content of saponin in the filtrate, but to separate the greater part of the ballast substances, without applying additional processing of the non-polar organic solvent, and thus remove the problem of its subsequent disposal. The use of macroporous anion exchanger AV-17-2S in a granular condition allows to increase the bandwidth of a solution of saponin and reagent to reduce the consumption of sorbent due to its higher capacitive characteristics. The use of 70% ethanol instead of 96% can reduce its costs.
1000 g of beet pulp, containing 0.2% saponin, insisted when heated to 80°from 1.0 DM3NaOH solution with a pH of 11.0 (ratio of the volume of extractant : the mass of pulp = 1:1) for 2 hours, advocated for 8 hours and filtered through a fabric filter. The obtained filtrate volume of 0.9 DM3containing 1.5 g/DM3saponins in Na+form was passed through a column of anion exchange resin AV-17-2P in the HE-form (grain size 0.5-1.0 mm). The diameter of the column - 2.0 cm, the layer height is 25 cm, the transmission rate of the solution is 1.0 cm3/min
Desorption of saponin with sorbent was carried out by passing 400 cm370%ethanol at a speed of 1.0 cm3/min
After distillation of the ethanol obtained 1.7 g of saponins with a net 80%. The output of saponins from the pulp (in recalculation on 100%saponin) was 68%. The residual content of saponins in the pulp is reduced 5 times which is 0.04% (0.4 g/kg). The number of operations per cycle - 5.
A method of obtaining a saponin from beet pulp, including the processing of raw materials with an alkaline reagent with stirring, settling and separation of the solid phase, sorption of saponin adsorbent, desorption of polar solvent and isolation of saponin obtained from the eluate, wherein the treatment with an alkaline reagent is carried out at a temperature of 80°C for 2 h followed by 8-hour sedimentation, as a sorbent use granular anion exchange resin AV-17-2P in the form, and desorption from the sorbent are passing 70% ethanol.
< / BR>where X = H, NH4showing immunostimulirutuyu activity
FIELD: organic chemistry, chemical technology, pharmacy.
SUBSTANCE: invention describes the improved method for preparing flumetasone (6α,9α-difluoro-11β,17α,21-trihydroxy-16α-methylpregna-1,4-diene-3,20-dione), flumetazone 21-acetate or its 17-carboxyl-androstene analogue of the formula (I) . Method involves interaction of benzoyl chloride with compound of the formula (II) in pyridine medium of its mixture with N,N'-dimethylacetamide to prepare 3-enol ester of the formula (IIIa) and it's the following interaction with 1-(chloromethyl)-4-fluoro-1,4-diazonium-bicyclo[2.2.2]octane-bis(tetrafluoroborate) in acetonitrile medium and water to prepare compound of the formula (IIIb) and the following removing the protective group in compound of the formula (IIIb) at the position C3 in medium of aqueous metabisulfite and ammonia to prepare compound of the formula (IV) . After the fluorination reaction of 9,11-epoxy group in compound of the formula (IV) using HF flumetasone 21-acetate is prepared followed by the selective hydrolysis with KOH in methanol (CH3OH) medium in the presence or absence of H2O2 to prepare compound of the formula (I) or flumetasone, respectively.
EFFECT: improved preparing method.
3 cl, 5 ex
FIELD: organic chemistry, steroids, pharmacy.
SUBSTANCE: invention relates to a new type of selective estrogens comprising steroid structure of the general formula (I) with nonaromatic ring A and free of bound hydroxyl group at carbon atom 3 wherein R1 means hydrogen atom (H), (C1-C3)-alkyl or (C2-C3)-acyl; R2 means hydrogen atom (H), α-(C1-C4)-alkyl, α-(C2-C4)-alkenyl or α-(C2-C4)-alkynyl; R3 means hydrogen atom (H) or (C1-C4)-alkyl at position 16 of steroid structure; R4 means ethynyl; R5 means hydrogen atom (H), (C1-C3)-alkyl or (C2-C3)-acyl; R6 means (C1-C5)-alkyl, (C2-C5)-alkenyl, (C2-C5)-alkynyl being each of that is substituted optionally with chlorine or fluorine atom; dotted line means the optional double bond. Compounds of the formula (I) elicit the selective affinity to ERα-receptors.
EFFECT: valuable properties of compounds and composition.
4 cl, 3 sch, 1 tbl, 8 ex
R1- (R2R3N(O)r)-, where r=0, 1, each of R2and R3independently - H, C1-6alkyl; or R1-
where q=0, - 1, Y-(CH2)m-, where m=1, 2, 3, 4, 5; or
R1- C1-6alkyl-CO-; R12Is n; X Is O or
where -(CH2)m-, where m=2; R6=H; R7=H, C1-6alkyl, C2-6alkenyl,2-6quinil, perhaps HE or substituted BASED; S=0, 1; each of the8and R9independently - H, HE, C1-6alkyl, R10CO., where R10’- H, C1-6alkyl