RU2048815C1 - Method for production of sodium salts of triterpene acids - Google Patents

Abstract

FIELD: biotechnology. SUBSTANCE: method involves treatment of fir resin in terpentine with aqueous solution of sodium bicarbonate followed by spray drying. The former process is carried out at 40-90 C, the latter at 115-125 C. Initial content of resin is 10-30 Thus prepared powder product has 62-74 content of main compound, its humidity being 5-9 EFFECT: simplifies the method. 1 tbl

Description

 The invention relates to the production of natural biologically active substances from plant materials and can be used in the chemical, chemical, perfumery, cosmetic, pharmaceutical and other industries.

 Triterpene acids (TTC) are part of the acidic part of the resin of the conifers from Abies species and are stronger acids than diterpenic ones. Na-salts of triterpenic acids can be used, for example, for the manufacture of cosmetic products, drugs, etc. A fairly technologically advanced method of obtaining them from resin is unknown.

 A known method of separating a mixture of di- and triterpenic acids by extraction of coniferous waste with a solution of chloroform: ethanol in a ratio of 1: 1, followed by treatment of the extract with a 5% aqueous solution of sodium bicarbonate. In the preparation obtained by the indicated method, Na salts of both di- and triterpenic acids are present.

 Closest to the proposed is a method consisting in processing a solution of resin in diethyl ether with a saturated aqueous solution of sodium bicarbonate. This method is intended for preparative isolation of TTK from fir gum and cannot be used in industrial technological processes due to the need to use volatile fire and explosive diethyl ether as a solvent. In addition, the use in this method of a foreign solvent complicates the technological scheme, since an additional stage of its regeneration is required.

 The aim of the invention is to simplify the process of separation from fir gum Na salts of TTK in a convenient powder form.

 The proposed method is as follows.

Fir sap were dissolved in turpentine, the resultant solution with a mass fraction of oleoresin 10-30% purified in a known manner from mechanical impurities and then treated with aqueous sodium bicarbonate at 50-90 ° ^C. After settling the separated aqueous solution of Na-salts TTC dewatered in a spray dryer at a temperature of 115-125 ^about C. Get a powdery product with a mass fraction of Na salts of TTK 62-74% water 5-9%
The object is achieved in that, instead of diethyl ether (t _heated ^to 34.5 C) was used turpentine (t _boiled 156-170 ° ^C) and the oleoresin saponification process is carried out in 10-30% strength turpentine solution at a temperature of 50-90 ° ^C. The advantage of the proposed method compared to the prototype is that it eliminates the need for the use and subsequent regeneration of extraneous volatile fire hazardous solvent. Turpentine is part of the feedstock: its mass fraction in fir gum is 38-40%. In addition, taking into account the thermolability of the product and its tendency to secondary transformations, the drying process is used by spraying an aqueous solution under conditions excluding these processes at a temperature of 115-125 ^about S.

EXAMPLES EXAMPLE 1 100 kg of fir oleoresin dissolved in 100 kg of turpentine, was purified from mechanical admixtures and at ⁹⁰ ° C was treated with 170 kg of a 5% aqueous solution of sodium bicarbonate. After settling, the aqueous layer is separated, washed with pure turpentine and the residual turpentine is removed from the aqueous solution. Get 160 kg of an aqueous solution of Na salts of TTK with a mass fraction of the basic substance of 7.5%. The solution is dried in a spray dryer at a temperature of 115 ^about C. Receive 18.5 kg of a powdery product with a mass fraction of Na salts of TTK 64% humidity 7.5 %
The results of the method (examples 1-3) and control examples (4-8) are presented in the table.

When using a 5% turpentine gum resin solution for saponification (example 4), a large consumption of solvent is required, which is not economical, but with a 35% or higher solution (example 5), a stable emulsion forms and a poor separation of the aqueous and organic phases. When the saponification temperature below 50 ^{° C} (Example 6) is also poorly separated aqueous phase turpentine. When the drying temperature of the aqueous solution Na-salts TTC below 115 ^C. (Example 7) obtained strongly wetted product, at elevated temperatures (Example 8) occurring undesirable thermal transformation of the base material.

 The method is tested in laboratory and experimental conditions. An enlarged batch of the drug for testing in healthcare has been developed. The proposed method is simple to implement, for its implementation, existing equipment is used and the publication of special devices is not required. It can easily be carried out at any wood-chemical enterprise, where a comprehensive technology for processing fir resin is conducted. The processing technology of fir resin, including the obtained TTK sodium salts by the proposed method, has been laid down and is being implemented in the project for the re-profiling of Leskhimpharmia MP (Barnaul).

Claims (1)

METHOD FOR PRODUCING SODIUM SALTS OF TRITERPENIC ACIDS by treating fir resin in an organic solvent with an aqueous solution of sodium bicarbonate, characterized in that turpentine is used as an organic solvent, and the treatment is carried out when the resin is contained in turpentine solution 10 30% at 50 90 ^o С and the target product is dried by spraying in hot air at 115 125 ^o C.

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