Method of extraction of saponins

 

(57) Abstract:

The invention relates to an improved method of isolation and purification of saponins. Purification of saponins produced by nonionic macroporous sorbent Styroform 1-Midah that allows you to simplify the allocation process and get saponins with a high degree of purity in water-soluble form. The selection of saponins from the waste of sugar manufacture by reducing the concentration of these substances in the effluent 15-20 times.

The invention relates to methods for isolating saponins from sugar beet waste of sugar manufacture, and can be used in the pharmaceutical and cosmetic industries, as well as to reduce the receipt of saponins in the environment.

Known methods for isolating saponins from the rhizomes of sugar beet, sugar beet pulp and prettification sediment, which are based on multistage extraction in various solvents (Nagorno C. A., jijina R. T. , Kartashov, A. K. // Sugar industry. - 1966, 8. - S. 39-43; Patent 90934, RAF, 1985; Sasazuka Tabashi, Makoto Endo, Hiwatashi vacuum tube audio amplifying circuit Hiroshi // Seitogijutsi kenkyukaishi - Proc. Res.Soc.Jap. Sugar Refin. Technol. - 1995. - C. 57-62).

The closest analogue is the allocation method with the I Century A., Gigina R. T., Kartashov, A. K. // Sugar industry. - 1966, 8. - S. 39-43).

The method is based on the ability of saponins to dissolve in alkaline environments and alcohols and lose solubility in acidic aqueous solutions. From root saponins extracted by processing them with a solution of NaOH with a further presidenial upon acidification with hydrochloric acid. Subsequent cleaning is performed using a multi-stage extraction of saponins ethanol, alternating presidenial them in an acidic environment.

The disadvantages of this method are the duration and multi-stage (16 operations per cycle) process. Selected saponins are insoluble in water (H+form, to redefine them in an easy to use water-soluble form leads to further complication of the process.

The claimed invention allows to simplify the process for the isolation of saponins from the rhizomes of sugar beet and waste of sugar manufacture, to obtain a product with a high degree of purity in water-soluble form, to reduce the content of saponins in the effluent of sugar mills in 15-20 times.

The technical problem is solved by the fact that the allocation of saponins known manner (Nagorno C. A., jijina R. T., Kartashov, A. K. // industrial Sugar is by saponins transferred to water-soluble NH4+- form by treatment with ammonium hydroxide solution with a pH of 11.0 pass through the macroporous non-ionic adsorbent Styroform 1 - Midah a speed of 0.1 m/h with subsequent desorption of 96% ethanol and distillation of the latter with the final product.

The choice of a macroporous non-ionic adsorbent Styroform due to its high specificity to the saponins, contributing to the preferential sorption of these compounds from dilute aqueous solutions with a concentration of 2.0 mg/DM3.

The sorbent is a type of polystyrene nets, by their chemical nature similar to the copolymers of styrene and divinylbenzene, but with a radically different structure, and is called supersewn (C. A. Davankov, S. C. Rogozhin, M. P. Tsyurupa / Journal of structural chemistry. - 1973, I. 48, 12. - S. 2964-2967). Such polymers do not get the traditional methods of copolymerization of monomers and cross-linking chains of polystyrene in solution or in the swelled state, bifunctional compounds forming in the final grid bridges rigid structure (M. P. Tsyurupa. Supersewn polystyrene - new type of polymer nets. Abstract. dis....Prof. chem. Sciences. M., 1985. - 48 S.). As cross-linking agents used 4,4-bis-chloro-IU the I bridges the following structure:

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When the content of cross-linking bridges over 40% of the grid called the "supersewn" polymers. Supersewn sorbents have high kinetic characteristics and ease of regeneration and can be used for separation of biological fluids into components (M. P. Tsyurupa, V. A. Davankov, V. F. Selemenev, etc. //Applied biochemistry and Microbiology. - 1985. - so 21. - 1. - S. 7225-7274).

This sorbent was used for separation of nucleic acids, having in its composition glycoside and carboxyl groups (B. F. Selemenev, G. J. Oros, I. Rudenko, O. I. Stukalov, M. P. Tsyurupa, V. A. Davankov. A method of obtaining nucleic acid and amino acid from Baker's yeast autolysates, the application 93032352/13 (031326)).

Similar functional groups and are in saponins.

As confirmation of this method serves two examples associated with the separation of saponins from the rhizomes of sugar beet and from the wastewater of sugar production.

Example 1. 130 g of crushed roots of sugar beet, containing 0,33% saponins, insisted upon heating to 60oWith tenfold with respect to the mass of raw material volume (1,3 DM3) NaOH solution with pH=11.0 V for 1 hour, filtered poluchenii sediment contains saponins, was filtered through a glass filter, THEN 16 and washed directly on the filter model HC1 solution with pH=1.0 to completely remove sugar (sample-naphthol). Washed from sugar precipitate was dried at a temperature of 105oWith that mass was 3.5 g of saponins - 12%. Saponins were insoluble in water N+form.

The residue was treated with 280 cm3the ammonium hydroxide solution with a pH of 11.0, while saponins were converted into water-soluble NH4+form.

The resulting solution containing saponins ~ 1.5 g/DM3was passed through a column Packed with 10 g of sorbent Styroform 1-Midah in the swelled state. The amount of sorbent granules of 0.5-1.0 mm column Diameter 2.0 cm, height of layer 30,3 cm, bandwidth solution of 0.5 cm3/min.

Desorption of saponins with sorbent was carried out by passing 300 cm396% ethanol at a rate of 0.5 cm3/min.

After distillation of ethanol was obtained 0.32 g of saponins with a purity of 82%. The output of the composition of the raw material in terms of 100% saponin was 61%. The number of operations per cycle is 10.

Example 2. 5 DM3wastewater of sugar production (mixture of wastewater category III, containing 370 mg/DM3Sapo is the notes of the deposition saponins within 12 hours. The precipitate was filtered through a glass filter, THEN 16, and, without drying, was treated with 1,2 DM3the ammonium hydroxide solution with a pH of 10.0. The resulting solution containing ~ 1.5 g/DM3saponins was passed through a column containing 40 g of sorbent Styroform 1-Midah in the swelled state. The column diameter 3.0 cm, the layer height 53 cm, bandwidth solution of 0.5 cm3/min.

Desorption of saponins from the spent sorbent transmission 1,0 DM396% ethanol. After distillation of ethanol received 1.47 g of sediment, containing 87% saponins. The yield was 65% of the initial content in the runoff in terms of 100% saponin. The residual content of saponins in runoff decreased 17 times and amounted to 22 mg/DM3. The number of operations per cycle - 7.

Method of extraction of saponins from sugar beet waste of sugar manufacture by deposition upon acidification of the alkaline extract of the rhizomes, pulp press station or waste water, characterized in that the crude saponins transferred to water-soluble NH4+-form by treatment with ammonium hydroxide solution with a pH of 11.0, adsorb on macroporous non-ionic sorbent Styroform 1-Midah a speed of 0.1 m/h with subsequent desorption of 96% ethanol,

 

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