The method of obtaining sterols

 

(57) Abstract:

Usage: as an intermediate product in the synthesis of vitamin D2. The inventive product ergosterol and a mixture of sterols fungistasis. Reagent 1: Baker's yeast. Reagent 2: alcoholic alkali. Reagent 3: hydrochloric acid, which is added to the mother liquor after the separation from it of ergosterol to pH 6,0 - 7,5, after which the sterols isolated. table 1.

The invention relates to the production of sterols from yeast, in particular of ergosterol and related sterols from Baker's yeast.

Known methods of obtaining sterols from various microorganisms, in particular of ergosterol and its derivatives from yeast, representing waste citric acid, penicillin, sulfite liquor, beer brewing, bread baking (1-4). Methods of obtaining sterols based on the hydrolysis Pilipinas fractions of various yeast and extracting it with an organic solvent (such as petroleum ether, benzene and other) free ergosterol and separately or simultaneously derivatives of ergosterol (ethers) and other sterols present in the biomass, yeast, for example, ubiquinone-9.

The output of sterols and, in particular Albolote sterols, as well as the cheapest source of raw materials.

Known industrial method of obtaining sterols from Baker's yeast or mycelial penicillin, namely ergosterol (provitamin D) by acid hydrolysis of yeast and extraction of ergosterol raw ethyl alcohol, followed by double recrystallization raw alcohol-benzene solution to obtain pure ergosterol, which then receive vitamin D2(5).

The method involves complex processing of raw materials to produce ergosterol and protein residue as fodder product.

However, acid hydrolysis destroys proteins, but not the lipid fraction, which is extracted together with ergosterol and then partially deposited with him, reducing the quality of ergosterol raw. In addition, in the present conditions of labour protection because of the toxicity of benzene in production with it not working. While the mother liquor in the crystallization process of ergosterol from the first stage attaches to the ergosterol crude, and with the second crystallization is removed from the process. However, the process of recrystallization may not be continuous, since the mother liquor with time more and more enriched by other sterols, saponified lipids of calamaretti ergosterol.

The closest to this invention is a method of obtaining sterols from Baker's yeast by hydrolysis and extraction of the alcohol in the alkali with the release of ergosterol and separation of the mother liquor followed by crystallization from him sediment mixture of sterols and returning the alcohol to the process (6).

The method involves the separation of the mother liquor with a mixture of sterols containing hydrolysates of proteins, nucleic acids, sodium hydroxide and other impurities in the first stage of purification of ergosterol raw during crystallization of ergosterol from alcohol solution. While separated from ergosterol liquor is on the crystallization of sterols with the purpose of distillation of alcohol on recovery and return to the process.

However, fallen during crystallization to precipitate the sterols and impurities at the present time are a waste product and go for the emission, which reduces the overall yield of sterols present in the original yeast, and in particular of ergosterol. Together with ergosterol in the sediment remain the accompanying useful sterols, such as lanosterol, zimecterin and others representing independent interest as a mixture of sterols as a separate product.

The way pout in waste.

The objective of the invention is to provide a process of obtaining sterols, providing an increase in the yield of sterols from Baker's yeast, in particular of ergosterol in the amount of sterols as a separate finished product, i.e., the method providing, in one process simultaneously with the free ergosterol additionally useful product mixture of sterols.

The invention is directed to solution of the problem, ensuring the achievement of the mentioned technical result, as well as providing a positive effect, consisting in a complex and rational use of raw materials Baker's yeast, excluding the release of sterols in the waste, reducing waste total production.

The solution of the stated problem and obtaining the mentioned technical result is achieved due to the fact that the method of obtaining sterols by hydrolysis and extraction of the Baker's yeast alcohol alkali emitting ergosterol and separation of the mother liquor with subsequent crystallization of sterols and returning the alcohol in the process, what is new is the fact that before the crystallization mother liquor is neutralized with hydrochloric acid to a pH of 6.0-7.5 and produce sterols WPI is in the process of the first cleaning (affinely) alcohol to the crystalline state of ergosterol, provides subsequent crystallization from him sediment sterols, cleaned from impurities. This is ensured by the fact that the mother liquor coming from a pH of 10-12, neutralized with hydrochloric acid to pH 6,0-7,5 that allows you to select sterols in crystalline form.

As a result of neutralization of the cells in the specified conditions during the subsequent crystallization of the precipitate the sterols in normal conditions (20aboutC for 2 h) method allows to obtain a crystalline product containing a mixture of sterols: ergosterin 60-70% zimecterin 12-15% larosterna 10-14% and the rest of other sterols, represents an independent commercial product, conventionally named fumisterie. If necessary, a mixture of sterols (Foresteria) can be allocated free ergosterol in a known manner. Allocated as a separate product in the hydrolysis of Baker's yeast in the production of provitamin D ergosterol fungistasis can be used as a bioactive additive and emulsifier in cosmetic products. Thus, this method allows to increase the overall yield of sterols, including ergosterol in the mixture of other sterols and get this mixture of sterols as an independent copulae a white crystalline powder with a content of the mass fraction of sterols not less than 40% calculated on the dry substance.

The selection of a mixture of sterols (Foresteria) from Baker's yeast along with a free ergosterol in one technological process due to the described method and conditions of its carrying out was unknown.

The method is as follows.

In a reactor with a stirrer, termobahia and reflux condenser load under stirring pressed Baker's yeast (GOST 171-69) with the content of ergosterol 0,6-1,2% of dry substance, ethyl alcohol rectified and solid cheshireman sodium hydroxide. The mixture is heated to boiling (80-82aboutC), boiled for 6 h, after which the hot extract is filtered off on a suction filter. Sediment "protein waste removed. The filtrate is evaporated to the dry matter content of 34-37% (refractometrically), is cooled in the mold until 18-20aboutC and at this temperature, stirred for 6-10 hours the Precipitate of ergosterol raw filtered off on a suction filter, the mother liquor is oparka for the regeneration of the spirit. Ergosterol raw paste is subjected to a double-cleaning-affinati, i.e., boiled for 10 min with 15 and 20-fold volume 65aboutthe aqueous alcohol at 80aboutC and filtered. The filter remains ergosterol, which is dried at 60aboutWith and pass on photosynthesis of vitaminaboutC. the Yield is 1.7-1.9 kg per 1 t yeast, or 0,17-0,19%

The mother liquor with a pH of 10-12, obtained in the separation of ergosterol in the process of its dual clean (affinely) containing sterols yeast, sodium hydroxide, hydrolysates of proteins and nucleic acids, neutralized with stirring, diluted hydrochloric acid (in a ratio of conc. HCl water 1 2 to a pH of 6.0 to 7.5 (potentiometric), cooled to 18-20aboutC and at this temperature crystallized for 2 hours, after which the precipitate is filtered off on a suction filter and washed with 65% alcohol or water, then dried in a vacuum dryer until the volatile content of not more than 5% Receive a white crystalline powder containing not less than 40% of sterols, besieged by digitonin, i.e., 3--a hydroxyl group in the molecule.

Technology method of obtaining sterols confirmed by specific examples.

P R I m e R 1. In a reactor with a capacity of 2 m3with a stirrer, termobahia and reflux condenser load with stirring 600 kg of compressed yeast species Laccharomyces serevisiae humidity 72-75% with the content of ergosterol 0,6-1,2% on S. century 975 litres of rectified spirit and 100 kg cashflowing sodium hydroxide. The mixture is heated to boiling 80-82aboutC, boiling 6 h, after which the hot extract Phil is etnicheskie), cool in the mould up to 18-20aboutC and at this temperature, stirred for 8 hours the Precipitate of ergosterol raw 4.2kg filtered on a suction filter, the mother liquor is passed to oparka for the regeneration of the spirit.

Ergosterol raw paste is subjected to 2-fold purification-affinati, i.e., boiled for 10 minutes first 15, then 20-fold volume of 65% aqueous alcohol and filtered. The filter remains ergosterol, and the mother liquor with sterols with the first and second stages of purification unite and separate. The resulting gasteren dried at 60aboutWith and send to the photosynthesis of vitamin D2. Affilirovanny ergosterol contains 85% of the basic substance (S. C.), up to 3% moisture. So pl. 157-160aboutC. the Yield amounts to 75-80% of the content in yeast, 1.75-1,82 kg of 1 t yeast, or 0.17% of the mass of the initial yeast.

The mother liquor with a pH of 10-12 in number 500-600 l containing caustic potash, sterols and yeast hydrolysates of proteins and nucleic acids (in the amount of 1.5-2.0 kg in terms of 1 t of the original yeast) is neutralized by stirring 4-6 l of diluted hydrochloric acid (1:2) to a pH of 6.8 (potentiometric), cooled to 20aboutC and at this temperature crystallized for 2 hours, after which the precipitate is filtered on a suction filter and washed with 100 l 65aboutthe aqueous alcohol, shesterin, containing 56.4% of sterols, besieged by digitonin (i.e., the 3-hydroxyl group in the molecule). The output of sterols 0,053% of the yeast.

The quality of the product meets THE 64-0431-5.01-91. The total yield of sterols amounted to 0.23% by weight of yeast.

The data presented in the table.

P R I m e R s 2-5. Similarly, the test method of obtaining sterols by neutralizing the mother liquor with different pH.

The results highlight Foresteria of Baker's yeast are presented in the table.

The METHOD of OBTAINING STEROLS by hydrolysis and extraction of the Baker's yeast alcohol alkali emitting ergosterol and separation of the mother liquor with subsequent crystallization of sterols and returning the alcohol in the process, characterized in that before the crystallization mother liquor is neutralized with hydrochloric acid to pH 6,0 - 7,5, after which the Sterol isolated.

 

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