The allocation method betulinol

 

The invention relates to methods of isolating biologically active substances from waste wood, namely the allocation method Betulinol of the outer layer of birch bark (bark). The allocation method Betulinol includes extraction of the crushed bark of aliphatic hydrocarbons. When this extraction is carried out 3-5 h hexane, at the end of the extract is treated with an equal volume of water. The aqueous layer is separated and precipitated from hexane precipitate is filtered off. Hexane is removed completely and use it again. For extraction use the bark fraction 0,5-5,0 mm Method allows to obtain a sufficiently high yield of pure Betulinol without additional purification, suitable for carrying out reactions of formation of glycosides and Betulinol acid, and to increase the completeness of extraction of the total number of triterpene compounds, the main component of which is Betulinol, to reduce the extraction time. 2 C.p. f-crystals, 2 tab., 2 Il.

The invention relates to methods of isolating biologically active substances from waste wood, namely the allocation method Betulinol of the outer layer of birch bark (bark).

Betulinol - Pyh triterpene alcohol lobanovo is soluble in water, sparingly soluble in chloroform, carbon tetrachloride, hexane, ethanol, isopropanol. Betulinol used in pharmaceutical, perfumery and food industry as an anti-inflammatory and antioxidant, as well as raw materials for the synthesis of glycosides and Betulinol acid.

A method of obtaining Betulinol from birch bark, including its activation at a temperature of 180-260oC, a pressure of 2-5 MPa for 60-300 seconds simultaneously with the alkaline hydrolysis, followed by boiling in ethanol for 2-5 minutes. After filtration, the alcohol is distilled off, the precipitated precipitate is washed and dried (RF Patent 2074876). The disadvantage of this method overestimates the yield of betulin 34%, which is significantly higher content of betulin in the bark of various species of birch trees. The total content of Betulinol in the bark of birch trees 10-30% by weight of absolutely dry raw material and depends on the location and growth conditions (P. Jaaskelainen Betulinol and its utilization /Paperi ja Puu - Pap. Och. Fra - 1981. - #10 - p. 599-603).

Described is a method of obtaining betulin, involving the extraction of 90-95% ethyl alcohol at a temperature of 70-75oSince, in the presence of activated charcoal (RF Patent 2172178). A method of obtaining Betulinol by extraction with isopropyl alcohol, pre-izm) extraction of birch bark with white spirit for 2 hours at a temperature of 155oC, followed by treatment of the extract water concentration solution of hydroaxe sodium, to separate the precipitated precipitated sodium derivatives of fatty and triterpene acids. The yield was 14% with a purity of basic substance 87-88%. To obtain Betulinol high purity precipitated residue was subjected to recrystallization from various solvents. The disadvantages of these methods is not a high yield of secreted product and a low content of Betulinol.

Closest to the technical essence and the achieved result of the allocation method betanol described in (Eckerman Ch., Ekman R. Comparison of solvents for extraction and crystallisation of betulind arom bisch bark Waste / Paperi ja Puu. Och Tra - 1985. #3 - p. 100-106). It provides for the allocation of betanol bark by extraction with organic solvents followed by recrystallization of extractives, the main of which is butanol. As extractants tested simplest alcohols, diethyl ether, acetone, aliphatic hydrocarbons and their chlorinated. In particular, the used solvent LIAV-200, which is a mixture of aliphatic hydrocarbons with BP. 163oWith, extraction they spend 8 hours after removal of the solvent get dry is a - low content of Betulinol, long extraction process.

The objective of the invention is to obtain a clean Betulinol without further purification, to reduce the extraction time.

The problem is solved by the proposed allocation method Betulinol, including extraction of shredded bark aliphatic hydrocarbons. As the aliphatic hydrocarbon used hexane, extraction spend 3-5 hours, after which the extract is treated with an equal volume of water. The aqueous layer is separated and precipitated from hexane precipitate is filtered off. Hexane is removed completely and use it again. For extraction use the bark fraction 0,5-5,0 mm and

The proposed method is to prepare bark to extraction by mechanical grinding with a rotary knife mill and subsequent extraction with hexane in the device socket within 3-5 hours.

The extract obtained was washed with distilled water, after separation falls crystalline precipitate containing 92-97% Betulinol. Then the water is separated from the extract. The precipitate is filtered off and dried. The output of this product is 5-8% by weight of air-dried bark taken for extraction (stage I).

Next extract Wendy solvent return for the next extraction process. The precipitate is washed with water and dried. The output amounted to 15-20% by weight of the extracted product with a basic substance content of 60-70% (stage II).

In the proposed method failed due to the choice of solvent (hexane) and the conditions of selection (precipitation water) without additional purification to obtain a product containing 92-97% Betulinol, while reducing the time of extraction.

Thus, the proposed method is new and allows to obtain a non-obvious technical result.

Fig.1 is a chromatogram of the product obtained by precipitation with water (stage I).

Fig.2 is a chromatogram of a mixture of triterpene compounds (II stage).

Example 1. 100 grams of powdered bark (fraction of 0.5-5.0 mm) is loaded into the extraction cartridge device socket, and in the receiving flask placed in a water bath, pour 1 liter of hexane. Extraction was carried out for 4 hours. The extract is treated with one liter of distilled water. When the delamination roll a white crystalline precipitate. Then separate the water from the extract. The precipitate is filtered off and dried. The product yield is 8 grams containing Betulinol 97% (Fig.1).

Then the extract was evaporated on a rotary vacuum evaporator, in this fall, Osada rasaut for the next extraction process. The precipitation triterpene compounds is filtered off, washed and dried. The output was 20 grams.

It is known that the pharmacological action of drugs made from birch bark impact triterpene compounds in combination, and their interrelation between activity and chemical composition of the drugs are not well understood. Therefore, the second stage of obtaining a dry extract of birch bark, which gives the product which is a mixture of triterpene compounds, is no less important than the first.

Maximum extraction rate achieved by pre-shredding bark and use of the instrument of socket, extraction in which, during the whole process, is the pure solvent. The end of the extraction process was determined by the chromatographic method.

Here is a comparison of the results of the proposed method and the known (table. 1).

Gas chromatographic method for the quantitative determination of Betulinol and triterpene compounds in the extract confirms the complexity of the investigated product. Identified three main components: Betulinol, lupeol and methyl ether of Betulinol acid. Quantitative calculation of the concentration of the components produced programs is th way obtaining pure Betulinol and the total number of triterpene compounds depending on the time of extraction and the degree of shredding bark. As can be seen from the table.1, the extraction process is almost ends after 4 hours, the yield of pure Betulinol (stage I) and the total number of triterpene compounds (stage II) was 28%.

Thus, the proposed method allows to obtain a sufficiently high yield of pure Betulinol suitable for carrying out reactions of formation of glycosides and Betulinol acid, and to increase the completeness of extraction of the total number of triterpene compounds, the main component of which is Betulinol, to reduce the extraction time.

Claims

1. The allocation method Betulinol, including extraction of shredded bark aliphatic hydrocarbons, characterized in that the extraction was performed with hexane within 3-5 h after the extract is treated with an equal volume of water, then the aqueous layer was separated, filtered residue, precipitated from hexane, and then remove the hexane fully.

2. The method according to p. 1, characterized in that use shredded bark fraction 0,5-5,0 mm and

3. The method according to PP.1 and 2, different the

 

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11 cl, 1 tbl, 9 ex

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