SU884703A1 - Method of separating biologically active substances from propolis - Google Patents

Description

(54) METHOD FOR ISOLATING BIOLOGICALLY ACTIVE The invention relates to a process for the production of biologically active substances for cosmetic preparations from propolis by extraction. The known method of obtaining biologically active substances from propolis by extraction with a mixture of ethyl alcohol and water, followed by filtration 1. However, this method does not completely confer flavonoids, which is associated with the choice of solvents (alcohol, water). The closest in technical essence and the achieved result is the method of separation of biologically active substances from propolis by extraction with a mixture of ethyl alcohol and water 2.; The disadvantage of the known method is incomplete separation of biologically active substances, since the use of only ethyl acetate / water and water in the K1 quality as solvents does not ensure the wide range of biologically active constituents of the policy, in addition, this method does not completely separate mechanical impurities and natural contaminants. knowledge. SUBSTANCES FROM PROPOLIS The purpose of the invention is a more complete isolation of biologically active substances from propolis. The goal is achieved by adding glycerin to the mixture of ethyl alcohol and water, providing 75-85, 5-10 and 1015 wt.% In a mixture of ethyl alcohol, glycerin and water, and the ratio of propolis: extractant is 1: 5, the extraction is carried out at 35-45 ° C, followed by cooling to (-5) (-8) C, and the residue after extraction is treated with mink oil at 75-85 ° C and the balance: mink oil is 1: 2. The method is carried out as follows. Natural propolis is cooled to a temperature not lower than —SPN, then ground to a granule size of 2–4 cm. Ground propolis and the solvent — glycerin and ethyl alcohol are loaded into the reactor and heated to 40 t with stirring. At this temperature, the propolis is extracted for 4 hours. Then the extracted mixture is cooled with cold water to 20 i 5C and pereassayut in another reactor. While stirring, cool the extracted mixture for 5-6 hours to (-5) - (- 8) С The cooled mixture is filtered on a suction filter under a vacuum of 0, 0.01 MPa (0.6 ± 0.1 kgf / cm).

Extraction of the residue of propolis with mink oil is carried out at 80 ± 5 ° C for 3 hours. The hot mixture is filtered at sot with a suction filter under a vacuum of 0.06 to, 01 MPa (0.6 ± 0.1 kgf / cm).

The hot filtrate - propolis oil extract is discharged into a storage tank.

In order to completely isolate biologically active substances from propolis, a series of experiments was carried out in order to select solvents and their optimum ratios, as well as for comparison with a known method.

Table 1

From the above tests can be seen. that the most complete absorption of flavonoids (up to 70%) was achieved with a plant, solvent containing, wt.%:, Ethyl alcohol 75-85. Water 10-15 Glycerin 5-10 63.0 65.0 68.0 70.0

23.9 17.8 16.0 13.2

From the experiments it can be seen that the optimal propolis: solvent ratio is 1: 5, since at a ratio of 1: 2, 1: 3, 1: 4 there is an incomplete release of flavonoids, and at a ratio of 1: 6 and 1: 7, the consumption of solution 70, 0 70 , 0

10.4 9.1

40 bodies and, accordingly, the concentration of flavonoids is reduced.

To determine the optimal temperature for the most complete extraction of waxes, balms and resins from water-alcohol-glycerin extract, using a solvent consisting of ethyl alcohol and glycerin, the yield of flavonoids is reduced. To determine the policy: solvent ratio, the results are given in table. . 2. Table 2

experiments were conducted, the results of which are given in Table 3.

T a b l and c a 3

Contents of socks, balzates, resins in alcohol-glitz rin mixture, wt. %

5 0.5

From the experiments it can be seen that a decrease in temperature contributes to the complete absorption of socks, balms, and tar in an alcohol-glycerin mixture. Already at -5 ° C, all waxes, balms and resins are picked up, and at elevated temperatures there are still waxes, balms and resins in the alcohol-glycerin mixture.

To determine the optimal ratio of the balance of propolis: mink oil, experiments were conducted, the results

which are given in tab., 4,

T a b l and c a 4

: i

Recoverable substances

Extraction

Propolis flavonoid fraction

, Flavones - chrysin, tektohrizin and other flavonols - galangin, alpine ramnocytrin, campherid.

Flavonones - pinocembrin, pinobrostin derivatives of quercetin Aromatic acids - coffee, ferulova, brown, benzoic acid Aromatic aldehydes - vanillin, isovanilin

Water soluble vitamins B, C, PP Wax part of propolis:.

free hydrocarbons 10%, fatty acids 15%

esters, mainly cerotinic acid derivatives 70%;

bsshieam oil

It is seen from the experiments that the optimum ratio of propolis residue: mink oil is 1: 2, since the 1: 1 ratio of solvents for balsams, waxes and resins is incomplete, while at a ratio of 1: 3 the consumption of normal oils increases and, accordingly, the concentration of waxes, balsams and resins in the extract.

dates for determining the optimal

0 The temperature in the process of extraction of the residue of propolis with mork oil was carried out experiments, the results of which are given in table. five.

Table 5

five

T, “C

Dissolving waxes, balms, resins in mink oil, wt.%

20

From the experiments it is clear that temperatures

30 does not provide complete extraction of waxes, balms and resins, therefore, the yield is reduced. Applying a temperature higher reduces the quality of the product35.

Substances extracted at each stage of extraction are listed in Table. 6

Table

P ji and Me p 1. Natural propolis is cooled in a refrigerator not lower, then ground on a grinder to a granule size of 2-4 cm. 10 kg are loaded into an enameled reactor with a steam jacket with a capacity of 100 liters, equipped with an enamelled core stirrer and thermometer. crushed propolis and solvent of the following composition:

kg weight,%. Ethyl alcohol

96%, w / o 41.35 82.7

Water6.00 12.0

Glycerol

94% 2.65 5.3

Include the stirrer and the heating of the reactor. Heat the contents of the reactor to .40 t 5 C. At this temperature, extraction of propolis is carried out with stirring for 4 hours. The extractable mixture is cooled in cold water to 20 ± 5 ° C and absorbed into another reactor equipped with a root stirrer and water jacket. With stirring, cool the extracted mixture for 5-6 hours to (-5) - (- 8) s. The cooled mixture is filtered on a suction filter under vacuum C, 06t 0.01 MPa (0.6 ± 0.1 ksg / cmD ).

The filtrate - a water-alcohol extract of propolis in the amount of 53 kg, containing 7 kg of the flavonoid fraction of propolis or 70% of propolis, is collected in a storage container. .

The propolis residue insoluble in the solvent mixture is 3 kg or 30% of the taken propolis.

The total volume of the filtrate solution contains wt.%: Water and ethyl alcohol 81.8; glycerin 5.0; Flavonoid fraction 13.2.

3 kg of dried propolis residue and 6 kg of mink oil are loaded into a clean enamelled reactor with a steam-water, 25-liter jacket equipped with a root agitator and a thermometer. Include the stirrer and the heating of the reactor. The contents of the reactor are heated with stirring at sot 5 ° C for 3 hours. The hot mixture is discharged from the reactor and at 80 filtered on a suction filter under vacuum p, 06 ± 0.01 MPa (0.6 t 0.1 ksg / cm

The hot filtrate - an oil extract of propolis in the amount of 7, 1 kg, containing 16% of propolis or 1.6 kg of the wax part of propolis, is released into a storage tank.

The oily filtrate contains, wt%: Propolis 22.0; 78.0 mink oil / on the filter there are mechanical impurities in the amount of 1.4 kg or 14% of taken propolis, which is thrown away.

Example 2. Natural propolis is cooled in the refrigerator, not like (-10) C, then ground to

a grinder to size of granules - 2.-4 cm.

In a clean enameled reactor with a steam-water jacket with a capacity of 5,100 liters, equipped with an in-line stirrer and thermometer, 10 kg of crushed propolis and the solvent of the following composition are loaded;

kg wt.% Q Ethyl alcohol

96%, w / o 34.0 85.0 Water - 4.0 10., O Glycerin 2.0 5.0 Switch on the stirrer and heating of the reactor. Heat the contents of the reactor to 40 ± 5 ° C; At this temperature, extraction of propolis is carried out with stirring for 4 hours.

The extracted mixture is cooled with cold water to 20 t and absorbed into another reactor equipped with a root agitator and water jacket. While stirring, cool the extracted mixture for 5-6 hours to (-5) - (-8) s. The cooled mixture of filter- 5 ruts on the suction filter with a vacuum of 0.0610.01 MPa (0.610.1 kgf / cm -).

Filt.t - water-alcohol extract of propolis in the amount of 42.8 kg, containing 6.8 kg of the flavonoid fraction of propolis or 68% of

Taking proprilis is collected in a storage tank.

The insolubility in the solvent mixture is propolis a. 3.2 kg or 32% of propolis. , The total volume of the filtrate solution contains, wt%: water and ethyl alcohol 79.0; glycerin 5.0; The propagolum flanoid fraction 16.0.

A clean enameled reactor 0 with a vapor-water jacket with a capacity of 25 liters, equipped with a root stirrer and a thermometer, is loaded with 3.2 kg of dried residue of propalis and 6.4 kg of mink oil. Include the stirrer and the heating of the reactor. The contents of the reactor are heated, stirring at 801 5s for 3 hours.

The hot mixture is discharged from the reactor and filtered on a suction filter with a vacuum of 0.06 ± 0.01 MPa (0.610.1 kgf / cm).

The hot filtrate, an oil extract of propolis in the amount of 7.5 kg containing 16% of the taken propolis or 1.6 kg of the wax portion of propolis, is discharged into a storage tank.

The oil filtrate contains, wt%: Zvoskova part of propolis 21.0; mink oil 79.0 ..

0 On the filter there are mechanical impurities in the amount of 1.4 kg or 14% of the taken propolis, which are emitted

Example 3. Natural propolis is cooled in a hopper not lower than temperature (), then crushed on a grinder to a granule size of 2-4 cm. A clean enameled reactor with a steam-lined jacket with a capacity of 100 liters, equipped with an enamelled core stirrer and a thermometer loaded 30 kg crushed pr polis and solvent the following composition: kg wt.% Ethyl alcohol 96%, w / v. 42.50 75.0 Glycerol 94% by 5.5 10.0 Include the agitator and the reactor heating. Heat the contents of the reactor to 40t 5 ° C. At this temperature, extraction of propolis is carried out with stirring for 4 hours. The extracted mixture is cooled with cold water to 20 t 5 ° C and absorbed into another reactor equipped with a root agitator and a water jacket. While stirring, cool the extracted mixture for 5-6 hours to (-5) - (-8) sec. The cooled mixture is filtered on a Nutsch-Liltre under a vacuum of 0.0610.01 MPa (6.6 t ± 0.1 kgf / cm -). The filtrate - a water-alcohol extract of propolis in the amount of 61 kg, containing 7.0 kg of the Llavonoid fraction of propolis or 70% of the taken propolis, is collected in a storage tank. The propolis residue insoluble in the solvent mixture is 3 K or 30% of the taken propolis. The total volume of the filtrate solution contains, wt%; water and ethyl alcohol 80.5; glycerin 8.0; flavonoid fraction 11.5. In a clean enamelled reactor with a steam-water jacket, 25 l in capacity, equipped with a root agitator and a thermometer, 3 kg of dried residue, propolis and 6 kg of mink oil are loaded. Include a stirrer and reactor heating. The contents of the reactor are heated, stirring, at 80 1. For 3 hours. The hot mixture is discharged from the reactor and at 80 ± filtered on a suction filter under a vacuum of 0.06 t 0.01 MPa (0.6 i 0.1 kgf / see) The hot filtrate — an oil extract of propolis in the amount of 7.1 kg, containing 16% of the taken propolis or 1.6 kg of the wax portion of propolis, is discharged into a storage tank. The oil filtrate contains, wt.%: The wax portion of propolis 22.0 mink oil 72.0. . On the filter there remain mechanical impurities in the amount of 1.4 kg or 14% of the taken propolis, which are removed. The use of ethyl alcohol, glycerin and water as a solvent makes it possible to isolate a wider range of biologically active substances from propolis. extracts, balms, waxes, resins use mint oil. Due to the low setting temperature, mink oil has a high extracting ability, which is associated with high surface tension. Therefore, mink oil is the optimal extracting component in the extraction of resins, waxes and balsam of propolis. Thus, with the above separation of propolis for cosmetic purposes, a hydroalcoholic glycerin extract is obtained, consisting of flavonoids and containing all the biologically active components of propolis, whose soft extraction regimes ensure the preservation of the biologically active components of flavonoids, and the optimum ratio of solvents ensures speeding up the extraction process, completeness of extraction and optimal concentration of flavonoids in the extract; in the technology of preparation of cosmetic preparations pre-. The introduction of a water-alcohol-glycerin extract into the technological process at a temperature above 50 ° С was considered. An extract of balsams, resins and propolis waxes on mink oil is obtained. Propolis waxes add shine to the cream. Mixed with mink oil, it is a useful cosmetic additive. The technology of making cosmetic preparations provides for the introduction of an oil extract, balms, waxes and resins into the technological process at 8.090 ° C. Also, fractions of mechanical impurities and propolis contaminants are obtained, which are emitted. Formula of the invention. A method for separating biologically active substances from propolis by extraction with a mixture of ethyl alcohol and eoda, characterized in that glycerin is added to the mixture of ethyl alcohol and water in order to more completely release the substance, providing the ratio in a mixture of ethyl alcohol, glycerol and water 75-85, 5-10 and 10-15 wt.%, Respectively, and the ratio of propolis: extract 1: 5, the extraction is carried out at 35-45 ° C. Followed by cooling to (-5) - (- 8) C, and the residue after extraction is treated with mink oil at and the balance: mink layer l.-i-. Sources of information, PIAShje into account in the examination 1. Scientific research and opinions about the composition, properties of propolis and its use for therapeutic purposes. Bucharest, Apimondii, 1975, p. 25 2. New research on the Apitheria (Second International Educational Symposium on Apitherapy. Bucharest 2 September 7, 1976), Apimondius, Thorrest, 1976, p. 155-157 (prototype)

Claims (1)

Claim The method of isolating biologically active substances from propolis by extraction with a mixture of ethyl alcohol and childbirth is characterized in that, in order to more fully isolate the substance into a mixture of ethyl alcohol. This and water add glycerin, providing a ratio in the mixture of ethyl alcohol, glycerol and water of 75-85, 5-10 and 10-15 wt.%, respectively, and the ratio of propolis: extract 1: 5, extraction is carried out at 35-45 ° С subsequent cooling to (-5) - (- 8) ° C, and the residue after extraction is treated with mink oil at 75-85 ^ 0 and • V ratios of the residue: mink oil 1: 2.