Method for vacuum ultrasound extraction of bioactive propolis compounds

IPC classes for russian patent Method for vacuum ultrasound extraction of bioactive propolis compounds (RU 2372928):

A61P29 - Non-central analgesic, antipyretic or antiinflammatory agents, e.g antirheumatic agents; Non-steroidal antiinflammatory drugs (NSAIDs)

A61P17/02 - for treating wounds, ulcers, burns, scars, keloids, or the like

A61K35/64 - Insects, e.g. royal jelly

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FIELD: medicine.

SUBSTANCE: raw material is grinded that is followed with vacuum ultrasonic extraction with 80% ethyl alcohol at 18-20°C.

EFFECT: invention allows simplifying the process and improving product purity.

1 ex

The invention relates to medicine and relates to a method of allocation of propolis raw biological groups and labile compounds used as a drug of the drug, "Propolis tincture 10% concentration in the alcohol solution of 80% concentration, with a shelf life of three years and improvement in all indicators, introduced in Pharmacological article, thereby reducing the recovery process and improve the quality of propolis raw stabilize all physico-chemical and technological properties of the substance, alcoholic propolis.

In order to improve the quality of propolis tincture and enhance the yield of biologically active compounds from the depths of pieces of propolis raw to 100% extraction we have developed a vacuum-ultrasonic technology of extraction of biologically active compounds at low temperature (18-20°C), which ensures the safety of all labile components and prevents the passage of the solvent, the associated inactive substances (waxes) and other compounds, due to the high purity of the end of extraction process that ensures the stability of all readings monograph "Propolis tincture".

As a prototype of the proposed positive solution Method to obtain propolis extract alcohol (EN 2073519 - (5). Nedostreljannaja vacuum extraction of propolis raw is the constant evaporation under vacuum 96% ethanol feed vapors in the cooling device, that leads to considerable loss of cooling water and the loss of ethanol 2-5%if you use a closed cycle, it will be a great loss of energy consumption for cooling water, 3-4 cycle evaporation of ethanol 96% and return it to wyborny cube, i.e. in the reactor. Extractable substances that remain in the evaporator Cuba, when re-filling the cube precipitate will be dissolved, what is undesirable after each cycle, so the remains must be constantly removed from the intermediate tank, which is time consuming and leads to great cost of time. The proposed vacuum extraction is not aimed at the creation of dosage forms of propolis tincture, it gives evaporation to a dry residue, such vacuum technology does not take into account the percentage of propolis raw, so you cannot calculate propolis tincture containing 10% propolis raw content of polyphenols, flavonoids, phenolic hydroxyl groups, heavy metals, microbial limits, antimicrobial activity under Pharmacopoeial article of the Ministry of health and social development.

Shown in the patent table reflect the degree of extraction of solids from propolis raw 96% ethanol at 45°With vacuum method, one stripped off to the dry residue. Extraction of 96% ethyl alcohol reduces the output of propol the sa-raw water-soluble biologically active substances. The precipitate vacuum method is used only for animals that are reflected in the technical specifications, in particular, for trudnozazivate RAS surface layers of the skin of animals, but not in medicine.

In the proposed patent the aim of the invention is the elimination of all the above drawbacks. For this purpose we have developed a vacuum-ultrasonic extraction the extraction of biologically active compounds from propolis raw 80% ethanol, at low temperatures (16-20°C), while increasing the degree of extraction of extractive substances from the depths of pieces of propolis raw, vacuum-ultrasonic device leads to the fact that propolis raw loses flexibility and becomes brittle, it disappears high adhesion.

Vacuum ultrasound allows to obtain fine particles of propolis raw, in alcohol, which leads to high extraction of biologically active substances. Therefore, the extraction is carried out at low temperature, which ensures the safety of all labile components and prevents the passage in the extract associated, undesirable substances (wax) and other compounds, which results in high purity of the final product, i.e. propolis tincture.

Example 1.

For this frozen propolis raw crushed in the crushing plant. Crushed in the crushing set is VCE propolis - raw is placed in purified water, mix thoroughly and leave to stand for 10-15 minutes. Pop-up on the surface of the water particles of wax and other impurities are removed, deposited on the bottom of the tank particles propolis raw collected on a stainless steel sieve and dried at room temperature 20-25°C during the day. Weigh the dried propolis raw and loaded into a glass column No. 1, diameter 0, 2 m, height 1 m from the filter at the bottom of the device. In column No. 1 load 10 kg of propolis raw in another tank or column prepared 80% ethanol 90 HP In a glass column No. 1 set ultrasonic device in the middle of crushed propolis raw and plug it in the electrical network of an alternating current. Use the power vacuum ultrasonic installation is negligibly small, only 5 volts, and the weight is only 200,

Column No. 1 sealed to the upper edge of the column attach the vacuum hose connected to the vacuum membrane pump and tank, where prepared with ethanol 80% ethanol for 10% of the content of propolis in alcohol solution. In column No. 1, in the upper part is the gauge, which will control the negative pressure in the column No. 1.

Start the extraction carried out in the following way: cover the bottom of the faucet in the column No. 1 include vacuum membrane the ASAS and when the vacuum reaches 0,65-0,75 MPa in column No. 1, manually control the flow of 80% ethanol, so that the pressure did not fall below 0.6 MPa. When the column No. 1 is filled with ethyl alcohol 80% in the amount of 30 liters, the lower the crane column is closed when the vacuum reaches 0,65-0,75 MPa, the upper crane column No. 1 block, include a vacuum membrane pump, in the fall of rarefaction periodically include a vacuum pump.

The first vacuum-ultrasonic extraction is carried out in the column No. 1 for 3 hours, at a content of 80% ethanol in the amount of 30 l after 3 hours, turn off the vacuum and lower the crane switch in the tank for collecting propolis tincture and under the pressure of the extract is filtered and flows into the collection vessel of the extractant. After removal of the extract column No. 1 again fill 80% ethyl alcohol, as in the beginning of the process, in the amount of 30 l and perform the same process, but stand for 1.5 hours, this is the second extraction of the same raw propolis.

A third extraction of propolis raw in column No. 1 is carried out, as the previous one, but stand one hour, only to have full use of the prepared 80% ethanol for 10 kg of propolis raw.

Thus, the proposed vacuum altasnova extraction of propolis raw is more effective in obtaining EC the paths of propolis alcohol and technologically has a number of advantages in comparison with known methods. Improve all indicators of the quality control of propolis tincture included in the Pharmacopoeia article, and meet all the standards prescribed by the specification "Propolis tincture".

The method of producing propolis extract alcohol by crushing raw materials, extraction with ethyl alcohol under vacuum followed by filtration, characterized in that the extraction of 80%ethyl alcohol spend vacuum-ultrasonic method at 18-20°C.