RU2402923C1 - Method for production of aqueous propolis extract - Google Patents

Abstract

FIELD: food industry.

SUBSTANCE: invention relates to technology of natural raw materials processing, in particular to production of aqueous propolis extract, and may be used in food, chemical and pharmaceutical, medical, liquor and biotechnological industries. Method includes freezing of propolis, its grinding down to powdery state, mixing of prepared propolis with distilled water, at the same time mass ratio of powdery propolis and water makes 1:10. Extraction is carried out by ultrasound in cavitation mode for 2.5 hr continuously, at the same time in process of extraction mixture temperature is gradually increased up to 50-60°C. Then extract is cooled and filtered.

EFFECT: invention makes it possible to produce aqueous propolis extract with maximum preservation of biologically active substances in extract.

3 cl, 1 ex

Description

The invention relates to a technology for processing raw materials of natural origin, in particular the preparation of an aqueous extract of propolis, and can be used in the food, chemical, pharmaceutical, medical, distillery and biotechnological industries to regulate the functions of the human body at physiological boundaries.

It is known that propolis (bee glue) is a product of the biological activity of bees, a biologically active substance (BAS) and is a solid mass of brown-brown color with a greenish tint, highly soluble in alcohol and poorly soluble in water. Propolis contains: a mixture of resins (a mixture of organic acids) and balms 55%, wax 30%, essential oil 10%, pollen 5%, vitamins A, C, group B and other trace elements, including aluminum, vanadium, iron , calcium, silicon, manganese, strontium. Propolis contains cinnamon alcohol, cinnamon and benzoic acid, tannins, chrysin, galangin, etc. It contains series, glycocol, aspartic and glutamic acids, alanine, tryptophan, phenylalanine, and leucine. More than 20 compounds that are represented by three groups of biologically active substances: acids, polyphenols, and compounds of an isoprenoid structure are isolated from propolis. The composition of propolis depends on the place and time of its collection.

Propolis is used in folk medicine as a prophylactic and therapeutic agent. Propolis is known to be harmful to some bacteria, in particular pyogenic (streptococci, staphylococci). It activates the functions of protective mechanisms in the human body, and is also used in veterinary medicine. Under its influence, phagocytosis intensifies, the content of a special protective protein (properdine) in the blood increases, the production of specific antibodies against pathogens and toxins increases. Propolis helps strengthen tooth enamel; most microorganisms do not become resistant to it. It is a non-specific immunosuppressant and increases the activity of antibiotics.

A known method of obtaining an aqueous preparation of propolis, which consists in processing the propolis raw material with an aqueous-organic solvent, separating the obtained extract from the precipitate, drying the extract to obtain propolis and dissolving the powder in water. An aqueous solution of the propolis preparation had an antibacterial effect (see patent of the European Patent Office No. EP 0109993, IPC A61K 8/02, A61K 8/98, A61K 35/64, published on 06/13/1984).

The disadvantage of this method of obtaining an aqueous preparation of propolis is the length of the process of obtaining it (about 10 days), as well as the need to use organic solvents for the extraction of propolis. This complicates the process of obtaining an aqueous extract of propolis.

There is also a known method of preparing a propolis extract, which purifies propolis from mechanical impurities, grinds it and extracts it with water, while extracting it by passing electric current through water until the extract reaches pH 7. Electric current is passed through water through oppositely charged electrodes placed in water, moreover, propolis is placed in the cathode zone, which is separated from the anode by means of a filter partition, while before extraction mineral salts are additionally introduced into water. In particular cases, the propolis extract contains propolis from 1 to 30 wt., In particular from 2 to 10 wt., More specifically 2 or 10 wt. (See RF patent for the invention No. 2090089, IPC A23L 1/076, AK61/35/64, publ. September 20, 1997).

However, the known method has the following disadvantages: firstly, due to the low temperature of the solvent, a low yield of biologically active substances, mainly unsaturated fatty acids, for example 10-hydroxy-2 decenoic acid; secondly, the presence of mineral salts clogs the aqueous propolis extract. Even when filtered, part of them will go into solution, which in turn affects the quality of the propolis aqueous extract. As a result, the scope of the final product is limited, for example, in eye practice; thirdly, the short shelf life of the final product. This complicates the process of preparing an aqueous extract of propolis.

A known method of obtaining an aqueous extract of propolis, which consists in the fact that the raw propolis is subjected to extraction with an aqueous solution of mineral salts, through which an electric current is passed, the electric current is transmitted using two oppositely charged electrodes, one of which is attached propolis, while at least at least one of the electrodes is made of silver, propolis in the amount of 0.5-4.0 g / cm2 is applied and fixed on the surface of the silver electrode, the pulsating electric current is tight with a speed (1.5-18.0) • 10-3 A / cm ^{2 of a} silver electrode is passed for 3-6 hours, starting from a current frequency of 50 Hz with increasing current frequency for 3-5 hours to 1000 Hz, then change the polarity of the electrodes and an electric current of the same density is passed for at least 10 minutes, after which the resulting propolis aqueous extract is cooled. The near-electrode space of the silver electrode is filled with an aqueous solution of mineral salts or mineral water with a salt concentration of at least 4 g / l, and the near-electrode space of the second electrode is filled with distilled water (see RF patent for the invention No. 2303988, IPC A61K 5/64, publ. 10.08. 2007).

The disadvantage of this method is the complex process of obtaining an aqueous extract of propolis, which leads to a rise in price of the finished product.

Closest to the proposed technical solution is a known method of obtaining an aqueous extract of propolis, including grinding, freezing, mixing the prepared propolis with water and extraction, while propolis is crushed to a powdery state, mixed with a portion of the water with a stabilizer necessary for extraction, treated with ultrasound and insist, then the remaining water is added to the treated mixture, while the water is first ionized with micro and macro elements, for example, by letting it through shungite and an electrolyzer, and silver ions are taken as a stabilizer, the ratio of powdered propolis to water is 1: 0.5, and extraction is carried out by heating the mixture to 80-90 ° C, followed by cooling and filtering. Ultrasound treatment is carried out for 20-30 minutes (see RF patent for the invention No. 2185181, IPC A61K 35/64, publ. July 20, 2002).

However, the disadvantage of this method is also a complex process for obtaining an aqueous extract of propolis, which leads to a rise in price of the finished product.

The objective of the present invention is to simplify the process of obtaining an aqueous extract of propolis and increase the shelf life of the finished product.

The technical result achieved in solving this problem is to provide the possibility of maximum output into the extract of intracellular fluids with the biologically active substances contained in them.

The specified technical result is achieved by the fact that in the method of obtaining an aqueous extract of propolis, including freezing propolis, grinding it to a powder state, mixing prepared propolis with water and extraction while increasing the temperature of the mixture, followed by cooling and filtering, according to the invention, the mass ratio of powdered propolis and distilled water is 1:10, and the extraction is carried out by ultrasound in the cavitation mode for 2.5 hours continuously, while in percent sse extraction gradually raise the temperature of the mixture to 50-60 ° C.

It is advisable to grind propolis after freezing into a powder with a particle size of 2 to 4 mm, and to cool the aqueous extract of propolis after extraction to a temperature of not more than 10 ° C.

With a mass ratio of powdered propolis and distilled water equal to 1:10 (i.e. 10% concentration), the optimal amount of biologically active substances in the extract is ensured. Water dissolves from 7 to 11% propolis, while boiling does not increase the concentration of the solution. At a lower concentration, a too small amount of biologically active substances in the extract is obtained, and at a higher concentration, biologically active substances are more difficult to separate from the feedstock. The proposed concentration is determined experimentally and provides a complete and comprehensive extraction of biologically active compounds of various nature, providing the necessary level and spectrum of specific activity of the target product and its quality.

Carrying out extraction by ultrasound in the cavitation mode for 2.5 hours continuously allows you to most fully extract biologically active compounds, the complex of which provides the necessary level and spectrum of specific activity of the target product. With a shorter extraction time, the completeness of depletion of the feedstock is not ensured, and with a longer extraction time, an over-consumption of the extractant is possible.

The shelf life of the finished product (aqueous extract of propolis) in a mixture of powdered propolis with distilled water is significantly increased, since propolis has an antimicrobial and antiseptic effect.

As a result of processing the mixture with ultrasound in the cavitation mode due to the intense interaction of the extractant with the extractant with a high frequency of ultrasonic exposure and the cavitation interaction mechanism, an effective extraction process occurs. This treatment allows maximum removal of intracellular fluids with the biologically active substances contained in them. Moreover, the extraction process is not only much faster, but also at much lower temperatures, which is important for substances that decompose or oxidize at high temperatures, in particular, to preserve the biological activity of protein compounds of the feedstock. The use of an ultrasonic apparatus for obtaining an aqueous extract of propolis allows for active extraction with ultrasound throughout the process, while creating the opportunity to obtain an aqueous extract of propolis with any fractions at different temperatures.

Propolis extract obtained by gradually increasing the temperature during extraction to 50-60 ° C contains more unsaturated and free acidic compounds, as well as decenic acid, than in the native stock solution.

A method of obtaining an aqueous extract of propolis is as follows.

The propolis raw material is cleaned of mechanical impurities and frozen, for example, in a refrigerator, while the freezing temperature is selected from the interval (-10 ° C) - (- 18 ° C), and freezing is carried out for no more than 3 hours. As a result of cooling, propolis becomes fragile. Then, frozen propolis is crushed into fine fractions into a powder with particles from 2 to 4 mm, for example, on a hammer mill M-8M type (manufactured by Pchelotehnopark LLC, Ryazan Region, Rybnoe city) or another type.

To carry out the extraction, the calculated amount of distilled water is poured into a container with powdered propolis (GOST 6709-72. Distilled water. Technical conditions. - M .: Standards Publishing House, 1996, reprint), while the mass ratio of powdered propolis to distilled water is 1 :10. Then an ultrasonic generator is connected, for example, the well-known ultrasonic device “UZUMI-15” (manufacturer of TRIMA LLC, Saratov) is used, power consumption 750 V • A, ultrasonic vibration frequency 38 kHz, ultrasonic power 550 V • A (see , for example, URL: http://www.trima.ru/autoservice/uzumi_ind.htm (accessed: 04/02/2009)), and conduct active extraction under cavitation conditions for 2.5 hours. A qualitative effect of active extraction is achieved due to the formation in the fluid of ultrasonic cavitation - pressure pulses that occur when the closure of cavitation voids, the influence of microflows and microflows of a cavitating solution in an ultrasonic field on the surface of particles of propolis crushed into powder. In the process of extraction, a gradual increase in temperature to 50-60 ° C.

Then, the resulting aqueous solution is cooled to ambient temperature, wax is removed from the surface of the propolis aqueous solution, for example, manually or by some other device. Next, the aqueous solution is filtered through belting or another similar type of filter. Filtration is carried out in a dry container of dark glass or stainless steel. Ready-to-use propolis aqueous extract is packaged in prepared containers.

Example. Propolis was taken to prepare an aqueous solution of propolis, and it was purified from mechanical impurities. Then propolis, crushed into pieces no larger than 20 mm, was frozen in a freezer in a domestic refrigerator to a temperature of -10 ° C for at least 3 hours to completely freeze it and crushed in an M-8M mill to a powder state with particles no more than 1-A mm . Propolis, crushed into fractions of 2-4 mm, has a large surface for extraction, which increases the extraction of biologically active substances, such as flavonoids, phytocides, unsaturated fatty acids (decenes), resins, essential oils, etc. As a result, the quality of the propolis extract increases. Then, powdered propolis was poured with distilled water at room temperature in a mass ratio of 1:10, i.e. 0.5 l of water and 50 g of propolis (10% solution). The resulting mixture was placed in an ultrasonic unit “UZUMI-15” and processed for 2.5 hours in the cavitation mode with a gradual increase in temperature to 55 ° C without access of light. Next, the solution was cooled and filtered through a paper filter. Then, the resulting propolis aqueous extract was packaged in a clean, dry, odorless container. Due to the fact that distilled water was used and the product was stored at a temperature of no more than 10 ° С (in the refrigerator), the shelf life of the propolis extract without changing its properties was 10 months.

From an aqueous extract of propolis obtained in accordance with the proposed invention, a water-soluble propolis powder was obtained. For this, the aqueous propolis extract was dried, for example, freeze-drying was used. The water-soluble propolis powder was convenient for storage and transportation. To prevent caking during storage, propolis powder was diluted with an inert filler, such as glucose.

Thus, for the preparation of an aqueous extract of propolis according to the proposed method does not require the development of special equipment, while the process is relatively simple and has a low cost.

Obtained by the proposed method, an aqueous extract of propolis can be used as a general strengthening agent with antioxidant and adaptogenic properties, contributing to an increase in the working capacity and resistance of the human body to adverse environmental factors. Propolis aqueous extract is intended for a wide range of consumers, has strong immunoprotective properties, promotes wound healing, is non-toxic, does not have autogenic, immunotoxic and teratogenic activities.

Claims (3)

1. A method of obtaining an aqueous extract of propolis, including freezing propolis, grinding it to a powder state, mixing the prepared propolis with water and extracting while increasing the temperature of the mixture, followed by cooling and filtering, characterized in that the mass ratio of powdered propolis to distilled water is 1 : 10, and the extraction is carried out by ultrasound in the cavitation mode for 2.5 hours continuously, while the temperature of the mixture is gradually increased during the extraction process and up to 50-60 ° C. 2. The method according to claim 1, characterized in that propolis, after freezing, is ground into a powder with a particle size of 2 to 4 mm. 3. The method according to claim 1, characterized in that the cooling of the aqueous extract of propolis after extraction is carried out to a temperature of not more than 10 ° C.