SI8711835A8 - Process for preparing a liquid ethanol extract of propolis - Google Patents

Abstract

The process is carried out by extracting the propolis at a low temperature, such as not above 20 DEG C, with an ethanol/water mixture with exposure to ultrasound of a certain frequency for a brief time, such as 25 minutes, in a closed system and subsequently decanting the resulting suspension and separating the clear propolis extract from the solid particles. The resulting propolis extract is distinguished by a high biological activity.

Description

The present invention relates to the field of food chemical technology, pharmacy and beekeeping, and in particular to a new process for the production of a high quality liquid ethanol extract of propolis useful as an (auxiliary) drug.

A technical problem

There was a need to find a new, technologically advanced, rapid and rational process for the preparation of a liquid ethanol extract of propolis, without the formation of resinous aggregates, with high product activity; which was not possible with the classic extraction method.

The state of the art

Propolis is a natural bee crop. It is collected on buds and other parts of plants and used in their living space to close openings and cracks and to isolate dead foreign bodies (insects and other animals) in the hive to prevent the spread of infection. It coats honeycomb cells before storing their crops, such as in honeycomb. honey and pollen. Propolis is a specific complex bioactive substance that consists of over 60 different compounds. The basic ingredients are various resins, waxes, essential oils and pollen. Important bioactive constituents of propolis are plant dyes, the most important of which are flavones or yellow plant dyes, such as chrysin and tectocrysin, flavonones such as pinostrombin, pinocembrin and quercetin with derivatives, and flavonols such as ramnocytrin, galangin and isoalpinin. Contains aromatic substances such as isovaniline, acetoxybetulenol and aromatic acids such as cinnamon, benzoic, caffeine, ferula and proteacetate acid, and esters of these acids with benzyl alcohol, pentonyl alcohol, phenethyl alcohol and cinnamal alcohol (EM Schneidege, J. Ari .Zeunke - Die Pharmazie Nr. 34, 1979 - 103). Most of these substances are antimicrobial and fungistatic, which is also characterized by the action of propolis extract.

By dissolving propolis in ethanol, the resinous, brown, thermoplastic and sticky mass dissolves to some extent. After some time they are eliminated from the solution

- 3 waxes. According to the method known so far (C. Braileanu et al., Die Propolis; Apimondia Verlag, Bucharest 1975, p. 147), the propolis extract is prepared by soaking the propolis for 10 days in an alcohol / water mixture (with an alcohol content of 30 to 96%). at a ratio of 1: 10. The suspension is occasionally stirred. After 10 days, the solution is filtered off and used as such.

This method of preparing a propolis extract has problems ranging from poor extraction, a lengthy process, poor yield, to bonding the resin to the walls of the container and mixer. Resinous aggregates are formed which are only difficult and incomplete to dissolve in the extraction solvent, which also causes the extraction efficiency to be very low. With the condition of the solution for several days in the air, some of the constituents are oxidized, which results in reduced activity of the final extract. A major problem with the classic method of extraction of propolis is also the poor dissolution of the resinous and waxy part of propolis, which leads to the subsequent extraction of waxes and further processing to the clogging of filter devices.

Documentation: L.Vechet: Die Propolis, Apimondia Publishing House, Bucharest 1975, p. 48 - 52; J.Metzner, E. Schneidewind, and E.Friedrich: Die Pharraazie, 32/1977, p. 730; J.Metzner, H.Bekemeier, M.Paintz, and E.Schneidewind: Die Pharmazie, 34/1979, p.97; M.Paintz and J.Metzner: Die Pharmazie, 34/1979, p. 839; A. Stojko and Others: Arzneimitt. Forsch. - Drug.Reg., 28/1978, p. 35; S.Scheller et al .: Arzneimitt.Forsch. - Drug.Res., 27/1977, p. 1547.

Description of solution to a technical problem with implementation examples

The inventors, however, were the first to come up with the idea of trying to extract propolis on an ultrasonic extractor on which medicinal herbs are extracted and which was also procured for this purpose. First, several extraction tests were performed on a laboratory ultrasonic extractor, and then the experiments were performed on an industrial (600 L) apparatus. The first efficiencies were low and the color of the extract product was not adequate. With great inventive effort and lengthy experiments, we found a new process of the invention that solves the technical problems mentioned.

We have now surprisingly found that in a technologically advanced, rational way, a high quality, liquid ethanol extract of propolis is obtained by a process that is ground by grinding propolis, such as with a particle size of up to 5 mm, briefly extracted over a minute to 25 minutes, by a mixture of ethanol and water in a volume of 70:30 to 90:10 as 87:13, in a closed system using ultrasound at a frequency of 18 to 25 kHz, and clear the resulting suspension by decanting and centrifugation.

If desired, concentrate the extract to max. solids content of 80%, e.g. in a vacuum, e.g. 1.47 to 0.5 kPa.

Compared to the known method of extraction of propolis, our process has great advantages and novelties, such as:

- 4a extraction is carried out at low temperatures, which is essential in order not to destroy bioactive thermolabile substances; at lower extraction temperatures between 273 and 290 K (0 to 17 ° C), the solubility of the waxes in the extraction solvent is low and, consequently, the subsequent isosomalisation of the wax is greatly reduced and the other active substances are nevertheless completely dissolved;

the extraction efficiency is extremely high, exceeding 96% (calculated on the dry weight of the input raw material); the extraction time is extremely shortened, i.e. only 25 minutes;

consumption of ethanol is more rational;

extraction requires less labor; extraction requires less space than conventional extraction

- 5 raacerations, where many stainless tanks are also used, which is a waste in the present process; the extraction efficiency is extremely high, because by breaking down the cells with ultrasound, it captures the possibility of extracting all bioactive substances, enabling the production of a more active propolis extract compared to conventional maceration;

Due to the modern process of extraction in a closed system, the possibility of oxidation of the active ingredients is also greatly reduced and thus a high activity extract can be obtained;

ultrasonic extraction of propolis yields an extract with a high content of bioactive flavonoids, the value of which, after chemical analysis, is at least 4% calculated on the hyperiside;

high antimicrobial activity of propolis extract obtained by ultrasonic extraction has been demonstrated, which is assumed to be due to the high content of flavonoids.

Based on our research to date, we find that: Propolis extract, when used locally, has antibacterial action on a wide range of bacteria, especially gram negative, which causes inflammation of the mucous membranes and skin, has an inhibitory effect on the growth of various fungi, has a pronounced local anesthetic action, accelerates the regeneration of skin epithelial cells. topical application, anti-inflammatory (anti-inflammatory) effect at local application, anti-viral effect (on Herpes simplex virus, influenza virus) (M.Likar and B.Filipič: antimicrobial activities of ethanol extract of propolis conducted at the Faculty of Medicine, Institute of Microbiology in Ljubljana from 1979 to 1986).

Based on the above documentation and the results of numerous biological and clinical tests in dermatology, dentistry and otolaryngology, the ethanol extract of propolis is used in inflammation of the mouth and throat, for the local treatment of wounds, ulcers and abrasions, for the protection of the body against certain viral infections (influenza , herpes) and incorporated into lubricants as an anti-inflammatory agent (for sunburn and jellyfish burns).

The propolis extract is used as a 5 to 80% solution in a mixture of ethanol and water in a volume ratio of 60:40 to 96: 4. For topical use, ethanol extract of propolis is used in the form of 5 to 80% ethanol extract of propolis and in the form of an ointment. In the form of tablets, capsules and dragees, it is suitable for oral and sublingual use and in the form of suppositories for rectal use. To protect against infection, propolis extract is used by incorporating it into honey and combining it with royal jelly and pollen.

The invention is explained by the following embodiments.

EXAMPLE 1

Preparation of extract_

The propolis is ground on a mill hammer into small particles with a maximum diameter of 3 mm. A 500 liter minimum of 87% by weight ethanol solution is prepared in the extraction vessel. .20 kg of ground propolis is added to the extractor while stirring. After 25 minutes of extraction with an ultrasound frequency of 18 to 25 kHz, allow the propolis extract to decant for a minimum of 2 hours, then filter.

Filtration is done through pressure filters with cartridges of rapid filter paper. The thus obtained clear propolis extract was concentrated in a column concentrator in a vacuum of 1.47 to 0.5 kPa by means of a heat pump to the desired concentration of 5 to 80% of the dry matter in the extract. The concentration is carried out at temperatures up to a maximum of 290 K (17 ° C).

EXAMPLE 2

Tablet composition <.............

Ingredients mg / tablet propolis extract _ £ 80% -en) 17.5 vitamin C 1.5 oil Menthae piperitae 0.7 sucrose 681.3

701,00 mg

EXAMPLE 3

Ointment composition

Ingredients propolis extract (80%) neutral ointment base g / 100 g ointment

Claims (1)

PATENT APPLICATION A process for the production of a liquid ethanol extract of propolis, characterized by stem to grind propolis as a particle size up to 5 mm, briefly within a minute to 25 minutes, is extracted with a mixture of ethanol and water in a volume of 70:30 to 90:10 , preferably 87:13 at? 73 <T <2-90 K (0 to 17 ° C) in a closed system using ultrasound at a frequency of 18 to 25 kHz and clear the resulting suspension by decantation and centrifugation.