WO2021118499A1

WO2021118499A1 - A propolis product not containing alcohol and alcohol derivatives, and a method for its production

Info

Publication number: WO2021118499A1
Application number: PCT/TR2020/051118
Authority: WO
Inventors: Derviş TÜRKİŞ
Original assignee: Arilardan Gida Sanayi̇ Ve Ti̇caret Li̇mi̇ted Şi̇rketi̇
Priority date: 2019-12-11
Filing date: 2020-11-17
Publication date: 2021-06-17
Also published as: TR201919878A1

Abstract

A method for obtaining a propolis-based product having standard features, which can be used as direct or raw material, obtained by extracting propolis without using alcohol and alcohol derivatives and as having high active substance content.

Description

A PROPOLIS PRODUCT NOT CONTAINING ALCOHOL AND ALCOHOL DERIVATIVES, AND A METHOD FOR ITS PRODUCTION

TECHNICAL FIELD

The invention relates to a production method by which propolis is obtained without using alcohol and alcohol derivatives, and as having high active substance content.

PRIOR ART

The structure of propolis varies according to the type of the plant from which it is collected, to the manner by which it was collected by the bee, and to the manner it is used. As taken from the hive, it consists of 50% resin and vegetable balsam, 30- 50% wax, 10% essential oils, 5% pollen, and 5% amino acids and minerals.

Since it contains wax and impurities, propolis cannot be consumed as it is obtained from the hive. It is necessary to perform an extraction process to extract the active substances after these impurities are removed. The extraction method and solvent that is used, in turn, have a direct impact on the ratio of the active substance in the propolis that is obtained. Various solvents and methods are used for this purpose. Ethanol solutions constitute the extraction solvent that is most widely used in propolis. However, the bitter taste, irritant nature and adverse health impacts of such alcoholic solvents limit their amounts of use, reducing their applicability in certain medical practices (such as application to the eye), paediatric cases, and in the pharmaceutical and cosmetics industry. Therefore, recently, extracts have been prepared using water or a water-propylene glycol mixture in order to extend its field of application. However, upon examination of the literature referring to extraction practices using water, it is seen that the active substance transfer is very low. WHO (World Health Organisation) indicates that the daily maximum consumption amount of propylene glycol must be 25 mg/kg body weight, which limit restricts the product’s use especially in children. An examination of the literature indicates that vegetable oils are used as well as solvents such as ethanol, water and polyethylene glycol [4, 5, 6, 7, 8, 9]. In a study conducted by Kubiliene et al. (2015), different extraction solvents have been tried on propolis. Water, ethyl alcohol, polyethylene glycol and olive oil have been used as solvents. The results of the study demonstrate that the total phenolic substance amounts are considerably low in extracts obtained from extractions performed by using water and vegetable oils (1.6 ±0.4 and 0.5 ±0.2 mg GAE/ml, respectively). The active substance ratios in the samples extracted by using 70% ethyl alcohol and polyethylene glycol-water mixture, however, have been found to be 12.7 ± 1.2 mg GAE/ml and 10.7 ± 1.2 mg GAE/ml, respectively [8]. In a study performed by Pujirahayu et al. (2014), the propolis samples have been extracted in water, 70% ethanol, propylene glycol, olive oil, and extra virgin coconut oil. Upon examination of the results, it is seen that the lowest antioxidant value and flavonoid amount is available in the propolis extracted in olive oil, water and extra virgin coconut oil [9].

It is seen in the sources of literature that propolis extraction is generally performed by extended-shaking with a solvent, or brief processing in an ultrasonic bath and microwave [1 , 2, 3, 5 6, 7] Although the method of extraction by shaking is effective in terms of high active substance transfer, the duration of the process is long. Active substance transfer is achieved in a short space of time in extraction using microwave, but this also causes the transfer of undesired substances such as wax. Also, after a certain period of time the active substances degrade, causing a decrease in the amount of the active substance in the extract. In this sense, the ultrasonic method is considered to be a more suitable method in terms of both active substance transfer and duration [3]

In prior art no. TR 2015/04984, acid and base extraction has been performed, and it is indicated that the product has subsequently become neutralised. Since changing the ambient conditions changes the product’s solubility, problems are foreseen in the ultimate product stability, in addition to the absence of a process step relating to the standardisation of the product.

In prior art no. TR 2014/ 10587, propolis has been extracted by using only water, and it is indicated in scientific literature that the active substance amount of the product would be low as a result of extractions performed in this manner. BRIEF DESCRIPTION OF INVENTION

The present invention relates to a water-based propolis product having the same characteristics, which has high active substance content, and a method to produce such product, in order to eliminate the above-mentioned disadvantages and to bring new advantages to the technical field in question.

In order to carry out all of the objectives mentioned above, which the following detailed description shall reveal, the present invention is a water-based standard propolis product having high active substance content, and a method for its production. Accordingly, the novelty in question involves a standard propolis product that contains water as a carrier substance, that is extracted without using alcohol or alcohol derivatives, that has a total phenolic substance amount of 10,000-50,000 mg GAE/L, that contains 10-150 flavonoid substances, and that has a wax amount of 1 -20%.

A preferred embodiment of the invention relates to a method for obtaining a propolis-based product having standard features, which can be used as direct or raw material, obtained by extracting propolis without using alcohol and alcohol derivatives and as having high active substance content. The method comprises the process steps of breaking down the propolis raw materials by using a breaker, removing the wax contained in the broken-down propolis, mixing the propolis, from which the wax was removed, with a solvent, the H⁺ ion concentration of which has been changed, for extraction in the manner of obtaining an extract, checking the phenolic substance amount and number of flavonoid substances of the extract, continuing the extraction if such amount and number are not suitable, filtering or centrifuging the extract in order to remove undissolved impurities, and packaging the extract from which the impurities have been removed. A preferred embodiment of the invention comprises the process step of obtaining a wax percentage in the range of 10-60% in the propolis raw materials, and a total phenolic substance amount between 60,000-200,000 mg GAE/L.

A preferred embodiment of the invention comprises the process step of sieving the propolis grains by using a wire mesh, adjusted according to the size of said grains in order to remove the wax from the broken-down propolis.

A preferred embodiment of the invention comprises the process step of spreading the broken-down propolis in a 2-3 cm-thick layer on a porous tray.

A preferred embodiment of the invention comprises the process step of spreading the broken-down propolis on a porous tray, and then heating it up to 50-80 C° in a heater.

A preferred embodiment of the invention comprises the process step of reducing the amount of removed wax to 20% or below.

A preferred embodiment of the invention comprises the process step of setting the H⁺ ion concentration of the solvent mixed with the propolis, from which wax was removed, to the range of 10-8-10-10.

A preferred embodiment of the invention comprises the process step of mixing the propolis and the solvent mixed with the propolis from which the wax was removed, for 30-60 minutes at 40-60 °C temperature, under minimum 3-bar pressure, in a homogeniser operating at a speed of 3000-7000 revs/min.

A preferred embodiment of the invention comprises the process step of setting the phenolic substance amount of the extract to the range of 10,000-50,000 mg GAE/L, and as containing a number of flavonoid substances in the range of 10-150.

A preferred embodiment of the invention comprises the process step of centrifuging the extract for 30-40 min at 4,000-8,000 revolutions. A preferred embodiment of the invention comprises the process step of filtering the extract by gradually passing it through 100-micron, 50-micron and 10-micron filters.

A preferred embodiment of the invention comprises the process step of dosing the water-based propolis product into disposable air- and light-proof packages at the filling machine. A preferred arrangement of the invention is a propolis product produced in accordance with any one of the above process steps.

DETAILED DESCRIPTION OF INVENTION

In this detailed description, the propolis product that is the subject of the invention and the process for producing such product are explained by way of non- exhaustive examples given merely for ensuring a better understanding of the subject.

The method for preparing the standard water-based propolis product having high active substance content, which is the subject of the invention, comprises the process steps described in the following section:

The propolis obtained from beekeepers is first analysed to check its wax percentage, total phenolic substance amount, and residue content. The raw material is returned if any nonconformity is found. The propolis that is found suitable is stored at -18 - -25 C° temperature. The propolis to be used in production is broken down into small pieces by using a breaker, thereby increasing the number of extraction surfaces.

Due to the wax and impurities it contains, propolis cannot be consumed in this form. The propolis is spread evenly at a thickness of 2-3 cm on a porous tray having a collection chamber, designed specifically for removing wax, and which is of a structure and size that would allow its being placed in an oven, and is exposed to 50-80°C temperature. During the process, the melting wax is removed from the propolis as it flows out of the pores. The process is continued until the flow of the wax is complete. The amount of the wax remaining in the propolis is checked through an analysis to verify the effectiveness of the process. The upper platform of the porous tray, on which the propolis was placed, is removed and placed under - 18 C° temperature to chill the propolis. The propolis, the stickiness of which is eliminated and is given a brittle nature in this manner, is removed from the platform by scraping.

The propolis from which the wax has been removed is placed in a closed stainless- steel tank. For extracting the phenolic components in the propolis, the solvent’s FT ion concentration is set to a range of 10 ⁷-10 ¹° and is mixed in the tank for 30-60 minutes at 40-60°C temperature. The propolis:solvent ratio is set according to the propolis amount desired in the end product. In order to increase the effectiveness of the extraction process during mixing, the product is mixed by using a homogeniser (3000-7000 rev/min) under high pressure (min 3 bars).

During the process, the amount of phenolic substances is checked to determine the effectiveness of the extraction process. If the desired active substance amount is not achieved at the end of the analysis, the extraction process is continued.

When the analysis reveals that the desired active substance amount has been reached, the undissolved portion is removed by centrifuging (4,000-8,000 revolutions, 30-40 min) or filtration (by gradually passing through 100-micron, 50- micron and 10-micron filters).

The obtained propolis is placed in the filling chambers, and then put into disposable, practical and hygienic packages. The amount of propolis in each package is fixed, whereby a fixed amount of water-based propolis of standard character is offered.

Since the standard water-based propolis with high active substance content, the process steps of which have been described above, and which is the subject of this invention, contains no alcohol or alcohol derivative, it is suitable for continuous use by any age group. The active substance amount of the obtained propolis product is equal to, or higher than, the active substance amount of products on the market that are extracted by using alcohol and alcohol derivatives. The recommended consumption amount of propolis extracts on the market presented in dropper bottles is indicated as number of drops according to age. Since the product that is the subject of the invention is presented in a disposable package, consumers do not have to calculate the amount they need to consume. Since the package is disposable and sealed, the product is prevented from contacting air, by which the product properties are preserved.

Claims

1. A method for obtaining a propolis-based product having standard features, which can be used as direct or raw material, obtained by extracting propolis without using alcohol and alcohol derivatives and as having high active substance content, characterised in that it comprises the following process steps: a) the propolis raw material is broken down by using a breaker, b) the wax contained in the broken-down propolis is removed, c) the propolis from which the wax has been removed is mixed with a solvent the H⁺ ion concentration of which has been changed, and is extracted in the manner of obtaining an extract, d) the extract’s phenolic substance amount and number of flavonoid substances are checked, and extraction is continued if this amount and numbers are not suitable, e) the extract is filtered or centrifuged to remove the undissolved impurities, f) the extract, from which the impurities have been removed, is filled into packages.

2. A method according to Claim 1 , characterised in that it comprises the process step of obtaining a wax percentage in the range of 10-60% in the propolis raw materials, and a total phenolic substances amount between 60,000-200,000 mg GAE/L.

3. A method according to any of the preceding claims, characterised in that it comprises the process step of sieving the propolis grains by using a wire mesh, adjusted according to the size of said grains in order to remove the wax from the broken-down propolis.

4. A method according to any of the preceding claims, characterised in that it comprises the process step of spreading the broken-down propolis on a porous tray at a thickness of 2-3 cm.

5. A method according to Claim 4, characterised in that it comprises the process step of spreading the broken-down propolis on a porous tray, and then heating it up to 50-80C° in a heater.

6. A method according to any of the preceding claims, characterised in that it comprises the process step of reducing the amount of removed wax to %20 or below.

7. A method according to any of the preceding claims, characterised in that it comprises the process step of setting the H⁺ ion concentration of the solvent mixed with the propolis, from which the wax was removed, to the range of 10⁸-1 O ¹⁰.

8. A method according to any of the preceding claims, characterised in that it comprises the process step of mixing the propolis and the solvent mixed with the propolis from which the wax was removed, for 30-60 minutes at 40-60 °C temperature, under minimum 3-bar pressure, in a homogeniser operating at a speed of 3000-7000 revs/min.

9. A method according to any of the preceding claims, characterised in that it comprises the process step of setting the phenolic substance amount of the extract to the range of 10,000-50,000 mg GAE/L, and as containing a number of flavonoid substances in the range of 10-150.

9. A method according to any of the preceding claims, characterised in that it comprises the process step of centrifuging the extract for 30-40 min at 4,000-8,000 revolutions.

10. A method according to any of the preceding claims, characterised in that it comprises the process step of filtering the extract by gradually passing it through 100-micron, 50-micron and 10-micron filters.

11. A method according to any of the preceding claims, characterised in that the water-based propolis product is filled at the filling machine by being dosed into disposable air- and light-proof packages.

12. The propolis product obtained through the method that is according to any of the preceding claims.