KR100514123B1 - Preparation for water-soluble propolis extracts - Google Patents

Abstract

The present invention extracts the sealed bridge bridge using a solvent containing ethanol, precipitates the insoluble resin component by heating and concentrating with water, and then cools it again to solidify the resin component and remove the suspension. It is related with providing the method of obtaining the water-soluble transparent propolis extract obtained by adding ethanol to an aqueous solution, adding and mixing alumina, filtering, and centrifuging.

Description

Preparation method of water soluble propolis extract {Preparation for water-soluble propolis extracts}

 Propolis is derived from the Greek word. Propolis is a combination of pro, meaning city, and polis, meaning city, which is a bee building and secreting it to prevent the invasion of pests and bacteria from the outside and to prevent infection.

The main ingredient of propolis is flavonoid, which is yellow to yellowish green depending on the type of tree to be collected. It contains cinnamic acid and kumaric acid and has a unique fragrance. It contains more than 50% of resin component, which is very viscous and hygroscopic. Have Propolis is known to contain excellent functional ingredients since ancient times and has been used in the treatment of various diseases in the public.

Propolis is a substance used by bees to prevent and strengthen honeycomb gaps and protect them from the outside. It is a salivary secretion of bees containing resin, beeswax and various enzymes collected from trees. And insect resistance.

Generally, propolis extracts are made by extracting the barley collected from the honeycomb with alcohol or water and mixtures thereof to obtain a dissolved component. Baek-Seok et al. Proposed a method for preparing a liquefied propolis extract using lipase, sorbitol, and alcohol in Korean Patent Publication No. 10-1997-0039866, and Yuhan Corporation propolis that is difficult to be water-soluble in Korean Patent 10-1992-0014532. The method of preparing a propolis extract with a water solubility is added to the extract of cyclodextrin, and Korean Patent No. 90-7005 proposes a method for preparing a propolis extract using ethanol and using it as a honeycomb fragrance. Seibutsu Chemical Co., Ltd. presents a preparation method of extracts extracted by the method of setting the pH of the solution to 5.5-7.0 in Korean Patent Publication No. 10-1997-0011639, and Korea Ginseng Research Institute in Korea Patent 10-1998-0022075 Propolis extract with high solubility by adding solvate and lecithin Has been proposed a method, such as choechangha presents a manufacturing method of the Republic of Korea accommodate the addition of the protease, lipase, cellulase, Pectinase dehydratase such as in Patent 10-1996-0030725 liquid extract. In addition, US Pat. No. 6,153,228 suggests a method for preparing a propolis extract from which a strong odor is removed.

Propolis contains various vitamins, minerals, flavonoids, aromatic unsaturated compounds, and so on, and its solubility in water is not easy to process for food. Among the solvents that can dissolve it, it is possible to use edible alcohol as an alcoholic beverage. It can be easily dissolved and obtain a very transparent dark brown extract, but since ethanol is contained in the solvent, it has become a lot of restriction for use in food. In addition, in the presence of ethanol, in the presence of ethanol, when dissolved, or ingesting an ethanol state containing these resin components, it was very inconvenient to dissolve in the mouth and adhere to the teeth. .

In order to solve the above problems, the present invention provides a method for obtaining a transparent propolis extract in aqueous solution by removing the resin components contained in the propolis extract causing various inconveniences.

In the present invention, the rod bridge obtained from the honeycomb is extracted for 1 to 3 hours at 60 to 80 degrees Celsius using an ethanol solvent of 70 to 95% (v / v) to dissolve and extract the components dissolved in ethanol. 1 to 3 times the volume of water was added, and concentrated under vacuum to remove ethanol to a volume of 1/3, cooled to 0 to 4 degrees Celsius to remove the beeswax component formed by precipitation in the upper layer, and again obtained 0.5 ~ 3 times of the volume of the extract is concentrated and vacuum concentrated to remove the ethanol by evaporation, cooling it to below 20 degrees Celsius or less to remove the precipitated resin component, and the particle size is 100 ~ 500. 1-5% (w / v) of micron porous alumina was added, mixed at room temperature, filtered, and ethanol was added to the extract obtained by centrifugation again to a concentration of 15% (v / v) or less to improve transparency. It constitutes the present invention by a method of obtaining a propolis extract of transparent water-soluble.

The rod bridge obtained from the honeycomb contains various foreign substances and must be extracted with an appropriate solvent. For this purpose, ethanol, which is edible ethanol, is used to make the concentration of ethanol at 70-96% (v / v), add it to the volume of 1-5 times the weight of the rod bridge, and warm it to 60-90 degrees Celsius, and then 1 ~ While stirring for 3 hours, the propolis component soluble in ethanol is extracted. Ethanol has a drawback that the yield is remarkably lowered when it is less than 70% (v / v) and the fat-soluble components are not dissolved. 96% (v / v) is currently the highest concentration that can be obtained for food in Korea, and 99% ( v / v) above edible anhydrous ethanol is no problem using it. At this time, the boiling point of ethanol is 78 ~ 79 degrees, so if the 90 degrees Celsius some pressure occurs, the vessel must be able to withstand the pressure. The reason for warming is to increase the solubility and to accelerate the dissolution. After the extraction process, this is filtered to remove insoluble foreign matter, and then 1 ~ 3 times of water of the obtained filtrate is added and mixed, and then concentrated in vacuo so that the volume is 1/3. In this process, most of the ethanol is removed by evaporation with water. Concentration by adding water is to reduce the concentration of ethanol to completely remove the beeswax components. The volume of water added before concentration depends on the concentration of ethanol in the extract, but add water so that the total ethanol concentration is 30-50% (v / v). This is because if the concentration of ethanol is too high, the wax component is completely dissolved and it is difficult to remove it completely even if it is supercooled. If the concentration of ethanol is too low, the resin component, etc., in addition to beeswax, elutes at once, so that the yield of the water-soluble component is lowered. The concentrated solution obtained by adding water is ethanol content of 5 ~ 30% (v / v) level is cooled to 0 ~ 4 degrees Celsius to remove the beeswax component precipitated. This is because the beeswax components dissolved and extracted in ethanol are removed as ethanol is removed in the concentration process, so that the solubility is reduced and precipitated. This is filtered off, and again, 1 ~ 3 times of the concentrate is added to water, and then concentrated in vacuo to make the volume less than 30% (v / v) of the volume before concentration, and then the contents do not freeze below 20 degrees Celsius. The resin component separated by cooling to a degree is filtered off. This is because the ethanol component contained in the extract is evaporated with water by azeotropic action and the resin components in the remaining solution are precipitated and removed by precipitation due to the lower concentration of ethanol. The resin component is dark brown to black and becomes a very sticky liquid with fluidity above 40 degrees Celsius. However, when cooled to 20 degrees Celsius or less, the resin becomes semi-solid and can be easily removed. If it is not cooled, the resin components are in a liquid phase, which not only easily filters the filter, but also has good fluidity, such that complete filtration is not easy and requires a long time. Cooling temperature is less than 20 degrees Celsius so that the contents do not freeze. The contents do not freeze at 0 degrees Celsius because they contain small amounts of ethanol. Therefore, it can be said that the temperature to cool is 20 degrees Celsius or less and 0 degrees or more. To the suspension obtained in the filtrate, 1-5% (w / v) of porous alumina having a particle size of 100 to 500 microns was added and mixed at room temperature, followed by filtration and centrifugation to obtain an extract of the suspension. The concentration is below 15% (v / v) to obtain a completely water soluble clear propolis extract. The reason for adding alumina in the above is to remove the off-flavor of propolis to eliminate the rejection when ingested. The alumina is porous so that strong aromatic components are adsorbed and removed together with the alumina. After addition of alumina, filtration and centrifugation to completely remove the suspended solids, the extract becomes a suspension phase. Adding a small amount of ethanol breaks down the emulsion in the suspension, resulting in a clear, water-soluble propolis extract. The added ethanol is 15% (v / v) or less in total concentration. This is because the ethanol content of the product finally obtained when the excess ethanol is added causes problems as a food, and ethanol is to add the minimum amount to make the suspension transparent.

Propolis extract obtained by the above method is a completely water-soluble transparent extract to remove the off-flavor having a sense of rejection when ingestion is very easy to take propolis extract can be utilized for a variety of uses, such as edible and pharmaceutical.

Hereinafter, the present invention will be described through examples. However, the examples do not limit the scope of the present invention.

Example 1

2kg of alcohol and water were added to 1kg of Bongyo and added to 2L, and mixed for 3 hours at 80 degrees Celsius. This was filtered through a filter paper to remove insoluble components and 2.2L of the filtrate. To this was added 3.3 L of water and concentrated in vacuo to finally reach a volume of 1.3 L. This was cooled for 4 hours at 2 degrees Celsius to remove white or off-white beeswax that precipitated on top. 1.5L of water was added thereto, and the resultant was concentrated in vacuo to finally reach 2L, and then cooled to 20 degrees Celsius to remove dark brown or black resin components precipitated at the bottom by precipitation, and the upper layer suspension was collected to obtain 1.3L. . . 30 g of porous alumina of 100-500 microns was added thereto and mixed for 3 hours. This was centrifuged at 2,000 rpm for 10 minutes to separate the supernatant to obtain 1.2 L of suspension. 100 ml of alcohol was added thereto to make the suspension transparent and 1.3 L of the final extract was obtained. The extract thus obtained was easy to ingest with little odor causing rejection and complete water solubility.

The present invention relates to a method for producing a propolis extract having a variety of pharmacological functions, so that the existing extracts using ethanol as a solvent in a state that does not remove it completely solves the inconvenience such as adsorption on the teeth when ingested Since it eliminates off-flavor and has a sense of rejection when ingested, it is possible to contribute to the improvement of health as it is widely used as a material of food and medicine as an extract with various functions of propolis.

Claims (3)

Extraction by adding a mixture of water and ethanol to the Bong bridge as a solvent, adding water to it, vacuum concentration to evaporate ethanol and cooling it to remove beeswax, and adding water and vacuum concentration to remove ethanol and cooling to precipitate As a process for producing a propolis extract obtained by the step of removing the resin to be removed, the step of removing the odor component by adding porous alumina and the step of adding ethanol to the obtained suspension to destroy the emulsion to obtain a transparent liquid, a) the concentration of ethanol in the extraction process is 70-95% (v / v), the extraction temperature is 60-80 degrees, the extraction time is 1-3 hours, b) In the beeswax removal process, 1 ~ 3 times of water is added to the filtrate obtained in the extraction process, and concentrated in vacuo to remove ethanol by reducing the volume to 1/3 or less, and cooling it to 0 ~ 4 degrees Celsius to solidify the beeswax component to the upper layer. Is a process of precipitation and removal, c) In the resin component removal step, 0.5-3 times of water is added to the filtrate obtained in the beeswax removal process of b), concentrated in vacuo, and evaporated to remove ethanol, and cooled to not freeze below 20 degrees Celsius to solidify the resin component. Is the process of removing d) removing the off-flavor components, adding 1-5% (w / v) of porous alumina with a particle size of 100-500 microns to the suspension obtained in the resin component removal process of c), mixing at room temperature, separating and removing Is, e) in the process of making the suspension transparent, adding ethanol to the suspension obtained in d) to break the emulsion to obtain a transparent liquid, and at the same time the concentration of ethanol in the obtained liquid to be 15% (v / v) or less. A water-soluble propolis extract manufacturing process obtained by. delete delete