KR20040043319A - The process of making food additive using propolis - Google Patents

Abstract

PURPOSE: A method of producing a food additive by extracting propolis in a solvent of distiller's dried grain with solubles(alcohol) and distilled water and then removing wax from the extract is provided. The produced food additive is not sticky or coagulated while maintaining good palatability and thus can be applied to various food and beverage products. CONSTITUTION: Propolis is finely ground, mixed 3 times with distiller's dried grain with solubles(alcohol) and extracted after refluxing 3 times for 3hr. Thereafter, the extract is filtered at 12hr intervals while storing for 3hr in a freezing chamber at -20deg.C, the filtrate is concentrated in a vacuum concentrator. Candies and beverages contain 0.5 to 2.0% by weight and 0.04% by weight of the propolis food additive, respectively.

Description

The process of making food additive using propolis

The present invention relates to a method for producing food additives using propolis, and more particularly, a method for extracting active ingredients from propolis ingot using alcohol (alcohol) and less provocative odor peculiar to propolis, It relates to an extraction method using water as a solvent in order to take advantage of convenient taking.

The origin of propolis is derived from the Greek word, which is a combination of pro and urban polis, which is used by bees to protect the beacon from bacterial contamination.

Propolis has a characteristic scent like a mixture of cinnamon, vanilla, etc., 50% to 55% resin and fragrance, 25% to 35% beeswax, 10% pollen, 5% organic and It is composed of inorganic materials.

The main components of propolis are flavonoids, which vary depending on the type of plant from which the resin is collected and the location of harvest.

As a physical property of propolis, specific gravity is 1.127, and it is easy to be broken into solid state at 15 ℃ but becomes soft at 30 ℃, and starts to dissolve above 60 ℃.

Propolis is a substance used by honeybees to strengthen their rooms, such as the gaps in the honeycomb, to preserve honey. It is made from the salivary secretions of bees containing hard resin, beeswax and various enzymes collected from trees. Unlike insects, harmful germs and viruses are not found at all, and it is estimated that pathogens and viruses are sterilized without knowing that honey bees are always in contact with propolis.

On the basis of this fact, the possibility of antimicrobial properties of propolis was found out and it is known to have various pharmacological effects and has been used as a folk remedy for the treatment of allergic rhinitis, asthma and dermatitis from all over the world.

In addition, in Eastern Europe, it is widely used for antiseptic, bacteriostatic, astringent, jingyeong, anti-inflammatory and anesthetic effects, ranging from cosmetics, health foods and toothpaste components. Especially in dermatology, wound treatment, tissue regeneration, burns, and neurodermatitis. It is also used for psoriasis, herpes, and bacterial eczema.

Propolis has generally been extracted and used by organic solvents such as ethanol, but in recent years, extracts using supercritical carbon dioxide or extracts using water have been utilized. The results of research on the difference in efficacy have been published.

As a technology for processed products using conventional propolis, Korean Patent No. 90-7005 proposes a method of preparing propolis extract using ethanol and using it as a bee flavour. As an example of commercializing propolis, Montana Co., Ltd. Propolis creams, propolis sprays, and propolis hard capsules are available.

Propolis is a useful food material that contains various vitamins, inorganic ingredients, various flavonoids, betulen, betulenol, isovanillin and aromatic unsaturated acids, but it has very low solubility in water and turbidity occurs when water is added. At the same time, solid lumps were formed, adhered to the base wall, and the formation thereof was very difficult to be edible, making it difficult to develop into a product.

In addition, ethanol extract contains a lot of ethanol, so it is difficult to develop it as processed food, and if alcohol is contained in food, the tax must be paid. When taking the extract as it is, it is lost due to tangling to the wall of the cup. There was a lot, even if taking the problem was very uncomfortable to take the adsorbed on the ceiling and teeth of the mouth.

In order to solve the above problems, the present invention provides a method for optimizing the extraction conditions of the active ingredient, and also remove the wax that is stuck to the ceiling and teeth or turbidity occurs when taking.

1 is a flavonoid of 100% alcohol extract of propolis analyzed using high performance liquid chromatography

Figure 2 is flavonoids of propolis-water extract analyzed using high performance liquid chromatography

Figure 3 is a polyphenolic compound of 100% alcohol extract of propolis analyzed using high performance liquid chromatography

4 is a polyphenolic compound of propolis water extract analyzed using high performance liquid chromatography

Figure 5 shows the nitrite scavenging activity according to the concentration, pH of propolis water extract

Propolis alcohol extract has an excellent antioxidant effect, including the effect of preventing the oxidation of edible fats and oils, and also has the effect of inhibiting the formation of carcinogens such as nitrite scavenging action, and water extracts can cause food poisoning in humans. There is an excellent antimicrobial activity against bacteria, namely Bacillus cereus, Staphylococcus aureus, Vibrio parahemorariticus, and also has a high antimicrobial activity against Streptococcus mutans bacteria that cause tooth decay.

The physiological activity of the extract as described above is determined by the polyphenol component contained in the extract, flavonoids and polyphenol components were identified by high-speed liquid chromatography, and the contents of the present invention will be described in detail through test examples and examples. .

Example 1 Preparation of Alcohol Extract

1 kg of propolis ingot was finely ground, and the extract prepared by three times reflux extraction at 70 ° C. for 3 hours was stored at -20 ° C. in a freezer for 3 days to remove wax components. The filtrate filtered with a filter at time intervals was concentrated with a vacuum condenser to completely remove the solvent to obtain an alcohol extract.

The recovery amount was 47.85% with respect to the dry powder, and the extract had the unique fragrance component contained in the original ingot.

Example 2 Preparation of Water-Soluble Extract

1 kg of propolis ingot was finely ground with a grinder, and the extract prepared by refluxing three times at 90 ° C. for 3 hours with distilled water of 10 times was stored at -20 ° C. freezer for 3 days to remove wax components. The filtrate was filtered through a filter at 12-hour intervals and concentrated under reduced pressure to obtain a water-soluble extract. The yield was 10% with respect to the dry powder of propolis, and the extract was reddish brown. Had.

Test Example 1: Analysis of various flavonoids

Fravonoid compounds showing various physiological activities such as anti-cancer, antioxidant, anti-cavity and antifungal effects were analyzed using 100% alcohol extract and propolis extract.

1 and 2 are added to 5 mg of ethanol and 6M hydrochloric acid to 500mg of propolis 100% alcohol extract and water extract and then cooled to reflux for 2 hours in a 95 ℃ water bath.

The extract was analyzed by high-performance liquid chromatography using 50 ml of a flask and a 50 ml round bottom flask with 50% ethanol. Table 1 below shows the amount of flavonoids in the propolis extract.

Unit: mg / g 100% alcohol extract Water extract One Mycetin 0.09 1.17 2 Quercetin 0.23 1.17 3 Apigenin 0.77 0.27 4 Camperol 1.04 0.54 Total Full Lavonoid Content 2.13 3.15

Test Example 2 Analysis of Various Polyphenol Compounds

Figures 3 and 4 show that in order to analyze various polyphenolic compounds contained in 100% alcoholic extracts of Ppopolis and water extracts, 500 ml of each extract was mixed with 100 ml of distilled water and 100 ml of epiacetate in a separatory funnel. After repeating this process three times, the epiacetate extract was combined, anhydrous sodium sulfate was added, the filtrate was completely concentrated with a rotary vacuum concentrator, and analyzed by high-performance liquid chromatography. The amount of polyphenol compound contained.

Unit: mg / g 100% alcohol extract Water extract One Garlic Exid 0.39 9.76 2 Chlorogenic acid 0.39 1.92 3 Catechin Tr 1.05 4 Epigallocatechin gallate 0.43 0.61 5 Epicatechin 0.18 1.52 6 Epicatechin gallate 0.09 1.42 Total Polyphenol Compound Content 1.48 16.28

Test Example 3: Antioxidant Test of 100% Alcohol Extract of Popopolis

The propolis extract prepared according to Example 1 was diluted at each concentration and used as a material for the antioxidant test.

Using soybean oil as a substrate, 0.1% of propolis alcohol extract was added to 100 g of oil and fat, and then stored at 50 ° C. in a constant temperature, and then flattened in a revolving triangle flask over time to measure peroxide value according to AOCS method.

In other words, add 10 mL of chloroform, 15 mL of acetic acid, and 1 mL of saturated potassium iodide, and shake for 1 minute, leave for 5 minutes in the dark, shake with 75 mL of distilled water, and titrate with 0.01 normal sodium thiosulfate solution. Was measured.

Peroxide value of soybean oil was not significantly different between the control and the control group at the beginning of storage, but from the 8th day, 32.73 meq / kg was added without the sample. meq / kg.

Particularly, after 10 days of storage, the peroxide value of 100% alcohol extract added to propolis was 10.69-18.94 meq / kg, and the fresh state of the initial storage was maintained, while the sample-free added product showed 110.36 meq / kg on the 16th day of storage. Has been shown to inhibit rancidity of fats and oils.

Test Example 4: Nitrite scavenging test of water extract of propolis

Nitrite scavenging activity was measured by adding samples to 1 mL of 1 mM sodium nitrate solution by concentration, and adjusting the pH of the reaction solution to 1.2, 4.0, and 6.0 using 0.1 N hydrochloric acid and 0.2 M citric acid buffer solution. The final volume was set to 10 mL.

After reacting the solution at 37 ° C for 1 hour, 1 mL of each reaction solution was added, 5 mL of 2% acetic acid solution and 0.4 mL of grease reagent were added and mixed well, and the mixture was left at room temperature and absorbance was measured to measure nitrite scavenging activity. It was.

The nitrite scavenging activity was measured by adding the water extract prepared according to Reference Example 2. As a result, the nitrite scavenging activity was 63% when 100 μg was added, and the nitrite scavenging activity was 90% when 500 μg was added. , Showed the highest activity at pH 1.2 of stomach acid (Fig. 5).

Test Example 5: Antibacterial test using propolis 100% alcohol and water extract

The antimicrobial activity was used the paper disk (Ψ8 mm) method.

In other words, the culture medium for each strain was dispensed into Petri dishes to solidify the plate, and 100 μl of the bacteria cultured for 24 hours was plated with a sterile rod to absorb 5 mg of each extract, and then the paper disk on which the solvent of the extract was evaporated was placed on the plate. Placed and cultured according to the culture conditions of each strain was measured and compared the diameter of the inhibitory ring around the disk.

100% alcohol extract showed high activity against Bacillus cereus, Bacillus subtilis and Staphylococcus aureus, whereas water extract caused Bacillus, low temperature bacteria Listeria monocytogenes and Vibrio sepsis. It showed high activity against Vibrio parahemoriaticus bacteria.

Example 1:

Formulation for the preparation of propolis candy was mixed with 450 g and 550 g of starch syrup and sugar, and then concentrated in a vacuum concentrator, and then 100% ethanol extract of propolis 0.5, 1, 2% and weight 1 of syrup and sugar. % And powder were added at a ratio of 1%, mixed, injected into a mold, cooled, and then separated from the mold to prepare a candy.

Propolis Candy

Formulation example (% by weight) Candy containing 0.5% of extract Candy with 1% extract Candy with 2% extract Candy containing 1% of powder + 1% of extract Sugar 55% 55% 55% 55% corn syrup 45% 45% 45% 45% Propolis 100% Alcohol Extract 0.5% 1.0% 2.0% 1% powder, 1% extract

When the candy is prepared by blending the raw materials, it is possible to obtain a candy effective for antioxidant, anticancer and antimicrobial activity.

Example 2:

To prepare a propolis drink, 400 ml of propolis water extract was used, and the first extract was used as an herbal extract, an apple concentrate, an auxiliary ingredient, citric acid as an acidifier, oligosaccharide as a sweetener, liquid fructose, sugar, xylitol, and honey. After preparing the prototype, the sensory test was conducted several times to select the four components and ratios of the final prototype in consideration of formulation suitability, manufacturing characteristics and quality characteristics.

Propolis Beverage Manufacturing

Formulation example (% by weight) A B C D Apple Juice Concentrate 4.0% 4.5% 5.8% 5.8% Jujube extract - 2.7% 2.1% 2.1% honey 3.5% - - - oligosaccharide 2.8% 3.4% 2.9% 2.9% Liquid fructose 1.0% 3.9% 2.5% 5% Sugar 2.0% 2.5% 3.8% - Xylitol 0.1% 0.2% 0.3% 0.3% Citric acid 0.015% 0.014% - -

When the beverage was prepared by blending the raw materials, a beverage having excellent aroma and functionality unique to propolis could be obtained.

Food additives using the propolis prepared by the present invention can be used in a variety of food and drink products without difficulty due to the phenomenon of forming or sticking solid lumps while maintaining a good palatability.

Claims (4)

Finely grinding the propolis collected from the honeycomb after drying; Mixing three times the weight of the spirits with respect to the ground propolis; Extracting the solution after refluxing three times for three hours after alcohol mixing; Removing the wax by filtration with a filter at 12 hour intervals while keeping the extract in a freezer at -20 ° C. for 3 days; Concentrating the filtered solution in a vacuum condenser to remove the solvent comprising a method for producing a food additive using a propolis. The candy according to claim 1, wherein the propolis additive contains 05 to 2.0% by weight. Finely grinding the propolis collected from the honeycomb after drying; Mixing 10 times the amount of distilled water with respect to the ground propolis; Mixing distilled water and refluxing three times at 90 ° C. for three hours to extract the solution; Removing the wax by filtration with a filter at 12 hour intervals while keeping the extract in a freezer at -20 ° C. for 3 days; Concentrating the filtered solution in a vacuum condenser to remove the solvent comprising a method for producing a food additive using a propolis. 4. A beverage according to claim 3, wherein the propolis additive contains 0.04% by weight.