JP4574742B1 - Propolis composition - Google Patents

Abstract

Provided is a propolis composition that contains only one type of composition component other than propolis extract, has no air bubbles, contains an active component of propolis at a high concentration, has good fluidity, and does not precipitate components. A method for producing the propolis composition is provided in a simple process.
A propolis composition comprising a propolis extract and a cellulose derivative. A first step of extracting the propolis bulk with a hydrophilic organic solvent and solid-liquid separation of insoluble matter to obtain a propolis extract; a second step of preparing a cellulose derivative solution by diluting the cellulose derivative with a hydrophilic organic solvent; And a third step of concentrating and preparing a mixed solution obtained by adding and mixing the cellulose derivative solution to the propolis extract, and a method for producing a propolis composition.
[Selection figure] None

Description

The present invention relates to a propolis composition, in particular, the active ingredients of propolis contained at a high concentration, is directed to a uniform propolis composition may system fluidity.

  Propolis is a dark brown gluey or waxy substance collected from beehives, including resin, flower buds, pollen, essential oils, bee secretions, etc., and is a parent of flavonoids, polyphenols, terpenoids, etc. Contains oily components, hydrophilic components such as organic acids and polysaccharides, vitamins, minerals, etc., and may have useful effects such as antibacterial action, antioxidant action, anti-inflammatory action, immunoregulatory action, anticancer action Are known. Propolis is applied to the nest entrance in the bee society and has an important role in preventing the entry of foreign enemies, reinforcing and maintaining the nest and disinfecting the nest, and has been used as a folk medicine mainly in Eastern European countries. There is a history. Since many of the active ingredients of propolis are insoluble in water, when used as a health food, propolis is extracted with ethanol or the like and taken as a propolis extract (tincture type) or a preparation (tablet, hard capsule, soft capsule).

  When propolis is continuously ingested as a health food, it is desirable if a preparation containing a high concentration of the active ingredient of propolis can be ingested, since the useful action of the active ingredient of propolis can be enjoyed only by ingesting a small amount of preparation each time. However, when the propolis extract is highly concentrated, the propolis extract extracted with ethanol or the like is concentrated to a high concentration, but the concentration causes precipitation of components and the system becomes non-uniform, producing a formulation such as a soft capsule. When trying to do so, it becomes difficult to produce a uniform preparation. Therefore, conventionally, there has been proposed a propolis composition containing an active ingredient of propolis at a high concentration and having a uniform system without precipitation of the ingredient. For example, there is a propolis composition obtained by reacting an enzyme with a composition of propolis extract, fat and oil and lysolecithin having a specific fat content (see Patent Document 1). Moreover, there exists a propolis composition which contains a propolis extract and saponin, improves dispersibility in water, and does not precipitate insoluble components in water (see Patent Document 2).

Japanese Patent Laid-Open No. 10-327803 JP-A-6-197734

  However, a propolis composition containing an active ingredient of propolis at a high concentration is preferable because the composition component other than the propolis extract is less likely to prevent the action of the composition component. However, the propolis composition described in Patent Document 1 is a propolis composition. In addition to the extract, three kinds of composition components are included. Moreover, the manufacturing process of a propolis composition is complicated. Furthermore, since the propolis composition described in Patent Document 2 contains saponin, the dispersibility in water is improved, but it may be foaming and difficult to use.

The present invention has been made in view of the above circumstances, and contains only one type of composition component other than the propolis extract, has no air bubbles, contains an active component of propolis at a high concentration, has good fluidity, and precipitates the component. It is an object of the present invention to provide a propolis composition that does not occur .

The inventors of the present invention have made various studies to solve the above problems and have arrived at the present invention. That is, the present invention is obtained by concentrating the mixture was added and mixed hydroxypropylcellulose propolis extract, propolis composition content of hydroxypropyl cellulose and said 0.06 to 0.33 wt% der Rukoto Is the gist.

  According to the propolis composition of the present invention, the mixture obtained by adding and mixing the cellulose derivative to the propolis extract is concentrated, and even if the concentration is increased, insoluble components are not precipitated and the concentrate is not separated. Since it has good fluidity, when it is formulated, it is possible to enjoy the useful action of the active ingredient of propolis only by continuously taking a small amount of the preparation. Moreover, it is not necessary to consider the action of composition components other than the propolis extract, and furthermore, since there is no bubble property, the handleability is good.

  The propolis composition of the present invention is produced by concentrating a mixed solution obtained by adding and mixing a cellulose derivative solution to a propolis extract.

  The propolis used for the propolis extract is not particularly limited, and the production area such as Brazilian, Japanese and Chinese is not limited.

  The solvent used for the extraction of the propolis extract is preferably a hydrophilic organic solvent. Examples of the hydrophilic organic solvent include ethanol, 1,3-butylene glycol, propylene glycol, glycerin, and the like, or a mixture thereof. When propolis is used as a health food, ethanol widely used as a food additive is preferable. The concentration of the hydrophilic organic solvent is preferably 70% by volume (V / V%) or more, and more preferably 80% by volume or more. If the concentration of the hydrophilic organic solvent is less than 70% by volume, the yield of the active ingredient contained in the propolis may be reduced.

  Examples of the cellulose derivative include methyl cellulose and hydroxypropyl cellulose (hereinafter sometimes referred to as “HPC”) that can be used in foods, and HPC that can use ethanol as a solvent is preferable in consideration of the intended use. The cellulose derivative is preferably prepared to 0.1 to 2.0 w / v%, more preferably 0.2 to 0.5 w / v% with the above hydrophilic organic solvent. When the concentration of the cellulose derivative is less than 0.1 w / v%, the amount of the cellulose derivative solution added to the propolis extract increases, and when it exceeds 2.0 w / v%, the viscosity increases and preparation becomes difficult.

  The method for producing a propolis composition according to the present invention comprises a first step of extracting a propolis bulk with a hydrophilic organic solvent, solid-liquid separation of insoluble matter to obtain a propolis extract, and diluting a cellulose derivative with a hydrophilic organic solvent. The second step of preparing the cellulose derivative solution and the third step of concentrating and preparing the mixed solution obtained by adding and mixing the cellulose derivative solution to the propolis extract. That is, the raw propolis bulk is coarsely pulverized, and the soluble components are extracted by refluxing with a hydrophilic organic solvent. The extraction temperature is room temperature to 90 ° C, preferably 50 to 70 ° C. When the extraction temperature is less than room temperature, the yield of the active ingredient contained in the propolis is lowered, and when it exceeds 90 ° C., the active ingredient may be denatured. The amount of the extraction solvent used is 2 to 10 times (volume) with respect to the propolis bulk, and preferably 5 to 6 times with respect to the propolis bulk. If the amount of the hydrophilic organic solvent used is less than 2 times, the yield of the active ingredient contained in the propolis may be reduced, and if it exceeds 10 times, the concentration process takes time. The obtained extract is cooled, and the insoluble matter is solid-liquid separated to obtain a propolis extract.

  A cellulose derivative solution prepared in advance is added to and mixed with the obtained propolis extract, and the mixture is concentrated. Even if the concentration of the solid content derived from propolis is increased by concentration, a stable propolis composition having good fluidity and free from insoluble components can be obtained. The good flowability of the propolis composition means a physical property that does not cause trouble because the viscosity is high when the propolis composition is commercialized. For example, the propolis composition is blended in a soft capsule. It refers to fluidity that facilitates work. Further, the content of the cellulose derivative in the final propolis composition is preferably 0.01 to 5.0% by weight (w / w%), more preferably 0.05 to 0.08% by weight. When the cellulose derivative content is less than 0.01% by weight, the fluidity of the propolis composition is improved, but the solid content concentration in the propolis composition is increased, and insoluble components may be precipitated, exceeding 5.0% by weight. In addition, the fluidity of the propolis composition becomes poor and difficult to handle.

  The method for concentrating the mixture of the propolis extract and the cellulose derivative solution is not particularly limited as long as the extract can be removed, and examples thereof include an atmospheric concentration method and a vacuum concentration method.

  The dry residue, that is, the solid content of the concentrated propolis composition is preferably 40 to 80% by weight (w / w%), more preferably 50 to 70% by weight. If the solid content of the propolis composition is less than 40% by weight, the active ingredient in the propolis composition is reduced and the amount of the final preparation increases, so the amount to be consumed increases, and if it exceeds 80% by weight, the viscosity increases. However, the fluidity becomes poor, so that it becomes difficult to handle and sometimes solidifies.

  The propolis composition of the present invention can be filled into a soft capsule and formulated into a powder, or powdered using various auxiliaries such as excipients, or formed into tablets or pills. When formulated, since the active ingredient of propolis is contained at a high concentration, it is possible to enjoy the useful action of the active ingredient of propolis even if the amount of the preparation taken every time is small.

  EXAMPLES Next, although an Example is given and this invention is demonstrated, this invention is not limited to a following example.

[Example 1] (Production of propolis composition (1))
(Manufacture of propolis extract)
200 g of Brazilian propolis bulk was coarsely pulverized, 1 L of 95% by volume primary ethanol was added thereto, and reflux extraction was performed with an extractor-concentrator for 2 hours. After extraction, the mixture was refrigerated overnight, and the insoluble material was separated into solid and liquid to obtain 900 mL of a propolis extract having a solid content of 10.1% by weight.

(Production Example 1-1)
Take 200 mL of the propolis extract obtained above, add 50 mL of 1 w / v% HPC (Nippon Soda Co., Ltd .: Cerney H) dissolved in 95% by volume primary ethanol, and add the resulting mixture to the rotary evaporator. And 40 g of a propolis composition having a solid content of 47.8% by weight was obtained. The concentration of HPC in the propolis composition was 1.25% by weight.

(Production Example 1-2)
Take 200 mL of a portion of the propolis extract obtained above, add 50 mL of 0.5 w / v% HPC (Nippon Soda Co., Ltd .: Cerney H) dissolved in 95% by volume primary ethanol, and rotate the resulting mixture. Concentration under reduced pressure using an evaporator gave 40 g of a propolis composition having a solid content of 46.7% by weight. The concentration of HPC in the propolis composition was 0.63% by weight.

(Production Example 1-3)
Take a 200mL portion of the propolis extract obtained above, add 25mL of 0.5w / v% HPC (Nippon Soda Co., Ltd .: Cerney H) dissolved in 95% by volume primary ethanol, and rotate the resulting mixture Concentration under reduced pressure using an evaporator gave 37 g of a propolis composition having a solid content of 65.1% by weight. The concentration of HPC in the propolis composition was 0.33% by weight.

  The propolis compositions of Production Example 1-1 to Production Example 1-3 all had stable physical properties with good fluidity and no insoluble components were precipitated. The fluidity of the propolis composition was best in Production Example 1-3, followed by Production Example 1-2 and then Production Example 1-1. Since all of the production examples had good fluidity, they could be easily blended for soft capsule preparations.

Regarding Production Example 1-1 to Production Example 1-3, p-coumaric acid, standard component content (equivalent to p-coumaric acid) was changed from Japan Health and Nutrition Food Association “Propolis Food Standards Standards; The measurement was performed according to “Partial revision standard component content” on May 15. Artepilin C was also measured under the same conditions. p-Coumaric acid and artepiline C are the content per dry residue (solid content). The p-coumaric acid equivalent amount refers to the concentration (w / w%) of the total dry residue (solid content) converted to the weight of p-coumaric acid. The HPLC conditions are as follows.
Liquid chromatographic conditions Pump: PU-2089 PLUS (JASCO) Flow rate 1.2mL
Column: SUPELCOSIL 5-9196 15cm × 4.6mm × 5μm (SUPELCOSIL)
Column oven: CO-2060 PLUS 50 ℃ (JASCO)
Detector: UV275nm UV-2075 (JASCO)
Injection volume: 10μL
The results are shown in Table 1.

  When the propolis extract of Table 1 is compared with the dry residue in the production example, and then the concentration of p-coumaric acid, standard component content (equivalent to p-coumaric acid), and Artepilin C are compared, the production example is p-coumaric. It can be seen that the acid, standard component content (equivalent to p-coumaric acid), and artepilin C are concentrated without deteriorating.

[Example 2] (Production of propolis composition (2))
(Manufacture of propolis extract)
In order to further improve the fluidity of the propolis composition containing the active ingredient of propolis at a high concentration, a pilot test in which the amount of HPC added was reduced was conducted. 15 kg of Brazilian propolis bulk was coarsely pulverized, 75 L of 95% by volume primary ethanol was added thereto, and the mixture was refluxed and extracted for 2 hours in a stirring tank of an extraction and concentration apparatus. After extraction and storage in the refrigerator overnight, the insoluble matter was separated into solid and liquid to obtain 45 L of propolis extract having a solid content of 9.9% by weight.

(Production Example 2-1)
To the above propolis extract, 2.625 L of 0.2 w / v% HPC (Nippon Soda Co., Ltd .: Celny H) dissolved in 95% by volume primary alcohol was added, and the resulting mixture was concentrated under reduced pressure to obtain a solid content of 70.8 8210 g of a weight percent propolis composition was obtained. The concentration of HPC in the propolis composition was 0.06% by weight. Even when the obtained propolis composition was carried out on an actual pilot scale, insoluble components did not precipitate, the system was stable, the fluidity was good and the physical properties were easy to handle.

  For Production Example 2-1, p-coumaric acid, standard component content (equivalent to p-coumaric acid), and Artepiline C were measured in the same manner as in Example 1.

  From Table 2, it can be seen that Production Example 2-1 is concentrated without deteriorating p-coumaric acid, standard component content (equivalent to p-coumaric acid), and Artepillin C. Even when the solid content in the propolis composition was as high as 70% by weight, it was possible to prepare a propolis composition having a stable liquid and improved fluidity.

Example 3
Hereinafter, although the compounding example of the propolis composition of this invention is given, this invention is not limited to the said compounding example.
(Formulation example 1) Soft capsule Propolis composition (solid content 70% by weight) 80mg
Safflower oil 190mg
Beeswax 15mg
Glycerin fatty acid ester 15mg
<Wrapping material>
Gelatin, glycerin

(Formulation example 2) Pills Propolis composition (solid content 60% by weight) 77mg
Propolis composition powder 157.5mg
Rice germ 31.5mg
Soy fiber 28mg
Starch 21.5mg
Shortening 17.5mg
Rice bran 7mg
Maltose extract

  In addition, it is not limited to the above-mentioned propolis that the cellulose extract can be used to produce a concentrated extract, but can also be applied to an ethanol preparation concentrate of herbal extracts such as corn, ginger, ginseng and elephant. For example, 600 mL of 95% by volume primary ethanol was added to 100 g of dried bean paste, reflux extraction was performed for 2 hours, and 550 mL of a liquid filtered through a nylon cloth was obtained. Of these, 200 mL of the solution concentrated under reduced pressure using an evaporator left a precipitate for 1 day.However, a solution obtained by adding 50 mL of 0.5 w / v% HPC to 250 mL of umami extract and concentrating the dry residue to 2 wt% It became a uniform liquid with a little viscosity. In addition, no separation was observed after 1 week of standing.

The propolis composition of the present invention is useful in the field of health foods and cosmetics because it contains an active ingredient of propolis at a high concentration and does not precipitate insoluble components with good fluidity .

Claims (1)

It is obtained by concentrating the mixture was added and mixed hydroxypropylcellulose propolis extract, propolis composition content of hydroxypropylcellulose is characterized from 0.06 to 0.33 wt% der Rukoto.