JP2007135516A - Propolis powder coated product and method for producing the same, and propolis-containing food product - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a propolis powder coated product which prevents the deterioration of useful ingredients derived from propolis and is excellent in temporal stability, to provide a method for producing the same, and to provide a propolis-containing food product. <P>SOLUTION: The propolis powder coated product has a fat-based coating layer having a melting point of 40°C on the surfaces of propolis powder particles. The propolis powder particle has a structure produced by coating the surface of propolis powder with the powder of propolis water extract or with esterified starch. The propolis powder is preferably composed of the powder of a propolis alcohol extract. The method for producing the propolis powder coated product comprises a process for coating the surface of the propolis powder with the powder of a propolis water extract or with esterified starch to prepare the propolis powder particles, and a process for mixing and stirring the propolis powder particles with fatty coating material having an average particle diameter of 0.1 to 50 μm at an impact average load of 0.01 to 10N. A propolis-containing food product contains the propolis powder coated product. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

  The present invention relates to a propolis powder coating useful as a health food material and the like, a method for producing the same, and a propolis-containing food containing the propolis powder coating.

  Propolis bulk is a glue-like substance produced by bees using shoots and resinous substances of various plants as raw materials. Propolis mass has antibacterial and anti-inflammatory effects, as described in Aristotle's Animal Journal compiled in the 4th century BC as “therapeutic agent for skin diseases, cuts and infections” It has been known for a long time, and recently, research results have been reported that components contained in the propolis block are useful for cancer treatment. The propolis bulk contains a variety of useful components such as cinnamic acid derivatives such as p-coumaric acid and artepillin C, flavonoids, other various minerals, and vitamins. In particular, artepilin C, which is a cinnamic acid derivative, is extremely useful because it has high anticancer activity. With regard to propolis, new effects and effects will be discovered in the future, and it is expected to contribute greatly to the promotion of human health.

  Propolis bulk is usually a propolis extract extracted with ethanol, hydrous ethanol, supercritical carbon dioxide, etc. in order to remove contaminants such as dust mixed during collection and to make useful components more efficient. Used as a raw material for health foods, etc. Such propolis extract may be supplied as a liquid product such as a drink, but many are powdered and supplied in dosage forms such as powders and granules, or compressed powders and granules. They are supplied as molded tablets or as capsules filled in gelatin capsules.

  When pulverizing a propolis extract, generally, a method of obtaining a propolis extract powder by mixing an excipient such as starch or dextrin with the propolis extract, followed by hot-air drying or freeze-drying. . However, in the propolis extract powder produced in this manner, when stored for a long period of time, the fluidity of aggregation or solidification frequently occurs and the stability over time is high. It was extremely difficult to maintain the quality for a long time.

  In order to solve such a problem, for example, Patent Document 1 discloses a method for producing a propolis powder in which a powder containing an ethanol extract of propolis and a powder of an aqueous extract of propolis are mixed. In the propolis powder produced by this method, since the powder interstices and the surface of the powder containing the ethanol extract of propolis are intercalated and coated with the powder of the water extract of propolis as a fluidizing agent, respectively, the ethanol extraction It reduces the stickiness (cohesiveness) and solidification (consolidation) of the product, and has high fluidity and processing characteristics.

On the other hand, Patent Document 2 discloses dehydrating and drying a propolis aqueous dispersion obtained by emulsifying and dispersing a mixture of propolis extract and octenyl succinate esterified starch in the presence of water by powerful mechanical stirring. Discloses a method for producing a powdered propolis composition. In the powdered propolis composition produced by the method of Patent Document 2, since the esterified starch adheres firmly to the surface of the propolis particles, the esterified starch covers the surface of the propolis particles. It is easy to disperse in water without forming a resinous condensate.
JP-A-11-9201 Japanese Patent Laid-Open No. 2003-219814

  However, the propolis powder and the powdered propolis composition produced by the methods of Patent Documents 1 and 2 are not sufficient in both stickiness and solidification during long-term storage, leaving room for further improvement. Has been. In particular, when these propolis powders and powdered propolis compositions are filled in hard capsules and stored for a long period of 3 months or more, there is a high possibility that the powder in the hard capsules solidifies. With regard to this type of health food, there is a good possibility that it will be stored for 3 months or more in the store and at the user's store during distribution. There are great expectations from people.

  Furthermore, in the development of a material aimed at improving the storage stability, it is also important to prevent the deterioration of useful components contained in the material. That is, in a powder containing a propolis extract, deterioration of useful components such as Artepillin C is likely to proceed due to ultraviolet rays, oxygen in the air, etc., and thus when producing health foods and the like using such a powder, It is an extremely important issue to maintain the aging stability of these useful components over a long period of time.

  As a result of intensive research under these circumstances, the present inventors have coated the surface of propolis powder particles having a specific composition with a powder of an oil-based coating material having a specific melting point. The present inventors have found that a propolis powder coating capable of maintaining high quality with respect to fluidity for a long period of time can be obtained. Furthermore, in the propolis powder coating obtained in this way, it was also found that deterioration of useful components such as Artepillin C can be effectively suppressed, and deterioration in appearance such as coloring and browning can also be suppressed. . And based on these knowledge, it came to complete this invention.

  An object of the present invention is to provide a propolis powder coating and a propolis-containing food that can suppress deterioration of useful components derived from propolis and are excellent in stability over time. Another object of the present invention is to provide a method for producing a propolis powder coating which can suppress the deterioration of useful components derived from propolis and can easily produce a propolis powder coating excellent in stability over time. There is to do.

  In order to achieve the above object, the invention described in claim 1 is a propolis powder coating having an oil-based coating layer on the surface of the powder particles of propolis, wherein the powder particles of propolis are propolis The surface of the powder is coated with a powder of water extract of propolis or esterified starch, and the greasy coating layer is composed of a greasy coating material having a melting point of 40 ° C. or higher. To do.

  The propolis powder coating according to claim 2 is characterized in that, in the invention according to claim 1, the propolis powder is composed of a propolis alcohol extract powder or a propolis hydrous alcohol extract powder. .

  The propolis powder coating according to claim 3 is the invention according to claim 1 or 2, wherein the powder particles of the propolis and the oil-based coating material are in a weight ratio of 25:75 to 99: It is made to contain in 1 range.

  The invention according to claim 4 is a method for producing the propolis powder coating according to any one of claims 1 to 3, wherein the method is provided on the surface of the propolis powder. The step of preparing the powder particles of the propolis by coating the powder of the water extract of the above or the esterified starch, and 0.01 to 10 N of the powder of the oil-based coating material with respect to the powder particles of the propolis And the step of mixing and stirring at the collision average load, the gist of the oil-based coating material having an average particle diameter of 0.1 to 50 μm.

  The gist of the propolis-containing food according to claim 5 is that it contains the propolis powder coating according to any one of claims 1 to 3.

  According to the present invention, it is possible to provide a propolis powder coating and a propolis-containing food that can suppress deterioration of useful components derived from propolis and are excellent in stability over time. According to the present invention, it is possible to provide a method for producing a propolis powder coating which can suppress the deterioration of useful components derived from propolis and can easily produce a propolis powder coating excellent in stability over time.

Hereinafter, one embodiment which materialized the propolis powder coating material of the present invention, its manufacturing method, and a propolis containing foodstuff is described.
The propolis powder coating of the present embodiment is composed of powder particles of propolis and an oil-based coating layer that covers the surface of the powder particles, and has a granular shape as a whole. In this propolis powder coating, since the powder particles of propolis are physically shielded from ultraviolet rays, moisture and oxygen in the air through the oil-based coating layer, Artepillin C contained in the powder particles Such deterioration of useful components as described above is suppressed, and a decrease in fluidity due to moisture absorption is effectively suppressed. For this reason, the propolis powder coating is excellent in stability over time because high quality is maintained over a long period of time with respect to fluidity and residual ratio of useful components.

  Propolis powder particles contain the propolis bulk or an extract thereof. The propolis bulk contains useful components having various useful physiological functions, including artepilin C. On the other hand, the propolis extract is an extract obtained by carrying out a predetermined extraction step on the propolis bulk to facilitate use (ingestion) of specific components contained in the propolis bulk. Examples thereof include an aqueous extract of propolis, an alcohol extract of propolis, an aqueous alcohol extract of propolis, an organic solvent extract of propolis, a supercritical extract of propolis, and a micellized extract of propolis.

  Incidentally, in this embodiment, for example, the propolis extract is subjected to the first extraction step on the propolis bulk and then the second extraction step on the residue (solid content) recovered after the step. The extract obtained by carrying out is also included. In this case, the extraction solvent used in the first extraction step is different from the extraction solvent used in the second extraction step. For example, it is possible to obtain an alcohol extract by extracting the propolis bulk with water and then extracting the residue (solid content) after the water extraction with alcohol. Included in the concept of propolis extract in form.

  The alcohol used for obtaining the alcoholic extract of propolis and the hydrous alcoholic extract is preferably a lower alcohol such as methanol, ethanol, butanol, propanol or isopropanol. Incidentally, in the alcoholic extract obtained by extracting the propolis bulk with alcohol, chlorogenic acid, p-coumaric acid, caffeic acid, dicaffeoylquinic acid, tricaffeoylquinic acid, dolpanin, flavonoids, artepilin C, baccharin, etc. Contains useful components at high concentrations. An organic solvent extract of propolis can be obtained using a known organic solvent such as acetone or hexane. In this embodiment, propolis ingots of all production areas such as South American countries including Brazil, Asian countries such as China and Japan, European countries, North American countries, Oceania countries and the like can be used.

The propolis powder particles have a structure in which the surface of the propolis powder is coated with a powder of an aqueous extract of propolis or an esterified starch (hereinafter referred to as a coating component).
Propolis powder is formulated to provide propolis-derived useful ingredients such as Artepillin C to the propolis powder coating. Propolis powders include: Propolis bulk pulverized product, propolis alcohol extract powder, propolis hydrous alcohol extract powder, propolis water extract powder, propolis organic solvent extract powder, propolis super A powder of a critical extract, a powder of a micelle extract of propolis, or the like can be used. Any of these propolis powders may be a dry powder product, and the drying method is not particularly limited, and may be dried by any method such as a vacuum drying method, a spray drying method, or a freeze drying method. In addition, the propolis powder may be used alone or in combination of two or more thereof.

  In addition, since propolis powder contains useful components derived from propolis at high concentrations, the propolis bulk pulverized product, the propolis alcohol extract powder, the propolis hydrous alcohol extract powder, and the propolis organic solvent At least one selected from powder of extract, powder of supercritical extract of propolis and powder of micellarized extract of propolis is preferably used, from powder of alcohol extract of propolis and powder of hydrous alcohol extract of propolis At least one selected is particularly preferably used.

  The propolis powders preferably used as listed above contain useful components derived from propolis such as Artepillin C at high concentrations, while being sticky (cohesive) and solidifying due to moisture absorption. It has the property of easily expressing (consolidation). Propolis water extract powder that can be used as propolis powder contains useful components derived from propolis such as Artepillin C at a high concentration, and has high hydrophilicity and hygroscopicity. Even so, it is difficult to cause a decrease in fluidity. Here, as propolis powder, pulverized propolis bulk, powder of propolis alcohol extract, powder of hydrous alcohol extract of propolis, powder of organic solvent extract of propolis, powder of supercritical extract of propolis and Propolis powder coating manufactured using at least one selected from the powder of micelle extract of propolis is used as the first propolis powder coating, and manufactured using the powder of water extract of propolis as the powder of propolis The resulting propolis powder coating is used as the second propolis powder coating.

  The coating component consists of a powder of water extract of propolis or esterified starch. The esterified starch is not particularly limited, but octenyl succinic esterified starch is preferably used. Both the water extract powder and esterified starch of propolis are sparingly oil-soluble, preventing the oil-soluble component in the propolis powder from oozing out into the oil-based coating layer, and the powder of the propolis powder. It makes it easy to form an oil-based coating layer on the surface. Furthermore, all of these coating components have high hydrophilicity and hygroscopicity, and even if they absorb moisture, it is difficult to cause a decrease in fluidity. It exerts the role of suppressing moisture absorption of the powder of propolis and consequently suppressing the expression of the adhesiveness and solidification of the powder particles.

  In addition to the above-described propolis powder and coating components, the propolis powder particles of the present embodiment may contain other components. The other components are not particularly limited, but powders of known excipients such as starch, lactose and dextrin are preferably used in order to facilitate the formation of propolis powder particles.

  Since the propolis powder particles of the present embodiment have the above-described structure, the coating components that have high hydrophilicity and hygroscopicity and do not easily decrease fluidity even when moisture is absorbed are propolis powder and fats and oils. It is interposed between the system coating layers. For this reason, mixing of the powder particles of the propolis and the oil-based coating layer is facilitated, and as a result, an efficient oil-based coating layer can be formed. Furthermore, in this case, before the moisture in the air that cannot be completely blocked by the oil-based coating layer and permeate the oil-based coating layer reaches the propolis powder, the coating component preferentially Since it is adsorbed, the moisture absorption of the propolis powder is suppressed, and as a result, the adhesiveness and solidification of the propolis powder coating are easily suppressed.

  In the present embodiment, the powder particles of propolis preferably have an average particle size of 10 to 350 μm, and particularly preferably have an average particle size of 40 to 280 μm. When the average particle diameter of the propolis powder particles deviates from the above range, it is highly likely that it is difficult to appropriately form a uniform oil-based coating layer on the surface of the propolis powder particles.

  Incidentally, in the propolis powder particles using esterified starch as a coating component, the blending ratio of esterified starch is preferably 0.1 to 1 part by weight of the solid content derived from propolis contained in the propolis powder. 20 parts by weight, more preferably 1 to 10 parts by weight, particularly preferably 3 to 8 parts by weight. When the blending ratio of the esterified starch is less than 0.1 parts by weight relative to 1 part by weight of the solid content derived from propolis, the effect of facilitating the formation of an oil-based coating layer on the surface of the propolis powder particles is sufficiently exerted On the contrary, when it exceeds 20 parts by weight, the content of useful components contained in the propolis powder coating is unfavorably lowered.

The oil-based coating layer is made of powder of an oil-based coating material, and is formed so as to cover the surface of each propolis powder coating.
The oil-based coating material of the present embodiment needs to have a melting point of 40 ° C. or higher in order to prevent an unfavorable situation such as the fusion of the propolis powder coatings in a high temperature environment such as summer. is there. Examples of the oil-based coating materials include animal oils such as beef tallow, pork tallow and fish oil, vegetable oils such as soybean oil, rapeseed oil, cottonseed oil, corn oil and coconut oil, hydrogenated oils of these animal and vegetable oils, rice wax, beeswax, carnauba wax, Waxes such as canderia, fatty acid metal salts, fatty acids, phospholipids, glycolipids, monoglycerides, diglycerides and the like can be used, but vegetable hardened fats and oils are particularly preferably used. These oil-based coating materials may be used alone or in combination of two or more.

  The oil-based coating layer is preferably formed to have a uniform thickness of 1 to 30 μm, more preferably 1 to 10 μm over the entire surface of the powder particles of each propolis. When the thickness (average value) of the oil-based coating layer is less than 1 μm, the effect of physically blocking ultraviolet rays, moisture and oxygen in the air is not sufficiently exerted, and conversely the thickness of the oil-based coating layer ( When the average value) exceeds 30 μm, the content of useful components contained in the propolis powder coating is relatively unfavorable. The oil-based coating material powder preferably has an average particle size of 0.1 to 50 μm. When an oil-based coating material having an average particle diameter outside the above range is used, it is difficult to form a homogeneous oil-based coating layer having the desired thickness described above.

  In the propolis powder coating of this embodiment, the propolis powder particles and the oil-based coating material are preferably contained in a weight ratio of 25:75 to 99: 1. That is, in the propolis powder coating, the content of the propolis powder particles is preferably in the range of 25 to 99% by weight. In this case, it is possible to produce a propolis powder coating with an increased content of useful components while maintaining high fluidity, and to maintain a high residual rate of useful components over a long period of time. It becomes very easy to provide a possible propolis powder coating.

  The propolis-containing food of the present embodiment is a food containing the propolis powder coating. Propolis-containing foods include health food preparations such as capsules such as hard capsules and soft capsules, powder preparations and tableting preparations, beverages dissolved in water and hot water, and other health foods as food ingredients In addition, it can be used by adding to general processed foods.

Next, the manufacturing method of the propolis powder coating material of this embodiment is demonstrated.
The method for producing a propolis powder coating according to the present embodiment includes a step of preparing powder particles of propolis by coating the surface of the propolis powder with a coating component (hereinafter referred to as a preparation step), and the preparation step. And a step of mixing and stirring the powder particles of the propolis prepared in step 1 and the powder of the oil-based coating material (hereinafter referred to as a mixing step).

In the preparation step, the surface of the propolis powder is coated with the coating component by mixing the propolis powder and the coating component according to a predetermined method.
In this embodiment, the powder particles of propolis using the powder of water extract of propolis as a coating component can be prepared by the method of Patent Document 1, for example. In this case, the powder of water extract of propolis is manufactured by pulverizing the water extract of propolis obtained by water extraction of the propolis bulk, or the propolis bulk is extracted with ethanol or hydrous ethanol It is preferable to produce the residue (solid content) obtained by pulverizing a water extract of propolis obtained by further water extraction. In addition, it is possible to add excipients such as dextrin and lactose to the aqueous extract of propolis for pulverization, and a propolis powder coating containing a high concentration of useful components derived from propolis is provided. Therefore, it is preferable not to add an excipient. And the powder of the water extract of propolis after pulverizing in this way can be made into propolis powder particles by being mixed with the powder of propolis by a mixing device such as a food processor.

For pulverization of the water extract of propolis, a direct concentration method by heating at normal pressure, a vacuum concentration method, a spray drying method, a freeze drying method, etc. can be adopted, and a freeze drying method or a spray drying method is preferable. Adopted. In particular, the aqueous powder of propolis obtained by freeze-drying (freeze-dried powder) is a powder having large voids in a packed state, that is, its apparent specific gravity is smaller than those obtained by other drying methods. Become a powder. The apparent specific gravity refers to the apparent weight per unit volume including the gap between powder particles. The apparent specific gravity value is influenced by the filling state of the powder, and is not a value that is uniquely determined, but when the apparent specific gravity of the lyophilized powder is measured without applying vibration or pressure, 0.01 Values in the range of ~ 0.5 g / cm ³ are shown. When the powder of the water extract of propolis having such a small specific gravity is arranged so as to cover the surface of the powder particles of propolis, the oil-based coating layer that is extremely efficient with respect to the surface of the powder particles Can be formed.

  On the other hand, powder particles of propolis using esterified starch as a coating component can be produced by the method of Patent Document 2, for example. In this case, after the propolis powder and the esterified starch powder are both dissolved in water to form a stable aqueous dispersion, the aqueous dispersion is dried and pulverized to obtain the propolis powder particles. Manufactured. In pulverizing the aqueous dispersion, esterified starch having high hydrophilicity forms an interface structure that covers the surface of the propolis powder in the aqueous dispersion. Forms a structure covering the surface of the propolis powder. Note that when the aqueous dispersion is pulverized, a spray drying method or a freeze drying method is preferably employed in order to facilitate the transition of the interface structure to the structure of the propolis powder particles as it is.

  In the mixing step, an oil-based coating layer is formed on the surface of the propolis powder particles. This mixing process is implemented, for example using the stirrer 10 shown in FIG. The stirrer 10 includes a main shaft stirring blade 11 and a sub-shaft stirring blade 12 that stirs in a direction orthogonal to the main shaft stirring blade 11 in the stirring tank 13. Propolis powder particles and oil-based coating material powder are respectively charged, and in the stirring tank 13, the propolis powder particles and the oil-based coating material powder are mixed and stirred while colliding with each other. At this time, the powder of the oil-based coating material is coated on the surface of the powder particles of the propolis, and a uniform oil-based coating layer is formed on the surface of each propolis powder coating.

  In the mixing step, it is preferable that the powder of the propolis and the powder of the oil-based coating material are mixed and stirred under a condition such that a collision average load of 0.01 to 10 N (Newton) is obtained. If the collision average load at the time of mixing and stirring deviates from the above range, it is difficult to form a homogeneous oil-based coating layer having a desired thickness. The collision average load is obtained by the following formula 1.

ただし、上記式中、Ｆは衝突平均荷重（Ｎ）、ｒ_１及びｒ_２はプロポリスの粉体粒子及び油脂系被覆材料の粉末の各粒子の平均半径（ｍ）、ｍ_１及びｍ_２はプロポリスの粉体粒子及び油脂系被覆材料の粉末の各粒子の平均質量（ｋｇ）、Ｙ_１及びＹ_２はプロポリスの粉体粒子及び油脂系被覆材料の粉末の各粒子のヤング率（ｋｇ／ｍ・sec^２）、ν_１及びν_２はプロポリスの粉体粒子及び油脂系被覆材料の粉末の各粒子のポアソン比、Ｖは衝突速度（ｍ／sec）を示す。

In the above formula, F is the collision average load (N), r ₁ and r ₂ are the average radius (m) of the powder particles of the propolis and the powder of the oil-based coating material, and m ₁ and m ₂ are the propolis. The average mass (kg) of each particle of the powder particles and the oil-based coating material powder, Y ₁ and Y ₂ are the Young's modulus (kg / m · sec ² ), ν ₁ and ν ₂ are Poisson's ratios of the propolis powder particles and the oil-based coating material powder, and V represents the collision velocity (m / sec).

  The adjustment of the collision average load differs depending on the types of the stirring blades 11 and 12, but for example, the peripheral speed of the main shaft stirring blade 11 is about 0.1 to 20 m / second, and the peripheral speed of the auxiliary shaft stirring blade 12 is 0.01 to 10 m. / Second can be adjusted. The mixing ratio of the powder of the propolis and the powder of the oil-based coating material is usually selected in the range of 25:75 to 99: 1 by weight, but the preferable mixing ratio is the propolis powder coating. Varies depending on the average particle size.

  That is, when the average particle diameter of the propolis powder coating is R μm, the amount of the oil-based coating material added to the total weight of the propolis powder coating is preferably 300 / R to 3000 / R wt%. When the addition amount of the oil-based coating material is lower than 300 / R, a sufficient thickness of the oil-based coating layer is not formed, so that the temporal stability of the propolis powder coating is lowered. Conversely, when the amount of the oil-based coating material added is higher than 3000 / R% by weight, not only the content of the propolis powder particles is lowered, but also the oil-based coating material is easily consolidated during mixing and stirring. A uniform oil-based coating layer cannot be formed, and as a result, a propolis powder coating that tends to cause deterioration of useful components is produced. Incidentally, the mixing and stirring time varies depending on the stirring conditions and cannot be unconditionally determined, but usually about 30 to 60 minutes is sufficient.

  In the production method of the present embodiment, in order to suppress the deterioration of useful components during production, a cooling gas containing no oxygen as much as possible at 20 ° C. or less, for example, in a cooled nitrogen gas atmosphere or a cooled carbon dioxide atmosphere. Mixing and stirring is preferably performed. As a result, the temperature of the propolis powder can be suppressed to 30 ° C. or lower throughout the mixing and stirring step, and deterioration of useful components due to temperature rise and moisture absorption during mixing and stirring can be suppressed. Thus, a propolis powder coating with an average particle diameter of 50 to 300 μm having a homogeneous oil-based coating layer having a thickness of 1 to 30 μm, preferably 1 to 10 μm, on the surface of the powder particles of propolis is efficient. Well manufactured.

Next, the operation of the propolis powder coating will be described.
The propolis powder coating of this embodiment includes a propolis powder containing a useful component such as Artepilin C at a high concentration. In the first propolis powder coating of the present embodiment, the propolis powder is likely to exhibit adhesiveness and solidification properties due to moisture absorption, and thus tends to cause a decrease in fluidity. On the other hand, in the first propolis powder coating of the present embodiment, since the oil-based coating layer capable of effectively blocking the transmission of moisture, oxygen and light is formed so as to cover the surface, the powder of propolis Are effectively protected from moisture, oxygen and light degradation. As a result, the deterioration of useful components can be suppressed, and the expression of tackiness and solidification of the propolis powder coating can be suppressed to have high fluidity.

  Further, in this propolis powder coating, the coating components (powder of water extract of propolis or esterified starch) are contained in the powder particles of propolis. Since the coating component has high hydrophilicity, it selectively adsorbs moisture that cannot be completely blocked by the oil-based coating layer and permeates the oil-based coating layer, thereby producing a propolis powder. Demonstrates the effective suppression of moisture absorption. As a result, since the expression of tackiness and solidification in the propolis powder is suppressed, it is easy to maintain the fluidity of the propolis powder coating in a high state. In addition, in this propolis powder coating, since the oil-based coating layer has a melting point of 40 ° C. or higher, the particles of the propolis powder coating are hardly fused even in a high temperature environment such as summer. This makes it easy to maintain quality related to fluidity.

  Therefore, the first propolis powder coating is excellent in stability over time because it is easy to maintain high quality over a long period of time with respect to fluidity and residual ratio of useful components. In particular, in this first propolis powder coating, the hygroscopic action on the powder of propolis is doubly blocked by both the oil-based coating layer and the coating components, so that the quality relating to fluidity is maintained at a high level. The effect to do is remarkably excellent. Moreover, since the oil-based coating layer also prevents the propolis powder from being irradiated with light such as ultraviolet rays, it is also possible to suppress undesired coloring such as browning of the propolis powder coating.

  Incidentally, in the case of the second propolis powder coating of the present embodiment, the expression of stickiness and solidification due to the powder of the water extract of propolis as the powder of propolis is hardly caused from the beginning. There is almost no decrease in the fluidity of the powder coating. Therefore, it is easier for the second propolis powder coating to maintain a higher fluidity over a longer period than the first propolis powder coating.

The effects exhibited by the above embodiment will be described below.
-Since the propolis powder coating of this embodiment has an oil-based coating layer on the surface of the propolis powder particles, the moisture absorption of the propolis powder is suppressed, and the propolis powder coating is adhesive and solidified. It is possible to make it difficult to express properties and to effectively suppress deterioration of useful components due to oxygen and light. For this reason, in this propolis powder coating, since it becomes easy to maintain high quality over a long period of time with respect to fluidity and residual ratio of useful components, it is excellent in stability over time. In particular, in the propolis powder coating containing a powder of alcohol extract of propolis or a powder of hydrous alcohol extract that easily develops tackiness and solidification, it has the effect of remarkably suppressing the development of tackiness and solidification. The point is important.

  Furthermore, in the propolis powder coating of this embodiment, since the coating component is disposed on the surface of the powder particles of propolis, the coating component causes the oil-soluble component in the propolis powder to be applied to the oil-based coating layer. Can prevent seepage. In addition, in this propolis powder coating, the high hydrophilicity of the coating component effectively suppresses the moisture absorption of the propolis powder, thereby suppressing the expression of stickiness and solidification due to the propolis powder. In addition, it is easy to maintain the fluidity of the propolis powder coating in a high state. In addition, in the propolis powder coating according to the present embodiment, since the oil-based coating layer has a melting point of 40 ° C. or higher, the particles of the propolis powder coating are fused even in a high temperature environment such as summer. This makes it easy to maintain quality related to fluidity.

  -According to the manufacturing method of the propolis powder coating material of this embodiment, it is possible to form a uniform and thin oil-based coating layer on the surface of the powder particles of propolis very simply and inexpensively. For this reason, in the obtained propolis powder coating, since the powder of propolis existing inside the coating and the outside of the coating are blocked by the oil-based coating layer, moisture absorption due to moisture, oxygen and light and Propolis powder can be effectively protected from deterioration. Accordingly, it is possible to easily produce a propolis powder coating material that can suppress deterioration of useful components and is excellent in stability over time.

  In particular, since the manufacturing method of the present embodiment does not include a step of pulverizing the powder, the propolis powder is not exposed on the surface of the propolis powder coating. For this reason, the coating effect by the oil-based coating layer can be maintained over a long period of time, and a product having a uniform particle size can be easily produced. Moreover, when manufacturing by mixing stirring using the stirrer 10, since the process which heats the powder of propolis to high temperature (for example, 60 degreeC or more) is not essential, it becomes possible to suppress deterioration of a useful component easily. In particular, when manufacturing in a low temperature and nitrogen atmosphere, the deterioration of useful components can be remarkably prevented, so that the quality of the propolis powder coating can be greatly improved.

  Furthermore, according to the manufacturing method of this embodiment, since it is easy to form the thickness of the oil-based coating layer uniformly, a high-quality propolis powder coating can be easily manufactured. On the other hand, when the oil-based coating layer is formed, the drying process can be omitted compared to the case of the water-soluble coating layer, so that it is not necessary to expose the propolis powder to high temperature and high humidity conditions for a long time. In addition, it is possible to suppress deterioration of useful components, adhesiveness and solidification, and to improve the quality of the propolis powder coating. Moreover, according to the manufacturing method of this embodiment, since it is easy to form an oil-based coating layer thinly, the propolis powder coating containing a solid content derived from propolis at a high content of 40 to 99% by weight Can be manufactured. In particular, a propolis powder coating containing 60 wt% or more of a solid content derived from propolis is very excellent in terms of cost and availability.

  -The propolis-containing food according to the present embodiment can suppress deterioration of useful components derived from propolis and contains a propolis powder coating excellent in stability over time, and thus maintains high quality over a long period of time. Is easy. Further, the propolis-containing food of the present embodiment can be ingested as a powder, ingested as a beverage dissolved in water or hot water, or used as a food material for general processed foods as well as health foods. Therefore, it can be used for a wide range of purposes and is convenient. In particular, since it has extremely high temporal stability compared to conventional propolis powder, it is important that it can be developed in the general food field. In addition, in the field of health food preparations having product forms such as hard capsules, soft capsules, tableting preparations, etc., the product quality assurance period can be greatly extended, and processing such as filling into hard capsules and tableting properties can be performed. It is also important that the property is good.

  EXAMPLES Next, although an Example demonstrates this invention further in detail, this invention is not restrict | limited at all by these examples. In the following examples, the average particle size was measured using a laser diffraction particle size distribution analyzer SALD-2100 manufactured by Shimadzu Corporation.

(Reference Example 1)
10 kg of starch hydrolyzate (Pine Flow manufactured by Matsutani Chemical Industry Co., Ltd.) is put into a cake mixer and stirred at a low speed, and then the ethanol extract of Brazilian propolis bulk is extracted with 95% ethanol. (Liquid concentrated to 60% by weight) was added little by little. After the whole became a uniform mixture, this mixture was dried at 50 ° C. for 24 hours by a shelf type hot air dryer. The dried product was cooled, pulverized with an impact pulverizer, and then passed through an 80 mesh sieve to obtain 18.4 kg of a propolis ethanol extract powder (apparent specific gravity 0.85). The powder of Reference Example 1 contains 47% by weight of a solid content derived from propolis and has an average particle diameter of 90 μm.

(Reference Example 2)
15 kg of Brazilian propolis bulk is pulverized with a pulverizer (Pulverizer manufactured by Fuji Paudal Co., Ltd.) and sieved with a vibration sieve (manufactured by Koei Sangyo Co., Ltd.). .5 kg was obtained. After adding 80 kg of water at 50 ° C. to 10 kg of the pulverized propolis mass, water extraction was performed at 45 ° C. for 5 hours while stirring at low speed with a mixer. The obtained water extract of propolis was filtered with a coarse filter cloth (polyester raw silk fabric) until there was no residual moisture, and 77 kg of crude filtrate was obtained. Next, 1 kg of diatomaceous earth (silica 100F manufactured by Chuo Silica Co., Ltd.) was added to the crude filtrate and stirred, followed by filtration with a multistage pressure filter equipped with No2 filter paper (Advantech Toyo Co., Ltd.). As a result, 77 kg of filtrate was obtained. 45 kg of this filtrate was concentrated under reduced pressure with a low temperature concentrator (Okawara Seisakusho Co., Ltd.) until the solid content was 20% by weight, and then freeze-dried with a freeze vacuum dryer (Nihon Vacuum Technology Co., Ltd.). did. The obtained freeze-dried product was pulverized to obtain 870 g of a powder of an aqueous extract of propolis colored with a light brown color (apparent specific gravity 0.1).

  Finally, 400 g of the ethanol extract of propolis obtained in Reference Example 1 was added to 24 g of the water extract powder of Propolis obtained and mixed with a food processor to obtain the powder of Propolis 2 (Propolis of Propolis). Powder particles). The powder of Reference Example 2 was produced according to the production method of Patent Document 1, and contained 50% by weight of a solid content derived from propolis and had an average particle diameter of 70 μm.

(Reference Example 3)
2 kg of octenyl succinic esterified starch (National Starch Purity Gum BE) was added to 6 kg of water and dissolved while heating. To this solution was added 2.9 kg of an ethanol extract of Brazilian propolis bulk (extracted with 95% ethanol and then concentrated to a solid content of 70% by weight), and a homomixer (a homomixer manufactured by Tokushu Kika Kogyo Co., Ltd.) was added. After stirring for 30 minutes with MK-II), the mixture was cooled to room temperature to prepare an emulsified dispersion. In the homomixer, stirring was performed by rotating the stirring blade at a rotation speed of 6000 rpm. Next, the prepared emulsified dispersion was spray-dried with a spray dryer (manufactured by Okawahara Chemical Co., Ltd.) to obtain 3.5 kg of the powder of Reference Example 3 (propolis powder particles). The powder of Reference Example 3 was produced according to the production method of Patent Document 2, and contained 50% by weight of a solid content derived from propolis and had an average particle size of 100 μm.

Example 1
20 parts by weight of powder of rapeseed oil having an average particle size of 10 μm (melting point: 65 ° C.) and 80 parts by weight of powder having an average particle size of 70 μm obtained in Reference Example 2 (solid content content derived from propolis: 50% by weight) The mixture was stirred using the stirrer 10 shown in FIG. The mixing and stirring conditions are as follows: the diameter D1 of the main shaft stirring blade 11 is 1.1 m, the diameter D2 of the sub shaft stirring blade 12 is 0.3 m, the peripheral speed of the main shaft stirring blade 11 is 5 m / sec, The speed was set to 1 m / second, and the nitrogen gas cooled to 10 ° C. was blown into the stirring tank 13 of the stirrer 10 while adjusting the average collision load to 0.06 N. The average collision load was calculated on the assumption that the powder particles of Reference Example 2 collided with the wall surface.

  By stirring and mixing with the stirrer 10 for about 40 minutes, a propolis powder coating having an average particle diameter of 90 μm (a solid content of 40% by weight derived from propolis) was obtained. The obtained propolis powder coating had high fluidity and good handleability as compared with the propolis powder particles of Reference Example 2 used as a raw material.

(Example 2)
In Example 1, it manufactured similarly to Example 1 except having changed the compounding quantity of the powder of the reference example 2 and the powder of rapeseed oil oil into 60 weight part and 40 weight part, respectively. As a result, a propolis powder coating (with a solid content of 30% by weight derived from propolis) having an average particle size of 80 μm was obtained. The obtained propolis powder coating had high fluidity and good handleability.

(Example 3)
20 parts by weight of powdered rapeseed oil (melting point: 65 ° C.) having an average particle diameter of 10 μm and 80 parts by weight of powder having an average particle diameter of 100 μm (solid content content derived from propolis of 50% by weight) obtained in Reference Example 3 were used. Thus, a propolis powder coating was produced in the same manner as in Example 1. As a result, a propolis powder coating (with a solid content of 30% by weight derived from propolis) having an average particle size of 120 μm was obtained. The obtained propolis powder coating had high fluidity and good handleability.

Example 4
The hard capsule encapsulated product of Example 4 was obtained by encapsulating the propolis powder coating obtained in Example 1 in a hard capsule made of gelatin.

(Example 5)
The hard capsule encapsulated product of Example 5 was obtained by encapsulating the propolis powder coating obtained in Example 3 in a hard capsule made of gelatin.

(Comparative Example 1)
Example 1 using 20 parts by weight of powdered rapeseed oil (melting point: 65 ° C.) having an average particle diameter of 10 μm and 80 parts by weight of ethanol extract of propolis having an average particle diameter of 90 μm obtained in Reference Example 1 A powder coating was produced in the same manner as described above. As a result, a powder coating having an average particle size of 110 μm was obtained.

(Comparative Example 2)
By encapsulating the powder coating obtained in Comparative Example 1 in a hard capsule made of gelatin, a hard encapsulated product of Comparative Example 2 was obtained. In addition, in this comparative example, since the fluidity | liquidity of the powder coating material used was bad, the workability | operativity at the time of enclosure work was bad.

(Comparative Example 3)
The hard-encapsulated product of Comparative Example 3 was obtained by encapsulating the propolis powder particles obtained in Reference Example 2 in a hard capsule made of gelatin.

<Evaluation of stability over time 1>
The propolis powder particles of Reference Examples 2 and 3, the propolis powder coating of Examples 1 to 3 and the powder coating of Comparative Example 1 are each put into a bag with a zip (trade name: Lami Zip) together with an equal amount of air. And stored at room temperature in a sealed state. And about each sample of these reference examples 2 and 3, Examples 1-3, and the comparative example 1, while investigating the fluidity | liquidity after storing for a predetermined | prescribed storage period, the residual rate of Artepillin C was calculated | required, respectively. In addition, as shown in the following Table 1, the predetermined storage period indicates immediately after production, after 3 months, and after 6 months. These results are shown in Table 1 below.

By the way, the investigation of fluidity was judged by visually observing the state of each sample when the zipped bag was grasped by hand and shaken.
Further, the residual ratio of artepilin C was determined as follows. First, a predetermined amount of each sample stored for a predetermined storage period was added to ethanol and sufficiently stirred, and then subjected to ultrasonic treatment with an ultrasonic vibrator. Subsequently, each ethanol solution after sonication was filtered to obtain a filtrate, and then each filtrate was concentrated under reduced pressure to obtain a concentrated solution. After quantifying the amount of each concentrate obtained in a 10 ml volumetric flask, a portion of each concentrate was analyzed by high performance liquid chromatography, whereby the artepilin C contained in each concentrate was analyzed. Concentration was measured. Using the measured concentrations of artepilin C, the residual rate (%) of artepilin C in each sample when stored for a predetermined storage period was determined. The high performance liquid chromatography column is: Capcell Pak ACR (4.6 × 250 mm) manufactured by Shiseido, column temperature: 40 ° C., moving bed: 70% methanol + 1% acetic acid, measurement time: 40 minutes, flow rate: 1 The measurement was carried out under the conditions of 0.0 ml / min and measurement wavelength: UV 200 to 400 nm (UV 280 nm cut).

表１より、プロポリスの粉体粒子の表面に、融点４０℃以上の油脂系被覆層が形成されてなる各実施例のプロポリス粉体被覆物では、いずれも長期間に亘ってプロポリスの粉末（プロポリスのエタノール抽出物の粉末）の固結が防止されて高い流動性を発揮するとともに、アルテピリンＣの経時安定性が高められていたことが示された。なお、各実施例のプロポリスの粉体粒子では、プロポリスの水抽出物の粉末及びエステル化澱粉のいずれが表面に被覆されている場合でも、同様に高い流動性及びアルテピリンＣの経時安定性を有していたことも確認された。

From Table 1, in the propolis powder coatings of the respective examples in which an oil-based coating layer having a melting point of 40 ° C. or higher is formed on the surface of the propolis powder particles, all of the propolis powder (propolis) It was shown that the solidification of the ethanol extract powder) was prevented and high fluidity was exhibited, and the stability of artepilin C with time was enhanced. It should be noted that the propolis powder particles of each Example have high fluidity and stability over time with Artepilin C, regardless of whether the surface of the aqueous powder of propolis or the esterified starch is coated. It was also confirmed that

<Evaluation of stability over time 2>
Each of the hard capsule encapsulated products of Examples 4 and 5 and Comparative Examples 2 and 3 was put in a bag with a zip (trade name: lami zip) together with an equal amount of air (humidity 75%) and stored in a sealed state at 40 ° C. . And about each sample of these Examples 4 and 5 and Comparative Examples 2 and 3, the change of the property after storage for the storage period shown in following Table 2 was evaluated by seeing with the naked eye, respectively. The results are shown in Table 2.

表２より、実施例１，３の各プロポリス粉体被覆物はいずれも、ハードカプセル中においても高い経時安定性を発揮していた。

From Table 2, each of the propolis powder coatings of Examples 1 and 3 exhibited high temporal stability even in the hard capsule.

Further, the technical idea that can be grasped from the embodiment will be described below.
-The propolis powder is a pulverized propolis mass, a powder of a propolis alcohol extract, a powder of a hydrous alcohol extract of propolis, a powder of an organic solvent extract of propolis, a powder of a supercritical extract of propolis and a propolis. The propolis powder coating according to claim 1, comprising at least one selected from powders of micellar extracts.

  The powder of the water extract of the propolis or the esterified starch is disposed between the powder of the propolis and the oil-based coating layer. The propolis powder coating according to Item.

  The propolis powder coating has a homogeneous oil-based coating layer having a thickness of 1-30 μm made of the oil-based coating material on the surface of the powder particles of the propolis, and an average particle in the range of 50-300 μm The propolis powder coating according to any one of claims 1 to 3, which has a diameter.

  The content of the oil-based coating material is 300 / R to 3000 / R wt% [wherein R represents an average particle diameter (μm) of the propolis powder coating]. The propolis powder coating according to any one of claims 1 to 3.

  5. The propolis powder according to claim 4, wherein in the mixing and stirring step, the powder of the oil-based coating material and the powder particles of the propolis are mixed and stirred in a cooling gas atmosphere of 20 ° C. or less. A method for producing a coating.

Sectional drawing which shows typically the stirrer used by embodiment and the Example.

Claims (5)

A propolis powder coating having an oil-based coating layer on the surface of the propolis powder particles,
The propolis powder particles have a structure in which the surface of the propolis powder is coated with a powder of water extract of propolis or esterified starch,
The oil-based coating layer is made of an oil-based coating material having a melting point of 40 ° C. or higher.   2. The propolis powder coating according to claim 1, wherein the propolis powder is a powder of an alcohol extract of propolis or a powder of an aqueous alcohol extract of propolis. 3.   3. The propolis powder coating material according to claim 1, wherein the propolis powder particles and the oil-based coating material are contained in a weight ratio of 25:75 to 99: 1. . A method for producing a propolis powder coating according to any one of claims 1 to 3,
The method comprises the steps of: preparing a powder particle of the propolis by coating the surface of the powder of the propolis with the powder of the water extract of the propolis or the esterified starch; Mixing and stirring the powder of the oil-based coating material at a collision average load of 0.01 to 10 N,
The method for producing a propolis powder coating, wherein the oil-based coating material powder has an average particle size of 0.1 to 50 µm.   The propolis containing food containing the propolis powder coating according to any one of claims 1 to 3.

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