JP5004198B2 - Method for producing powder composition - Google Patents

Description

  The present invention relates to a method for producing a microencapsulated powder composition containing a fragrance, a sweetener, a seasoning, an acidulant or a functional substance, mainly for use in an oral composition such as chewing gum. More specifically, flavoring, sweeteners, seasonings, acidulants or functional substances can be released into the oral cavity by mastication at the desired timing, lasting for a long time, excellent in heat resistance and storage stability, and fluid The present invention relates to a method for producing a powder composition that is excellent in resistance to blocking.

  Conventionally, microencapsulation technology has been used in various fields for the purpose of imparting heat resistance to core materials, improving stability, preventing moisture absorption, and improving sustained release and sustainability. In particular, in the field of fragrances, research has been actively conducted as a method for solving the problems caused by the volatility and instability of fragrances, and the fragrances are contained in matrices of carbohydrates, sugar alcohols, and other carbohydrates. A method to contain the material has been developed.

  In particular, in flavors, sweeteners, seasonings, acidulants and functional substances for use in chewing gum, both chewing gum is quickly released at a desired timing and lasts for a long time as it is chewed. Is required. Therefore, a technique for imparting sustained release to a fragrance or the like using a microencapsulation technique has been developed.

  Such techniques include, for example, an encapsulated composition in which an active ingredient is encapsulated in a mixture of high molecular weight polyvinyl acetate and a hydrophobic plasticizer such as triglyceride (Patent Document 1), a perfume as an aqueous solution of a water-soluble wall material, Emulsified in the presence of a compound having a valent metal ion and a gel-forming ability, spray-dried to a powder, then insolubilized with a polyvalent metal salt, dried again to a powder, and then melted animal and plant hardened oil and Active ingredients such as a coating powder flavor (Patent Document 2), a high-sweetness sweetener of 0 to 55% by weight, and a wall material such as polyvinyl acetate. A sustained release structure formed by extruding a mixture containing ingredients (Patent Document 3), a first intense sweetener encapsulated in a first core coating, And a delivery system (Patent Document 4) containing a second external hydrophilic coating containing up to the solubility limit of the second coating of the second sweetener, after removing content components of the cells such as yeast, There is disclosed a microcapsule (Patent Document 5) in which a fragrance or the like is encapsulated in a microbial cell, and a saccharide, a high-intensity sweetener, a protein, a polyhydric alcohol, or the like is attached to the surface.

  However, since polyvinyl acetate used in Patent Documents 1 and 3 is a component that is also used as a chewing gum base material (1), when blended in chewing gum, it easily mixes with the base material during chewing, (2) Since the temperature for melting polyvinyl acetate is high, there is a problem of volatilization and deterioration when a fragrance is used as a core substance. (3) Poly Vinyl acetate has disadvantages such as being unable to be used for purposes other than chewing gum base and fruit or fruit skin coatings, including when included in pharmaceutical preparations, under the Japanese Food Sanitation Law. . Further, the methods of Patent Documents 2 and 4 have a drawback that the process is very complicated. Further, even in the method using the yeast cell wall of Patent Document 5, the flavor persistence is still not sufficient.

  On the other hand, shellac is known as a coating agent and has been conventionally used to form a thin film on the surface of food, medicine, etc. by dissolving in an alcohol solution or an alkaline solution for the purpose of forming a glossy film. . The purpose of these coatings is to protect the contents by utilizing the water resistance and acid resistance of shellac, or to make it a brightening agent. Further, it is easy to chew or change the surrounding pH. The film was physically and chemically broken, and it was possible to eat and drink internal foods and to ingest medicines. As a technique for microencapsulation using shellac, for example, an aqueous solution of shellac having a pH of 6.0 to 9.0 is added to and mixed with an edible substance emulsion, powder flavor, acidulant, sweetener and the like. , A method for obtaining an excellent sustained-release dry product having high thermal stability by drying (Patent Document 6), emulsified preparations, powdered flavorings, acidulants, sweeteners and other substances to be dispersed, and powdered shellac into shellac A method of obtaining an excellent sustained-release dried product with high thermal stability by adding an alcohol solution, mixing, drying and then pulverizing is disclosed (Patent Document 7).

  However, the methods of Patent Documents 6 and 7 are methods in which a thin film capsule is formed on a core substance using an ethanol solution or an alkaline aqueous solution. Usually, the shellac film formed by these methods is very thin. Moreover, since it has brittleness, once the membrane is broken, the content components easily flow out to the outside, and it cannot be said that it has sufficient sustained release and sustainability. In addition, in order to form a thick and strong shellac film by these methods, a large amount of shellac ethanol solution or alkaline aqueous solution must be prepared, and a large amount of ethanol or water is distilled off for drying. It had the disadvantage of being disadvantageous in terms of work and economy.

  Therefore, there is a need for a microencapsulation technique that can be easily and easily manufactured and that is highly sustainable.

JP 62-215349 A JP-A-4-293454 JP-A-5-292890 JP-A-6-14739 International Publication WO2003 / 041509 Pamphlet JP 2009-55850 A JP 2009-55851 A

  The problem to be solved by the present invention is that at the time of production, even if a highly volatile substance such as a fragrance is used as a core substance, there is no dissipation due to volatilization, and the fragrance, sweetener, seasoning, acidulant, functional substance The core material such as is completely encapsulated, excellent in heat resistance and storage stability, high in fluidity of the powder, hardly blocking even in a high humidity environment, and further, when blended in chewing gum, etc. An object of the present invention is to provide a method for producing a powder composition in which the release of a core substance by mastication occurs gradually and lasts for a long time.

  In order to solve the above-mentioned problems, the present inventors diligently studied a material for a wall material for enclosing a fragrance and the like and an enclosing method. As described above, shellac has been conventionally used after being dissolved in an alcohol solution or an alkali solution, coated, and dried to form a film. As described above, since this film has a thin film and is brittle, once the film is broken, the content components tend to flow out to the outside, and it has the disadvantages that it takes labor and cost to manufacture. . However, the shellac heated to a molten or semi-molten state and then solidified by cooling was very high in both strength and elasticity, and it was expected to be useful as a coating material for microcapsules. Therefore, the present inventors mixed powdered core material and powdered or flaky shellac in a powder state, heated and melted the mixture, cooled and solidified, and pulverized to obtain a powder. In particular, the inventors have found that microcapsules in which the release of the core substance is extremely slow can be obtained by a very simple method, and have completed the present invention.

  Thus, in the present invention, the powdered core material and powdered or flaky shellac are mixed in a powder state, and the mixture is heated to a molten or semi-molten state, and then cooled, solidified, and pulverized. The present invention provides a method for producing a powder composition.

  In the present invention, the powdered core substance is at least one selected from powder flavors, powder sweeteners, powder seasonings, powder acidulants and powder functional substances. A manufacturing method is provided.

  Furthermore, the present invention provides an average particle diameter (median diameter) of 10 μm to 2000 μm when the particle size of the powdered core substance is measured on a volume basis by a dry method using a laser diffraction / scattering particle size distribution measuring device. The present invention provides a method for producing the above powder composition.

  Furthermore, the present invention provides a method for producing the above powder composition, wherein shellac is contained in the powder composition in an amount of 5% to 70% in terms of mass.

  Furthermore, the present invention provides a method for producing the above-mentioned powder composition, wherein the heating temperature for making the molten or semi-molten state is 50 ° C. to 110 ° C.

  The powder composition obtained by the present invention is excellent in sustained release, and when blended in chewing gum, the sustainability of a core material such as a fragrance, sweetener, seasoning, acidulant, and functional substance is extremely high. . In addition, the sustained release can be easily adjusted by using a particle size of the core substance or shellac together with a carbohydrate-based material such as sugar or sugar alcohol. In addition, even if a material that is volatile and easily deteriorates, such as a fragrance, is used as a core substance, the temperature of heating and melting is low. In addition, shellac that has been re-solidified after heating and melting has high heat resistance, and thus has heat resistance, and the core substance remains sufficiently even after being baked after being used for baked goods. Further, since the inclusion is completely completed, the storage stability of the core substance is good. Furthermore, since the surface of the powder is covered with solidified shellac, the powder has high fluidity and is less likely to block even in a high humidity environment.

  In the present invention, any material that can be used as the core substance can be used as long as it is a material that is intended to have sustained release properties by microencapsulation. In addition, since these materials are once mixed with powdered or flaky shellac in a powder state in a later step, it is necessary to be a powdered material. Among these materials, powder flavors, powder sweeteners, powder seasonings, powder acidulants and powder functional substances can be exemplified as particularly preferable materials.

  The fragrance used in the present invention is not particularly limited, and any natural extract such as various natural essential oils, extracts, oleoresin, resinoids, synthetic fragrance compounds, or blended fragrances prepared by using these may be used. Can do. Examples of natural essential oils include citrus essential oils such as orange, lemon, lime, and grapefruit, and plant essential oils such as flower essential oil, peppermint oil, spearmint oil, and spice oil. Examples of natural product extracts include cola nuts. Oily extracts such as extract, coffee extract, vanilla extract, cocoa extract, tea extract and spice extract, resinoids and their oleoresins, and synthetic fragrance compounds include, for example, , "Survey on the use of food fragrance compounds in Japan" (FY 2000 Health and Welfare Research Report; Japan Fragrance Industry Association published in March 2001), "Synthetic fragrance chemistry and product knowledge" (March 22, 2005 supplement) Issuance of revised editions written by Motoichi Into, Chemical Industry Daily, etc. At least one synthetic fragrance selected from the group of esters, alcohols, aldehydes, ketones, phenols, ethers, lactones, hydrocarbons, nitrogen-containing and / or sulfur-containing compounds, acids, etc. It can be illustrated.

  The sweetener that can be used in the present invention is not particularly limited, and examples thereof include acesulfame K, sucralose, aspartame, neotame, disodium glycyrrhizinate, thaumatin, saccharin and a salt thereof, rakan extract, licorice extract, rebaudio High-sweetness sweeteners such as Cyudo A, Stevia extract, Enzyme-treated Stevia extract, Neohesperidin dihydrochalcone; Sugar alcohols such as xylitol, erythritol, sorbitol, maltitol, paratinite, reduced starch candy; sugar, glucose, Examples thereof include saccharides such as fructose, maltose, lactose, galactose, maltose and trehalose.

  The seasoning that can be used in the present invention is not particularly limited, and examples thereof include sodium L-aspartate, DL-alanine, glycine, L-glutamic acid, sodium L-glutamate, succinic acid, monosodium succinate, and L-theanine. Amino acid-based or nucleic acid-based seasonings such as 5′-ribonucleotide disodium and 5′-ribonucleotide dicalcium can be exemplified.

  The acidulant that can be used in the present invention is not particularly limited. For example, citric acid, monopotassium citrate, tripotassium citrate, trisodium citrate, fumaric acid, monosodium fumarate, DL-malic acid, DL -Sodium malate, DL-tartaric acid, L-tartaric acid, DL-sodium tartrate, L-sodium tartrate, acetic acid, sodium acetate, succinic acid, sodium succinate and the like can be exemplified.

  The functional substance that can be used in the present invention is not particularly limited, and examples thereof include spice extract, caffeine, quina extract, gentian extract, theobromine, naringin, sagebrush extract, and tannin bitters; β -Carotene, paprika dye, food red No. 2, food yellow No. 5, riboflavin, Anato dye, cacao dye, gardenia blue pigment, gardenia yellow pigment, cochineal pigment, chlorophyll, beet red, grape skin pigment, safflower yellow pigment, marigold Natural pigments such as pigments, beech mushroom pigments, purple potato pigments, lac pigments, rutin; fat-soluble vitamins such as liver oil, vitamin A, vitamin A oil, vitamin D, vitamin B12, riboflavin butyrate, natural vitamin E mixture, coenzyme Q10 Class: Vitamin B1, Vitamin B2, Bi Water-soluble vitamins such as Min B6, folic acid, nicotinic acid, vitamin C, vitamin P; soybean oil, rapeseed oil, corn oil, olive oil, palm oil, safflower oil, sunflower oil, rice oil, beef tallow, pork oil, fish oil Animal and vegetable oils and fats such as: rosin, copal, dammar, elemi, ester gum, and other vegetable resins; processed edible fats and oils such as medium chain saturated fatty acid triglycerides having 6 to 12 carbon atoms, and edible oily materials thereof be able to.

  In the present invention, a fat-soluble liquid core material used as a core material, such as a fragrance or other fat-soluble material, is powdered by pulverizing in advance by a method such as spray drying, vacuum drying, or freeze drying. It can be. In the preparation of the powdered core substance, the fragrance material mixture and the fat-soluble functional substance, for example, fatty acid monoglyceride, fatty acid diglyceride, fatty acid triglyceride, propylene glycol fatty acid ester, sucrose fatty acid ester, polyglycerin fatty acid ester , Lecithin, modified starch, sorbitan fatty acid ester, kiraya extract, gum arabic, tragacanth gum, guar gum, caraya gum, xanthan gum, pectin, alginic acid and its salts, carrageenan, gelatin, casein, dextrin, monosaccharides, disaccharides, polyols, etc. It can be obtained by emulsifying using a surfactant or an appropriate excipient and drying by a drying method such as spray drying, vacuum drying, freeze drying and the like.

  Of the above core materials, the solid core material is also preferably in a powder form. As a method for obtaining a powder, when the particle size of the solid core substance is large, it can be pulverized using a general pulverizer used in food production such as a hammer mill and a feather mill.

  The particle size after pulverization can be adjusted by combining the state of the dried product to be pulverized, the apparatus used for pulverization, and the pulverization time. Furthermore, when it is desired to make the particle sizes uniform, it is possible to obtain particles in a desired range by using a sorting device such as a vibrating sieve.

  The particle size of these powders is 10 μm to 2000 μm, preferably 20 μm to 1000 μm, as an average particle size (median diameter) when measured on a volume basis by a dry method using a laser diffraction / scattering particle size distribution analyzer. More preferably, it can illustrate in the range of 50 micrometers-500 micrometers. In the present invention, the powdered core material is mixed with powdered or flaky shellac in a later step, and melted and solidified. However, when the particle size is larger than 2000 μm, the inclusion by shellac is uniform. In addition, the capsule collapses and the core substance is easily eluted, and the sustainability is deteriorated, and the effects of the present invention are not exhibited. In addition, when the particle size is smaller than 10 μm, the inclusion is performed well, but the core substance does not elute forever, and it becomes difficult to express flavor, taste, function, and the like.

  The powdered core material is then mixed with powdered or flaky shellac. Shellac is parasitized by trees such as leguminosae and mulberry departments, and the resinous material (stick rack) that sucked sap and secreted outside the body was crushed, sieved, washed with water, insect shells and wood, It is a natural resin obtained by removing a water-soluble dye or the like to obtain a seed rack and then purifying it after being melted or in solution, followed by filtration. Shellac includes a wax-containing product from which shellac wax has not been removed and a dewaxed product from which shellac wax has been removed, and a shellac-derived natural pigment that has been bleached or decolorized. Bleached shellac is produced by dissolving seed rack in an aqueous alkali solution, bleaching with sodium hypochlorite, neutralizing the alkali with an inorganic acid and precipitating shellac. Bleached dewaxed shellac can be obtained by removing the wax by filtration during the manufacturing process. Shellac is recognized by the FDA (US Food and Drug Administration) as a GRAS substance (a substance generally accepted as safe).

  Shellac dissolves slowly but well in ethanol at room temperature, but is insoluble in water and only insoluble or swells in organic solvents other than ethanol. In addition, it is a thermosetting resin and is easily melted by heat. However, once it is thermoset, it is not easily attacked by heat or a solvent.

  The shellac that can be used in the present invention can be any of refined shellac, bleached shellac, decolorized shellac and the like. Commercially available shellac is sold in the form of powder or flakes, but any shape can be used. These commercially available shellacs can be obtained from, for example, Gifu Shellac Co., Ltd., Nippon Shellac Industry Co., Ltd., Koyo Chemical Co., Ltd.

  In the present invention, first, a powdery core substance and powdered or flaky shellac are mixed in a powdered state. In mixing, the ratio of powdered or flaky shellac to the entire mixture is 5% to 70%, preferably 10% to 60%, more preferably 20% to 50% in terms of mass. When the ratio of the powder or flaky shellac to the whole mixture is less than 5%, the coating of the core material is insufficient, the durability is deteriorated, and the effect of the present invention is not exhibited. In addition, when the ratio of powder or flaky shellac to the whole mixture exceeds 70%, the inclusion is performed well, but the core substance does not elute forever, and it becomes difficult to express flavor, taste, function, etc. End up.

  In the present invention, other excipients may be added to the powder mixture of the powdered core substance and the powder or flaky shellac as long as the effects of the present invention are not impaired. By adding other excipients, it is possible to adjust the sustained release and sustainability, such as slightly reducing the sustained release and shortening the sustainability. Examples of excipients that can be used include polymer excipients such as dextrin, modified starch, starch, and arabic gum; sugars such as sugar, glucose, fructose, maltose, lactose, galactose, maltose, and trehalose; xylitol, Examples thereof include sugar alcohols such as erythritol, sorbitol, maltitol, palatinit, and reduced starch candy.

  The mixing ratio of these excipients adjusts the sustained release and sustainability of the finished powder composition as appropriate within the range of 0% to 50% in terms of mass with respect to the whole powder mixture before heating and melting. Can be determined.

  In the present invention, the powdered core material, the powdered or flaky shellac, and, if necessary, the excipient are then mixed in a powder state. Once mixed in the powder state, in the melting or semi-melting by heating in the subsequent process, the core material is surrounded by a melted or semi-molten shellac, and solidified by cooling to solidify the core material. The included capsule is completed. Mixing in a powder state can be performed by a powder mixer such as a stirring pot, a kneader, a nauter mixer, a ribbon mixer, and an extruder.

  In the present invention, these powder mixtures are then heated to bring the shellac and / or excipients into a molten or semi-molten state. The temperature for melting or semi-melting at this time can be 50 ° C to 110 ° C, preferably 70 ° C to 110 ° C. When the temperature is lower than 50 ° C., the shellac is not melted or semi-molten, so that a uniform matrix cannot be formed, which is not preferable. Moreover, when temperature exceeds 110 degreeC, the thermal deterioration of core substances, such as a fragrance | flavor and a functional substance, may occur, and is not preferable.

  These apparatuses for heating the mixture to melt the sugar into a semi-molten state may be heated as it is when the powder mixer has a heating device such as a jacket. Heating and extrusion may be performed continuously by feeding into a heated biaxial extruder. Moreover, when using a biaxial extruder, mixing of powder-melting by heating or semi-melting-extrusion can also be performed continuously.

  The molten or semi-melted product by heating can be solidified by taking out from the apparatus and then placing it on a tray or the like to form a thin film or string. At this time, the matrix can be efficiently solidified by cooling the back side of the tray or the like with a cooler. In addition, when extrusion is performed using a biaxial extruder or the like, it can be solidified by cooling due to deprivation of heat of vaporization caused by extrusion under a cooling atmosphere or extrusion under a reduced pressure atmosphere.

  In the present invention, the obtained solidified product is then pulverized using an appropriate pulverizer to obtain a powder composition. Examples of the pulverizing apparatus include pulverizers such as a vibration mill, a ball mill, a feather mill, and a hammer mill. By passing through an outlet having an appropriate mesh size or opening size using these pulverizers, a powder composition having an appropriate particle size according to the purpose of use can be obtained.

  The powder composition obtained by the above-described method of the present invention is less susceptible to thermal deterioration of the core material during production, and since it is completely clathrated by shellac, it has excellent sustained release, excellent sustainability, heat resistance, It has good storage stability, high fluidity as a powder, and does not easily block even in a high humidity environment.

  Examples of foods and drinks to which the powder composition of the present invention can be added include, for example, chewing gum, baked confectionery, tablet confectionery, candy, powder soup, snack food, processed meat products, instant food, retort food, cooked food, taste Various foods and drinks such as foods and drinks and other foods and drinks can be mentioned. By adding appropriate amounts of these foods and drinks as flavorings, sweeteners, seasonings, acidulants or functional compositions, during processing and storage It is possible to provide foods and drinks that can suppress changes in these components, exhibit sustained release and sustainability during eating and drinking, and can achieve satisfaction.

  The following examples further illustrate the present invention.

[Reference Example 1] Preparation of menthol powder fragrance 300 g of modified starch (Purity Gum BE: manufactured by NSC Japan) and 400 g of dextrin (Paindex (registered trademark) No. 1: manufactured by Matsutani Chemical Co., Ltd.) were dissolved in 1300 g of soft water. Thereafter, 300 g of menthol was added and emulsified with a homomixer to an emulsified particle size of about 0.5 μm to 2 μm to obtain an O / W emulsion. This emulsion is spray dried using a mobile minor type spray dryer (manufactured by GAE Process Engineering Co., Ltd.) at a hot air inlet temperature of 150 ° C., an exhaust air temperature of 80 ° C. and an atomizer speed of 20000 rpm, and menthol is 30%. 1000 g of powdered fragrance | flavor containing was obtained (reference product 1). As a result of measuring the particle size of Reference Product 1 on a volume basis by a dry method using a laser diffraction / scattering particle size distribution analyzer, the average particle size (median diameter) was 45.7 μm.

[Example 1]
Reference product 1 (100 g) and powdered shellac 100 g are mixed in advance, heated and melted with a biaxial extruder EA-20 (manufactured by Suehiro EPM), and extrusion melt-molded with a die having a screen size of 2 mm × 12 holes. went.

Extrusion conditions: Temperature when the mixture is melted: 92 ° C
Die surface set temperature: 70 ° C
Product temperature when extruded from the die: 81 ° C
Screw rotation speed: 60rpm
The extruded mixture is placed in a string so as not to overlap the stainless steel tray, blown to cool to room temperature and solidified, and then the obtained granule is pulverized and sieved with 30 mesh to obtain 200 g of a powder composition. (Invention product 1: containing 15% menthol and 50% shellac).

[Example 2]
Reference product 1 (70 g) and powdered shellac 130 g are mixed in advance, heated and melted with a biaxial extruder EA-20 (manufactured by Suehiro EPM), and extrusion melt-molded with a die of a screen 2 mm × 12 holes. went.

Extrusion conditions: Temperature when the mixture is melted: 92 ° C
Die surface set temperature: 70 ° C
Product temperature when extruded from the die: 81 ° C
Screw rotation speed: 60rpm
The extruded mixture is placed in a string so as not to overlap the stainless steel tray, blown to cool to room temperature and solidified, and then the obtained granule is pulverized and sieved with 30 mesh to obtain 200 g of a powder composition. (Invention product 2: menthol 10.5%, shellac 65% contained).

[Example 3]
Reference product 1 (160 g) and powdered shellac 40 g are mixed in advance, heated and melted with a biaxial extruder EA-20 (manufactured by Suehiro EPM), and extrusion melt-molded with a die having a screen size of 2 mm × 12 holes. went.

Extrusion conditions: Temperature when the mixture is melted: 92 ° C
Die surface set temperature: 70 ° C
Product temperature when extruded from the die: 81 ° C
Screw rotation speed: 60rpm
The extruded mixture is placed in a string so as not to overlap the stainless steel tray, blown to cool to room temperature and solidified, and then the obtained granule is pulverized and sieved with 30 mesh to obtain 200 g of a powder composition. (Invention product 3: menthol 24%, shellac 20% contained).

[Example 4]
Reference product 1 (180 g) and powdered shellac 20 g are mixed in advance, heated and melted with a biaxial extruder EA-20 (manufactured by Suehiro EPM Co., Ltd.), and extrusion melt-molded with a die of a screen 2 mm × 12 holes. went.

Extrusion conditions: Temperature when the mixture is melted: 92 ° C
Die surface set temperature: 70 ° C
Product temperature when extruded from the die: 81 ° C
Screw rotation speed: 60rpm
The extruded mixture is placed in a string so as not to overlap the stainless steel tray, blown to cool to room temperature and solidified, and then the obtained granule is pulverized and sieved with 30 mesh to obtain 200 g of a powder composition. (Invention product 4: 27% menthol and 10% shellac).

[Example 5]
Reference product 1 (100 g), dextrin (paindex No. 1: made by Matsutani Chemical Co., Ltd.) 50 g and powdered shellac 50 g are mixed in advance and heated with a biaxial extruder EA-20 (made by Suehiro EPM). After melting, extrusion melt molding was performed using a die having a screen of 2 mm × 12 holes.

Extrusion conditions: Temperature when the mixture is melted: 92 ° C
Die surface set temperature: 70 ° C
Product temperature when extruded from the die: 81 ° C
Screw rotation speed: 60rpm
The extruded mixture is placed in a string so as not to overlap the stainless steel tray, blown to cool to room temperature and solidified, and then the obtained granules are crushed and sieved with 30 mesh to obtain 180 g of a powder composition. (Invention product 5: containing 15% menthol and 25% shellac).

[Comparative Example 1]
Reference product 1 (194 g) and powdered shellac 6 g are mixed in advance, heated and melted with a biaxial extruder EA-20 (manufactured by Suehiro EPM), and extrusion melt-molded with a die having a screen size of 2 mm × 12 holes. went.

Extrusion conditions: Temperature when the mixture is melted: 92 ° C
Die surface set temperature: 70 ° C
Product temperature when extruded from the die: 81 ° C
Screw rotation speed: 60rpm
The extruded mixture is placed in a string so as not to overlap the stainless steel tray, blown to cool to room temperature and solidified, and then the resulting granule is pulverized and sieved through a 30 mesh powder composition containing menthol 180 g (comparative product 1: 29.1 menthol, containing 3% shellac) was obtained.

[Comparative Example 2]
After dissolving 300 g of modified starch (Purity Gum BE: manufactured by NSC Japan) and 400 g of dextrin (Paindex No. 1: manufactured by Matsutani Chemical Industry Co., Ltd.) in 1300 g of soft water, 300 g of menthol was added and emulsified particles with a homomixer Emulsification was performed to a diameter of about 0.5 μm to 2 μm to obtain an O / W emulsion. Next, 400 g of 25% shellac aqueous solution having pH 7.0 was added to and mixed with this O / W emulsion, and this emulsion was heated using a mobile minor type spray dryer (manufactured by GAE Process Engineering Co., Ltd.) at a hot air inlet temperature of 150 ° C. Spray drying was performed at an exhaust air temperature of 80 ° C. and an atomizer rotational speed of 20000 rpm to obtain a dried product. The obtained dried product was sieved with 30 mesh to obtain 1100 g of a powdered fragrance (Comparative product 2: containing 27.3% menthol and 9.1% shellac).

[Comparative Example 3]
After dissolving 300 g of modified starch (Purity Gum BE: manufactured by NSC Japan) and 400 g of dextrin (Paindex No. 1: manufactured by Matsutani Chemical Industry Co., Ltd.) in 1300 g of soft water, 300 g of menthol was added and emulsified particles with a homomixer Emulsification was performed to a diameter of about 0.5 μm to 2 μm to obtain an O / W emulsion. Next, 1000 g of 25% shellac aqueous solution of pH 7.0 was added to and mixed with this O / W emulsion, and this emulsion was heated at a hot air inlet temperature of 150 ° C. using a mobile minor type spray dryer (manufactured by GAE Process Engineering Co., Ltd.). Spray drying was performed at an exhaust air temperature of 80 ° C. and an atomizer rotational speed of 20000 rpm to obtain a dried product. The obtained dried product was sieved with 30 mesh to obtain 1250 g of a powdered fragrance (Comparative product 3: containing 24% menthol and 20% shellac).

[Comparative Example 4]
Reference product 1 (100 g) was mixed with 41.5 g of powdered shellac in advance, and then 41.5 g of shellac ethanol solution in which equal amounts of shellac were mixed and dissolved in 95% ethanol in terms of mass. The mixed product was extruded with a 0.7 mm screen using an extrusion granulator basket ruser (manufactured by Fuji Paudal Co., Ltd.) and dried with a vacuum dryer at 1 Pa, 60 ° C. for 15 hours. The obtained dried product was sieved with 30 mesh to obtain 162.25 g of a dried product (Comparative product 4: containing 18.5% menthol and 38.4% shellac).

Flavor dissolution test 1 (Aroma testing and sensory evaluation of chewing gum)
To the chewing gum base shown below, the reference product 1, the present invention products 1 to 5 or the comparative products 1 to 4 are respectively added so that the menthol content in the chewing gum is 0.18%, and the mixture is usually used with a high shear mixer. The mixture was mixed at about 50 ° C. by the method, and after cooling, it was subjected to pressure forming by rolling on a roll to prepare 3 g of chewing gum.

  The chewing gum obtained was sensorially evaluated for the duration and strength of the menthol aroma when chewing gum was chewed by a panel of 10 experts. At that time, the menthol feeling continues to feel to a certain extent even after chewing, so after chewing for a certain period of time, chewing is interrupted and sensory evaluation is performed at that time, and chewing is resumed when the menthol feeling disappears. Then, sensory evaluation of chewing for the next time was performed. In the above test, mastication was performed for 7 minutes, 5 minutes, and 3 minutes for a total of 15 minutes to compare the persistence of menthol expression. In addition, each feature and overall evaluation are described. The average evaluation results are shown in Table 1.

Chewing gum base composition Raw material Blending amount Chewing gum base 100 parts by weight Sugar 250
Glucose 40
Corn syrup (Bx85) 60
Glycerin 3
Reference product 1, product of the present invention or comparative product Amounts listed in Table 1

  As shown in Table 1, the reference product 1 containing no shellac showed a sharp flavor peak after about 1 minute, and then the flavor decreased sharply and the flavor disappeared after about 5 minutes. In addition, menthol-specific irritation and bitterness were felt. On the other hand, the product 1 of the present invention prepared by the method of the present invention (containing 50% shellac) showed a flavor peak after 5 to 9 minutes, then decreased gradually, and the flavor was sustained for 15 minutes or more. . In addition, the sensation and bitterness peculiar to menthol was alleviated, and it had a strong and mild flavor. Further, both of the present invention product 2 containing 65% shellac and the present invention product 3 containing 20% shellac have slightly different peak times. After that, a gentle decrease was observed, the flavor lasted for 15 minutes or more, and the irritation and bitterness peculiar to menthol were alleviated, resulting in a mild flavor. In the present invention product 4 (containing 10% shellac), the expression of flavor was slightly sharp from the beginning of mastication, and the appearance of the peak was earlier than that of the present invention products 1 to 3, but the duration was long and peculiar to menthol. Good with little irritation and bitterness. The product 5 of the present invention uses dextrin as an excipient in addition to shellac, but the peak appeared slightly earlier than the product 1 of the present invention, but other than that, it was almost the same as the product 1 of the present invention. The expression of flavor was shown. Therefore, it was found that the time until the appearance of the flavor peak was accelerated by using an excipient in addition to shellac.

  On the other hand, the comparative product 1 (shellac content 3%) with reduced shellac use has a sharp expression of flavor, a menthol-specific irritation and bitterness, and the disappearance of the flavor is quick, after 7 minutes. Almost no flavor was felt.

  Comparative product 2 (shellac 9.1 content%) is a product obtained by adding a shellac alkaline aqueous solution in advance at the time of preparation of menthol powder fragrance as a core substance, that is, emulsifying menthol, and then obtaining a powder by spray drying. The expression of the flavor is weak, and a peak is felt relatively early (3 to 4 minutes). However, it did not last long and disappeared around 6 minutes. Comparative product 3 (containing 20% shellac) was obtained by increasing the amount of shellac used in comparative product 2, but the flavor was weak and unclear and had a peak at 8 to 10 minutes, but not so conspicuous, 13 It disappeared around minutes. Comparative product 4 (containing 38.4% shellac) was encapsulated using an ethanol solution of shellac instead of the heating and melting method of the present invention, but the expression of flavor was weak and unclear, 8-10. There was a peak at the minute, but it was not very noticeable and disappeared around 12 minutes.

Test reference product 1 relating to moisture absorption stability, products 1 to 5 of the present invention, and comparative products 1 to 4 were sampled in a petri dish by 5 g each and spread uniformly over the powder, then at a temperature of 40 ° C. and a relative humidity of 60% for 5 hours. The moisture absorption test was conducted. The results are shown in Table 2.

  As shown in Table 2, the reference product 1 (powder flavor of menthol) was not blocked, but the fluidity was slightly lowered and the influence of moisture absorption was observed.

  On the other hand, it was found that the products 1 to 5 of the present invention maintained a completely good state even after the moisture absorption test, and the stability under high humidity was extremely good.

  Comparative product 1 (shellac content 3%) in which the amount of shellac used was reduced, comparative product 2 (containing shellac 9.1%) obtained by spray drying after adding a shellac alkaline aqueous solution in advance during emulsification of menthol, Instead of the comparative product 3 (containing 20% shellac) and the comparative product 4 (containing 38.4% shellac) encapsulated in an ethanol solution of shellac in place of the heating and melting method of the present invention, both of them were completely after the moisture absorption test. The good state was maintained and the stability under high humidity was very good.

[Reference Example 2] (Preparation of lemon powder flavor)
After 300 g of modified starch and 400 g of dextrin were dissolved in 1300 g of soft water, 300 g of lemon oil was added and emulsified with a homomixer to an emulsified particle size of about 0.5 μm to 2 μm to obtain an O / W emulsion. Using a mobile minor type spray dryer (manufactured by GAE Process Engineering Co., Ltd.), this emulsion is spray-dried at a hot air inlet temperature of 150 ° C., an exhaust air temperature of 80 ° C., and an atomizer speed of 20000 rpm, and 30 ml of lemon oil is obtained. % Powder fragrance 1000% was obtained (reference product 2). As a result of measuring the particle size of Reference Product 2 on a volume basis by a dry method using a laser diffraction / scattering particle size distribution analyzer, the average particle size (median diameter) was 60.4 μm.

[Example 6]
Reference product 2 (100 g) and powdered shellac 100 g are mixed in advance, heated and melted with a biaxial extruder EA-20 (manufactured by Suehiro EPM), and extrusion melt-molded with a die having a screen size of 2 mm × 12 holes. went.

Extrusion conditions: Temperature when the mixture is melted: 92 ° C
Die surface set temperature: 70 ° C
Product temperature when extruded from the die: 81 ° C
Screw rotation speed: 60rpm
The extruded mixture is placed in a string so as not to overlap the stainless steel tray, blown to cool to room temperature and solidified, and then the obtained granule is pulverized and sieved with 30 mesh to obtain 200 g of a powder composition. (Invention product 6: containing 15% lemon oil and 50% shellac).

[Comparative Example 5]
In Example 6, except that the extrusion conditions were changed as follows, the same operation as in Example 6 was performed to obtain 200 g of Comparative Product 5 (containing 15% lemon oil and 50% shellac).

Extrusion conditions: Temperature when the mixture is melted: 140 ° C
Die surface set temperature: 127 ° C
Product temperature when extruded from die: 134 ° C
Screw rotation speed: 60rpm

[Comparative Example 6]
After dissolving 300 g of modified starch (Purity Gum BE: manufactured by NSC Japan) and 400 g of dextrin (Paindex No. 1: manufactured by Matsutani Chemical Industry Co., Ltd.) in 1300 g of soft water, 300 g of lemon oil was added and emulsified with a homomixer. Emulsification was performed to a particle size of about 0.5 μm to 2 μm to obtain an O / W emulsion. Next, 1000 g of 25% shellac aqueous solution of pH 7.0 was added to and mixed with this O / W emulsion, and this emulsion was heated at a hot air inlet temperature of 150 ° C. using a mobile minor type spray dryer (manufactured by GAE Process Engineering Co., Ltd.). Spray drying was performed at an exhaust air temperature of 80 ° C. and an atomizer rotational speed of 20000 rpm to obtain a dried product. The obtained dried product was sieved with 30 mesh to obtain 1250 g of a powdered fragrance (Comparative product 6: containing lemon oil 24% and shellac 20%).

[Comparative Example 7]
Reference product 2 (100 g) was mixed with 41.5 g of powdered shellac in advance, and then 41.5 g of shellac ethanol solution in which shellac was mixed and dissolved in 95% ethanol in an equivalent amount by mass. The mixed product was extruded with a 0.7 mm screen using an extrusion granulator basket ruser (manufactured by Fuji Paudal Co., Ltd.) and dried with a vacuum dryer at 1 Pa, 60 ° C. for 15 hours. The obtained dried product was sieved with 30 mesh to obtain 162.25 g of a dried product (Comparative product 7: containing lemon oil 18.5% and shellac 38.4%).

Flavor dissolution test 2 (Aroma testing and sensory evaluation of chewing gum)
Add the reference product 2, the present invention product 6 or the comparative products 5 to 7 to the same base material as the flavor elution test 1 so that the lemon oil content in the chewing gum is 0.18%, and use a high shear mixer. The mixture was mixed at about 50 ° C. by a conventional method, and after cooling, it was subjected to pressure forming by rolling onto a roll to prepare 3 g of chewing gum.

  The obtained chewing gum was sensoryly evaluated by the same method as in dissolution test 1 for the duration and strength of the lemon aroma when chewing gum was chewed by a panel of 10 experts. The average evaluation results are shown in Table 3.

  As shown in Table 3, the reference product 2 containing no shellac showed a sharp flavor peak after about 1 minute, and then the flavor decreased sharply and the flavor disappeared after about 5 minutes. On the other hand, the product 6 of the present invention prepared by the method of the present invention (containing 50% shellac) showed a peak of flavor after 5 to 9 minutes, then decreased gradually, and the flavor was sustained for 15 minutes or more. . Moreover, it had a fresh aroma and flavor of lemon. Although the comparative product 5 which raised the heat-melting temperature had the same fragrance expression as the product 6 of the present invention, it was poor in the freshness of the lemon top and felt a slightly deteriorated odor. Comparative product 6 (containing 20% shellac) is a product obtained by adding a shellac alkaline aqueous solution in advance at the time of preparing a lemon powder flavor as a core substance, that is, emulsifying lemon oil, and then obtaining a powder by spray drying. The expression of was weak, unclear, and had a peak at 8-10 minutes, but was not very noticeable and disappeared around 13 minutes. Comparative product 7 (containing 38.4% shellac) was encapsulated using an ethanol solution of shellac instead of the heating and melting method of the present invention, but the expression of flavor was weak and unclear, 8-10. There is a peak at the minute, but it was not so noticeable and disappeared around 12 minutes.

Test Reference Product 2 for Storage Stability 2, Invention Product 6 and Comparative Products 5 to 7 were each taken in a 7 cm × 11 cm plastic bag of 30 g, sealed, and subjected to a storage test at 40 ° C. in a dark place for 4 weeks. . The sample after storage was diluted in 0.1% water (0.07% only for the reference product 1), and sensory evaluation was performed by 10 well-trained panelists. Table 4 shows the average sensory evaluation results of 10 people.

  As shown in Table 4, the reference product 2 (powder flavor of lemon oil) had a strong lemon odor due to storage, but the product 6 of the present invention maintained a fresh flavor of lemon even after a storage test. However, it was found that no deterioration odor was felt and the storage stability was very good. On the other hand, the comparative product 5 in which the heating and melting temperature was raised decreased the fresh fragrance of the lemon and felt a deteriorated odor of the lemon. Comparative product 6 (containing 20% shellac) is a powder obtained by spray drying after adding a shellac alkaline aqueous solution in advance when preparing a lemon powder fragrance as a core substance, that is, emulsifying lemon oil. The fresh scent of lemon was slightly weakened and a slightly deteriorated odor was felt. Furthermore, comparative product 7 (containing 38.4% shellac) was encapsulated using an ethanol solution of shellac instead of the heating and melting method of the present invention, but the fresh aroma of lemon was slightly weakened. A slight odor was felt. Therefore, according to the present invention, the powder composition obtained by mixing the core material and shellac in a powder state, heating and melting, cooling, solidifying, and pulverizing is more than the powder composition coated with the shellac solution. It was shown that the storage stability was good.

[Reference Example 3] (Preparation of butter flavor powder fragrance)
After 300 g of modified starch and 400 g of dextrin are dissolved in 1300 g of soft water, 300 g of butter flavor (manufactured by Hasegawa Fragrance Co., Ltd.) is added and emulsified with a homomixer to an emulsified particle size of about 0.5 μm to 2 μm to obtain an O / W emulsion. Obtained. This emulsion is spray-dried using a mobile minor type spray dryer (manufactured by GAE Process Engineering Co., Ltd.) at a hot air inlet temperature of 150 ° C., an exhaust air temperature of 80 ° C. and an atomizer speed of 20000 rpm, and a butter flavor of 30 % Powder fragrance 1000% was obtained (reference product 3). As a result of measuring the particle size of Reference Product 3 on a volume basis by a dry method using a laser diffraction / scattering particle size distribution analyzer, the average particle size (median diameter) was 64.8 μm.

[Example 7]
Reference product 3 (100 g) and powdered shellac 100 g are mixed in advance, heated and melted with a biaxial extruder EA-20 (manufactured by Suehiro EPM), and extrusion melt-molded with a die of a screen 2 mm × 12 holes. went.

Extrusion conditions: Temperature when the mixture is melted: 92 ° C
Die surface set temperature: 70 ° C
Product temperature when extruded from the die: 81 ° C
Screw rotation speed: 60rpm
The extruded mixture is placed in a string so as not to overlap the stainless steel tray, blown to cool to room temperature and solidified, and then the obtained granule is pulverized and sieved with 30 mesh to obtain 200 g of a powder composition. (Invention product 7: containing 15% butter flavor and 50% shellac).

[Comparative Example 8]
After dissolving 300 g of modified starch (Purity Gum BE: manufactured by NSC Japan) and 400 g of dextrin (Paindex No. 1: manufactured by Matsutani Chemical Co., Ltd.) in 1300 g of soft water, 300 g of butter flavor (manufactured by Hasegawa Fragrance Co., Ltd.) is added. The emulsion was emulsified with a homomixer to an emulsified particle size of about 0.5 μm to 2 μm to obtain an O / W emulsion. Next, 1000 g of 25% shellac aqueous solution of pH 7.0 was added to and mixed with this O / W emulsion, and this emulsion was heated at a hot air inlet temperature of 150 ° C. using a mobile minor type spray dryer (manufactured by GAE Process Engineering Co., Ltd.). Spray drying was performed at an exhaust air temperature of 80 ° C. and an atomizer rotational speed of 20000 rpm to obtain a dried product. The obtained dried product was sieved with 30 mesh to obtain 1250 g of a powder fragrance (Comparative product 8: containing 24% butter flavor and 20% shellac).

[Comparative Example 9]
Reference product 3 (100 g) was mixed with 41.5 g of powdered shellac in advance, and then 41.5 g of shellac ethanol solution in which shellac was mixed and dissolved in 95% ethanol in an equal amount by mass. The mixed product was extruded with a 0.7 mm screen using an extrusion granulator basket ruser (manufactured by Fuji Paudal Co., Ltd.) and dried with a vacuum dryer at 1 Pa, 60 ° C. for 15 hours. The obtained dried product was sieved with 30 mesh to obtain 162.25 g of a dried product (Comparative product 9: containing 18.5% butter flavor and 38.4% shellac).

Sensory evaluation (mixed into baked goods)
According to the following formulation, cookie dough is mixed, and the reference product 3, the inventive product 7, the comparative product 8 or the comparative product 9 is added to the cookie so that the content of butter flavor in the cookie is 0.2%. The cookie was prepared by extending to 5 mm, cutting to a size of 3 cm × 3 cm, baking for 15 minutes in an oven heated to 170 ° C., and cooling.

The obtained cookie was subjected to sensory evaluation by a professional panel of 10 people. The average evaluation results are shown in Table 5.
(Cookie dough formulation example)
Soft flour 100.0 parts by mass Powdered sugar 60.0
Shortening 30.0
Nonfat dry milk 5.0
Salt 1.0
Sodium bicarbonate 0.8
Ammonium bicarbonate 1.0
Water 18.0
Perfume composition (reference product 3, invention product 7, comparative product 8, comparative product 9) Addition amount of Table 5

  As shown in Table 5, Reference Product 3 containing no shellac had a buttery flavor but was weak and did not feel much of its characteristics. However, the product 7 of the present invention was good with a fresh but fragrant characteristic scent spreading in the mouth. On the other hand, when preparing a butter flavor powder fragrance as a core substance, that is, using a comparative product 8 in which powder was obtained by spray drying after adding an aqueous shellac aqueous solution in advance during emulsification of butter flavor, and an ethanol solution of shellac Each of the encapsulated comparative products 9 had a stronger butter flavor than the reference product 3, but the characteristics were not felt so much, and the freshness and spread in the mouth were insufficient. Therefore, it was shown that the product of the present invention coated with shellac by heat extrusion melting has high thermal stability.

[Example 8]
Aspartame 100 g (manufactured by Ajinomoto Co., Inc .: hereinafter referred to as reference product 4) and 60 g of powdered shellac are mixed in advance, heated and melted with a biaxial extruder EA-20 (manufactured by Suehiro EPM), and screen 2 mm × 12 Extrusion melt molding was performed with a hole die.

Extrusion conditions: Temperature when the mixture is melted: 82 ° C
Die surface set temperature: 60 ° C
Product temperature when extruded from the die: 71 ° C
Screw rotation speed: 60rpm
The extruded mixture is placed in a string so as not to overlap the stainless steel tray, blown to cool to room temperature and solidified, and then the obtained granules are pulverized and sieved with 30 mesh to obtain 160 g of a powder composition. (Invention product 8: containing 62.5% aspartame, 37.5% shellac).

Flavor elution test 3 (Aroma test and sensory evaluation on chewing gum)
Add 0.75% of the reference product 4 (aspartame) or 1.2% of the product 8 of the present invention to the chewing gum base shown below, mix at about 50 ° C. using a high shear mixer, and cool. It was press-molded on the rear roll to prepare 3 g of chewing gum.

  The obtained chewing gum was sensorially evaluated by the same method as the flavor elution test 1 for the duration and intensity of sweetness when chewing gum was chewed by a panel of 10 experts. The average evaluation results are shown in Table 6.

Chewing gum base material Raw material Blending amount Chewing gum base 270 parts by weight Sorbitol 90
Hydrogenated palm oil 60
Corn syrup (Bx85) 30
Glycerin 3

  As shown in Table 6, the reference product 4 reached a sweetness peak in 1 minute and almost no sweetness was felt after 5 minutes, whereas the product 8 of the present invention had a low sweetness peak immediately after the start of chewing, Sweetness persisted even after 15 minutes from chewing, and it was confirmed that the flavor persistence was high.

[Example 9]
100 g of anhydrous powdered citric acid (produced by Iwata Chemical Co., Ltd.): hereinafter referred to as reference product 5) and 60 g of powdered shellac are mixed in advance and heated with a biaxial extruder EA-20 (produced by Suehiro EPM). Then, extrusion melt molding was performed using a die having a screen size of 2 mm × 12 holes.

Extrusion conditions: Temperature when the mixture is melted: 82 ° C
Die surface set temperature: 60 ° C
Product temperature when extruded from the die: 71 ° C
Screw rotation speed: 60rpm
The extruded mixture is placed in a string so as not to overlap the stainless steel tray, blown to cool to room temperature and solidified, and then the obtained granules are pulverized and sieved with 30 mesh to obtain 160 g of a powder composition. (Invention product 9: containing 62.5% citric acid and 37.5% shellac).

Flavor elution test 4 (Aroma test and sensory evaluation on chewing gum)
0.75% of Reference product 5 (anhydrous powdered citric acid) or 1.2% of the product 9 of the present invention was added to the same base material as the flavor elution test 1 and about 50 ° C. by a conventional method using a high shear mixer. The mixture was cooled, and after cooling, it was press-molded on a roll to prepare 3 g of chewing gum.

  The obtained chewing gum was sensorially evaluated by the same method as the flavor elution test 1 for the duration and strength of sourness when chewing gum was chewed by a professional panel of 10 people. Table 7 shows the average evaluation results.

  As shown in Table 7, the reference product 5 reached a sour peak in 1 minute and almost no sourness was felt after 5 minutes, whereas the product 9 of the present invention had a low sour peak immediately after the start of chewing, Even after 15 minutes from chewing, the sourness was maintained, and it was confirmed that the sourness was high.

Claims (3)

The average particle diameter (median diameter) when measured on a volume basis by a dry method using a laser diffraction / scattering particle size distribution measuring device is 10 μm to 2000 μm, powder flavor, powder sweetener, powder seasoning, powder One or more powdery core materials selected from acidulants, powdered bitters, powder pigments and powdered vitamins , and powdered or flaky shellac are mixed in a powder state, and these mixtures are heated. A method for producing a sustained-release powder composition, which is cooled, solidified, and pulverized after being melted or semi-molten. The method for producing a sustained-release powder composition according to claim 1, wherein shellac is contained in the powder composition in an amount of 5% to 70% in terms of mass. The method for producing a sustained-release powder composition according to claim 1 or 2, wherein a heating temperature for obtaining a molten or semi-molten state is 50 ° C to 110 ° C.