JP2005194419A - Perfume capsule and bathing agent containing the same - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a perfume capsule excellent in long-period persistency and stability of perfume, being stable to sodium hydrogencarbonate, sodium sulfate, or the like, not causing deterioration thereby and free from deterioration and capable of retaining good aroma over a long time when charged into a water kept at a relatively high warm temperature of 38-42°C, and to obtain a bathing agent in which the perfume capsule is formulated. <P>SOLUTION: The perfume capsule is obtained by encapsulating a perfume ingredient by using a modified pregelatinized starch as an encapsulating material. The modified pregelatinized starch comprises, as at least a part, at least one kind of starch of modified pregelatinized starches forming an aqueous solution having ≥50 cps viscosity when measuring the viscosity at 30°C after heating the starch for 5 min at 80°C in a form of 20% aqueous solution. The bathing agent is obtained by formulating the perfume capsule. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  The present invention relates to a perfume capsule and a bath containing the same. More specifically, the present invention is excellent in long-term stability, does not deteriorate or deteriorate in fragrance even when exposed to a high temperature for a long period of time, can release a good fragrance over a long period of time, and is a bath agent. It is related with the fragrance | flavor capsule which is hard to produce a degeneration by components, such as sodium sulfate contained in etc., and the bath agent which mix | blended this fragrance | flavor capsule.

In a conventional bath agent, various fragrances are blended in order to enhance the feeling of use, but the volatility of the fragrance blended in the bath agent varies, and it is necessary to adjust the aroma well.
However, bathing agents containing fragrances have different characteristics of the components that make up the fragrances, and are used in warm water at a relatively high temperature such as 38 to 42 ° C., so the balance of the fragrances tends to be lost during use. The present condition is that a pleasant fragrance cannot be maintained for a long time.

  In many of the conventional powder baths, a mixture of sodium hydrogen carbonate and sodium sulfate is used as a base, but the fragrance component is inferior in stability to the base, and accordingly, during storage and use There is a problem that fragrance changes easily.

  Therefore, in order to improve the stability of the fragrance component in the bath agent, a fragrance powder for bath agent in which the fragrance is mixed and dispersed in dextrin or gum arabic is known. However, even if this bath fragrance powder is blended in the bath tub, it is difficult to smoothly adjust the fragrance and control the volatilization of the fragrance. In addition, the fragrance component is likely to be altered by bases such as sodium bicarbonate and sodium sulfate, which are often contained in bathing agents, and it was difficult to maintain the fragrance well in the bathing agent for a long period of time. .

  It consists of a modified starch (such as a modified starch treated with octenyl succinic anhydride) that forms a low-viscosity aqueous solution for the purpose of improving the storage stability of perfume ingredients and spreading a good aroma during and after the washing process. Encapsulated perfume particles in which a specific perfume component is encapsulated in a matrix have been proposed (see Patent Document 1). However, the encapsulated fragrance particles have been developed for the purpose of giving a fragrance impact to the cleaning composition, and have not been developed for use in bathing agents. Therefore, when the encapsulated fragrance particles of Patent Document 1 are blended in a bath agent, the fragrance encapsulated in the capsule particles by a base such as sodium sulfate or sodium hydrogen carbonate that is often contained in the bath agent. It tends to change in quality and cause a decrease in fragrance, and a good fragrance cannot be maintained over a long period of time. Moreover, when the encapsulated fragrance particles of Patent Document 1 are put into a hot water for bathing, which is generally at a high temperature of 38 to 42 ° C., the fragrance easily disappears or modulates in a short time, and the fragrance capsule for bathing agents Is inappropriate.

Japanese translation of PCT publication No. 2002-513073

An object of the present invention is to provide a fragrance material that is excellent in storage stability, has a small decrease in fragrance and changes in quality even when stored at a high temperature for a long period of time, and can maintain a good fragrance over a long period of time.
Furthermore, the object of the present invention is excellent in stability to bases such as sodium hydrogen carbonate and sodium sulfate, which are often used in bathing agents. It is to provide a perfume material that does not easily occur.
In addition, the object of the present invention is to prevent the fragrance from deteriorating or deteriorating and to maintain a good fragrance even when it is blended in a bath agent and poured into hot water for bathing at a relatively high temperature of 38 to 42 ° C. It is to provide a perfume material that can be maintained over time.
And the objective of this invention is providing the bath agent excellent in the stability of fragrance and the sustainability which mix | blended the fragrance | flavor material which has the above-mentioned favorable characteristic.

The inventors of the present invention have continually studied to achieve the above object. As a result, a perfume capsule in which a perfume component is encapsulated using a modified pregelatinized starch as an encapsulating material is prepared. At that time, as a part of the modified pregelatinized starch, a 20% aqueous solution is formed and heated at 80 ° C. for 5 minutes. Use of at least one modified pregelatinized starch that forms an aqueous solution having a viscosity of 50 cps or more when measured at 30 ° C. provides excellent long-term storage stability, and reduces fragrance and changes in quality even when exposed to high temperatures. It has been found that a perfume capsule that hardly occurs and maintains a good fragrance over a long period of time can be obtained.
Furthermore, the present inventors have found that the perfume capsules formed using the specific modified pregelatinized starch are not easily affected by sodium bicarbonate or sodium sulfate, which are often used in bathing agents, and have excellent stability. Therefore, it has been found that when the fragrance capsule is blended in a bath agent, a bath agent excellent in storage stability capable of maintaining a good fragrance over a long period of time can be obtained.
Moreover, when the bathing agent which mix | blended the fragrance | flavor capsule formed using the said specific modified | denatured pregelatinized starch was thrown into the hot water for bathing of comparatively high temperature like 38-42 degreeC, It was found that the fragrance is less likely to deteriorate or deteriorate, and the original good fragrance is maintained in hot water for a long time.

  Furthermore, the present inventors made a fragrance capsule using the specific modified pregelatinized starch that forms an aqueous solution having a viscosity of 50 cps or more when measured at 30 ° C. after being heated at 80 ° C. for 5 minutes in a 20% aqueous solution. In forming the fragrance, the modified pregelatinized starch that forms an aqueous solution having a viscosity of 50 cps or more is used in combination with the modified pregelatinized starch that forms an aqueous solution having a viscosity of less than 50 cps when measured under the same conditions as described above. We found that capsules have excellent characteristics of long-term storage stability and sustainability of fragrance, and moreover, when blended into bathing agents, a strong fragrance is gradually released over a long period of time. Based on this, the present invention has been completed.

That is, the present invention
(1) A fragrance capsule in which a fragrance component is encapsulated using a modified pregelatinized starch as an encapsulating material, and at least a part of the modified pregelatinized starch constituting the encapsulating material is made into a 20% aqueous solution at 80 ° C. A fragrance capsule characterized by using at least one modified pregelatinized starch that forms an aqueous solution having a viscosity of 50 cps or more when measured at 30 ° C. after heating for 30 minutes.

And this invention,
(2) A fragrance capsule in which a fragrance component is encapsulated using a modified pregelatinized starch as an encapsulating material, and is a 20% aqueous solution as a modified pregelatinized starch forming an encapsulating material, and after heating at 80 ° C. for 5 minutes, 30 At least one modified pregelatinized starch that forms an aqueous solution having a viscosity of 50 cps or more when measured at 0 ° C, and a viscosity of less than 50 cps when measured at 30 ° C after heating at 80 ° C for 5 minutes in a 20% aqueous solution. It is a fragrance | flavor capsule characterized by using together the at least 1 sort (s) of the modified pregelatinized starch which forms the aqueous solution which has.

Furthermore, the present invention provides
(3) Modified encapsulated starch that forms an aqueous solution having a viscosity of 50 cps or more when measured at 30 ° C. after heating at 80 ° C. for 5 minutes in a 20% aqueous solution in an encapsulating material, and 80 ° C. in a 20% aqueous solution. The ratio of the modified pregelatinized starch that forms an aqueous solution having a viscosity of less than 50 cps when measured at 30 ° C. after heating for 5 minutes at a ratio of the former: latter = 10: 90 to 80:20 (2) Perfume capsules; and
(4) A modified pregelatinized starch that forms an aqueous solution having a viscosity of 50 cps or more when measured at 30 ° C. after being heated at 80 ° C. for 5 minutes in a 20% aqueous solution has a viscosity of 100 cps or more when measured under the same conditions. The perfume capsule according to any one of (1) to (3) above, which is a modified pregelatinized starch that forms an aqueous solution;
It is.

And this invention,
(5) The fragrance capsule according to any one of (1) to (4), wherein the fragrance component is contained at a ratio of 20 to 90% by mass based on the total mass of the fragrance capsule;
(6) The fragrance capsule according to any one of the above (1) to (5), which contains limonene as a fragrance component; and
(7) The fragrance capsule according to any one of (1) to (6), wherein limonene is contained in a proportion of 50% by mass or more based on the mass of the fragrance component;
It is.

Furthermore, the present invention provides
(8) A bathing agent containing the fragrance capsule according to any one of (1) to (7).

The fragrance capsule of the present invention is excellent in scent sustainability and stability, and even after long-term storage, especially after long-term storage at high temperature, there is little deterioration and deterioration of the scent, and a good scent can be maintained over a long period of time. .
The perfume capsules of the present invention are stable against bases such as sodium bicarbonate and sodium sulfate, which are often used in bathing agents, and are not easily altered. Therefore, the bath containing the fragrance capsule of the present invention, the fragrance component contained in the bath is not easily altered by the base, and thereby can maintain a good fragrance over a long period of time,
The bathing agent containing the fragrance capsule of the present invention is less likely to cause a decrease in fragrance or alteration when placed in hot water for bathing such as 38 to 42 ° C. Can be held over time.
In particular, as a denatured pregelatinized starch forming an encapsulating material, a denatured pregelatinized starch that forms an aqueous solution having a viscosity of 50 cps or more when measured at 30 ° C after heating at 80 ° C for 5 minutes in a 20% aqueous solution, and The fragrance capsule of the present invention formed by using a modified pregelatinized starch that forms an aqueous solution having a viscosity of less than 50 cps when measured under the same conditions is more excellent in the long-term storage stability and sustainability of the fragrance, and is also a bath agent Releases a strong fragrance gradually over a longer period of time when blended in.

The present invention is described in detail below.
The fragrance capsule of the present invention is a fragrance capsule encapsulating a fragrance component using a modified pregelatinized starch as an encapsulant, wherein at least a part of the modified pregelatinized starch forming the encapsulant is a 20% aqueous solution. Modified pregelatinized starch that forms an aqueous solution having a viscosity of 50 cps or more when measured at 30 ° C after heating at 80 ° C for 5 minutes [hereinafter this modified pregelatinized starch is referred to as “modified pregelatinized starch (≧ 50 cps; 20% aq)”] It is necessary to consist of at least one of the above.
At that time, as the modified pregelatinized starch (≧ 50 cps; 20% aq), only one kind may be used or two or more kinds may be used in combination.
Among them, the modified pregelatinized starch (≧ 50 cps; 20% aq) has a viscosity of 100 cps or more, particularly 100 to 200 cps when measured at 30 ° C. after heating at 80 ° C. for 5 minutes in a 20% aqueous solution. A modified pregelatinized starch that forms an aqueous solution is more preferably used.

Denatured pregelatinized starch is a paste obtained by swelling or dissolving modified starch in water or hot water and rapidly dehydrating and drying it in the state of glue, and is dispersed in water at room temperature.・ Swells and can easily reproduce paste. Examples of the modified starch that forms the base of the modified pregelatinized starch include various modified starches such as oxidized starch, derivative starch (starch acetate ester, starch phosphate ester, various starch ether phosphates, cross-linked starch, etc.).
In the present invention, as a denatured pregelatinized starch (≧ 50 cps; 20% aq), among the above-mentioned denatured pregelatinized starches, a 20% aqueous solution is used and heated at 80 ° C. for 5 minutes and then measured at 30 ° C. Any modified pregelatinized starch that forms an aqueous solution having a viscosity can be used. Among them, the pregelatinized hydrolyzed starch that forms an aqueous solution having a viscosity of 50 cps or more is capable of maintaining the fragrance in a perfume capsule, and releasing it slowly. It is preferably used from the standpoints of effects, scent alteration prevention, and the like.

  The modified pregelatinized starch (≧ 50 cps; 20% aq) used in the fragrance capsule of the present invention is conventionally known, and various products are sold. In the present invention, commercially available products can be used as appropriate. . Specific examples of the modified pregelatinized starch (≧ 50 cps; 20% aq) that can be suitably used in the present invention include “N Creamer 46” manufactured by National Starch & Chemical Co., Ltd.

In the present invention, only the modified pregelatinized starch (≧ 50 cps; 20% aq) may be used as the modified pregelatinized starch for forming the capsule, or the modified pregelatinized starch (≧ 50 cps; 20% aq). In addition, other modified pregelatinized starches may be used in combination.
Among them, in the present invention, when the denatured pregelatinized starch forming the encapsulating material is measured together with the denatured pregelatinized starch (≧ 50 cps; 20% aq) and a 20% aqueous solution heated at 80 ° C. for 5 minutes and then measured at 30 ° C. It is more preferable to use a modified pregelatinized starch that forms an aqueous solution having a viscosity of less than 50 cps (hereinafter, this modified pregelatinized starch may be referred to as “modified pregelatinized starch (<50 cps; 20% aq)”).
As a modified pregelatinized starch that forms an encapsulating material, a combination of modified pregelatinized starch (≧ 50 cps; 20% aq) and modified pregelatinized starch (<50 cps; 20% aq) can improve the long-term storage stability and durability of the scent. It is possible to obtain a fragrance capsule which is more excellent and can maintain a strong fragrance with a good fragrance over a long period of time when it is blended in a bath agent and gradually releases a strong fragrance over a longer period of time.

  Modified pregelatinized starch (<50 cps; 20% aq) is a modified starch, oxidized starch, derivative starch (starch acetate, starch phosphate, various starch ether phosphates, cross-linked starch, etc.) A paste-like product prepared by swelling or dissolving starch (modified starch) in water or hot water was obtained by rapidly dehydrating and drying the paste in the form of a paste. Modified pregelatinized starch (≧ 50 cps) As well as 20% aq), which is conventionally known and various products are sold. In the present invention, commercially available products can be used as appropriate. Specific examples of modified pregelatinized starch (<50 cps; 20% aq) that can be suitably used in the present invention include “Purity Gum BE” and “Capsule” manufactured by National Starch & Chemical Co., Ltd. .

  By using a modified pregelatinized starch (≧ 50 cps; 20% aq) and a modified pregelatinized starch (<50 cps; 20% aq) that form aqueous solutions having different viscosities, and adjusting the blending ratio of the two, Bases (such as sodium sulfate and sodium hydrogen carbonate) that can adjust the volatilization rate and volatilization pattern of the perfume ingredients from the capsules and are contained in products such as bathing agents that contain the perfume capsules. It is possible to prevent the fragrance ingredient from being altered or deteriorate with time, and to maintain a good fragrance for a longer time.

In the fragrance capsule of the present invention, the ratio of the modified pregelatinized starch in the encapsulated material from the viewpoints of ease of manufacture of the fragrance capsule, long-term storage of the fragrance capsule, scent sustainability, sustained release performance, feel during use, etc. [The ratio of the entire modified pregelatinized starch including the modified pregelatinized starch (≧ 50 cps; 20% aq)] is preferably 50% by mass or more based on the total mass of the encapsulated material, and is 60 to 100 mass. %, More preferably 70 to 95% by mass.
Moreover, the ratio of the modified pregelatinized starch (≧ 50 cps; 20% aq) in the encapsulating material is the modified pregelatinized starch used as the encapsulating material from the viewpoints of scent sustainability, sustained release performance, feel during use, etc. It is preferably 15% by mass or more, more preferably 20% by mass or more, and still more preferably 20 to 80% by mass based on the total mass.

  In addition, when using a modified pregelatinized starch (≧ 50 cps; 20% aq) and a modified pregelatinized starch (<50 cps; 20% aq) as the modified pregelatinized starch as the encapsulating material, Although it can be adjusted according to the type and amount of the flavor component to be encapsulated, in general, [denatured pregelatinized starch (≧ 50 cps; 20% aq)]: [denatured pregelatinized starch (<50 cps; 20% aq) ] = 10: 90 to 80:20 is preferable from the viewpoints of ease of formation of the fragrance capsule, sustained release of the fragrance from the fragrance capsule, processability, and the like, and 20:80 to 70:30. The mass ratio is more preferable.

The encapsulating material forming the fragrance capsule of the present invention is mainly composed of modified pregelatinized starch and contains modified pregelatinized starch (≧ 50 cps; 20% aq) as at least a part of the modified pregelatinized starch. It may consist only of modified pregelatinized starch or may contain other components along with the modified pregelatinized starch.
Preferable examples of other components that can be used with the modified pregelatinized starch include saccharides. Specific examples of saccharides in that case include monosaccharides such as glucose, fructose, mannose, galactose, xylose, arabinose and ribose, disaccharides such as maltose, lactose and sucrose, dextrins obtained by hydrolyzing starch with acid or enzyme, Examples thereof include sugar alcohols such as mannitol, sorbit, and malbit, and one or more of these can be used, and among these, dextrins are preferably used.

When the fragrance capsule of the present invention contains other components such as the above-mentioned saccharides as a part of the encapsulating material, the use ratio of the other components is 50% by mass or less based on the total mass of the encapsulating material. It is preferable that it is 45 mass% or less, and it is further more preferable that it is 5-30 mass%.
The fragrance capsule of the present invention is a part of the encapsulated material together with the above-mentioned modified pregelatinized starch from the viewpoint of ease of production of the fragrance capsule, sustainability of the fragrance in the fragrance capsule, sustained release, and feel during use. It is preferable that saccharides (particularly dextrins) are contained in a proportion of 5 to 30% by mass, particularly 10 to 20% by mass, based on the total mass of the encapsulating material.

  As a fragrance | flavor component enclosed with the fragrance | flavor capsule of this invention, as long as it is a fragrance | flavor component used for a normal scented product, any may be sufficient. In particular, when the fragrance capsule of the present invention is used as a bath agent or the like, as a fragrance component, for example, a hydrocarbon-based fragrance such as limonene, pinene, γ-terpinene, caryophyllene; phenylethyl alcohol, terpineol, paxanol, geraniol, nerol, Alcohol flavors such as linalool and cis-3-hexenol; Aldehyde flavors such as lyial, citral, aldehyde C-8, aldehyde C-9, aldehyde C-11, hexylcinnamic aldehyde, vanillin, and heliotropin; Mention may be made of ketone-based fragrances such as phenone, woody flow, damascon, and ISOE super; other fragrances such as musks, eugenol, coumarin, etc. The fragrance capsule of the present invention is one of the fragrances described above as a fragrance component or It may contain more species.

  The types of flavor components that can be used in the flavor capsule of the present invention include, for example, eggplant-type flavors, forest flavor-type flavors, Japanese cypress-type flavors, rose-flavor-type flavors, jasmine flavor-type flavors, lavender-type flavors, and chamomile-type flavors. And so on.

  The content of the fragrance component in the fragrance capsule can be adjusted according to the kind of fragrance and the use of the fragrance capsule, etc., but the ease of manufacture of the fragrance capsule, the strength of the fragrance, the persistence of the fragrance, the feel during use, etc. In general, the content is preferably 20 to 90% by mass, more preferably 40 to 70% by mass based on the total mass of the fragrance capsule.

  The size (particle size) of the fragrance capsule of the present invention is not particularly limited, but it is easy to manufacture, uniform mixing when blended in a bath agent, etc., fragrance divergence, fragrance persistence, feel during use, etc. In general, the average particle diameter is preferably 30 to 200 μm, and more preferably 60 to 100 μm.

The method for producing the fragrance capsule of the present invention is not particularly limited, and any method may be used as long as the above-described fragrance capsule of the present invention can be produced smoothly. Generally, after the modified pregelatinized starch is dispersed or dissolved in water or hot water alone, or after other components such as the modified pregelatinized starch and sugar are dispersed or dissolved in water or hot water, the perfume ingredients are added there. And then using an emulsifier such as a homomixer or homogenizer to prepare an oil-in-water emulsion and evaporating the water from the emulsion by a process such as freeze drying or spray drying. The fragrance capsules of the invention can be produced.
At that time, by setting the emulsion size (oil droplet size) of the fragrance component in the emulsion to 0.5 to 10 μm, particularly 0.5 to 1.0 μm, the average particle size is 30 to 200 μm, especially A perfume capsule of 60 to 100 μm can be produced smoothly.

The perfume capsules of the present invention can be used for bathing agents, cleaning agents, bleaching agents and the like. The perfume capsules of the present invention are sodium sulfate and sodium bicarbonate, which are often used as a base in bathing agents, even when placed in relatively hot water such as 38 to 42 ° C. It is difficult to cause deterioration or deterioration with time. Therefore, the perfume capsule of the present invention is suitable as a perfumed product for bathing agents, and therefore the present invention includes a bathing agent in which the perfume capsules of the present invention are blended.
The blending amount of the fragrance capsule in the bath agent can be adjusted according to the content of the fragrance component in the fragrance capsule, the kind of the fragrance component contained in the fragrance capsule, etc., but generally based on the total mass of the bath agent. 0.1 to 10% by mass is preferable from the viewpoint of fragrance strength, sustainability and solubility, and more preferably 0.5 to 5% by mass.

  In addition to the above-mentioned perfume capsules, the bathing agent of the present invention contains a moisturizer, enzyme agent, binder, disintegrant, foaming agent, dispersant, coloring agent, surfactant, buffering agent, stabilizer as necessary. One or two or more kinds of components conventionally blended in a bath agent such as a pH adjuster can be contained. Furthermore, the bath agent of this invention can contain another fragrance | flavor component with the fragrance | flavor capsule of this invention. The blending amount of the various components described above can be set to the same level as conventionally used in bathing agents. Moreover, the bath agent of this invention can devise 1 type (s) or 2 or more types of various medicinal components (For example, a hot spring component, a herbal medicine component, a plant extract etc.) as needed.

  The form of the bathing agent of the present invention is not particularly limited, but it is preferable from the viewpoint of handleability to form powders, granules, tablets, effervescent tablets and the like. Moreover, the bath agent of this invention can be distribute | circulated and sold by subdividing into an appropriate bag and a container for every one use, or filling it in bulk. Examples of such bags and containers include bags and containers formed from laminated films and sheets obtained by laminating polyethylene and other resin layers on aluminum foil, and synthetic resin containers manufactured by molding such as injection molding and press molding. Can be mentioned.

  The dose per bathing agent of the present invention can be appropriately adjusted according to the type and concentration of the active ingredient used in the bathing agent, the bath agent type, the bathing temperature, etc., but generally per 200 liters of bathing bath. About 5 to 200 g, particularly about 10 to 100 g is preferable. However, the amount is not necessarily limited.

Hereinafter, the present invention will be specifically described with reference to examples and the like, but the present invention is not limited to the following examples.
In the following examples, the viscosity of a 20% aqueous solution of modified pregelatinized starch (hereinafter sometimes referred to as “viscosity (20% aq)”) was measured as follows.

[Measurement of modified pregelatinized starch viscosity (20% aq)]
40 g of modified pregelatinized starch is added to 160 g of water at a temperature of 20 ° C. to make a 20% aqueous solution, which is heated to 80 ° C. with stirring, maintained at 80 ° C. with stirring for 5 minutes, and then cooled to 30 ° C. The viscosity of the aqueous solution immediately after reaching 30 ° C. was measured using a viscometer (“Tokimec Viscometer BM Type” manufactured by Tokimec Corporation; Spindle No. 1 30 rpm, Spindle No. 2 30 rpm).

<< Example 1 >> [Production of fragrance capsule (a) (fragrance ingredient: limonene)]
(1) Modified Purified Starch “Purity Gum BE” [National Starch & Chemical Co., Ltd .; Viscosity (20% aq) = 40 cps] 35 g, Modified Alphaized Starch “N Creamer 46” [National Starch & Chemical Co .; viscosity (20% aq) = 165 cps] 10 g and dextrin 10 g were dispersed in 200 g of water at a temperature of 20 ° C., then heated to 70 ° C. with stirring, and when the liquid became transparent, limonene After 55 g was added and mixed uniformly, an emulsion having an emulsion size of 0.5 to 1.0 μm was prepared using an emulsifier.
(2) The emulsion prepared in the above (1) was spray-dried (drying temperature 120 to 200 ° C.) to produce a fragrance capsule [fragrance capsule (a)] encapsulating limonene [containing limonene in the fragrance capsule (a) Amount = 50 mass%; average particle size of perfume capsules = 80 μm].

<< Example 2 >> [Production of fragrance capsule (b) (fragrance ingredient: limonene)]
(1) 45 g of the same modified pregelatinized starch “N Creamer 46” [viscosity (20% aq) = 165 cps] used in Example 1 and 10 g of dextrin were dispersed in 200 g of water at a temperature of 20 ° C. and stirred. The mixture was heated to 70 ° C. and when the liquid became transparent, 55 g of limonene was added and mixed uniformly, and then an emulsion having an emulsion size of 0.5 to 1.0 μm was prepared using an emulsifier. .
(2) The emulsion prepared in the above (1) was spray-dried (drying temperature 120 to 200 ° C.) to produce a fragrance capsule [fragrance capsule (b)] encapsulating limonene [containing the limonene in the fragrance capsule (b) Amount = 50 mass%; average particle size of perfume capsules = 80 μm].

<< Example 3 >> [Manufacture of fragrance capsule (c) (fragrance ingredient: cocoon type fragrance)]
(1) 35 g of the same modified pregelatinized starch “Purity Gum BE” used in Example 1 [Viscosity (20% aq) = 40 cps], modified pregelatinized starch “N Creamer 46” [Viscosity (20% aq) = 165 cps] 10 g of dextrin and 10 g of dextrin were dispersed in 200 g of water at a temperature of 20 ° C., and then heated to 70 ° C. with stirring. After adding 45 g (content 50 mass% or more) and mixing uniformly, an emulsion having an emulsion size of 0.5 to 1.0 μm was prepared using an emulsifier.
(2) In the fragrance capsule (c), the emulsion prepared in (1) above was spray-dried (drying temperature 120 to 200 ° C.) to produce a fragrance capsule [fragrance capsule (c)] in which an eggplant-type fragrance was encapsulated. Content of insulator-type fragrance = 45% by mass; average particle size of fragrance capsule = 80 μm].

<< Example 4 >> [Production of fragrance capsule (d) (fragrance ingredient: limonene)]
The same operation as in Example 3 was carried out except that limonene was used in place of the eggplant-type fragrance as the fragrance component, and a fragrance capsule [fragrance capsule (d)] encapsulating limonene was produced [of limonene in the fragrance capsule (d)] Content = 45% by mass; average particle size of perfume capsules = 80 μm].

<< Comparative Example 1 >> [Manufacture of fragrance capsule (e) (fragrance ingredient: limonene)]
(1) “Capsule” (National Starch & Chemical Co., Ltd.), a modified pregelatinized starch (pregelatinized hydrolyzed starch); 45 g of viscosity (20% aq) = 32 cps] and 10 g of dextrin in 200 g of water at a temperature of 20 ° C. After the dispersion, the mixture was heated to 70 ° C. with stirring, and 55 g of limonene was added when the liquid became transparent. After mixing uniformly, the emulsion size was 0.5 to 0.5 using an emulsifier. A 1.0 μm emulsion was prepared.
(2) The emulsion prepared in (1) above was spray-dried (drying temperature 120 to 200 ° C.) to produce a fragrance capsule [fragrance capsule (e)] encapsulating limonene [of the limonene in the fragrance capsule (e) Content = 50% by mass; average particle size of perfume capsules = 80 μm].

  The contents of the fragrance capsules (a) to (d) produced in Examples 1 to 4 and the fragrance capsule (e) produced in Comparative Example 1 are summarized as shown in Table 1 below.

<< Examples 5 to 9 >> [Production of bathing agents (A), (B), (C), (D1) and (D2)]
Any of the perfume capsules (a) to (d) produced in Examples 1 to 4 above, sodium sulfate and sodium hydrogen carbonate are mixed in the proportions shown in Table 2 below, and a powdery bath containing the perfume capsules Agents (A), (B), (C), (D1) and (D2) were produced, respectively. In the bath preparation (D2), as shown in Table 2, together with the fragrance capsule (d), a cocoon-type fragrance base [from the cocoon-type fragrance used in the production of the fragrance capsule (c) of Example 3 contained in limonene) Was used as a fragrance | flavor. The adjustment insulator type fragrance | flavor which cut | disconnected 50 mass% and made limonene content 25 mass%] was used.

<< Comparative example 2 >> [Production of bathing agent (E)]
The perfume capsule (e) produced in the above Comparative Example 1, sodium sulfate and sodium hydrogen carbonate were mixed in the proportions shown in Table 3 below to produce a powdered bath agent (E) containing the perfume capsule.

<< Comparative Examples 3 and 4 >> [Production of Bathing Agents (F) and (G)]
Instead of using perfume capsules, use non-encapsulated eggplant type perfume (manufactured by Takasago Perfume Industry Co., Ltd .; limonene content of 50% by mass or more) or limonene. Sodium hydrogen was mixed in the proportions shown in Table 3 below to produce fragrant powdered bathing agents (F) and (G), respectively.

<< Test Example 1 >>
Comparisons containing the bath capsules (A) and (B) of Examples 5 and 6 containing the perfume capsules (a) and (b) produced in Examples 1 and 2, respectively, and the perfume capsule (e) of Comparative Example 1 The bathing agent (E) produced in Example 2 and the bathing agent (G) produced in Comparative Example 4 containing an unencapsulated fragrance component (limonene) were stored at 45 ° C. for 1 week after the production of each bathing agent. After that, 1 g of each bathing agent was added to 1.5 liters of hot water at a temperature of 42 ° C. The fragrance strength and fragrance immediately after the addition, 20 minutes after the addition, and 1 hour after the addition are shown in Tables 4 and 5 below. According to the evaluation criteria shown in Fig. 6, the evaluation was made on a five-point scale by six expert panelists, and the average value was taken.

As can be seen from the results in Table 6 above, the bathing agents (A) and (B) of Examples 5 and 6 are modified pregelatinized starch comprising at least part of a modified pregelatinized starch (≧ 50 cps; 20% aq). As a result of blending the fragrance capsules (a) and (b) of the present invention in which limonene is encapsulated using as an encapsulating material, there is little change in fragrance even after 1 hour has passed after being poured into hot water at 42 ° C. Can maintain a refreshing fragrance for a long time.
In particular, the bathing agent (A) of Example 5 is a fragrance capsule formed using a modified pregelatinized starch (≧ 50 cps; 20% aq) and a modified pregelatinized starch (<50 cps; 20% aq) as an encapsulant ( As a result of blending a), even after 1 hour has passed since it was poured into 42 ° C. hot water, the strength and freshness (fragrance) of the fragrance decreased only slightly compared to immediately after the addition, which is extremely good. The fragrance was maintained.

On the other hand, the bathing agent (E) of Comparative Example 2 was obtained by using only the modified pregelatinized starch (<50 cps; 20% aq) without using the modified pregelatinized starch (≧ 50 cps; 20% aq) as the modified pregelatinized starch. By blending the fragrance capsule (e) of Comparative Example 1 in which limonene was encapsulated, the fragrance strength was greatly reduced at the time when it was put into 42 ° C. hot water for 1 hour and the change in fragrance was large. A nasty smell was produced.
Furthermore, the bathing agent (G) of Comparative Example 4 was blended directly as it was without encapsulating limonene, so that the scent of limonene was lost when it was poured into hot water at 42 ° C. for 1 hour. It was transformed into a bad smell.

<< Test Example 2 >>
The bathing agent (C) of Example 7 containing the fragrance capsule (c) produced in Example 3 and the bathing agent (F) of Comparative Example 3 in which the palm-type fragrance was directly blended as it was without being encapsulated were 5 ° C. And after storage for 1 week at 45 ° C. (stored in the air without packaging) 30 g of that was poured into 200 liters of 42 ° C. bath water, 20 minutes later and 1 hour immediately after being put into the bath water. In accordance with the evaluation criteria shown in Table 7 and Table 8 below, based on the strength and fragrance of the scent immediately after production of the bath preparation (F) of Comparative Example 3, When seven grades were evaluated by seven general panelists and the average value was taken, it was as shown in Table 9 below (rounded to the first decimal place).

As seen in the results of Table 9 above, the bath agent (D) of Example 9 is a modified pregelatinized starch containing at least a part of a modified pregelatinized starch (≧ 50 cps; 20% aq) [specifically, denatured starch] A fragrance capsule of the present invention in which a coconut-type fragrance is encapsulated using a pregelatinized starch (≧ 50 cps; 20% aq) and a denatured pregelatinized starch (<50 cps; 20% aq)] as an encapsulating material ( By blending c), both the storage at a low temperature of 5 ° C. and the storage at a high temperature of 45 ° C. showed little decrease in fragrance and deterioration, and excellent long-term storage stability. Moreover, even after 1 hour has passed since being put into 42 ° C. bath water, the change in fragrance was small and a strong fragrance was maintained, and the fragrance intensity gradually increased after being put into the bath water.
On the other hand, the bathing agent (G) of Comparative Example 3 has a strong fragrance strength when stored for one week at a temperature of 45 ° C. by directly blending the coconut-type fragrance without encapsulating it. As it decreased, the fragrance changed greatly, and the storage stability and stability to the base composed of sodium sulfate and sodium bicarbonate contained in the bath were inferior.

<< Test Example 3 >>
The bathing agent (D1) of Example 8 containing the fragrance capsule (d) produced in Example 4 and the bathing agent (G) of Comparative Example 4 in which limonene was blended as it was without being encapsulated were at 5 ° C and 45 ° C. After storing for 1 week (stored in the air in an exposed state without packaging), 1 g of the solution is put into a beaker containing 1.5 liters of hot water of 42 ° C., and immediately after charging, the scent after 20 minutes and 1 hour According to the evaluation criteria shown in Table 4 above, the strength was evaluated by 5 professional panelists, and the average value was taken. The result was as shown in Table 10 below.

As seen from the results of Table 10 above, the bathing agent (D1) of Example 8 is a modified pregelatinized starch containing at least part of a modified pregelatinized starch (≧ 50 cps; 20% aq) [specifically modified The perfume capsule (d) of the present invention in which limonene is encapsulated using a pregelatinized starch (≧ 50 cps; 20% aq) and a denatured pregelatinized starch (<50 cps; 20% aq)] as an encapsulating material. In addition to when stored at a low temperature of 5 ° C., the fragrance strength does not decrease when stored at a high temperature of 45 ° C., and is added to hot water at 42 ° C. for 1 hour. Only after the lapse of time, the intensity of the fragrance was not so lowered as compared to immediately after the addition.
On the other hand, the bathing agent (G) of Comparative Example 4 was directly blended as it was without encapsulating limonene, so that the fragrance strength was already greatly reduced when stored at a temperature of 45 ° C. for 1 week. .

<< Test Example 4 >>
The bath agent (D2) of Example 9 containing both the perfume capsule (d) encapsulating limonene produced in Example 4 and the unencapsulated cocoon-type fragrance base, and the unencapsulated cocoon-type fragrance alone 30 g of each of the bath preparations (F) of Comparative Example 3 blended directly into 200 liters of 42 ° C. bath water, and the balance of fragrance immediately after the bath water addition, after 20 minutes and 1 hour, was compared with the bath preparation of Comparative Example 3. Based on the incense tone balance immediately after the production of (F), five levels were evaluated by seven general panelists according to the evaluation criteria shown in Table 11 below, and the average value was taken. (Rounded to the first decimal place).

As seen from the results of Table 12 above, the bathing agent (D2) of Example 9 is a modified pregelatinized starch containing at least a part of a modified pregelatinized starch (≧ 50 cps; 20% aq) [specifically modified The perfume capsule (d) of the present invention in which limonene is encapsulated using a pregelatinized starch (≧ 50 cps; 20% aq) and a denatured pregelatinized starch (<50 cps; 20% aq)] as an encapsulating material. And a non-encapsulated cocoon-type fragrance base were blended, so that an almost good fragrance balance was maintained even after one hour had passed after being put into hot water at 42 ° C.
On the other hand, the bathing agent (F) of Comparative Example 3 was blended directly as it was without encapsulating the coconut-type fragrance, so that the fragrance balance was lost when 1 hour had passed after being poured into hot water at 42 ° C. It was.

<< Test Example 5 >>
(1) The insulator-type fragrance itself was dissolved in diethyl ether and analyzed by gas chromatography to obtain a chart shown in FIG.
(2) After storing the bathing agent (F) of Comparative Example 3 in which the coconut-type fragrance was blended as it was without being encapsulated at 5 ° C. and 45 ° C. for 1 week (stored in the air in an exposed state without packaging), 1 g thereof was dissolved in 5 ml of water (temperature 25 ° C.), the solution was extracted with diethyl ether, and the extract was analyzed by gas chromatography to obtain the charts shown in FIGS. 1 (ii) and (iii).

(3) Chart (i) of the cocoon type fragrance itself in FIG. 1 and chart (ii) after storage of the bath agent (F) blended in the bath agent without encapsulating the cocoon type fragrance (at 5 ° C.) As shown in the comparison between (preservation) and chart (iii) (storage at 45 ° C), in the bathing agent (F) in which the coconut-type fragrance is directly blended without being encapsulated, the limonene is greatly increased when stored at 5 ° C. In the case of storage at 45 ° C., almost the entire amount of limonene disappeared, and α-terpineol and p-menthane-1,8-diol appeared in both cases. From these results, in both cases of storage at 5 ° C. and storage at 45 ° C. (both when the storage temperature is low and high), limonene in the eggplant-type fragrance is a base in the bath agent ( It turns out that it is easy to receive alteration by the mixed base of sodium sulfate and sodium bicarbonate.

The fragrance capsule of the present invention has excellent scent sustainability and stability, is stable against components such as sodium hydrogen carbonate and sodium sulfate, is not easily altered, and has a relatively high temperature of 38 to 42 ° C. Even if it is poured into hot water, it does not easily cause a decrease in fragrance or alteration. Therefore, the fragrance capsule of the present invention is suitable as a fragrance material for various products, and can be effectively used as a fragrance material for bathing agents.
The bath agent of the present invention containing the fragrance capsule of the present invention can be effectively used as a bath agent because of its excellent fragrance sustainability and stability.

Chart (i) of the gas chromatographic analysis of the cocoon-type fragrance itself, obtained by extracting the bath additive of Comparative Example 3 containing the cocoon-type fragrance as it is without encapsulating it at 5 ° C. and extracting with diethyl ether Chart by gas chromatography analysis of the extract obtained (ii), Chart by gas chromatography analysis of the extract obtained by extracting the bathing agent (F) of Comparative Example 3 at 45 ° C. and then extracting with diethyl ether It is a figure which shows (iii).

Claims (8)

  A fragrance capsule in which a fragrance component is encapsulated using a modified pregelatinized starch as an encapsulating material, and at least part of the denatured pregelatinized starch forming the encapsulating material, heated to 80 ° C. for 5 minutes after heating at 80 ° C. A fragrance capsule characterized by using at least one modified pregelatinized starch which forms an aqueous solution having a viscosity of 50 cps or more when measured at 30 ° C.   A fragrance capsule in which a fragrance component is encapsulated using a modified pregelatinized starch as an encapsulant, and measured at 30 ° C after heating at 80 ° C for 5 minutes as a 20% aqueous solution as a denatured pregelatinized starch forming the encapsulant. At least one modified pregelatinized starch that forms an aqueous solution having a viscosity of 50 cps or more, and an aqueous solution having a viscosity of less than 50 cps when measured at 30 ° C. after being heated at 80 ° C. for 5 minutes after being made into a 20% aqueous solution. A fragrance capsule characterized by using in combination at least one kind of modified pregelatinized starch to be formed.   In the encapsulating material, a modified pregelatinized starch that forms an aqueous solution having a viscosity of 50 cps or more when measured at 30 ° C. after heating at 80 ° C. for 5 minutes in a 20% aqueous solution, and 20% aqueous solution at 80 ° C. for 5 minutes. The flavor according to claim 2, wherein the ratio of the modified pregelatinized starch that forms an aqueous solution having a viscosity of less than 50 cps when measured at 30 ° C after heating is a mass ratio of the former: the latter = 10:90 to 80:20. capsule.   A modified pre-gelatinized starch that forms an aqueous solution having a viscosity of 50 cps or more when measured at 30 ° C. after heating at 80 ° C. for 5 minutes in a 20% aqueous solution is an aqueous solution having a viscosity of 100 cps or more when measured under the same conditions. The perfume capsule according to any one of claims 1 to 3, which is a modified pregelatinized starch to be formed.   The fragrance | flavor capsule of any one of Claims 1-4 which contains a fragrance | flavor component in the ratio of 20-90 mass% based on the total mass of a fragrance | flavor capsule.   The fragrance capsule according to any one of claims 1 to 5, comprising limonene as a fragrance component.   The fragrance | flavor capsule of any one of Claims 1-6 which contains a limonene in the ratio of 50 mass% or more based on the mass of a fragrance | flavor component. A bath agent comprising the fragrance capsule according to any one of claims 1 to 7.

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