JP2006083071A - Solid preparation for fragrant cosmetic - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a solid preparation for fragrant cosmetics hardly suffering from deterioration in fragrance or changes in fragrance qualities at the time of use even after a long-term preservation. <P>SOLUTION: A perfume is incorporated with a solid preparation for fragrant cosmetics such as a powder or tablet bathing agent, a powder or tablet detergent, or the like as a locked-in type powder perfume. The solid preparation exhibits excellent long-term stability, suffers from neither deterioration nor degeneration in fragrance or in cooling and warm feeling effects, and can sustainedly exhibit good effects over a long period of time. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

  The present invention relates to a solid preparation for cosmetics containing a lock-in type powder fragrance. More specifically, the present invention is excellent in long-term stability, has no deterioration or deterioration in fragrance or cooling sensation effect, can release a good effect over a long period of time, and is included in bathing agents and detergents. The present invention relates to a solid preparation for cosmetics which is unlikely to be altered by components such as sodium sulfate, sodium hydrogen carbonate, surfactants and enzymes.

  Conventionally, powder pack, whitening powder, powder bath, tablet bath (bath tablet), bubble bath, deodorant powder, powder detergent, dishwasher detergent, powder bleach, slime remover, denture cleaner In these various cosmetic products, a fragrance is blended for adding a flavor to the cosmetic product. In addition, substances that give a cooling sensation effect or a warm sensation effect are blended in cosmetics as necessary. The blending of a fragrance, a cooling sensation agent, a warming sensation agent, etc. (hereinafter referred to as “perfume”, etc.) into a cosmetic product is carried out when the cosmetic product is in the form of powder or granules. Added to these base compositions, or powdered fragrances produced by spray drying (may contain cooling sensation agent, warming sensation agent, etc., if necessary) added to these cosmetic base compositions And is done by mixing. Further, when the cosmetic product is a tablet, it is manufactured by tableting a base composition containing the fragrance or the powder fragrance manufactured by the spray drying method. However, cosmetics in the form of powder, granule or tablet solid preparations contain various chemical substances. For example, mirabilite (sodium sulfate) is mainly used as the base material of the bath agent, and when the bath agent is foaming, a mixture of mirabilite and sodium hydrogen carbonate is used. In detergents, in addition to surfactants, mirabilite, sodium carbonate, sodium phosphate and the like are used as builders. In addition, various additives such as enzymes are also used, and some of the components constituting fragrances have poor stability against these chemical substances, and therefore some of the components that make up fragrances during storage. There is a problem that the ingredient balance of the fragrance is lost due to the decomposition of the substance, the fragrance quality and the fragrance intensity of the fragrance are changed, and as a result, the fragrance of the cosmetic product is changed, or the cooling effect is lowered. is there. In addition, cosmetic products made into various solid preparations are often packaged and supplied to the market. However, for example, limonene contained in a fragrance as a fragrance component is heat sealability of a packaging material used in the packaging. It is also conceivable that the resin is dissolved to give a sticky feeling to the cosmetic product at the time of opening, or that the package that has been separated during storage is opened. These problems are not limited to the case where the fragrance is directly added to the base material, and the same problem is caused even when the powder fragrance produced by the spray drying method is used. In addition, in other cosmetic products, there are substances that degrade the constituents such as fragrances, causing problems similar to bathing agents and detergents, and changes in the effect of cooling and warming. When it is supplied to the market, the problem of dissolution of the resin by the fragrance component occurs as in the case of bathing agents and detergents.

  On the other hand, the lock-in type capsule powder is a water-soluble core material in an amorphous matrix obtained by heating a carbohydrate such as a sugar together with a small amount of water as necessary, for example. Alternatively, an oil-soluble normal liquid substance is mechanically dispersed and sealed (locked-in), and then the core material is dispersed, and the contained matrix material is solidified by cooling as it is, and then finely pulverized, or the core material Using a single or twin screw extruder (extruder), the dispersion matrix is solidified by extruding it into a coolant such as a refrigerant through a die and then solidifying it, and then the core material is dispersed and contained. Alternatively, it is manufactured by pulverization or the like and is already known. In this lock-in type capsule powder, carbohydrates are usually used as a matrix material, so that the capsule can be colored, and the flavor components have excellent antioxidant and volatilization prevention properties. Has been used to grant. In particular, it is widely used in the production of candy, chewing gum and the like. Examples of the conventionally proposed lock-in type capsule powder for the flavor component or the production method thereof include the following.

(1) A method in which an aromatic oil (flavoring component) containing an antioxidant and a dispersant is dispersed in heated corn syrup, extruded and then pulverized (see Patent Document 1).
(2) A method comprising heating a mixture comprising a saccharide such as sucrose, starch hydrolyzate and an emulsifier, extruding the mixture with a flavor component into a cold solvent, molding and then grinding (see Patent Documents 2 to 5) .
(3) A method of adding flavor (flavoring ingredient) to a sugar aqueous solution in which maltose, lactose, maltotriose or raffinose and corn syrup, dextrin, maltodextrin are mixed in a specific proportion at a specific ratio and then drying (patented) Reference 6).
(5) A method of fixing essential oil or the like with an aqueous sorbitol solution or melt (see Patent Document 7).
(6) A method of fixing essential oil by mixing and heating solid corn syrup and glycerol or non-toxic glycol (see Patent Document 8).
(7) A small component selected from water-soluble carbohydrates such as fructose and a base material composed of a polymeric carbohydrate such as maltodextrin of DE20 or higher are mixed with a volatile flavor without adding water, A method of heating to the glass transition point or more of the substrate in an extruder having a screw, and then extruding, cooling, and molding to obtain a glassy inclusion (see Patent Document 9).

(8) Chemical starch and hydrogenated saccharide are contained in a weight ratio of 15:85 to 85:15 in terms of solid content, and the hydrogenated saccharide is xylitol, lactitol, maltitol, isomalt And a carbohydrate mixture that is one or more selected from hydrogenated corn syrup is heated to a melt, and a flavoring agent is added to the melt and mixed to obtain a uniform mixture, which is then rapidly extruded while extruding the uniform mixture. A method of obtaining a sugar-free (sugar-free or low-sugar) capsule by cutting or crushing the solid material obtained after cooling to solid (see Patent Document 10).
(9) a. Melt-mixing mono- or disaccharides, polysaccharides and water with aromatic oils, resulting in a particulate fragrance composition having a Tg below room temperature; and b. Production of particulate aroma composition by extruding the above homogeneous substrate at a temperature sufficient to form a melt that can solidify as a hard rubbery and amorphous material incorporating the aromatic oil upon cooling. (See Patent Document 11).
(10) Solid transport system for release of fragrance components obtained by extrusion, having an extruded sugar or sugar derivative matrix containing an effective amount of hydrophilic fragrance material (see patent document 12).

Japanese Patent Publication No. 34-5600 (corresponding to US Pat. No. 2,809,895) JP-A 49-62677 JP 52-94452 A JP 61-12248 A JP-T 61-502656 Publication Japanese Patent Publication No.52-37062 JP-A-49-132251 US Pat. No. 3,041,180 US Pat. No. 4,820,534 Japanese Patent No. 3190229 JP-T 9-507267 Special table 2002-528601 gazette

  These lock-in type capsule powders are conventionally blended or added to foods, etc., and during the storage or marketing of foods, the flavor components, flavors, etc. in the capsules are prevented from being volatilized and oxidized, and the foods are put in the mouth of consumers. When injected, flavor components in the capsule are released in the mouth, and are used to allow consumers to perceive the taste and aroma of food and the like with sufficient satisfaction. Therefore, the conventional lock-in type capsule powder has not been considered to be used for purposes other than the release of flavor components, flavors and the like in the mouth. A lock-in type powder fragrance is blended, and it is not considered to be used for maintaining a good fragrance over a long period of time by releasing the fragrance during use. As far as the applicant knows, there are no cosmetic solid preparations on the market.

An object of the present invention is to provide a solid preparation for cosmetics that has a reduced scent strength and a small change in fragrance during use even after long-term storage.
In addition, the object of the present invention is to deteriorate the blended fragrances by additives such as sodium sulfate, sodium carbonate, sodium phosphate, sodium hydrogen carbonate, detergents or enzymes, which are often used as a base ingredient of cosmetics. It is to provide a solid preparation for cosmetics.
Furthermore, this invention is providing the solid formulation for cosmetics which does not melt | dissolve the resin of the packaging material by a fragrance | flavor at the time of a preservation | save.
Moreover, this invention is providing the fragrance | flavor stabilization method of the solid preparation for cosmetics which prevents the fall of the fragrance | flavor of the solid preparation for cosmetics and the intensity | strength of fragrance in storage.

  The present inventors have intensively studied to solve the above-mentioned problems, and by incorporating a lock-in type powder fragrance using a fragrance as a core material of a lock-in type capsule powder into a solid preparation for cosmetics. In addition, after storing a cosmetic product for a long period of time, it is possible to obtain a solid preparation for cosmetic product that does not deteriorate in flavor and emits a good fragrance during use, and there is no leaching of the flavor component from the flavor powder. The present invention has been made based on this finding, and it has been found that dissolution of the resin used in the present invention can also be prevented.

That is, the present invention is a solid preparation for cosmetics characterized by containing a lock-in type powder flavor.
Moreover, the present invention is the above solid preparation for cosmetics, wherein the cosmetic is a bath agent or a detergent.
Furthermore, the present invention is a method for stabilizing the fragrance of a solid cosmetic preparation, characterized by using a lock-in type powder fragrance in the solid cosmetic preparation.

In the solid preparation for cosmetics of the present invention, since the fragrance is contained in a lock-in capsule, the fragrance does not volatilize or volatilize, and since the fragrance does not deteriorate due to oxidation, even after storage for a long time, It is possible to obtain a solid preparation for cosmetics that emits a strong and good scent when the cosmetic is used.
Further, the solid preparation for cosmetics of the present invention has the fragrance contained in the lock-in type capsule, so that the fragrance is hardly affected by the base material used in the cosmetic, and thus the scent during storage A solid preparation for cosmetics can be obtained without any decrease in odor or change in fragrance.
Moreover, since the fragrance | flavor is enclosed in the lock-in type capsule, the fragrance | flavor does not ooze out of a capsule in the solid formulation for cosmetics of this invention. For this reason, it does not adversely affect the heat sealing resin of the packaging material encapsulating the solid preparation for cosmetics with the fragrance, and the resin is dissolved by the fragrance component during storage, and the stickiness of the cosmetic product or damage to the packaging material may occur. Never happen.
In the present invention, when the cosmetic product is a bath agent or a detergent, a particularly excellent effect can be obtained.
In addition, when the cosmetic preparation of the present invention is a bath agent, the fragrance does not decrease for a long time and the fragrance does not change during use, and a good fragrance can be maintained for a long time.
In addition, according to the present invention, the aroma of the solid preparation for cosmetics is stabilized by incorporating the lock-in type powder fragrance into the solid preparation for cosmetics.

Hereinafter, the present invention will be described in more detail.
In the present invention, the solid preparation for cosmetics contains a lock-in type powder flavor. The lock-in type powder fragrance contained in the cosmetic solid preparation of the present invention may be used as long as the fragrance is used as the core material of the lock-in type capsule powder, and is used to form the lock-in type powder fragrance. There are no particular restrictions on the materials and production methods. For example, conventionally used matrix materials and fragrances can be used as the materials used, and the manufacturing method can be easily manufactured by a known manufacturing method. Here, as a known matrix material and production method, for example, the materials or production methods described in the patent literatures and the like previously described as the prior art can be mentioned, and the perfume is conventionally used for attaching a cosmetic product. Fragrances. However, as described above, in the present invention, any lock-in type powder fragrance may be used, and it is not particularly limited to known materials and known production methods.

  Specific examples of the matrix material of the lock-in type powder flavor of the present invention include monosaccharides, disaccharides, polysaccharides, sugar alcohols, polyols, sugar derivatives, modified starches, modified starches, and rubbers. More specifically, for example, sucrose, glucose, lactose, levulose, fructose, maltose, glucopyranosyl mannitol, glucopyranosyl sorbitol, ribose, dextrose, isomalt, sorbitol, mannitol, xylol, lactitol, maltitol , Pentatol, arabinose, pentose, xylose, galactose, starch, hydrogenated starch hydrolyzate, maltodextrin, agar, carrageenan, polydextrose and derivatives and mixtures thereof.

  Any of the above matrix materials is preferable as the matrix material of the lock-in type powder fragrance used in the present invention. Among them, a modified starch and a hydrogenated saccharide are converted in terms of solid content. 15:85 to 85:15 by weight, and the saccharide hydrogenated product is a carbohydrate mixture that is one or more selected from xylitol, lactitol, maltitol, isomalt and hydrogenated corn syrup (See Patent Document 10).

Here, the modified starch is a chemically treated starch, for example, an acid-treated starch (eg dextrin), an enzyme-treated starch (eg dextrin), or a heated starch (eg α-starch). , Oxidized starch, cross-linked starch and other starch derivatives (for example, see Non-Patent Document 1). As the dextrin, those having a low DE (Dextrose Equivalent = rotated sugar equivalent) value, particularly about 20 or less are preferably used. When the DE value is greater than about 20, the stability to moisture becomes poor. However, if the DE value is less than about 5, the viscosity at the time of mixing the flavor may be too high. A starch derivative is a highly modified starch in which the side chain of starch is modified with a hydrophilic group or a hydrophobic group. Specifically, starch derivatives such as starch phosphate, starch carboxy Mention may be made of starch ethers such as methyl ether and cross-linked starches such as phosphoric acid cross-linked starch. These starch derivatives are preferably used because they are superior in stability to moisture during storage of the resulting capsules compared to other modified starches. Further, as another factor for improving the moisture stability of the capsule, use of a modified starch having a large average molecular weight and a branched structure can be mentioned. Examples of the modified starch having a branched structure include a modified starch containing amylopectin in a high ratio. In particular, a modified starch containing about 80% by weight or more of amylopectin is preferably used.
Jhon M. DeMAN, “PRINCIPLES OF FOOD CHEMISTRY”, Second Edition, Van Northland Reinhold (New York), 1990, pp. 167-168

  Specific examples of such modified starch include modified starch derived from amioka starch, tapioca starch, waxy maize and the like. Of these, modified starch derived from waxy maize is particularly preferable. The most preferably used modified starch is a modified starch derived from waxy maize, and a starch derivative having a bulky three-dimensional structure that has a stronger interaction between the side chains of starch. Specific examples of such a modified starch include PURITY GUM 59, PURITY GUM BE, PURITY GUM 1773, N-LOK (all trade names, National Starch and And edible chemical starch produced by National Starch and Chemical Company). By using the above matrix, there is no deterioration due to base materials such as fragrances, and it becomes possible to gradually release the fragrance over a long period of time when using cosmetics, maintaining a strong fragrance with good fragrance over a long period of time. can do.

  Further, as another preferable matrix material, it has a viscosity of 50 cps (mPa · s) or more when measured at 30 ° C. after heating at 80 ° C. for 5 minutes as described in Japanese Patent Application No. 2004-3125. Examples include those using modified pregelatinized starch (hereinafter referred to as “modified pregelatinized starch (≧ 50 cps)”) as at least a part of the matrix material. The paste obtained by dissolving and adjusting is rapidly dehydrated and dried in the paste state, and can be easily reproduced by dispersing and swelling in normal temperature water. Modified starch that forms the base of starch includes oxidized starch, derivative starch (starch acetate ester, starch phosphate ester, various dengues). Emissions ether phosphoric acid, various modified starch such as crosslinked starch, etc.).

  Modified pregelatinized starch (≧ 50 cps) is conventionally known, and various products are sold. These commercially available products may be used as appropriate. For example, “N Creamer 46” manufactured by National Starch and Chemical Co., Ltd. may be mentioned as a commercially available product. These modified pregelatinized starches (≧ 50 cps) may be used with other modified pregelatinized starches. The modified pregelatinized starch used with these modified pregelatinized starches (≧ 50 cps) is, for example, a viscosity of less than 50 cps (mPa · s) when measured at 30 ° C. after heating at 80 ° C. for 5 minutes in a 20% aqueous solution. Modified pregelatinized starch (hereinafter referred to as “modified pregelatinized starch (<50 cps)”). Modified pregelatinized starch (<50 cps) is a modified starch (modified starch) such as hydrolyzed starch, oxidized starch, derivative starch (starch acetate ester, starch phosphate ester, various starch ether phosphates, cross-linked starch, etc.). ) Was swelled or dissolved in water or hot water to obtain a paste-like product which was obtained by rapidly dehydrating and drying the paste in the same state as in the case of modified pregelatinized starch (≧ 50 cps). Conventionally, various products are sold. Examples of commercially available products include “Purity Gum BE” and “Capsule” manufactured by National Starch and Chemical Co., Ltd. By using these in combination, it is possible to gradually release the fragrance over a longer period of time when the cosmetic product is used, and it is possible to maintain a strong fragrance with a good fragrance over a long period of time.

  By adjusting the blending ratio of the modified pregelatinized starch (≧ 50 cps) and the modified pregelatinized starch (<50 cps) that form aqueous solutions having different viscosities, the volatilization rate and volatilization pattern of the lock-in type powder flavor are well adjusted. be able to. In addition, it prevents the perfume ingredients from deteriorating or changing over time due to bases (such as sulfuric acid marking sheet thorium or sodium bicarbonate) contained in bathing agents and detergents. Can last. The blending ratio of the modified pregelatinized starch to the total amount of the matrix material is determined based on the matrix base material in terms of ease of production of the lock-in type powder fragrance, long-term storage, fragrance sustainability, performance of removal, and feel during use. Is preferably 50% by mass or more, more preferably 60 to 100% by mass, and still more preferably 70 to 95% by mass or more. The blending ratio of the modified pregelatinized starch (≧ 50 cps) is preferably 15% by mass or more, more preferably 20% by mass or more, and more preferably 20 to 80% by mass with respect to the total amount of the matrix material. Further preferred. In the case of using a modified pregelatinized starch (≧ 50 cps) and a modified pregelatinized starch (<50 cps), the use ratio is generally preferably 10:90 to 80:20, and preferably 20:20: More preferred is a mass ratio of 80 to 70:30.

  The modified pregelatinized starch may be used in combination with other components such as sugars. Examples of saccharides that can be used in combination include monosaccharides such as glucose, fructose, mannose, galactose, xylose, arabinose, and ribose, disaccharides such as mannose, lactose, and sucrose, and dextrins obtained by hydrolyzing starch with acid or enzyme. Examples thereof include sugar alcohols such as mannit, sorbit and malbit. Of these, dextrin is preferred. When modified pregelatinized starch (≧ 50 cps) is used as a matrix material, for example, when the formed lock-in type powder flavor is used in a powder or tablet bath, a relatively hot water such as 38 to 42 ° C. Even if put in, there is an advantage that the scent lasts for a long time.

  In the above, the viscosity value of a 20% aqueous solution of modified pregelatinized starch is determined by adding 40 g of modified pregelatinized starch to 160 g of water at a temperature of 20 ° C. to make a 20% aqueous solution, and stirring the aqueous solution up to 80 ° C. The mixture was heated and stirred at 80 ° C. for 5 minutes, then cooled to 30 ° C., and the viscosity of the aqueous solution immediately after reaching 30 ° C. was measured by a viscometer (“Tokimec Vismeter BM Type” manufactured by Tokimec Co., Ltd .; Spindle No. 1 30 rpm, Spindle No. 2 30 rpm).

  On the other hand, as the fragrance used in the lock-in type powder fragrance of the present invention, any fragrance may be used as long as it can be used for fragrance of cosmetics, including those conventionally used in solid preparations for cosmetics. It is not limited. The fragrance used may be a synthetic fragrance or a natural essential oil, and may be in any state such as a liquid, a paste or a solid. For example, as the fragrance component, hydrocarbon-based fragrances such as limonene, pinene, γ-terpinene, caryophyllene; alcohol-based fragrances such as phenylethyl alcohol, terpineol, paxanol, geraniol, nerol, linalool, cis-3-hexenol; Aldehyde fragrances such as citral, aldehyde C-8, aldehyde C-9, aldehyde C-11, hexyl cinnamic aldehyde, vanillin, heliotropin; ketone fragrances such as ionone, rosephenone, woody flow, damascon, and ISOE super Other fragrances such as musks, eugenol and coumarin; essential oils such as lemon oil, orange oil and peppermint oil; essences such as apple essence and strawberry essence That. The powder fragrance | flavor of this invention contains 1 type, or 2 or more types of these fragrance | flavor components.

  Examples of the fragrance component type include citrus type, for example, cocoon type fragrance, forest fragrance type fragrance, cypress fragrance type fragrance, rose fragrance type fragrance, jasmine fragrance type fragrance, lavender type fragrance, and chamomile type fragrance. However, depending on the fragrance and fragrance required for cosmetics, the desired fragrance or fragrance (citrus, fruity, green, floral, aldehyde, spicy, woody, sweet, mossy, musky, amber, animal, herbal, marine, And mint notes, etc.) can be prepared.

In addition to perfume, if necessary, solvent (ethanol, ethylene glycol, propylene glycol, etc.), emulsifier, solubilizer, retention agent / fragrance, cooling sensation / warming agent, enhancer, antioxidant, photodegradation prevention An additive such as an agent can be used as appropriate (see, for example, Non-Patent Document 2).
"Known and Conventional Techniques (Fragrance) Part 1 Perfume General", published on January 29, 1999, JPO

Moreover, these matrix materials, fragrance | flavors, and the additive used as needed are made into a lock-in type powder fragrance | flavor by the following methods, for example.
First, if necessary, water is added to the matrix material and heated to form a melt of the matrix material. In the case of adding water, the amount is desirably the minimum amount in which the matrix material is uniformly dispersed. For example, the amount is preferably about 3 to 40% by weight based on the matrix material. If the amount of water added is too large, it takes too much time to heat and lower the water content later, which is not preferable. The heating temperature is in the range of about 110 to 200 ° C., depending on the composition, but until the matrix material is melted and the water content is lowered to some extent. Preferably, it is boiled in a boiled kettle or the like until the water content is about 0.5 to 6% by weight. If the residual water content is too high at this point, the water content of the capsules obtained is increased, and the stability against water is deteriorated.

  Next, a fragrance | flavor is added to the obtained melt. At this time, other additives may be added as necessary. The stability of the obtained capsules with respect to moisture varies depending on the contents of moisture, fragrance, other additives, and the like, and if these contents are large during molding, the stability becomes worse. For this reason, it is desirable that the amount of the fragrance is about 20% by weight or less based on the matrix material. If the amount of the fragrance added is too small, the effect cannot be obtained. Therefore, the blending ratio of the fragrance to the matrix material is usually about 0.2 to 20% by weight, preferably about 1 to 15% by weight.

  The method of mixing the matrix material melt and the fragrance is not particularly limited as long as it is a method capable of obtaining a uniform mixture. For example, the matrix material may be used with an apparatus such as a high-speed stirrer (homodisper). A fragrance | flavor etc. may be added to the place which is stirring the melt of this, and also stirring may be continued and made uniform. At this time, when a dispersant or an emulsifier is blended in the fragrance or the like, a uniform dispersion of the fragrance or the like is easily obtained.

  Next, the obtained homogeneous mixture is transferred to an extruder (extruder), sealed, and then pressurized, and extruded from the extruder outlet (die). It is preferable that the extruder is preheated because the extrusion becomes smooth. Moreover, the extruder which consists of a pressure vessel with an extrusion plate which can perform a heating, mixing, and extrusion in the same container can also be used. That is, if a matrix material, added water, a fragrance, etc. are each introduced into an extruder using a feeder (feeder) consisting of a metering pump or the like, and heating, mixing, and extruding these in the extruder, A series of steps can be performed continuously without changing the container, and the production amount per hour can be increased, which is preferable. In particular, it is more preferable to have a structure (hereinafter referred to as “barrel”) capable of heating and mixing at the same time when the raw material is conveyed.

  Furthermore, an extruder composed of a pressure vessel having two or more screws is preferably used. An extruder having two or more screws is superior in conveying force and mixing force compared to an extruder composed of a single screw, and enables more stable production. In addition, an extruder having two or more screws has an excellent self-cleaning function in the container, and is easy to clean and maintain after use. An extruder having two or more screws in the barrel is particularly preferably used.

  On the other hand, the solidification of the matrix mixture is usually performed using a cooled refrigerant. For this reason, a refrigerant is put into a cooling tank and cooled to a low temperature as appropriate. It is desirable to select a refrigerant that does not harm humans, does not dissolve the matrix material, and can be easily removed from the surface of the obtained capsule powder. Examples thereof include alcohols such as ethanol and isopropyl alcohol. The cooling method of these refrigerants is not particularly limited, and can be freely selected according to the equipment such as cooling with dry ice or the like, or cooling with a device such as a cooler.

  The cooling temperature is a temperature sufficient for the homogeneous mixture extruded from the extruder die to be rapidly cooled and solidified, and a temperature at which the obtained solid does not soften. It is good to set to -30 degreeC. The solid material obtained here is obtained by rapidly cooling and solidifying a matrix material enclosing a fragrance. The pressure at which extrusion is performed varies depending on the type of raw material and the type of the extruder, but it is sufficient that the matrix material containing the fragrance is continuously extruded in a filament form from the extruder die. When using an extruder composed of a pressure vessel with an extrusion plate, it is preferable to apply a pressure of about 5 to 50 psig by means such as introducing nitrogen gas after sealing the extruder.

  The solid obtained by rapidly cooling while extruding the homogeneous mixture is cut or pulverized by means such as stirring to form a lock-in type powder fragrance. The obtained powder is separated into powder and refrigerant by means such as centrifugation. An anti-caking agent may be added to prevent re-consolidation of the powder. As the anti-caking agent, silicon dioxide, tricalcium sulfate, tricalcium phosphate and the like can be used. The addition amount of the anti-caking agent is preferably about 0.1 to 1% by weight with respect to the total weight.

  Next, the powder is dried. The drying method is not particularly limited, but it is necessary to select a method that does not destroy the capsule structure of the powder. Preferably, vacuum drying by means such as a vacuum rotary dryer is preferable. The water content of the capsule thus obtained is preferably about 6% by weight or less. Furthermore, if necessary, sieving or the like can be performed to obtain a lock-in type powder fragrance.

  The average particle size of the lock-in type powder fragrance is not particularly limited, but is usually 2 for example from the viewpoint of uniform mixing with a cosmetic base material, sustainability when using a fragrance, and feeling when used. The size is about 250 μm. The lock-in type powder flavors obtained in this way are powder pack, whitening powder, powder bath, tablet bath, bubble bath, deodorant powder, powder detergent, dishwasher detergent, powder bleach, slime remover, denture wash It is used for the purpose of imparting fragrance during use to cosmetics made into various solid preparations including agents. In particular, in powder baths or tablet-type baths, sodium sulfate or sodium hydrogen carbonate is used as a base material in the case of a foaming bath, and in detergents, in addition to surfactants, As a builder, sodium sulfate, sodium carbonate, sodium phosphate or the like is used. When the fragrance is a lock-in type powder fragrance, the fragrance is not affected by such a base compound and further by additives such as enzymes. Agents or detergents have good fragrance. For this reason, as cosmetics, a bath agent and a detergent are mentioned as preferable examples. Further, since the fragrance does not exude through the matrix of the lock-in type powder fragrance, there is no dissolution by the fragrance component of the heat sealing resin of the packaging material used for separating. For this reason, it can respond | correspond favorably with respect to the solid formulation for cosmetics sealed.

  When the cosmetic solid preparation of the present invention is a powder or tablet-type bath agent, a lock-in type powder flavor and, if necessary, a moisturizing agent on a base made of sodium sulfate or sodium hydrogen carbonate as a foaming agent , Enzyme agents, binders, disintegrants, dispersants, pigments, surfactants, buffers, stabilizers, pH adjusters, herbal medicine components, and the like can be blended.

  In addition, when the cosmetic solid preparation of the present invention is a powder or tablet type detergent, a surfactant and a builder include a lock-in type powder fragrance and, if necessary, a moisturizer, an enzyme agent, a disintegrant, a coloring agent, a buffer. An agent, an alkaline agent, a bleaching agent, a softening agent, an anti-deposition agent, a powdering agent, and the like can be blended.

  EXAMPLES The present invention will be specifically described below with reference to examples, but the present invention is not limited to the following examples.

Production Example 1: Production of lock-in type powder flavor A (sugar free type) 67.41 parts by weight of isomalt (palatinite), 4.40 parts by weight of purity gum 59, Paindex # 1 (manufactured by Matsuo Chemical Co., Ltd .; dextrin) 18 .36 parts by weight was heated with stirring with ion-exchanged water, and into a bowl-like solution, 9.54 parts by weight of lemon oil (manufactured by Takasago International Corporation), soybean lecithin (manufactured by Nisshin Eulio) 0.10 Part by weight, 0.18 part by weight of vitamin E (manufactured by Riken Vitamin Co., Ltd.) was added, and the whole was homogenized. After that, the filament was put into ethyl alcohol cooled to -10 ° C using an extruder. The mixture was extruded into a shape, rapidly cooled, then stirred and pulverized. Next, after removing ethyl alcohol by centrifugation, 0.73 parts by weight of calcium trisulfate was added as an anti-caking agent to prevent reconsolidation, thereby obtaining a lock-in type fragrance powder.

Production Example 2: Production of Lock-in Type Powder Fragrance B (Sugar Type) While stirring 50.54 parts by weight of granulated sugar and 39.45 parts by weight of Pindex # 1 (manufactured by Matsuo Chemical Co., Ltd .; dextrin) with ion-exchanged water Heated and boiled into a bowl-like solution, 9.00 parts by weight of lemon oil (manufactured by Takasago Kagaku Kogyo Co., Ltd.), 0.90 parts by weight of soybean lecithin (manufactured by Nisshin Oilio Co., Ltd.), vitamin E (manufactured by Riken Vitamin Co., Ltd.) ) After adding 0.18 parts by weight of a solution dissolved in ethyl alcohol and further stirring to homogenize the whole, using an extruder, the solution was made into filaments in ethyl alcohol cooled to -10 ° C. After extrusion and rapid cooling, the mixture was stirred and pulverized. Next, after removing ethyl alcohol by centrifugation, 0.73 parts by weight of calcium trisulfate was added as an anti-caking agent to prevent reconsolidation, thereby obtaining a lock-in type fragrance powder.

Example 1: Production of powder bath A A lock-in powder flavor obtained in Production Example 1 was added to 90 parts by weight of a bath base comprising 0.30 part by weight of anhydrous silicic acid and 99.70 parts by weight of neutral anhydrous sodium sulfate. 10 parts by weight of A was added and mixed. Next, this powder mixture was sealed with a heat sealer for each 10 g using a packaging sheet having a heat-sealable resin film on an aluminum foil.

Example 2: Production of powder bathing agent B Powder bathing agent in the same manner as in Example 1 except that 10 parts by weight of lock-in type powder fragrance B obtained in Production Example 2 was used instead of lock-in type powder fragrance A B was obtained and sealed in the same manner as in Example 1.

Comparative Example 1: Production of powder bath C C Lemon oil (manufactured by Takasago Fragrance Co., Ltd.) was added to 99.10 parts by weight of a bath base consisting of 0.30 parts by weight of anhydrous silicic acid and 99.70 parts by weight of neutral anhydrous sodium sulfate. .90 parts by weight was mixed, and then the obtained mixture was separated with a heat sealing machine to each 10 g using a packaging sheet having a heat-sealable resin film on an aluminum foil.

Test example 1
The powder bath A immediately after manufacture and the powder bath A to C after being stored in a 40 ° C. constant temperature bath for 1 week in a sealed state were subjected to the following evaluation test to evaluate the aroma. The results are shown in Table 3.

[Aroma evaluation test of bath salts]
Put 3 liters of 40 ° C hot water in a 3 liter beaker, put 1 bag (10 g) of powder bath, and evaluated the strength of the scent by sensory evaluation based on the following evaluation criteria by 5 expert panelists. . The evaluation result was based on the average score of five people.

Evaluation criteria:
5 points; 4 points with a strong lemon smell; 3 points with a fairly strong lemon smell; 2 points with a clear lemon smell; 1 point with a weak but lemon smell; little lemon smell

  From Table 3, the powder bath C produced by the conventional method has a large deterioration in aroma when dissolved in hot water after storage at 40 ° C. for 1 week, whereas the lock-in type powder flavor of the present invention is It can be seen that the blended powder baths A and B retain the same fragrance as that before storage even after storage at 40 ° C. for 1 week.

Test example 2
Samples were prepared under the following sample preparation conditions using powder baths A, B, C immediately after production and powder baths A, B, C after storage for 1 week in a 40 ° C. constant temperature bath. The amount of the fragrance component was calibrated under the above conditions, and the change with time of the fragrance component during storage was examined. Table 4 shows the results (the amount of the corresponding fragrance component after 7 days storage when each fragrance component immediately after production is 100.0; after correction by the internal standard).
(Sample preparation conditions)
Add 500 mg of powder bath to 100 mL of hot water at 42 ° C. Thereafter, extraction was performed with 100 mL of diethyl ether, 0.15 mL of the internal standard was added, and then the extract was concentrated to 0.5 mL to prepare a sample.
The internal standard is obtained by dissolving 25 μL (20 mg) of hexyl ether (carbon number 12) in 5 mL of diisopropyl ether and refrigerated.
(Gas chromatography measurement conditions)
Column: HP-20M 0.2 mm × 25 m (PEG column)
Start temperature 55 ° C, temperature increase condition 1.5 ° C / min, end point temperature 85 ° C
Introduction temperature: 250 ° C
FID temperature: 250 ° C
Carrier gas flow rate: 0.3 mL / min. (Constant flow)
Split ratio: 10: 1
Sample introduction amount: 2μL of autosampler

  From Table 4, in the powder bath C produced by the conventional method, the fragrance component deteriorated severely after storage at 40 ° C. for 1 week, whereas the powder of the present invention containing the lock-in type powder fragrance It can be seen that the powder baths A and B, which are bathing agents, have almost no deterioration of the fragrance component even after storage at 40 ° C. for 1 week.

Example 3: Production of powder detergent D 98.00 parts by weight of a commercial detergent base was mixed with 2.00 parts by weight of the lock-in type powder fragrance A obtained in Production Example 1, and this powder mixture was then placed on an aluminum foil. Using a packaging sheet having a heat-sealable resin film, it was sealed with a heat-sealing machine to each 20 g.

Comparative Example 3 Production of Powder Detergent E Mix 99.80 parts by weight of a commercial detergent base with 0.2 parts by weight of lemon oil EXG 5 hold, and then add this powder mixture to a heat-sealable resin film on an aluminum foil. Using the packaging sheet, it was sealed with a heat sealer for each 20 g.

Test example 3
Detergents D and E immediately after production and powder detergents D and E after being stored in a 40 ° C. constant temperature bath for 1 week in a sealed state were subjected to the following evaluation test to evaluate the fragrance strength. The results are shown in Table 5.

[Detergent aroma evaluation test]
Put one bath towel in the automatic washing machine, set the water volume low, start washing with 20g of the above detergent, and after 5 minutes of start, the expert panelists of the fragrance in the washing machine during washing 5 minutes Thus, sensory evaluation was performed based on the following evaluation criteria. The evaluation result was based on the average score of five people.

Evaluation criteria:
5 points; 4 points with a strong lemon smell; 3 points with a very strong lemon smell; 2 points with an obvious lemon smell; 1 point with a weak but lemon smell; little lemon smell

From Table 5, the powder detergent E produced by the conventional method has a significantly worse aroma at the time of washing after storage at 40 ° C. for 1 week than when the detergent just produced is used, whereas the lock of the present invention It can be seen that the powder detergent D containing the in-type powder fragrance retains the same fragrance as the detergent immediately after manufacture even after storage at 40 ° C. for 1 week.

Claims (3)

A solid preparation for cosmetics containing a lock-in type powder fragrance. The solid preparation for cosmetics according to claim 1, wherein the cosmetic is a bath agent or a detergent. A method for stabilizing the aroma of a solid preparation for cosmetics, wherein a lock-in powder flavor is used in the solid preparation for cosmetics.