Emulsion composition

Abstract

To provide an emulsion composition which has high emulsion stability, and includes, water, fat, cyclodextrin, and a water soluble gelatinizer.SOLUTION: There is provided an emulsion composition including, water, fat, cyclodextrin, and a prescribed water soluble gelatinizer, where a ratio of a blending amount of the fat and a total blending amount of the cyclodextrin and the water soluble gelatinizer is, in a mass ratio, (a blending amount of the fat: a total blending amount of the cyclodextrin and the water soluble gelatinizer) is, 1 or greater and less than 9: greater than 1 and equal to or less than 9.SELECTED DRAWING: None

Description

Technical Field

[0001] The present invention relates to an emulsified composition containing water, oil and fat, cyclodextrin, and a predetermined water-soluble gelling agent.

Background Art

[0002] Emulsified compositions containing oil and fat, water, cyclodextrin, and a water-soluble gelling agent are widely used in various fields such as pharmaceuticals, cosmetics, food and beverages.

[0003] Patent Document 1 discloses an emulsified composition containing water, an oily component, α-cyclodextrin, and as a gel-forming component, any one or more of agar, low-strength agar, galactomannan or glucomannan in combination with xanthan gum, carrageenan, furcellaran, gellan gum, native gellan gum.

[0004] Patent Document 2 discloses an emulsified composition characterized by containing oil and fat, water, cyclodextrin, etc., and also discloses that gums such as xanthan gum, guar gum, gum arabic CMC, carrageenan, locust bean gum, etc. may be used as stabilizers.

[0005] Patent Document 3 discloses an emulsified cosmetic obtained by mixing an aqueous raw material in which a water-soluble polymer compound such as pectin, tragacanth gum, gelatin, casein, sodium alginate, hydroxypropyl cellulose, hydroxyethyl cellulose, hydroxypropyl methylcellulose, methylcellulose, sodium polyacrylate, carboxyvinyl polymer is dissolved with an oily raw material for cosmetics, adding cyclodextrin, and emulsifying.

[0006] Non-Patent Document 1 describes that when xanthan gum and tragacanth gum were respectively added as emulsifying stabilizers to an oil-in-water emulsion obtained by emulsifying a 1:1 volume ratio sample of soybean oil and an aqueous cyclodextrin solution, the emulsification stability increased.

Prior Art Documents

Patent Documents

[0007]

Patent Document 1

Patent Document 2

Patent Document 3

Non-Patent Documents

[0008]

Non-Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0009] The inventors have found that a conventionally known emulsified composition containing oil and fat, water, cyclodextrin, and a water-soluble gelling agent has insufficient emulsification stability and may easily separate oil and water.

[0010] Therefore, an object of the present invention is to provide an emulsified composition containing oil and fat, water, cyclodextrin, and a water-soluble gelling agent, which has high emulsification stability.

Means for Solving the Problems

[0011] As a result of intensive studies to solve the above problems, the inventors have found that by blending at least one water-soluble gelling agent selected from the group consisting of carboxymethyl cellulose (CMC), xanthan gum, locust bean gum, guar gum, glucomannan, κ-carrageenan, ι-carrageenan, λ-carrageenan, tamarind gum, and gellan gum together with oil and fat, water, and cyclodextrin, an emulsified composition having high emulsification stability can be obtained.

[0012] And, by setting the ratio of the blending amount of the fats and oils in the emulsified composition to the total blending amount of cyclodextrin and the water-soluble gelling agent within the range of (blending amount of fats and oils: total blending amount of cyclodextrin and water-soluble gelling agent) of 1 or more and less than 9: 9 or less and more than 1 in terms of mass ratio, it has been found that the form (for example, powder) obtained by drying the emulsified composition has excellent heat resistance and moisture resistance and does not cause discoloration or dissolution even when subjected to high temperature and high humidity conditions.

[0013] Furthermore, it has been found that high emulsification stability is maintained also for the emulsified composition obtained by re-emulsifying the form obtained by drying in a solvent such as water.

[0014] The present invention is based on these novel findings and includes the following inventions. [1] An emulsified composition containing water, fats and oils, cyclodextrin, and at least one water-soluble gelling agent selected from the group consisting of carboxymethyl cellulose (CMC), xanthan gum, locust bean gum, guar gum, glucomannan, κ-carrageenan, ι-carrageenan, λ-carrageenan, tamarind gum, and gellan gum, wherein the ratio of the blending amount of the fats and oils to the total blending amount of the cyclodextrin and the water-soluble gelling agent is in the range of (blending amount of fats and oils: total blending amount of cyclodextrin and water-soluble gelling agent) of 1 or more and less than 9: 9 or less and more than 1 in terms of mass ratio. [2] The emulsified composition according to [1], wherein the water content is 10% by mass or less. [3] The emulsified composition according to [1] or [2], which has a powder form. [4] A re-emulsified composition comprising the emulsified composition according to [2] or [3] and a solvent. [5] The re-emulsified composition according to [4], further comprising an emulsifier. [6] The re-emulsified composition according to [4] or [5], further comprising an aqueous organic solvent. [7] A step of mixing water, oil and fat, cyclodextrin, and at least one water-soluble gelling agent selected from the group consisting of carboxymethyl cellulose (CMC), xanthan gum, locust bean gum, guar gum, glucomannan, κ-carrageenan, ι-carrageenan, λ-carrageenan, tamarind gum, and gellan gum to form an emulsified composition, wherein the ratio of the blending amount of the oil and fat to the total blending amount of the cyclodextrin and the water-soluble gelling agent is in the range of (the blending amount of the oil and fat: the total blending amount of the cyclodextrin and the water-soluble gelling agent) 1 or more and less than 9: 9 or less and more than 1 by mass ratio, and mixing is carried out so as to be in this range. A method for producing an emulsified composition, including this step. [8] A production method according to [7], further including a step of subjecting the obtained emulsified composition to a drying treatment. [9] The production method according to [8], wherein the water content of the emulsified composition is made 10% by mass or less by the drying treatment.

[10] A production method according to [8] or [9], further including a step of forming the obtained emulsified composition into a powder form.

[11] A method for producing a re-emulsified composition, including a step of mixing the emulsified composition of [2] or [3] with a solvent to form a re-emulsified composition.

[12] The production method according to

[11] , further mixing an emulsifier.

[13] The production method according to

[11] or

[12] , further mixing an aqueous organic solvent.

Advantages of the Invention

[0015] According to the present invention, it is possible to provide an emulsified composition containing oil and fat, water, cyclodextrin, and a water-soluble gelling agent, which has excellent emulsification stability.

Brief Description of the Drawings

[0016]

Figure 1

Mode for Carrying Out the Invention

[0017] The present invention relates to an emulsion composition containing water, fats and oils, cyclodextrin, and a predetermined water-soluble gelling agent.

[0018] In the present invention, "oil and fat" can utilize the oil and fat generally used in an emulsified composition, and both polar and non-polar ones can be used. Such oil and fat include, for example, plant-derived oil and fat (such as canola oil, rapeseed white pressed oil, soybean oil, corn oil, cottonseed oil, peanut oil, sesame oil, rice oil, rice bran oil, camellia oil, safflower oil, olive oil, linseed oil, perilla oil, egoma oil, sunflower oil, palm oil, tea oil, coconut oil, avocado oil, kukui nut oil, grape seed oil, cocoa butter, coconut oil, wheat germ oil, almond oil, evening primrose oil, castor oil, hazelnut oil, macadamia nut oil, rose hip oil, grape oil, cacao oil, jojoba oil, palm kernel oil, beeswax, candelilla wax, carnauba wax, etc.), paraffin, microcrystalline wax, ceresin, petrolatum, ozokerite, isostearyl alcohol, capryl alcohol, lauryl alcohol, stearyl alcohol, 2-octadecyl alcohol, myristyl alcohol, cetyl alcohol, phytosterol, cholesterol, stearic acid, isostearic acid, capric acid, lanolinic acid, lauric acid, myristic acid, palmitic acid, behenic acid, linoleic acid, linolenic acid, glyceryl monostearate, glyceryl monopalmitate, glyceryl monobehenate, glyceryl monomyristate, glyceryl monolaurate, glyceryl monolanolinate, glyceryl monolinoleate, glyceryl monolinolenate, glyceryl monooleate, glyceryl triisostearate, isopropyl myristate, glyceryl tri-2-heptylundecanoate, glyceryl tri-2-ethylhexanoate, 2-heptylundecyl palmitate, di-2-heptylundecyl adipate, cetyl isooctanoate, trimethylolpropane-2-trimethylolheptylundecanoate, propane-2-ethylhexanoate, pentaerythritol-2-heptylundecanoate, pentaerythritol-2-ethylhexanoate, cholesterol isostearate, diethyl phthalate, dibutyl phthalate and other synthetic ester oils, beef tallow, lard, lanolin, squalene, squalane, beeswax, sperm whale oil and other animal-derived oil and fat, silicone oil, etc., but are not limited thereto.In the present invention, the oil and fat is preferably a highly safe animal-derived or plant-derived oil and fat, and particularly preferably an edible vegetable oil having a food experience and high safety. The oil and fat may be used alone or in combination of different oils and fats.

[0019] In the emulsified composition of the present invention, the oil and fat can be contained in any amount as long as the ratio of the blending amount of the oil and fat detailed below to the total blending amount of cyclodextrin and the water-soluble gelling agent is within a predetermined range in terms of mass ratio. For example, it can be contained in an amount of 1% by mass or more, 3% by mass or more, 5% by mass or more, or 7% by mass or more, and the upper limit is not particularly limited, but for example, it can be 50% by mass or less, 40% by mass or less, 30% by mass or less, 20% by mass or less, or 10% by mass or less. The range of the amount of the oil and fat in the emulsified composition of the present invention can be represented by using two numerical values respectively selected from the numerical values of the lower limit and the upper limit. For example, the emulsified composition of the present invention contains the oil and fat in an amount appropriately selected from the range of 1% by mass to 50% by mass, 1% by mass to 30% by mass, or 1% by mass to 20% by mass, or 1% by mass to 10% by mass, preferably 5% by mass to 10% by mass, or 7% by mass to 10% by mass. When the amount of the oil and fat is less than 1% by mass, emulsification may be insufficient, or for example, a squeaky feeling may be felt when applied. On the other hand, when the amount of the oil and fat is more than 50% by mass, an oily feeling such as stickiness or greasiness may be strongly felt, and a desired feeling of use may not be obtained in the form of use in the intended application. In the present specification, the description of the amount of each component is shown in terms of mass% with the total mass of the emulsified composition of the present invention being 100% by mass.

[0020] In the emulsified composition of the present invention, water can be contained in any amount capable of emulsifying an oil and fat to form an oil-in-water emulsion together with cyclodextrin and a predetermined water-soluble gelling agent. For example, the emulsified composition of the present invention contains water in an amount of 15% by mass or more, 20% by mass or more, 30% by mass or more, 40% by mass or more, 45% by mass or more, 50% by mass or more, 60% by mass or more, or 70% by mass or more. The upper limit is not particularly limited, but can be, for example, 90% by mass or less, or 85% by mass or less. The range of the amount of water in the emulsified composition of the present invention can be represented by using two numerical values respectively selected from the numerical values of the above lower limit and upper limit. For example, the emulsified composition of the present invention can contain water in an amount appropriately selected from the ranges of 15% by mass to 90% by mass, 45% by mass to 90% by mass, or 70% by mass to 85% by mass. The amount of water contained in the emulsified composition of the present invention is preferably larger than the oil and fat in terms of volume ratio. For example, the content of the oil and fat and water can be in an amount exceeding 1:1 (oil and fat: water) in terms of volume ratio, for example, 1:2 or more, 1:3 or more, 1:4 or more, 1:5 or more, 1:6 or more, 1:10 or more, 1:15 or more, or 1:20 or more. The upper limit of the amount of water is not particularly limited, but can be 1:90 or less, 1:80 or less, 1:70 or less, 1:60 or less, or 1:50 or less. By adjusting the amounts of water and oil and fat contained in the emulsified composition of the present invention to the above ranges, a feeling of use with reduced oiliness such as stickiness and greasiness can be obtained.

[0021] "Cyclodextrin" means a cyclic non-reducing maltooligosaccharide having glucose as a constituent unit, and examples thereof include α-cyclodextrin having 6 glucose units, β-cyclodextrin having 7 glucose units, and γ-cyclodextrin having 8 glucose units. In the present invention, α-, β-, γ-cyclodextrins, their derivatives, and any combination thereof can be used. Examples of cyclodextrin derivatives include, but are not limited to, ethyl cyclodextrin, methyl cyclodextrin, hydroxyethyl cyclodextrin, hydroxypropyl cyclodextrin, methylamino cyclodextrin, amino cyclodextrin, carboxyethyl cyclodextrin, carboxymethyl cyclodextrin, sulfoethyl cyclodextrin, sulfoxyl cyclodextrin, acetyl cyclodextrin, branched cyclodextrin, cyclodextrin fatty acid ester, glucosyl cyclodextrin, maltosyl cyclodextrin, etc. Preferably, α-cyclodextrin is used. α-Cyclodextrin has high solubility in water and can obtain an emulsified composition with less roughness.

[0022] In the emulsified composition of the present invention, cyclodextrin can be included in an amount that can impart emulsification stability to an oil-in-water emulsion together with a predetermined water-soluble gelling agent and can provide a desired feeling of use in the form of use in the intended application, as long as the ratio of the blending amount of the oil and fat detailed below to the total blending amount of cyclodextrin and the water-soluble gelling agent is within a predetermined range in terms of mass ratio. For example, cyclodextrin can be included in the emulsified composition of the present invention in an amount of 0.5% by mass or more, 1% by mass or more, 2.5% by mass or more, 3% by mass or more, 4% by mass or more, 4.5% by mass or more, or 5% by mass or more. The upper limit is not particularly limited, but can be, for example, 15% by mass or less, 10% by mass or less, 9% by mass or less, 8% by mass or less, 7% by mass or less, or 6% by mass or less. The range of the amount of cyclodextrin in the emulsified composition of the present invention can be represented by using two numerical values respectively selected from the numerical values of the above lower limit and upper limit. For example, the emulsified composition of the present invention contains cyclodextrin in an amount of 0.5% by mass to 15% by mass, for example, 1% by mass to 15% by mass, 2.5% by mass to 10% by mass, 2.5% by mass to 9% by mass, 3% by mass to 9% by mass, 4% by mass to 8% by mass, 4.5% by mass to 9% by mass, or 5% by mass to 7% by mass, preferably 2.5% by mass to 9% by mass, or 4.5% by mass to 9% by mass, and can be included in an amount appropriately selected from these ranges. If the amount of cyclodextrin is less than 0.5% by mass, the emulsification stability of the composition may be insufficient. On the other hand, if it is more than 15% by mass, the viscosity of the composition may become too high or the feeling of squeak may become strong, and in either case, a desired feeling of use may not be obtained in the form of use in the intended application.

[0023] In the present invention, the "water-soluble gelling agent" generally refers to a substance that dissolves in water and imparts viscosity (which may also be called a thickener, thickening stabilizer, sizing agent, etc.). Examples of water-soluble gelling agents that can be used in the present invention include carboxymethyl cellulose (CMC), xanthan gum, locust bean gum, guar gum, glucomannan, κ-carrageenan, ι-carrageenan, λ-carrageenan, tamarind gum, and gellan gum. The water-soluble gelling agent may be used alone or in combination of different water-soluble gelling agents. More preferably, the water-soluble gelling agent is carboxymethyl cellulose (CMC), glucomannan, tamarind gum, and xanthan gum, which can impart particularly high emulsion stability to the emulsion composition of the present invention.

[0024] In the emulsion composition of the present invention, as long as the ratio of the blending amount of the oil and fat detailed below to the total blending amount of cyclodextrin and the water-soluble gelling agent is within a predetermined range in terms of mass ratio, the water-soluble gelling agent can be included in an amount that can impart emulsion stability to the oil-in-water emulsion together with cyclodextrin and obtain a desired feeling of use in the form of use for the intended purpose. For example, the emulsion composition of the present invention contains a water-soluble gelling agent in an amount of 0.05% by mass or more, 0.1% by mass or more, 0.2% by mass or more, or 0.3% by mass or more, and the upper limit is not particularly limited, but can be, for example, 1% by mass or less, 0.8% by mass or less, 0.7% by mass or less, 0.6% by mass or less, or 0.5% by mass or less. The range of the amount of the water-soluble gelling agent in the emulsion composition of the present invention can be represented by using two numerical values respectively selected from the numerical values of the above lower limit and upper limit. For example, the emulsion composition of the present invention can contain a water-soluble gelling agent in an amount appropriately selected from the ranges of 0.05% by mass to 1% by mass, 0.1% by mass to 1% by mass, 0.2% by mass to 0.8% by mass, or 0.2% by mass to 0.5% by mass. If the amount of the water-soluble gelling agent is less than 0.1% by mass, the emulsion stability of the composition may be insufficient. On the other hand, if it is more than 1% by mass, the viscosity of the composition may become too high, and in either case, a desired feeling of use may not be obtained in the form of use for the intended purpose.

[0025] In the emulsified composition of the present invention, the ratio of the blending amount of the oil and fat to the total blending amount of the cyclodextrin and the water-soluble gelling agent is in the range of (the blending amount of the oil and fat: the total blending amount of the cyclodextrin and the water-soluble gelling agent) 1 or more and less than 9: 9 or less and more than 1 in terms of mass ratio. For example, in the emulsified composition of the present invention, the blending amount of the oil and fat: the total blending amount of the cyclodextrin and the water-soluble gelling agent is, in terms of mass ratio, 1:9, 2:8, 3:7, 4:6, 5:5, 6:4, 7:3, or 8:2, preferably 5:5. In this ratio, when the blending amount of the oil and fat is less than 1 and the total blending amount of the cyclodextrin and the water-soluble gelling agent is more than 9, the emulsification and emulsion stability of the emulsified composition may be insufficient. Also, when the blending amount of the oil and fat is 9 or more and the total blending amount of the cyclodextrin and the water-soluble gelling agent is 1 or less, a strong oily feeling such as stickiness or greasiness may be felt in the emulsified composition, and in the dried product of the emulsified composition, sufficiently high heat resistance and moisture resistance may not be obtained. In any case, a desired feeling in use may not be obtained in the form of use in the intended application.

[0026] The emulsified composition of the present invention has high emulsion stability. More preferably, the emulsified composition of the present invention can maintain the emulsified state even after being subjected to high temperature (for example, about 100°C to 130°C) conditions, and has excellent emulsion stability with high heat resistance and no emulsion breakage.

[0027] The emulsified composition of the present invention has high emulsion stability regardless of the pH value. More preferably, the emulsified composition of the present invention can maintain the emulsified state even after being subjected to high temperature (for example, about 100°C to 130°C) conditions, and has excellent emulsion stability with high heat resistance and no emulsion breakage.

[0028] The form of the emulsified composition of the present invention is not particularly limited. In addition to the form having the above moisture content, it may also be provided in the form of a semi-solid / semi-liquid (gel, sol, etc.) or a dried product (e.g., powder, flake, etc.) prepared by reducing the moisture content. Such forms of semi-solid / semi-liquid (gel, sol, etc.) or dried product (e.g., powder, flake, etc.) can be obtained by subjecting the emulsified composition having the above moisture content to a conventionally known drying means to reduce the moisture content of the emulsified composition. Examples of such drying means include, but are not limited to, freeze-drying, heat drying, air drying, spray drying, drum drying, hot air drying, vacuum drying, etc. The moisture content of the emulsified composition after being subjected to the drying means can be appropriately selected according to the intended form. For example, in the case of a dried product form, it can be less than 15% by mass, 10% by mass or less, 5% by mass or less, or 1% by mass or less. The lower limit of the moisture content of the emulsified composition after being subjected to the drying means is not particularly limited, but can be 0% by mass or more, more than 0% by mass, 0.1% by mass or more, 0.5% by mass or more, 0.6% by mass or more, 0.7% by mass or more, or 0.8% by mass or more. The range of the moisture content of the dried product form can be represented by using two numerical values respectively selected from the above upper and lower limit values. For example, the moisture content of the emulsified composition can be 0% by mass to less than 15% by mass, more than 0% by mass to less than 15% by mass, 0.1% by mass to less than 15% by mass, 0.1% by mass to 10% by mass, 0.5% by mass to 5% by mass, 0.5% by mass to 1% by mass, 0.6% by mass to 1% by mass, 0.7% by mass to 1% by mass, or 0.8% by mass to 1% by mass. The emulsified composition after being subjected to the drying means may be used as it is, or alternatively, a suitable solvent (e.g., water, hot water, a mixture of a water-soluble organic solvent and water, etc.) may be added during use / to a suitable solvent and re-emulsified (which may be described as a "re-emulsified composition" in this specification) and used.

[0029] The emulsified composition after being subjected to the drying means, especially in the form of a dried product, has high heat resistance and moisture resistance and does not cause discoloration or dissolution even after being subjected to high temperature (e.g., about 100°C to 200°C) conditions and / or high humidity (e.g., about 95% humidity) conditions.

[0030] The re-emulsified composition has high emulsification stability, and more preferably, it can maintain the emulsified state even after being subjected to high temperature conditions (for example, about 100°C to 130°C), and has excellent heat resistance and high emulsification stability without causing emulsion breakage.

[0031] The re-emulsified composition has high emulsification stability regardless of the pH value, and more preferably, it can maintain the emulsified state even after being subjected to high temperature conditions (for example, about 100°C to 130°C), and has excellent heat resistance and high emulsification stability without causing emulsion breakage.

[0032] In addition, in this specification, unless otherwise specified, the "emulsion composition of the present invention" includes, in addition to the form having the above water content, forms such as semi-solid / semi-liquid (gel, sol, etc.) and dried bodies (for example, powders, flakes, etc.), as well as the form of the re-emulsified composition.

[0033] The emulsion composition of the present invention can be used as a base and included in applications such as food and drink products, cosmetics, external pharmaceuticals, pharmaceuticals (including quasi-drugs), chemical products, chemical finished products, agricultural chemicals, toiletries, spray products, paints, industrial thin film materials, surface modification materials, etc., and can be provided in a form for use in the intended application (for example, the form of a predetermined product, etc.).

[0034] The emulsified composition of the present invention can exhibit excellent heat resistance, whereby in the usage form for the purpose of using the emulsified composition of the present invention as a base, it can be subjected to high-temperature conditions in the processes such as its production, sterilization, storage, and use. For example, the usage form for the purpose of using the emulsified composition of the present invention as a base can be subjected to heat sterilization treatment, more specifically, high-temperature sterilization treatment at 100°C to 130°C (for example, retort sterilization treatment), and a product with less / no added preservatives and high safety can be provided. Also, for example, the emulsified composition of the present invention can be subjected to high-temperature conditions together with other raw materials, or can be immediately combined with other raw materials that have been subjected to high-temperature conditions, which not only contributes to the efficiency improvement of the manufacturing process and operations, but also enables the production of usage forms (for example, predetermined products, etc.) that could not be achieved conventionally because high-temperature conditions were avoided.

[0035] The emulsified composition of the present invention has high emulsification stability regardless of the pH value, and more preferably, it can maintain the emulsified state even after being subjected to high-temperature conditions (for example, about 100°C to 130°C), and has high heat resistance and excellent emulsification stability without causing emulsion breakdown. The pH value of the emulsified composition of the present invention is not particularly limited and can be appropriately set to the pH value desired in the usage form for the intended application. The pH value of the emulsified composition of the present invention can be adjusted using conventionally known and generally used pH adjusters. In this specification, the pH value of the emulsified composition of the present invention means the value measured at 25°C in accordance with JIS Z8802:2011. Thereby, for the usage form for the purpose of using the emulsified composition of the present invention as a base, it can be subjected to various pH conditions in the processes such as its production, sterilization, storage, and use, enabling the production of usage forms (for example, predetermined products, etc.) in various applications without being limited by the pH value.

[0036] In addition to the above components, the emulsified composition of the present invention may further contain, if necessary, components commonly used in the production of the form of use in the intended application, in an amount appropriate to the desired form of use, within the range that does not impair the effects of the present invention. Examples of such components include excipients, disintegrants, lubricants, binders, diluents, buffers, suspending agents, thickeners, preservatives, antibacterial agents, antiseptics, antioxidants, ultraviolet absorbers, colorants, pigments, dyes, coloring matters, lubricants, plasticizers, solvents, solubilizing agents, isotonic agents, flavoring agents, fragrances, sweeteners, flavor components, acidulants, seasonings, humectants, vitamins, surfactants, chelating agents, antibacterial agents, emulsifiers, water-soluble organic solvents, etc., but are not limited thereto.

[0037] The emulsified composition of the present invention can impart high emulsion stability to the oil-in-water emulsion by the combined use of the above cyclodextrin and water-soluble gelling agent. Therefore, in addition to these, it may be substantially free of emulsifiers generally used in the production of conventional emulsified compositions. In the present invention, "substantially free of emulsifiers" means that in the emulsified composition of the present invention, the emulsifier is not contained in a form in which it exerts an emulsifying action, and it is not intended that no emulsifier is contained at all. By being substantially free of emulsifiers, the present invention can provide a highly safe emulsified composition with less skin irritation, for example, when the emulsified composition of the present invention is applied to the skin. Further, the emulsified composition of the present invention can provide a smooth and moist feeling after washing by being substantially free of emulsifiers, for example, when the emulsified composition of the present invention is applied to the skin. Examples of "emulsifiers generally used in the production of conventional emulsified compositions" include glycerin fatty acid esters, organic acid monoglycerides, polyglycerin fatty acid esters, polyoxyethylene glycerin fatty acid esters, sorbitan fatty acid esters, propylene glycol fatty acid esters, polyoxyethylene fatty acid esters, polyglycerin condensed ricinoleic acid esters, sorbitan fatty acid esters, polyoxyethylene sorbit fatty acid esters, sucrose fatty acid esters, lecithin, enzymatically decomposed lecithin, polyethylene glycol, polypropylene glycol, etc., but are not limited thereto.

[0038] Alternatively, in the emulsified composition of the present invention, an emulsifier generally used in the production of conventional emulsified compositions may be appropriately selected and blended according to the usage form in the intended application within the range that does not impair the desired effects of the present invention described above. In the emulsified composition of the present invention, the emulsifier can be included in an amount that can obtain a desired feeling of use in the usage form in the intended application within the range that does not impair the desired effects of the present invention described above. For example, the emulsified composition of the present invention contains an emulsifier in an amount of 0.005% by mass or more, or 0.01% by mass or more, and the upper limit is not particularly limited, but can be, for example, 0.5% by mass or less, or 0.1% by mass or less. The range of the amount of the emulsifier in the emulsified composition of the present invention can be represented by using two numerical values respectively selected from the numerical values of the lower limit and the upper limit. For example, the emulsified composition of the present invention can contain an emulsifier in an amount appropriately selected from the range of 0.005% by mass to 0.5% by mass or less, or 0.01% by mass to 0.1% by mass.

[0039] By blending an emulsifier into the emulsified composition of the present invention, the adhesiveness of the emulsified composition can be suppressed / disappeared.

[0040] The emulsified composition of the present invention has water-soluble organic solvent resistance, and thereby can maintain an emulsified state and does not cause emulsion breakage even after being subjected to high-temperature conditions in the presence of a water-soluble organic solvent, more preferably in the presence of a water-soluble organic solvent, and can maintain excellent emulsion stability.

[0041] As used herein, the term "water-soluble organic solvent" generally refers to an organic solvent that, when mixed with water, dissolves in water and does not form a two-phase system (consisting of an organic phase and an aqueous phase), but forms a homogeneous phase. Examples include alcohols (e.g., methanol, ethanol, propanol, isopropanol, butanol, isobutanol, 2-butanol, tert-butanol, etc.), polyhydric alcohols (e.g., ethylene glycol, diethylene glycol, polyethylene glycol, propylene glycol, dipropylene glycol, polypropylene glycol, glycerin, glucose, etc.), glycol ethers (e.g., ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, etc.), alkanediols (e.g., 1,2-butanediol, 1,3-propanediol, 1,3-butanediol, 1,4-butanediol, etc.), amines (e.g., ethanolamine, diethanolamine, triethanolamine, etc.), amides (e.g., formamide, etc.), ketones (e.g., acetone, acetylacetone, etc.), nitriles (e.g., acetonitrile, etc.), nitrogen-containing solvents (e.g., 2-pyrrolidone, triethanolamine, etc.), sulfur-containing solvents (e.g., thiodiethanol, dimethyl sulfoxide, etc.), etc., but are not limited thereto. The water-soluble organic solvent can be appropriately selected according to the form of use in the intended application of the emulsified composition of the present invention. For example, it can be blended as a solvent for other components, etc.

[0042] The emulsified composition of the present invention can be produced by mixing and stirring water, fats and oils, cyclodextrin, a predetermined water-soluble gelling agent, and, if necessary, other components in the above amounts. All the components may be mixed and stirred together, or each component may be added sequentially separately or in any combination (the order does not matter) and then mixed and stirred. The emulsified composition obtained by mixing and stirring may be subjected to heat sterilization treatment.

[0043] Further, the emulsified composition obtained by mixing and stirring may be further subjected to a drying means if necessary. The drying means can be carried out by the above-mentioned conventionally known drying means, and the water content of the emulsified composition can be appropriately adjusted according to the target shape of the semi-solid / semi-liquid (gel, sol, etc.) or the dried body. The obtained dried body can be further subjected to crushing, grinding, or pulverization treatment to form powders, flakes, etc. if necessary. Other components may be mixed and stirred in the above amounts in the emulsified composition obtained by being subjected to the drying means, and / or it may be subjected to heat sterilization treatment.

[0044] The emulsified composition obtained by being subjected to the drying means can be used to produce a re-emulsified composition by further mixing, stirring, and re-emulsifying it with a suitable solvent if necessary. The solvent can be appropriately selected according to the form of use in the target application of the re-emulsified composition. For example, water, a mixture of a water-soluble organic solvent and water, etc. can be mentioned, and it can be included in an amount appropriately selected from the range of 15% by mass to 90% by mass, preferably 45% by mass to 90% by mass, more preferably 70% by mass to 85% by mass. Other components may be mixed and stirred in the above amounts in the obtained re-emulsified composition, and / or it may be subjected to heat sterilization treatment.

[0045] Hereinafter, the present invention will be described by way of examples, but the present invention is not limited to these examples.

Examples

[0046] Experiment 1: Evaluation of the Emulsion Stability of the Emulsified Composition (1) Preparation of the Emulsified Composition According to the composition of Table 1 below, each component was added and mixed to prepare an emulsion composition. As the water-soluble gelling agent, any one of carboxymethyl cellulose (CMC), sodium alginate, gum arabic, glucomannan, guar gum, pectin, κ-carrageenan, tamarind gum, gellan gum, xanthan gum, ι-carrageenan, locust bean gum, λ-carrageenan, phosphate-crosslinked starch, hydroxypropyl starch, hydroxypropylated phosphate-crosslinked starch, tragacanth gum, carboxyl vinyl polymer, sodium polyacrylate, hydroxypropyl cellulose, methyl cellulose, hydroxypropyl methyl cellulose, and hydroxyethyl cellulose was blended.

[0047] The mixing of each component was carried out by stirring at 20,000 rpm for 10 minutes using a hand blender. Each obtained composition (50 mL) was transferred to a conical tube (Falcon (registered trademark) conical tube 50 mL) and centrifuged at 3000 rpm for 1 minute. Then, the thickness (depth) of the aqueous phase, micelles, and oil phase was visually observed, and the ratio (%) of each phase was measured to evaluate the emulsion stability of each composition. The evaluation was performed as follows: those with a micelle ratio of 100% were rated as "◎", those with a micelle ratio of 70% or more and less than 100% were rated as "〇", and those with a micelle ratio of less than 70% were rated as "×".

[0048] Note that the amounts of each component in the table described below are shown in mass% with the amount of the obtained emulsion composition being 100 mass%. For fats and oils, α-cyclodextrin, and water-soluble gelling agent, food additives (food grade) were all used.

[0049]

Table 1

[0050] (2) Results Table 2 shows the water-soluble gelling agents added to the emulsion composition, the measured ratios of each phase, and the evaluation results. As is clear from these results, the emulsion stability of the emulsion composition varies depending on the water-soluble gelling agent added. When CMC, glucomannan, guar gum, κ-carrageenan, tamarind gum, gellan gum, xanthan gum, ι-carrageenan, locust bean gum, or λ-carrageenan was added, the micellar phase was maintained and high emulsion stability was shown. In particular, when CMC, glucomannan, tamarind gum, or xanthan gum was added, no separation of the aqueous and oil phases was observed, and remarkably high emulsion stability was confirmed.

[0051]

Table 2

[0052] Experiment 2: Evaluation of the interaction between α-cyclodextrin and water-soluble gelling agents in the emulsion composition To evaluate the interaction between α-cyclodextrin and water-soluble gelling agents in an aqueous solution, the enthalpy change (ΔH) was determined by isothermal titration calorimetry (ITC) according to a conventionally known method. That is, using an isothermal titration calorimeter (NANO ITC SV; TA Instruments), 10 μL of an aqueous solution of a water-soluble gelling agent (0.05 g / 100 mL) was added dropwise to an aqueous solution of α-cyclodextrin (25 g / 100 mL) every 180 seconds for 25 times (75 minutes), and the enthalpy value (μJ) was determined from the area of the 25th (final) titration peak.

[0053] The results are shown in Table 3. A positive enthalpy value, that is, an endothermic reaction, was observed only when CMC and xanthan gum, which showed high emulsification stability in Experiment 1 above, were used. This result suggests the presence of an interaction via hydration water between the water-soluble gelling agent and α-cyclodextrin. For example, it is conceivable that some of the water molecules hydrated to the water-soluble gelling agent form hydrogen bonds with α-cyclodextrin. Usually, the hydrogen bonds formed between water molecules are shorter in distance and higher in energy value than the hydrogen bonds formed between the water-soluble gelling agent and α-cyclodextrin, which cause intermolecular repulsion due to charged sites. Therefore, when some of the water molecules hydrated to the water-soluble gelling agent form hydrogen bonds with α-cyclodextrin, it is considered that an endothermic reaction occurs as a result of the difference in energy values. The transfer of heat (positive enthalpy value) suggests the presence of an interaction between the water-soluble gelling agent and α-cyclodextrin, and this interaction is considered to be the factor that causes high emulsification stability in Experiment 1 above.

[0054] [Table 3]

[0055] Experiment 3: Performance evaluation (texture) of the emulsified composition (1) Preparation of the emulsified composition According to the compositions in Table 4 below, each component was added and mixed to prepare the emulsified compositions of Examples 1-4 and Comparative Examples 1-4. The mixing of each component was carried out by stirring at 20,000 rpm for 10 minutes using a hand blender. For each of the obtained emulsified compositions, the following evaluation items were evaluated based on each criterion. The evaluation was performed on 4 subjects.

[0056] · Viscosity (creaminess): When placed on the palm and spread, if it has a good feeling of use like lightly spreading cream, it is marked as "〇"; if it has a feeling of use like spreading cream, it is marked as "△"; if it is impossible to obtain a feeling of use like spreading cream (the viscosity is too low or too high), it is marked as "×".

[0057] ·Emulsifying power after storage: After storing at 40°C for 7 days, if emulsification is maintained, it is marked as "〇"; if separation of water and oil is observed, it is marked as "×".

[0058] ·Slipperiness immediately after application: Immediately after applying on the palm, if there is no oily feeling (stickiness or greasiness), it is marked as "〇"; if there is an oily feeling, it is marked as "×".

[0059] ·Feeling after washing: After applying on the palm and then washing, if a smooth and moist feeling is observed, it is marked as "〇"; if a smooth and moist feeling is observed but there is also a slight oily feeling at the same time, it is marked as "△"; if a smooth and moist feeling is not observed, it is marked as "×". Note that the same results can be obtained whether only water is used for washing or hand soap is used. In this case, washing was performed using hand soap.

[0060] ·Heat sterilization: After retort sterilization (123°C, 50 minutes) and cooling to room temperature, if emulsification is maintained, it is marked as "〇"; if separation of water and oil is observed, it is marked as "×". Note that the amounts of each component in the table described below are shown in mass% based on the amount of the obtained emulsified composition being 100 mass%.

[0061]

Table 4

[0062] (2) Results The evaluation results for each of the obtained emulsified compositions are shown in Table 4. From the results of Examples 1 - 4, it was confirmed that the fats and oils are not limited to specific ones and various fats and oils can be utilized.

[0063] When polyoxyethylene glycol was used instead of the water-soluble gelling agent (Comparative Examples 1, 2, and 4), it was found that a feeling of spreading the cream could not be obtained, a decrease in emulsifying power after storage, a decrease in the feeling of use immediately after application and after washing, and a decrease in emulsifying power after heat sterilization were observed, and it was confirmed that the performance was inferior to that of the emulsified compositions of Examples 1-4 using the water-soluble gelling agent.

[0064] The emulsified compositions of the examples had a good feeling of use like gently spreading the cream. Among them, the emulsified compositions of Examples 1-3 had particularly excellent performance, and good results were obtained in all evaluation items. In Examples 1 and 2 where the content of α-cyclodextrin was relatively high in Examples 1-3, a slightly tight feeling (a feeling of squeak) was felt when applied compared to Example 3 where the content was relatively low, but it did not interfere with the good feeling of use.

[0065] Experiment 4: Powder Emulsified Composition (Freeze-Dried) (1) Preparation of Powder Emulsified Composition According to the composition shown in Table 5 below, each component was added and mixed to prepare an emulsified composition. The mixing of each component was carried out by stirring at 20,000 rpm for 5 minutes using a hand blender. Then, the obtained emulsified composition was freeze-dried (made into a vacuum state after freezing, and then freeze-dried at 20 °C for 16 hours) and pulverized to obtain a powder emulsified composition. Note that the amounts of each component in the tables described below are shown in mass% with the amount of the obtained emulsified composition being 100 mass%.

[0066]

Table 5

[0067] (2) Performance Evaluation of Powder Emulsified Composition (Texture) (i) The water content of the obtained powder emulsion composition was measured by an atmospheric pressure heating drying method in accordance with a conventional method. That is, the obtained emulsion composition was placed in a weighing can and precisely weighed (mass before drying), dried at 105°C for 5 hours, then transferred to a desiccator, allowed to cool for 1 hour, and precisely weighed (mass after drying). From the mass before drying and the mass after drying, the water content (mass %) of the powder emulsion composition was determined.

[0068] (ii) For the obtained powder emulsion composition, "viscosity (creaminess)", "emulsifying power after storage", "slimy feeling immediately after application", and "feeling of use after washing" were evaluated according to the same method and judgment criteria as described in the above "Experiment 3: Performance Evaluation (Texture)". As a control, a composition obtained by the same operation except that each component was added according to the composition in Table 5 above and mixed by hand without applying a shearing force (i.e., not making an emulsion composition) was used.

[0069] (3) Results (i) The measurement results of the water content are shown in Table 6 below. The measurement of the water content was performed using two separately prepared powder emulsion compositions as samples. The water content of the obtained powder emulsion composition was approximately 0.7 mass% and approximately 0.9 mass%, and on average, it was approximately 0.8 mass%.

[0070]

Table 6

[0071] (ii) The powder emulsion composition has a powdery form that is smooth and dry, while the control composition is a paste-like form in which a liquid oil and fat and powder are mixed, and a smooth and dry powdery form could not be obtained.

[0072] In addition, for the obtained powder emulsion composition, all of "viscosity (creaminess)", "emulsifying power after storage", "slimy feeling immediately after application", and "feeling of use after washing" received an evaluation of "〇". Similar to the emulsion composition of Experiment 3 above, when spread on the palm, it can be spread in a transparent state where an oil film forms quickly, has a good feeling of use, and when washed after application, a crispy feeling like when powder is applied and a moist feeling like when cream is applied were obtained simultaneously. On the other hand, for the control composition, when spread on the palm, liquid and solid separated, and a rough and grating feeling was felt, and a good feeling of use was not obtained.

[0073] Experiment 5: Powder Emulsion Composition (Spray Drying) (1) Preparation of Powder Emulsion Composition According to the composition in Table 5 above, each component was added and mixed to prepare an emulsion composition. The mixing of each component was carried out by stirring with a hand blender at 20,000 rpm for 5 minutes. Then, the obtained emulsion composition was spray-dried (190 °C) to obtain a powder emulsion composition.

[0074] (2) Performance Evaluation of Powder Emulsion Composition (Texture) (i) For the obtained powder emulsion composition, the moisture content (mass %) of the powder emulsion composition was determined by the same method as described in the above "Experiment 4: Powder Emulsion Composition (Freeze Drying)".

[0075] (ii) For the obtained powder emulsion composition, "viscosity (creaminess)", "emulsifying power after storage", "slimy feeling immediately after application", and "feeling of use after washing" were evaluated by the same method as described in the above "Experiment 4: Powder Emulsion Composition (Freeze Drying)".

[0076] (3) Results (i) The measurement results of the moisture content are shown in Table 7 below. The measurement of the moisture content was carried out using two separately prepared powder emulsion compositions as samples. The moisture content of the obtained powder emulsion composition was approximately 0.7 mass % and approximately 1.0 mass %, and the average was approximately 0.8 mass %.

[0077]

Table 7

[0078] (ii) For the spray-dried powder emulsion composition as well, similar to the freeze-dried one, it had a powdery form with a crispy texture, and all of "viscosity (creaminess)", "emulsifying power after storage", "slimy feeling immediately after application", and "feeling during use after washing" received an evaluation of "〇". Also, when spread on the palm, it could be spread in a transparent state where an oil film quickly forms, having a good feeling during use. Moreover, when washed after application, a crispy feeling like when applying powder and a moist feeling like when applying cream were obtained simultaneously. It was confirmed that similar characteristics can be obtained regardless of the drying treatment method.

[0079] From the above results, it became clear that by blending a water-in-oil emulsion containing water and oil with cyclodextrin and a predetermined water-soluble gelling agent in combination, an emulsion composition having high emulsification stability and a good texture like cream can be obtained. Also, the feeling during use when the emulsion composition is spread is unprecedented. It has a good texture like cream, and when washed with water or the like after application, it was confirmed that a crispy feeling like when applying powder and a moist feeling like when applying cream can be obtained simultaneously.

[0080] Furthermore, for the dried form (powder emulsion composition) obtained by subjecting the emulsion composition to a drying treatment, it was confirmed that when spread, it can be spread in a transparent state where an oil film quickly forms, and similar characteristics can be obtained. On the other hand, for the dried form obtained by subjecting it to a drying treatment without going through the emulsion composition having the high emulsification stability, such characteristics were not obtained. From this, it was confirmed that the good characteristics in the dried form are also due to maintaining an emulsion state without solid-liquid separation, and are caused by the emulsion composition before being subjected to the drying treatment having high emulsification stability.

[0081] Experiment 6: Evaluation of the heat resistance of the powder emulsion composition (1) Preparation of the powder emulsion composition According to the compositions shown in Tables 8 - 10 below, each component was added and mixed to prepare an emulsion composition. The mixing of each component was carried out by stirring with a hand blender at 20,000 rpm for 5 minutes. Subsequently, the obtained emulsion composition was freeze - dried (made into a vacuum state after freezing, and then freeze - dried at 20°C for 16 hours), and pulverized to obtain a white powder emulsion composition.

[0082] (2) Heat resistance test of the powder emulsion composition The obtained powder emulsion compositions were respectively placed in a dry heat sterilizer (Hirayama Manufacturing Co., Ltd.) and heat - treated at 105°C (product temperature) for 13 hours. After the heat treatment was completed, they were taken out from the dry heat sterilizer, cooled to room temperature, and the changes in each powder emulsion composition were visually evaluated. As a control, conventionally known white powdered fats and oils (N Neopowder A and N Neopowder P (NOF Corporation)) were used, and heat - treated in the same manner, and the changes were visually evaluated.

[0083] (3) Results The evaluation results of the heat resistance of each powder emulsion composition are also shown in Tables 8 - 10 below. In Table 8 - 10, for the powder emulsion composition after the above heat treatment, the measurement results of the moisture content (mass%) obtained by the same method as described in the above "Experiment 4: Powder emulsion composition (freeze - dried)" are also shown. Hereinafter, the amounts of each component in the table are shown in mass% with the amount of the obtained emulsion composition being 100 mass%. Also, "mass before drying" and "mass after drying" indicate the total mass of the weighing can and the powder emulsion composition.

[0084]

Table 8

[0085]

Table 9

[0086] [Table 10]

[0087] From the above results, it was confirmed that the dry form (powder emulsified composition) obtained by subjecting the emulsified composition obtained by blending cyclodextrin and a predetermined water-soluble gelling agent in combination to an oil-in-water emulsion containing water and oil to a drying treatment has excellent heat resistance and does not cause dissolution or yellowing even when subjected to high-temperature conditions. Further, such excellent heat resistance was also confirmed when the powder emulsified composition of Example 23 was further subjected to a heat treatment under high-temperature conditions (13 hours at 200 °C (product temperature)). On the other hand, it was confirmed that all of the conventionally known powdered fats and oils used as controls changed color to dark yellow as a whole by heat treatment, and also became sticky, and the powder form was not maintained, showing poor heat resistance.

[0088] Comparative Example 25 is an example in which the ratio of the blending amount of fat and oil to the total blending amount of α-cyclodextrin and water-soluble gelling agent is 9:1 in terms of mass ratio (blending amount of fat and oil: total blending amount of α-cyclodextrin and water-soluble gelling agent). It was confirmed by heat treatment under high-temperature conditions that the whole turned yellow, the properties of the fat and oil were strongly manifested, stickiness occurred, adhesion formed lumps, the powder form was not maintained, and heat resistance was poor (Table 8).

[0089] Comparative Examples 212 and 213 are examples in which "gum arabic" and "dextrin" not included in the predetermined water-soluble gelling agent in the present invention were used. It was confirmed that the powder form before heat treatment was not maintained, such as yellowing and strong manifestation of the properties of the fat and oil resulting in stickiness, and heat resistance was poor (Table 10).

[0090] Experiment 7: Evaluation of the moisture resistance of the powder emulsified composition (1) Moisture resistance test of the powder emulsified composition Each powder emulsion composition (Examples 21 to 211, Comparative Examples 25 to 213) prepared in the above "Experiment 6: Evaluation of Heat Resistance of Powder Emulsion Composition", as well as conventionally known white powdered fats and oils (N Neopowder A and N Neopowder P (NOF Corporation)) were left in a thermo-hygrostat (PR-4KP, ESPEC Corporation) at 40°C and 90% humidity for 1 week for humidification treatment. After the completion of the treatment, they were taken out from the thermo-hygrostat, cooled to room temperature, and the changes in each powder emulsion composition were visually evaluated.

[0091] (2) Results The evaluation results of the moisture resistance of each powder emulsion composition are shown in Table 11-13 below. Table 11 also includes the measurement results of the moisture content (mass%) obtained by the same method as described in the above "Experiment 4: Powder Emulsion Composition (Freeze-Dried)" for the powder emulsion composition after the humidification treatment. In the table, "mass before drying" and "mass after drying" indicate the total mass of the weighing can and the powder emulsion composition.

[0092]

Table 11

[0093]

Table 12

[0094]

Table 13

[0095] From the above results, it was confirmed that the dried form (powder emulsion composition) obtained by subjecting an emulsion composition obtained by blending a cyclodextrin and a predetermined water-soluble gelling agent in combination to a water-in-oil emulsion containing water and fats and oils to a drying treatment has excellent moisture resistance and does not cause yellowing or caking even when subjected to high humidity conditions. On the other hand, all of the conventionally known powder fats and oils used as controls changed to dark yellow as a whole by the humidification treatment, had high hygroscopicity, and thus solidified and could not maintain the powder form, and were confirmed to have poor moisture resistance.

[0096] Comparative Example 25 is an example where the ratio of the blending amount of the oil and fat to the total blending amount of α-cyclodextrin and the water-soluble gelling agent is 9:1 in terms of mass ratio (blending amount of the oil and fat: total blending amount of α-cyclodextrin and the water-soluble gelling agent). By the humidification treatment, it was confirmed that the whole was yellowish, solidified to form lumps, could not maintain the powder form, and had poor moisture resistance (Table 11).

[0097] Comparative Examples 212 and 213 are examples where "gum arabic" and "dextrin" not included in the predetermined water-soluble gelling agent in the present invention were used. It was confirmed that the powder form before the humidification treatment, such as yellowing and high hygroscopicity resulting in solidification, could not be maintained and had poor moisture resistance (Table 13).

[0098] Experiment 8: Re-emulsified composition of the powder emulsified composition (1) pH resistance test and heat resistance test The powder emulsified composition of Example 23 prepared in the above "Experiment 6: Evaluation of the heat resistance of the powder emulsified composition" was added to water in a glass beaker to a concentration of 10% by mass, mixed, and re-emulsified to prepare an emulsified composition. The mixing of the powder emulsified composition and water was carried out by stirring at 300 rpm for 1 hour at room temperature using a magnetic stirrer (RS-4AN manufactured by AS ONE Corporation). Next, the pH value (25°C) of the obtained re-emulsified composition was adjusted to 2, 3, 4, 7, 9, and 10 respectively using a potassium phosphate buffer solution, and the emulsification breakdown state (or emulsification stability) and the presence or absence of adhesion to the glass beaker wall surface in each re-emulsified composition were visually evaluated. The emulsification breakdown state (or emulsification stability) was evaluated according to the following criteria. <Evaluation criteria> ◎: No change. Emulsification is maintained. 〇: Emulsification breakdown has not occurred, but some oil floating or water separation is observed. ×: Separation of the oil layer and the water layer is confirmed. Emulsion breaking has occurred.

[0099] Also, 30 mL of the re-emulsified composition adjusted to each of the above pH values (25 °C) was placed in a 100 mL beaker and heat-treated in a water bath at 90 °C (product temperature) for 5 minutes. After the heat treatment, it was taken out from the water bath and allowed to stand at room temperature for 30 minutes, and then the emulsion breaking state (or emulsion stability) in each emulsified composition was visually evaluated according to the above criteria.

[0100] (2) Results

[0101]

Table 14

[0102] The re-emulsified composition prepared by adding the powder emulsified composition to water and re-emulsifying was confirmed to maintain the emulsified state and not cause emulsion breaking at any of the pH values (25 °C) of 2, 3, 4, 7, 9, and 10, indicating that it has high pH tolerance and excellent emulsion stability.

[0103] Also, regardless of the pH value (25 °C), a large amount of adhesion was observed on the wall surface of the glass beaker containing any of the re-emulsified compositions. Such re-emulsified compositions may be useful in applications where adhesion is required (for example, but not particularly limited to, paints, etc.).

[0104] Also, regardless of the pH value (25 °C), it was confirmed that the emulsified state was maintained and no emulsion breaking occurred in any of the re-emulsified compositions after the heat treatment, indicating that they have high heat resistance and excellent emulsion stability.

[0105] Experiment 9: Re-emulsified composition with an added emulsifier (1) Various resistance tests To the re-emulsified compositions having pH values of 2, 3, 4, 7, 9, and 10 (25 °C) prepared in the above “Experiment 8: Re-emulsified Composition of Powder Emulsion Composition”, sucrose palmitate (P-1670, Mitsubishi Chemical Corporation) was added as an emulsifier in an amount of 0.01% by mass, and the mixture was mixed and stirred at room temperature for 1 hour. For each of the obtained re-emulsified compositions, the emulsification breakdown state (or emulsification stability), the presence or absence of adhesion to the glass beaker wall, and the emulsification breakdown state (or emulsification stability) after heat treatment were evaluated by the same method as described in the above “Experiment 8: Re-emulsified Composition of Powder Emulsion Composition”. Also, to evaluate the water-based organic solvent resistance of each of the above-obtained re-emulsified compositions, ethanol, acetone, or acetonitrile was further added to each of the re-emulsified compositions in an amount of 5% by mass, and the mixture was mixed and stirred. For each of the obtained re-emulsified compositions, the emulsification breakdown state (or emulsification stability) and the emulsification breakdown state (or emulsification stability) after heat treatment were evaluated by the same method as above.

[0106] (2) Results

[0107]

Table 15

[0108] It was confirmed that emulsification breakdown did not occur in any of the re-emulsified compositions having any pH value (25 °C) prepared by adding an emulsifier, and it was shown that excellent emulsification stability with high pH resistance was maintained even in the presence of an emulsifier.

[0109] Also, it was shown that no adhesion was observed on the wall of the glass beaker containing any of the re-emulsified compositions having the above pH values (25 °C), and the addition of an emulsifier could suppress / disappear the adhesiveness. Such re-emulsified compositions may be useful, for example, in applications different from those where adhesiveness is required (for example, but not particularly limited to, foods and beverages, etc.).

[0110] Furthermore, in any of the re-emulsified compositions having the above pH values (25°C), it was confirmed that the emulsified state was maintained after heat treatment and no emulsion breakage occurred, indicating that excellent emulsion stability with high heat resistance was maintained even in the presence of an emulsifier.

[0111] And in any of the re-emulsified compositions having the above pH values (25°C), it was confirmed that the emulsified state was maintained in the presence of ethanol, acetone, or acetonitrile and no emulsion breakage occurred, indicating that excellent emulsion stability with high water-soluble organic solvent resistance was confirmed. Also, in any of the above re-emulsified compositions to which ethanol, acetone, or acetonitrile was added, it was confirmed that the emulsified state was maintained after heat treatment and no emulsion breakage occurred, indicating that excellent emulsion stability with high heat resistance was maintained even in the presence of a water-soluble organic solvent. These results indicate that the re-emulsified composition can be used in combination with a water-soluble organic solvent that can also be used as a solvent or the like regardless of the pH value or the presence or absence of heat treatment.

[0112] Experiment 10: Sensory test of the taste situation of the re-emulsified composition (1) Preparation of the re-emulsified composition of the salt-containing powder emulsified composition According to the composition shown in Table 16 below, each component was added and mixed to prepare an emulsified composition. The mixing of each component was carried out by stirring at 20,000 rpm for 5 minutes using a hand blender. Then, the obtained emulsified composition was freeze-dried (at 20°C for 48 hours) and pulverized to obtain a salt-containing powder emulsified composition. Note that the amounts of each component in the table are shown in mass% based on the amount of the obtained emulsified composition being 100 mass%.

[0113]

Table 16

[0114] 0.8 g of the obtained salt-formulated powder emulsion composition and 99.2 g of water were mixed and stirred to prepare a re-emulsified composition. As a control, a saline solution prepared by mixing 0.4 g of sodium chloride and 99.6 g of water was used.

[0115] (2) Sensory evaluation method Eight panelists who had been trained regularly evaluated the flavor of the obtained re-emulsified composition according to the following procedures 1. to 8. 1. Rinse the mouth with an appropriate amount of water and spit it out. 2. Hold 10 g of the control saline solution in the mouth and spread it throughout the mouth. 3. At this time, the sensory evaluation was used as the first impression, and the saltiness intensity was evaluated by the VAS method. 4. After the first impression evaluation, swallow it, and after 1 minute, evaluate the second impression of the saltiness intensity by the VAS method. 5. Rinse the mouth with an appropriate amount of water. 6. Hold 10 g of the re-emulsified composition of the salt-formulated powder emulsion composition in the mouth and spread it throughout the mouth. 7. At this time, the sensory evaluation was used as the first impression, and the saltiness intensity was evaluated by the VAS method. 8. After the first impression evaluation, swallow it, and after 1 minute, evaluate the second impression of the saltiness intensity by the VAS method.

[0116] (3) Results The evaluation results of the above first impression and second impression of the control saline solution and the re-emulsified composition by each panelist are shown in Table 17 below. Furthermore, regarding the evaluation results, with the value of the first impression of the control saline solution as "100%", the results with each value expressed as a relative value are shown in Table 18 below, and with the value of the second impression of the control saline solution as "100%", the results with the value of the second impression of the re-emulsified composition expressed as a relative value are shown in Table 19 below, respectively.

[0117]

Table 17

[0118]

Table 18

[0119]

Table 19

[0120] It was confirmed that the re-emulsified composition of the salt-containing powder emulsion composition tended to have a stronger salty taste for both the first impression and the second impression compared to the control saline. In particular, it was shown that the salty taste was felt stronger for the second impression compared to the control saline. From these results, it was confirmed that by using the said emulsion composition as a carrier for the active ingredient, the active ingredient can be slowly released from the composition, and the active ingredient can act or be sensed over a longer period of time.

[0121] Experiment 11: Performance evaluation of the emulsion composition (application of a hydrophilic surface) (1) Test method In the above "Experiment 6: Evaluation of the heat resistance of the powder emulsion composition", the emulsion composition of Example 23 prepared according to the composition of Table 8 was used for the following tests. After applying any one of the following treatments 1. to 3. to the surface of a polyethylene resin (5 cm × 5 cm × 1 mm (thickness)), 100 μL of distilled water was dropped, and the angle (contact angle) formed between the surface of the liquid droplet and the resin surface was compared. 1. 1 mL of 100% ethanol was dropped onto the center of the polyethylene resin, and appropriate pressure was applied with a gloved hand to coat it evenly. After gently wiping off the excess ethanol with a Kimwipe, it was dried. 2. 1 mL of the emulsion composition of Example 23 was dropped onto the center of the polyethylene resin, and appropriate pressure was applied with a gloved hand to coat it evenly. After gently wiping off the excess emulsion composition with a Kimwipe, it was dried. 3. After applying the emulsion composition of Example 23 to the central part of the polyethylene resin in the same manner as in 2. above and drying it, 100% ethanol was applied and dried in the same manner as in 1. above.

[0122] (2) Results The state of the droplets dropped on the surface of the polyethylene resin subjected to each treatment is shown in Fig. 1. The contact angle of the distilled water droplets dropped on the surface of the polyethylene resin subjected to Treatment 3. was larger than that of the others, and it was confirmed that the wettability of the surface of the polyethylene resin was good (that is, the hydrophilicity was high). It is suggested that by Treatment 3., after applying the emulsion composition of Example 23 and then wiping with 100% ethanol, the hydrophilic part of the emulsion composition remains on the surface of the polyethylene resin, thereby enhancing the hydrophilicity of the surface.

[0123] Experiment 12: Performance Evaluation of Emulsion Composition (Smoothing of Skin Surface) (1) Test Method In the above-mentioned "Experiment 6: Evaluation of Heat Resistance of Powder Emulsion Composition", the emulsion composition of Example 23 prepared according to the composition in Table 8 was used in the following tests. The entire hand of the subject was thoroughly washed with hand soap to remove as much oil on the skin surface as possible. In this experiment, the same results can be obtained whether only water or a detergent such as hand soap is used for washing, but this time hand soap was used for washing. After applying any one of the following Treatments 1. to 3. to the surface of the pulp of the index finger of the left hand, the skin on the surface was observed with a stereomicroscope and its touch was subjected to a sensory test. 1. Untreated: The air was blown onto the pulp side of the index finger of the left hand with the blower function of a dryer for 10 minutes continuously. 2. After applying the emulsion composition of Example 23 to the surface of the pulp side of the index finger of the left hand, it was gently wiped and then the air was blown onto it with the blower function of a dryer for 10 minutes continuously. 3. After applying the emulsion composition of Example 23 to the surface of the pulp side of the index finger of the left hand, it was thoroughly washed with hand soap, gently wiped, and then the air was blown onto it with the blower function of a dryer for 10 minutes continuously.

[0124] (2) Results As a result of observing the ventral surface of the index finger of the left hand on which each treatment was performed under a stereomicroscope, when the emulsified composition of Example 23 was applied to the skin surface (Treatment 2, Treatment 3), compared with the untreated case (Treatment 1), it was confirmed that the surface irregularities and wrinkles were alleviated and the surface became smoother. This effect was more significantly confirmed in the case of washing (Treatment 3) after applying the emulsified composition of Example 23. In addition, the sensory evaluation results showed the same results. In the untreated case (Treatment 1), the skin surface felt hard and the rough feeling with resistance increased. However, when the emulsified composition of Example 23 was applied to the skin surface (Treatment 2, Treatment 3), the moist feeling of the skin surface was maintained and a smooth and slippery feeling was also felt.

[0125] From the above results, it was suggested that the emulsified composition obtained by blending a water-in-oil emulsion containing water and oil with cyclodextrin and a predetermined water-soluble gelling agent in combination, the dried form (powder emulsified composition) obtained by subjecting it to a drying treatment, and the re-emulsified composition of the dried form have excellent stability with various resistances and can be used in various applications.

Claims

1. An emulsified composition powder in the form of an oil-in-water emulsion, comprising water, oil and fat, cyclodextrin, and at least one of carboxymethylcellulose (CMC) or xanthan gum, wherein the ratio of the blending amount of the oil and fat to the total blending amount of the cyclodextrin and at least one of the CMC or xanthan gum is in the range of 1 or more and less than 9:9 or less and more than 1 in terms of mass ratio (the blending amount of the oil and fat: the total blending amount of the cyclodextrin and at least one of the CMC or xanthan gum), and the ratio of the blending amount of the cyclodextrin to the total blending amount of at least one of the CMC or xanthan gum is in the range of 2.5 / 0.35 to 8 / 0.3:1 in terms of mass ratio (the blending amount of the cyclodextrin: the total blending amount of at least one of the CMC or xanthan gum).

2. The powder of the emulsified composition according to claim 1, wherein the water content is 10% by mass or less.

3. A re-emulsified composition comprising the powder of the emulsified composition according to claim 1 or 2 and a solvent.

4. The re-emulsified composition according to claim 3, further comprising an emulsifier that does not contain cyclodextrin, CMC, and xanthan gum.

5. The re-emulsified composition according to claim 3 or 4, further comprising an aqueous organic solvent.

6. A step of mixing water, oil and fat, cyclodextrin, and at least one of carboxymethylcellulose (CMC) or xanthan gum to form an emulsified composition, wherein the ratio of the blending amount of the oil and fat to the total blending amount of the cyclodextrin and at least one of the CMC or xanthan gum is in the range of 1 or more and less than 9:9 or less and more than 1 in terms of mass ratio (the blending amount of the oil and fat: the total blending amount of the cyclodextrin and at least one of the CMC or xanthan gum), and the ratio of the blending amount of the cyclodextrin to the total blending amount of at least one of the CMC or xanthan gum is in the range of 2.5 / 0.35 to 8 / 0.3:1 in terms of mass ratio (the blending amount of the cyclodextrin: the total blending amount of at least one of the CMC or xanthan gum), and a step of subjecting the obtained emulsified composition to a drying treatment and further forming it into a powder form. A method for producing a powder of an emulsified composition in the form of an oil-in-water emulsion, comprising the steps.

7. The production method according to claim 6, wherein the water content of the emulsion composition is made 10% by mass or less by the drying treatment.

8. A method for producing a re-emulsion composition, comprising a step of mixing the powder of the emulsion composition according to claim 1 or 2 with a solvent to form a re-emulsion composition.

9. Furthermore, the production method according to claim 8, wherein an emulsifier not containing cyclodextrin, CMC, and xanthan gum is mixed.

10. Furthermore, the production method according to claim 8 or 9, wherein an aqueous organic solvent is mixed.

Images