JP2014019673A - Cosmetic raw material solution free of antiseptic agent and surfactant, preparation method of cosmetic and cosmetic raw material solution - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a cosmetic raw material solution free of an antiseptic agent and a surfactant and a preparation method thereof having mild and less stimulus to skin and high effect to skin with the small particle diameter of an emulsified particle, to provide a cosmetic using the cosmetic raw material.SOLUTION: The preparation method of a cosmetic raw material free of an antiseptic agent and a surfactant comprises the steps of: dissolving 0.01 to 0.1 mass% of a mixture containing agar and xanthane gum in water under heating, and obtaining the solution; aseptically filtering the solution with a filter having the pore size of 0.45 μm or less; and emulsifying the filtered solution with an aseptically filtered oil component added, and obtaining the emulsion having the average particle diameter of an emulsified particle of 20 μm or less.

Description

  The present invention relates to a cosmetic raw material liquid containing an oily component and free of preservatives and surfactants, a cosmetic and a method for preparing a cosmetic raw material liquid. More specifically, the present invention relates to a method for preparing a cosmetic in which the average particle size of the emulsified particles of the emulsion contained in the cosmetic raw material liquid is 20 μm or less.

  For cosmetic raw materials, emulsions composed of an oily component and a hydrophilic component are often used from the viewpoint of improving the feeling of use and penetrating into the skin. An example of the oil component is an essential oil such as rose oil. Rose oil is mainly used as a fragrance, but has the following beauty effects and is often used as a cosmetic raw material. The beauty effect of rose oil is, for example, skin tone, moisturizing effect, improvement of blood flow, improvement of sagging / dullness such as spots / wrinkles, antibacterial action, or relaxing effect. Most of the rose-derived ingredients contained in cosmetics are components that separate into the lower layer when steaming rose flowers and camellia, so-called rose water, and are components that separate into the upper layer during distillation. There are few cosmetics to which a certain rose oil itself is added. Rose water is naturally different from the components of rose oil and does not necessarily contain the active ingredient of rose oil. In order to use rose oil in cosmetics, it is necessary to disperse and emulsify in water, and a surfactant is usually used for dispersion and emulsification. In addition, a preservative is usually added to prevent the growth of microorganisms in cosmetics. However, it may be desired not to use preservatives and surfactants (preservative-free and surfactant-free) from the viewpoint of irritation to the skin.

  As a method for preparing a preservative-free cosmetic, for example, a method of aseptic filtration with a sterile 0.45 μm filter is a known technique.

  As a material for preparing surfactant-free cosmetics, a water-soluble polymer formulation (hereinafter referred to as a water-soluble polymer) composed of agar with a lower molecular weight than general agar and modified xanthan gum instead of a surfactant. (It is also called a formulation.) Has been reported (see, for example, Non-Patent Document 1). Non-Patent Document 1 describes an example in which the water-soluble polymer formulation is used in an amount of 1.5 to 2.0% by mass for cosmetics, and preparation of emulsions of a wide variety of oils such as highly polar oils. Application to emulsification is described. In the emulsion described in Non-Patent Document 1, according to FIGS. 5 and 6 of Non-Patent Document 1, particles having a particle size of 10 to 20 μm are scattered, but more than half of the emulsion particles have a particle size of 30 μm or more. The largest one is 69 μm in FIG. 5 and 105 μm in FIG. That is, it can be said that the emulsified particles having a very large particle size are dispersed as described in 3-1.

  By the way, it is known that a compound having a molecular weight of 500 daltons or less is absorbed by the skin (for example, see Non-Patent Document 2). The molecular weights of citronell, nerol, geraniol, etc., which are the main components in rose oil, are around 154 daltons and are clearly absorbed and absorbed by the skin.

International Publication WO2008 / 018643 JP 2003-201370 A

Fat and oil 63 volumes 65 pages (2010) J. et al. D. Bos, M.M. M. Meinardi; Exp. Dermatol 9 165 pages (2000)

  The cosmetics described in Non-Patent Document 1 contain methylparaben and propylparaben, and are not preservative-free. In the emulsion preparation method described in Non-Patent Document 1, an oil component is added to a water-soluble polymer preparation dissolved in water at a concentration of 1.8% by mass or more. However, an aqueous solution in which the water-soluble polymer preparation is dissolved at a concentration of 1.8% by mass or more has a high viscosity and is viscous, making aseptic filtration difficult. Furthermore, the particle size of the emulsified particles of the obtained emulsion is 30 μm or more with more than half of the particles, and oil droplets having a very large particle size are dispersed with respect to the pore size of the filter used for aseptic filtration. Aseptic filtration is also not possible. Moreover, although sterilization by an autoclave under high temperature pressurization, such as 120 degreeC, can be considered, a component may thermally decompose. Therefore, in the preparation method of Non-Patent Document 1, it is considered that a preservative must be added in order to prevent agar spoilage.

  An object of the present invention is to provide a cosmetic raw material solution that is mild and less irritating to preservative / surfactant-free skin, and has a high effect on the skin because the particle size of the emulsified particles is small, and a method for preparing the same. it can. Moreover, it is providing the cosmetics using the cosmetic raw material.

  Preservatives and surfactants are free by emulsifying oily components using a filtrate prepared by dissolving a mixture containing agar and xanthan gum in water at a very low concentration and filtering with a filter for aseptic filtration of 0.45 μm or less. It was found that a cosmetic raw material solution was obtained, and the present invention was completed. That is, the method for preparing a preservative / surfactant-free cosmetic raw material liquid according to the present invention is to heat a mixture containing agar and xanthan gum in water at a concentration of 0.01% by mass or more and 0.1% by mass or less. And a step of aseptically filtering the solution with a filter of 0.45 μm or less, and emulsifying the sterilized oily component into the filtrate so that the average particle size of the emulsified particles is 20 μm. And obtaining an emulsion which is the following.

  The preservative / surfactant-free cosmetic raw material liquid according to the present invention is a sterile dispersion medium in which a mixture containing agar and xanthan gum as an emulsifier is dissolved in water at a concentration of 0.01% by mass to 0.1% by mass. And an emulsion in which aseptic oily components are dispersed, and the average particle size of the emulsified particles in the emulsion is 20 μm or less.

  In the preservative / surfactant-free cosmetic raw material liquid according to the present invention, the oil component is preferably an essential oil. Since the surface area per unit mass of the essential oil can be increased, the effect on the skin can be further increased.

  In the preservative / surfactant-free cosmetic raw material liquid according to the present invention, the essential oil is preferably rose oil. It is possible to increase the penetration and absorption of the active ingredient of rose oil into the skin.

  The antiseptic / surfactant-free cosmetic according to the present invention comprises a whitening agent, a moisturizer, an anti-aging agent, an antiallergic / anti-inflammatory agent, a hair growth / hair restorer as a water-soluble active ingredient in the cosmetic raw material liquid according to the present invention. Or at least 1 sort (s) of the ultraviolet-ray inhibitor was mixed.

  INDUSTRIAL APPLICABILITY The present invention can provide a cosmetic raw material solution that is mild and less irritating to preservative / surfactant-free skin and has a high effect on the skin because the particle size of the emulsified particles is small, and a method for preparing the same. Further, a preservative / surfactant-free cosmetic using the cosmetic raw material can be provided.

  Next, the present invention will be described in detail with reference to embodiments, but the present invention is not construed as being limited to these descriptions. As long as the effect of the present invention is exhibited, the embodiment may be variously modified.

  The preparation method of the preservative / surfactant-free cosmetic raw material liquid according to the present embodiment is obtained by heating a mixture containing agar and xanthan gum to water at a concentration of 0.01% by mass or more and 0.1% by mass or less. A step of dissolving to obtain a solution; a step of aseptically filtering the solution with a filter of 0.45 μm or less; and an emulsified oil component added to the filtrate for emulsification, so that the average particle size of the emulsified particles is 20 μm or less. Obtaining an emulsion.

  In order to emulsify the oily component in water, the preparation method according to the present embodiment uses a mixture containing naturally-derived agar and xanthan gum instead of a normal surfactant. The agar is preferably low molecular agar. The low molecular weight agar referred to here is one having a smaller molecular weight than general agar. While the weight average molecular weight of general agar is 200,000 to 500,000, the weight average molecular weight of low molecular agar is preferably 10,000 to 100,000, more preferably 20,000 to 60,000. . Low molecular agar is, for example, the low molecular agar described in Patent Document 1, and unlike ordinary agar, the molecules of agar components (agarose and agaropectin) are cut short, and the weight average molecular weight is 10,000 to 100,000, The agar is preferably 20,000 to 60,000. The xanthan gum is preferably a modified xanthan gum. The modification method of xanthan gum is, for example, heat / acid treatment, heat treatment, hydrolysis treatment, and radiation irradiation treatment. The modified xanthan gum is preferably one having a lower molecular weight than general xanthan gum. The average molecular weight of the modified xanthan gum is preferably 100,000 to 1,000,000, more preferably 500,000 to 900,000, as determined by the viscosity method. The modified xanthan gum is, for example, a low molecular weight xanthan gum described in Patent Document 2. The low molecular weight xanthan gum is preferably obtained by adjusting the fermentation conditions of the genus Xanthomonas such as Xanthomonas campestris. In this case, the nitrogen content is adjusted to 0.15 N or less, particularly 0 N. It is preferable to carry out fermentation of Xanthomonas bacteria such as Xanthomonas campestris in the prepared medium. Specifically, the bacteria of the genus Xanthomonas are inoculated into a culture solution containing carbohydrates such as starch, glucose, and sucrose, adjusted to pH and temperature, and stirred and aerated. At this time, in order to obtain a normal xanthan gum having an average molecular weight of 1,500,000 to 3,500,000, it is necessary to adjust the pH to 6.0 to 7.5 and to culture at a temperature of 25 to 35 ° C. for about 2 days. However, when obtaining low molecular weight xanthan gum with an average molecular weight of 100,000 to 1,000,000, the fermentation rate is slowed by changing the conditions of pH and temperature, etc. Cultivation is performed by reducing the nitrogen content in the medium. The low molecular weight xanthan gum is preferably obtained by hydrolyzing xanthan gum, and the hydrolysis is preferably performed by acid or heating. The mixture containing agar and xanthan gum is preferably a mixture containing low molecular agar and modified xanthan gum. As a mixture containing low molecular agar and modified xanthan gum, for example, NOMCOAT (registered trademark) AG described in Non-Patent Document 1 as a commercial product can be used.

  The mixture containing agar and xanthan gum is added to water and heated so as to be finished into a solution having a concentration of 0.01% by mass to 0.1% by mass, preferably 0.03% by mass to 0.07% by mass. While stirring, dissolve. The heating temperature is preferably 50 ° C. or higher and 100 ° C. or lower, and more preferably 70 ° C. or higher and 80 ° C. or lower. When the concentration of the mixture containing agar and xanthan gum exceeds 0.1% by mass, the solution becomes viscous and it is difficult to filter with a filter for aseptic filtration of 0.45 μm or less. Further, even when a mixture containing low molecular agar and modified xanthan gum is used, filtration is similarly difficult. If it is less than 0.01% by mass, the emulsifying action is insufficient. In addition to the mixture and water, the solution may contain a polyhydric alcohol such as glycerin as long as the effects of the present invention are not impaired.

  As shown in Non-Patent Document 1, when a water-soluble polymer preparation is dissolved in water at a concentration of 1.8% by mass or more to prepare an emulsion-like cosmetic liquid containing an oil, the size of oil droplets in the generated emulsion More than half of the particles are 30 μm or more, and very large oil droplets are dispersed. Even if this emulsion of Non-Patent Document 1 is diluted by adding water until the concentration of the mixture of agar and xanthan gum becomes 0.01 to 0.1% by mass as in the present invention, the size of the oil droplets in the emulsion Will not change. In order to prepare an emulsion having a size of fine oil droplets having an average particle diameter of 20 μm or less, the inventors of the present invention initially adjusted the concentration of the mixture containing agar and xanthan gum to a low level, and the low concentration solution was used as an oil component. It was found that it was a big factor to be used for emulsification of the present invention, resulting in the present invention.

  Mixtures containing agar and xanthan gum contain high molecular weight xanthan gum, and some may not pass through the filter when filtered through a 0.45 μm filter for aseptic filtration, but only the filtrate components that pass through the filter are sufficient. It was a great feature of the present invention that the emulsifying effect of the oil component can be exhibited.

  In order to perform aseptic filtration of a solution obtained by adding a mixture containing agar and xanthan gum to water and dissolving it, it is preferable to use a filter for aseptic filtration having a spread of 0.45 μm or less. The aseptic filtration filter is, for example, a membrane filter or a ceramic filter. Further, a liquid capsule filter may be used. For aseptic filtration, a filter for aseptic filtration of 0.45 μm or 0.22 μm is usually used. However, in this embodiment, there is no particular limitation as long as the pore diameter of the filter for aseptic filtration is 0.45 μm or less. The filtration method is, for example, suction filtration or pressure filtration.

  The filter may be a flat plate type or a cartridge type.

  The oily component sterilized while stirring is dropped into a filtrate obtained by aseptically filtering a solution obtained by adding a mixture containing agar and xanthan gum to water. Although this step can be performed at room temperature, it is more preferably performed by heating. By warming, emulsification is accelerated and a good emulsified state is easily obtained. The temperature to be heated is preferably 40 to 70 ° C, and more preferably 45 to 55 ° C. When heating, a low-boiling component in the oily component may volatilize, so it is preferable to attach a reflux tube.

  Examples of the method for aseptically treating the oil component include aseptic filtration, ultraviolet irradiation, and autoclave treatment. Among these, the aseptic filtration method is preferable in that the influence on the physical properties of the oil component is small. As a filter for aseptic filtration used in the aseptic filtration method, for example, the same type as that used for aseptic filtration of a solution obtained by adding a mixture containing agar and xanthan gum to water and dissolving it can be used.

  In the present specification, the oil component is a component that becomes an oil phase in an emulsion, for example, fats, waxes, hydrocarbons, higher fatty acids, higher alcohols, esters, silicone oils, essential oils that are oily raw materials for cosmetics. Carotenoids. The fats and oils are, for example, olive oil, camellia oil, and macadamia nut oil. The wax is, for example, jojoba oil. The hydrocarbon is, for example, liquid paraffin. Higher fatty acids are, for example, palmitic acid and lauric acid. The higher alcohol is, for example, cetyl alcohol, 2-octyl docanol. The ester is, for example, 2-octyldodecyl myristate. Silicone oil is, for example, methylpolysiloxane. The essential oil is, for example, rose oil. The carotenodos are, for example, astaxanthin, retinal, retinoic acid, lutein, lycopene. Of these, the oil component is preferably an essential oil. When the oil component is an essential oil such as rose oil, the addition amount of the essential oil is preferably 0.01% by mass or more and 0.1% by mass or less, and 0.02% by mass with respect to the total mass of the cosmetic raw material liquid. More preferably, it is 0.07 mass% or less. If the amount of the essential oil added exceeds 0.1% by mass, emulsification may not be successful unless the concentration of the mixture containing agar and xanthan gum is increased. If it is less than 0.01% by mass, the effect of the essential oil may not be exhibited.

  The average particle size of the emulsified particles of the obtained emulsion is 20 μm or less. More preferably, it is 15 μm or less. When the average particle size of the emulsified particles exceeds 20 μm, the surface area per added mass of the oily component becomes relatively small, and the effect of obtaining high efficacy is not obtained while the amount of the oily component added is small. Here, the average particle diameter is an average value of the diameters of the emulsified particles measured under an optical microscope, and is measured by the following method. The emulsion is observed using an optical microscope, and the diameter of the emulsified particles appearing in the image is determined by the scale of a slide glass with a scale. This operation is repeated until the number of emulsified particles reaches 100 for the non-overlapping region, and the average value of the diameters is taken as the average particle size. The observation magnification is, for example, 70 to 100 times depending on the size of the emulsified particles.

  The preservative / surfactant-free cosmetic raw material liquid according to this embodiment is a sterile dispersion obtained by dissolving a mixture containing agar and xanthan gum as emulsifiers in water at a concentration of 0.01% by mass or more and 0.1% by mass or less. It is an emulsion in which a sterile oily component is dispersed in a medium, and the average particle size of the emulsified particles in the emulsion is 20 μm or less. The emulsion is a so-called O / W type in which oil droplets are dispersed in an aqueous phase, and the emulsified particles are oil droplets.

  The essential oil used in the present embodiment is generally referred to as an essential oil, and is a plant-derived aromatic / volatile oil. Essential oils are mainly composed of organic compounds such as volatile terpenes and aromatics contained in plants. Essential oils are often used as perfumes because they have a unique fragrance, but are said to have other aromatherapy effects and bactericidal action. Main essential oils used in this embodiment are collected from the following plants. Examples of those collected from flowers and buds include rose, ylang ylang, chamomile, and jasmine. For example, lavender, rosemary, mint and thyme are collected from the whole grass. Examples of materials collected from trees and bark include cypress, hiba, pine, and cinnamon. Examples of the material collected from the leaves include geranium, eucalyptus, basil, and ghetto. Examples of those collected from fruits and seeds include vanilla and perilla. For example, grapefruit is collected from the pericarp.

  The essential oil generally refers to one produced by a steam distillation method, but may be one produced by another solvent extraction method, compression method or supercritical extraction method, for example.

  In the present embodiment, the essential oil is preferably rose oil. The rose oil in the essential oil used in the present invention is collected from, for example, Damascus of the Rosaceae family and is generally called rose otto. The effects of rose oil include, for example, body effects such as calming feelings, anxiety or stress relief, effects on the skin, improving skin balance or hormonal balance, deodorizing effects, or promoting blood circulation. It is an effect on. The effects on the skin when used as a cosmetic are, for example, an astringent action that tightens the skin, a wrinkle and stain preventing action, and an anti-aging action on the skin.

  As described above, the main component of rose oil has the property of being osmotically absorbed by the skin. In this embodiment, since the particle size of the essential oil in the emulsion is as small as 20 μm or less, the surface area per unit mass of the added essential oil. Becomes larger and more easily absorbed. And the effect on skin, such as an astringent action and an antiaging action which an essential oil has, becomes remarkably high.

  Cosmetics other than the oil component can be added to an emulsion containing an oil component emulsified with a mixture of agar and xanthan gum to make a cosmetic product. The cosmetic raw material to be added is not particularly limited as long as it is water-soluble, and examples thereof include various active ingredients such as a whitening agent, a moisturizing agent, an anti-aging agent, an antiallergic / anti-inflammatory agent, a hair growth / hair restorer, and an ultraviolet ray preventing agent. Examples of the whitening agent include vitamin C or derivatives thereof, β-arbutin, α-arbutin, kojic acid, acerola extract, aloe extract, kudzu root extract, rice bran extract, and resorcinol derivative. Examples of the humectant include hyaluronic acid, low molecular weight hyaluronic acid or hyaluronic acid derivatives, collagen (including marine collagen and synthetic collagen), betaine, amino acid, trehalose, urea, oligosaccharide, glycerin, propylene glycol, 1,3 -Butylene glycol, polyethylene glycol, sorbitol, sodium lactate. Anti-aging agent has the effects such as active oxygen scavenging, oxidation prevention, photo-aging prevention, such as agaris koji extract, seaweed extract, fucoidin, licorice extract, β-1,3-glucan, Yeast extract, moon peach extract, guava extract. Examples of the antiallergic / antiinflammatory agent include ascorbic acid-2-glucoside, turmeric extract, chamomile extract, perilla extract, silk extract, tea extract, tranexamic acid, and biotin. Examples of the hair growth / restoration agent include water-soluble minoxidil and amino acids. Examples of the UV inhibitor include paraaminobenzoic acid (PABA), PABA glyceryl, and water-soluble benzophenones. Moreover, you may add well-known adjuvants other than an antiseptic | preservative and surfactant other than an active ingredient to cosmetics.

  Since the above-mentioned active ingredients are all water-soluble, they can be sterilized by filtering with a filter for aseptic filtration without heating. By adding the pre-sterilized active ingredient to the cosmetic raw material liquid according to the present embodiment, a preservative / surfactant-free cosmetic can be obtained.

  Next, although an example of the present invention is given and explained, the present invention is not limited to these examples.

Example 1
Put 640 parts of water in a container equipped with a reflux tube, add 0.32 part of a mixture of agar and xanthan gum (Nomcoat AG, Nisshin Oilio Co., Ltd.) while stirring at 70-80 ° C and stirring for another 2 hours. Stirring was continued. The resulting solution was aseptically filtered into a sterilized container with a liquid capsule filter (Acropack 1500, manufactured by Pall Corp., pore size 0.2 μm). Rose oil (Bulgarian Rose Otto essential oil, manufactured by Connect Co., Ltd.) pre-sterilized with a 0.45 μm filter for aseptic filtration (membrane filter, Acropack 20, manufactured by Pall) to where the filtrate was heated to 40-50 ° C ) 0.32 part was added and stirred for another hour to obtain an emulsion-like cosmetic raw material liquid (part A). On the other hand, 0.5 parts of sodium hyaluronate and 10 parts of sorbite solution are added to 360 parts of water in another container and dissolved while stirring at room temperature. This was aseptically filtered with a 0.45 μm filter for aseptic filtration (Part B). Part B was added to part A with stirring at room temperature, and part A and part B were mixed to obtain a cosmetic product.

(Example 2)
Put 640 parts of water in a container equipped with a reflux tube, add 0.20 parts of a mixture containing agar and xanthan gum (Nomcoat AG, manufactured by Nisshin Oilio Co., Ltd.) while stirring at 70-80 ° C. while stirring and adding 2 Stirring was continued for an hour. The obtained solution was aseptically filtered into a sterilized container with a pressure filter (stainless steel pressure filtration funnel, manufactured by Pole) equipped with a 0.45 μm filter for aseptic filtration. To the place where the filtrate was heated to 40 ° C. to 50 ° C., 0.13 parts of rose oil rose oil which had been sterile-filtered in advance with a 0.45 μm filter for aseptic filtration was added, and the mixture was further stirred for 1 hour. A cosmetic raw material liquid was obtained (part A). On the other hand, 0.3 parts of sodium hyaluronate, 1 part of water-soluble collagen, and 10 parts of glycerin were added to 360 parts of water in another container and dissolved at room temperature with stirring. This was filtered with a 0.45 μm filter for aseptic filtration (Part B). Part B was added to part A with stirring at room temperature, and part A and part B were mixed to obtain a cosmetic product.

(Example 3)
Put 640 parts of water in a container equipped with a reflux tube, add 0.32 part of a mixture containing agar and xanthan gum (Nomcoat AG, manufactured by Nisshin Oilio Co., Ltd.) with heating to 70-80 ° C. and stirring for 2 hours. Stirring was continued. The resulting solution was aseptically filtered into a sterilized container with a liquid capsule filter (Acropack 1500, manufactured by Pall Corp., pore size 0.2 μm). To the place where the temperature of the filtrate is heated to 40 ° C. to 50 ° C., 0.32 parts of rose oil rose oil which has been sterile-filtered in advance with a 0.45 μm filter for aseptic filtration and further stirred for 1 hour to give an emulsion A cosmetic raw material liquid was obtained (part A). On the other hand, 1.0 part of sodium hyaluronate, 20 parts of sorbite solution, and 1.0 part of aloe extract were added to 360 parts of water in another container and dissolved while stirring at room temperature. This was filtered with a 0.45 μm filter for aseptic filtration (Part B). Part B was added to part A with stirring at room temperature, and part A and part B were mixed to obtain a cosmetic product.

Example 4
Put 640 parts of water in a container equipped with a reflux tube, add 0.32 part of a mixture containing agar and xanthan gum (Nomcoat AG, manufactured by Nisshin Oilio Co., Ltd.) with heating to 70-80 ° C. and stirring for 2 hours. Stirring was continued. The resulting solution was filtered into a sterilized container with a pressure filter (stainless steel pressure filtration funnel, manufactured by Pall) with a 0.45 μm filter for aseptic filtration, and the temperature was increased to 40 to 50 ° C. After heating, 0.20 part of rose oil which was pre-sterilized with a 0.45 μm filter for aseptic filtration was added and stirred for another hour to obtain an emulsion-like cosmetic raw material liquid (part A). On the other hand, in a separate container 125 parts water, 40 parts sorbite solution, 60 parts dipropylene glycol solution, 20 parts α-arbutin, 10 parts yeast extract, 0.5 parts sodium hyaluronate, 5 parts betaine And 100 parts of ethanol were added and dissolved while stirring at room temperature. This was filtered with a 0.45 μm filter for aseptic filtration (Part B). Part B was added to part A with stirring at room temperature, and part A and part B were mixed to obtain a cosmetic product.

(Comparative Example 1)
Put 640 parts of water in a container equipped with a reflux tube, add 10 parts of a mixture of agar and xanthan gum (Nomcoat AG, manufactured by Nisshin Oilio Co., Ltd.) while stirring at 70-80 ° C and stirring, and further stirring for 2 hours. Continued. The resulting solution was sticky and was sterilized through a liquid capsule filter (Acropack 1500, manufactured by Pall Corp., pore size 0.2 μm), but could not be filtered.

(Comparative Example 2)
Without aseptic filtration, the solution of Comparative Example 1 was added with 72 parts of rose oil and further stirred for 1 hour to obtain an emulsion (emulsion before dilution). An emulsion obtained by diluting the emulsion before dilution with 27000 parts of water (emulsion after dilution) was sterilized through a liquid capsule filter (Acropack 1500, manufactured by Pall, pore size: 0.2 μm), but could not be filtered. .

(Average particle size measurement)
About the cosmetics of Examples 1-4, the average particle diameter of the emulsified particle | grains in an emulsion was calculated | required as follows. Using an optical microscope (Olympus BX40), observation was performed at a magnification of 100 times, and the diameter of the emulsified particles appearing in the image was determined by the scale of a slide glass with a scale. This operation was repeated until the number of emulsified particles reached 100 for the non-overlapping region, and the average value of the diameters was defined as the average particle size. Each average particle diameter is as shown in Table 1. Further, in the cosmetics of Examples 1 to 4, it was found that the average particle diameter of the emulsified particles in the emulsion was 20 μm or less, which was much smaller than the oil particle diameter described in Non-Patent Document 1. .

  By the way, when the average particle diameter of the emulsion before dilution and the emulsion after dilution of Comparative Example 2 were measured in the same manner as in the example, the average particle diameter of the emulsion before dilution was 98.7 μm. The average particle size of was 65.9 μm. It was confirmed that Comparative Example 2 could not be filtered because the emulsified particles remained large even in the diluted emulsion.

Claims (5)

  A step of dissolving a mixture containing agar and xanthan gum in water at a concentration of 0.01% by mass or more and 0.1% by mass or less under heating to obtain a solution; and sterilizing the solution with a filter of 0.45 μm or less. Preservative-free surfactant-free, characterized by having a step of filtering and emulsifying an oily component obtained by sterilization in the filtrate to obtain an emulsion having an average particle size of emulsified particles of 20 μm or less Preparation method of cosmetic raw material.   An emulsion in which a sterile oily component is dispersed in a sterile dispersion medium in which a mixture containing agar and xanthan gum as an emulsifier is dissolved in water at a concentration of 0.01% by mass or more and 0.1% by mass or less. A preservative / surfactant-free cosmetic raw material liquid, wherein the average particle size of the emulsified particles is 20 μm or less.   3. The preservative / surfactant-free cosmetic raw material liquid according to claim 2, wherein the oil component is an essential oil.   4. The preservative / surfactant-free cosmetic raw material according to claim 3, wherein the essential oil is rose oil.   The cosmetic raw material liquid according to any one of claims 2 to 4, wherein at least one of a whitening agent, a moisturizing agent, an anti-aging agent, an antiallergic / anti-inflammatory agent, a hair growth / hair restoration agent, or an ultraviolet ray preventing agent as a water-soluble active ingredient. A preservative / surfactant-free cosmetic characterized by mixing one species.