WO2014103742A1

WO2014103742A1 - Reverse vesicle composition and method for producing same

Info

Publication number: WO2014103742A1
Application number: PCT/JP2013/083382
Authority: WO
Inventors: 亘堀江; ウルフオルソン
Original assignee: ポーラ化成工業株式会社
Priority date: 2012-12-25
Filing date: 2013-12-12
Publication date: 2014-07-03
Also published as: TW201442732A

Abstract

The present invention addresses the problem of providing a stable reverse vesicle composition using lecithin. The means for solving this problem is a reverse vesicle composition comprising a reverse vesicle including lecithin and an oil solution that has a molecular weight greater than 114 g/mol and is liquid at 25°C.

Description

Reverse vesicle composition and method for producing the same

The present invention relates to an inverse vesicle, an inverse vesicle composition, an external preparation for skin using the same, and a method for producing them.

The technology of microencapsulating active ingredients and applying them inside and outside the living body is expected to be applied in the pharmaceutical and food fields as well as in the cosmetics field because of the advantages such as the effectiveness of the active ingredients in the capsules. Has been.
As a microencapsulation technique in the cosmetics field, a vesicle having a phospholipid such as lecithin as a bilayer component is conventionally known.

Lecithin is a natural lipid and is widely used as an emulsifier and stabilizer in the cosmetics and food fields.
Conventionally, vesicles using lecithin were mainly water-dispersed vesicles in which the hydrophilic groups of phospholipids were oriented outward and dispersed in an aqueous phase.

On the other hand, silicone surfactants are those obtained by introducing hydrophilic organic groups into silicone having water repellency, and are applied to various applications because of the ease of molecular design.
In particular, in the cosmetics field, low HLB silicone surfactants are used as emulsifiers in preparing W / O emulsions. High HLB silicone surfactants are used in hair care products such as O / W emulsions because they can impart slipperiness and antistatic effects to hair.

By the way, the following is known as an inverted vesicle in which the hydrophobic group of the amphiphile is oriented outward.
Patent Document 1 describes a reverse vesicle using a sucrose fatty acid ester. It also describes forming a water-in-oil emulsion by the three-phase emulsification method using the reverse vesicle as an emulsifier.
Patent Document 2 describes a reverse vesicle composition using sphingosines.

Non-Patent Document 1 describes the formation of reverse vesicles containing lecithin, and it is reported that specific lecithins form reverse vesicles in cyclohexane.
On the other hand, Non-Patent Document 2 shows that a lecithin having a carbon chain different from the above does not form a coexisting phase of an oil and a lamellar layer necessary for forming a reverse vesicle in the same oil agent.
Furthermore, Non-Patent Document 3 describes a reverse vesicle composition using tetraethylene glycol dodecyl ether.
Non-Patent Document 4 describes a reverse vesicle composition using a diglycerin fatty acid ester.
Non-Patent Document 5 describes a reverse vesicle composition using polyoxyethylene oleyl ether (C18: 1EO50.8).

The conventional reverse vesicle described above has been manufactured by mixing the lamellar phase and the oil agent, which are constituents of the reverse vesicle, by applying physical stirring force by hand stirring or ultrasonic irradiation (the above-mentioned patent documents, (See non-patent literature.)
In the conventional method for forming a reverse vesicle, the dispersion of the lamella phase into the oil can be performed with a weaker stirring force as the flexibility of the lamella phase increases. It is reported that it is important to swell with an oil component (Non-patent Document 6).

JP 2010-104946 A JP 2009-62365 A

Conventional water-dispersed vesicles are prone to exchange of water-soluble components because the aqueous phase exists inside and outside (bulk) the vesicle. Therefore, the water-dispersed vesicle composition has a problem that a water-soluble active ingredient cannot be stably retained.

On the other hand, as shown in Non-Patent Document 1, when lecithin and C4-lecithin are combined in cyclohexane, a reverse vesicle composition can be formed. When using lecithin, it was difficult to form reverse vesicles.
In addition, as shown in Non-Patent Document 1, it is necessary to add a salt such as NaCl in order to stably form an inverted vesicle in cyclohexane.

The present invention is intended to solve the above-described problems, and an object thereof is to provide a reverse vesicle composition using lecithin.

By the way, in forming the reverse vesicle, it is necessary that the surfactant is in a balanced state in which a bilayer film is formed.
Surfactants constituting reverse vesicles as described in

Patent Documents

1 and 2 and

Non-Patent Documents

3 and 4 have a small hydrophilic group, which indicates that the curvature of the bilayer film becomes positive when the hydrophilic group is further increased. This is because a bimolecular film is not formed.
Since such a bilayer component is easy to mix with oil, there is a problem that the bilayer membrane is likely to undergo structural change, and it is difficult to select a system for the entire composition.

On the other hand, as described in Non-Patent Document 5, in order to form a reverse vesicle using a surfactant having a long hydrophilic group, it is necessary to add an oil solvent having a small molecular weight in order to make the curvature negative. is there. However, an oil agent having an extremely small molecular weight is difficult to apply to an external preparation for skin due to safety issues.
For the above reasons, when examining an external preparation for skin containing reverse vesicles, there are great restrictions on the surfactants that can be selected.

The present invention is intended to solve the above-described problems, and an object thereof is to provide a novel reverse vesicle composition. In particular, even when a surfactant having a large hydrophilic group is used, it is possible to easily obtain a balanced state for forming a bilayer film, and to provide a technique for stably producing a reverse vesicle. And

On the other hand, in the conventional method for producing a reverse vesicle composition, when a large molecular weight oil agent is used, the oil agent cannot enter between the layers of the bilayer film, so that the lamellar phase becomes rigid and a fine reverse vesicle is obtained. It was difficult. In particular, when trying to obtain a reverse vesicle using a relatively large molecular weight oil that can be used safely in cosmetics and the like, it is necessary to give a large stirring force, which is also a problem in terms of production efficiency. there were.

The present invention is intended to solve the above-described problems, and an object thereof is to provide a novel method for producing a reverse vesicle composition. In particular, an object of the present invention is to provide a production method that facilitates the formation of a reverse vesicle composition as compared with the conventional method when an oil agent having a large molecular weight is used.

<Reverse vesicle composition containing lecithin>
The first aspect of the present invention for solving the above problems is a reverse vesicle composition containing lecithin and a reverse vesicle composition containing a liquid oil at 25 ° C. having a molecular weight of greater than 114 g / mol.
In the reverse vesicle composition of the present invention, the reverse vesicle of lecithin is stably formed in an oil agent.
Here, the stable formation of the reverse vesicle means that the composition containing the reverse vesicle is retained in the composition without phase separation into an oil and a lamellar phase. .

In a preferred embodiment of the present invention, the oil agent is selected from silicone oil, hydrocarbon oil, ester oil, natural animal and vegetable oil, and fluorine oil.
By using these oil agents, a highly safe reverse vesicle composition suitable for cosmetics is obtained.

In the preferable form of this invention, the said reverse vesicle composition contains the said oil agent 40 mass% or more.
A reverse vesicle composition containing 40% by mass of the oil agent has high reverse vesicle formation.

In the preferable form of this invention, the said reverse vesicle contains water.
When the reverse vesicle contains water, the formation property of the reverse vesicle is improved, and the reverse vesicle composition having higher stability is obtained. In addition, for example, a water-soluble component that is an active ingredient such as cosmetics can be held in the reverse vesicle. Moreover, the inside of a reverse vesicle can also be used as a reaction field.

In a preferred embodiment of the present invention, the content of the water in the inverse vesicle composition is not more than 1 mass times the content of the bilayer constituent components including lecithin.
By setting it as such a form, the reverse vesicle of a lecithin can be maintained more stably.

In the preferable form of this invention, the said reverse vesicle contains a water-soluble active ingredient.
An inverse vesicle composition containing such an inverse vesicle composition can function as a composition having various activities on biological tissues such as skin.

In a preferred form of the invention, the inverse vesicle composition of the invention is non-emulsifying.
The inverse vesicle composition in such a form has high stability.

Another aspect of the present invention is an external preparation for skin comprising the reverse vesicle composition of the present invention described above.
The external preparation for skin containing such a reverse vesicle composition can hold a water-soluble active ingredient in the reverse vesicle, and thus can stably hold the active ingredient in the preparation.

Another aspect of the present invention is a reverse vesicle comprising preparing a mixture by mixing lecithin and a liquid oil component having a molecular weight of greater than 114 g / mol at 25 ° C., and then shaking or stirring the mixture. It is a manufacturing method of a composition.
According to the production method of the present invention, a stable composition containing an inverted vesicle containing lecithin can be produced efficiently.

Another aspect of the present invention is a method for producing a reverse vesicle, which comprises recovering the reverse vesicle from the reverse vesicle composition described above.
Another aspect of the present invention is an external preparation for skin containing the reverse vesicle collected above.

<Reverse Vesicle Composition Containing Silicone Surfactant>
Moreover, this invention which solves the subject regarding the magnitude | size of the hydrophilic group mentioned above and the molecular weight of an oil agent is the reverse vesicle composition containing a silicone surfactant and water and a liquid agent at 25 degreeC.
The reverse vesicle composition of the present invention is such that a reverse vesicle containing a silicone surfactant and water is stably formed in an oil.
Here, the stable formation of the reverse vesicle means that the composition containing the reverse vesicle is retained in the composition without phase separation into an oil and a lamellar phase. .

In a preferred embodiment of the present invention, the silicone surfactant is selected from polyoxyethylene-modified silicone, polyoxypropylene-modified silicone, polyoxyethylene / polyoxypropylene-modified silicone, and polyglycerin-modified silicone.
By using these silicone surfactants, a reverse vesicle composition that can be used for a topical skin preparation or the like is obtained.

In a preferred embodiment of the present invention, the silicone surfactant has an HLB of 3 to 13.
By using such a silicone surfactant, the reverse vesicle formability of the silicone surfactant is improved.

In the preferable form of this invention, a reverse vesicle composition contains the said oil agent 40 mass% or more.
A reverse vesicle composition containing 40% by mass of the oil agent has high reverse vesicle formation.

In a preferred embodiment of the present invention, the content mass of the water is not more than 1 times the content mass of the bilayer membrane component containing the silicone surfactant.
By setting it as such a form, the reverse vesicle of a silicone surfactant can be maintained more stably.

In the preferable form of this invention, the said reverse vesicle contains a water-soluble active ingredient.
An inverse vesicle composition containing such an inverse vesicle can function as a composition having various activities on biological tissues such as skin.

In a preferred form of the invention, the inverse vesicle composition is non-emulsifying.
The inverse vesicle composition in such a form has high stability.

Another aspect of the present invention is a reverse vesicle composition comprising mixing a silicone surfactant, water, and an oil component that is liquid at 25 ° C. to prepare a mixture, and then shaking or stirring the mixture. It is a manufacturing method.
According to the production method of the present invention, a stable composition containing an inverted vesicle containing a silicone surfactant can be produced efficiently.

<The manufacturing method 1 of a reverse vesicle composition>
The present invention for solving the problems related to the method for producing the reverse vesicle composition described above,
Dissolving a bilayer component in a volatile solvent to obtain a first isotropic solution;
Mixing the first isotropic solution with an oil to obtain a second isotropic solution;
Volatilizing the volatile solvent in the second isotropic solution;
A volatilization step of forming a reverse vesicle of the bilayer component by volatilization of a volatile solvent;
Is a method for producing a reverse vesicle composition.
In this way, the bilayer component is dissolved in a volatile solvent to form an isotropic solution, then mixed with an oil agent, and then the volatile solvent is volatilized, so that the lamellar is removed from the isotropic solution. A reverse vesicle composition can be obtained by causing a phase transition to.
According to the method for producing an inverse vesicle composition of the present invention, an inverse vesicle composition is produced even in a system in which the bilayer component is difficult to disperse in an oil agent by physical stirring, for example, a system using an oil agent having a large molecular weight. It becomes possible to do.
In particular, an inverse vesicle composition containing fine inverse vesicles can be easily produced.

In a preferred embodiment of the present invention, the volatile solvent is selected from alcohols, hydrocarbons, aromatics, ketones, ethers, esters, volatile silicone oils, and isoparaffins.
By using the above as a volatile solvent, when it is assumed that the manufactured reverse vesicle composition is used for an external preparation for skin such as cosmetics, its safety can be improved.

In a preferred embodiment of the present invention, the oil agent is selected from silicone oil, hydrocarbon oil, ester oil, natural animal and vegetable oil, and fluorine oil.
By using these oil agents, when it is assumed that the manufactured reverse vesicle composition is used for an external preparation for skin such as cosmetics, its safety can be improved.

In the present invention, the bilayer component is not particularly limited. For example, when the obtained reverse vesicle composition is applied as a cosmetic component, lecithin and / or a nonionic surfactant are preferably mentioned.

In one embodiment of the present invention, the first isotropic solution may contain water that is not more than 1 times the content of the bilayer component.

In one form of the present invention, the second isotropic solution is a two-phase solution in which particles of the first isotropic solution are dispersed in the oil.
Depending on the volatile solvent, the volatile solvent and the oil may form one phase or two phases. In the latter case, the particles of the first isotropic solution are dispersed in the oil. By doing so, a reverse vesicle can be manufactured.

In a preferred embodiment of the present invention, the volatile solvent is volatilized under reduced pressure.

The present invention relates to a method for producing a reverse vesicle composition comprising a reverse vesicle containing lecithin and an oil agent which has a molecular weight greater than 114 g / mol and is liquid at 25 ° C.
Moreover, this invention relates to the manufacturing method of the reverse vesicle composition containing a silicone surfactant and water, and the reverse vesicle composition containing an oil agent liquid at 25 degreeC.

The present invention also relates to a method for producing an external preparation for skin, comprising mixing the reverse vesicle composition produced by the production method described above with other components.

<The manufacturing method 2 of a reverse vesicle composition>
In addition to the above production method, the present invention for solving the problems related to the production method of the reverse vesicle composition described above,
Mixing the bilayer component and the oil and heating to obtain an isotropic solution;
A cooling step for cooling the isotropic solution;
Forming a reverse vesicle of the bilayer component by the cooling; and
Is a method for producing a reverse vesicle composition.
In this way, an isotropic solution is prepared by mixing and heating a bilayer component and an oil agent, and cooling this to cause a phase transition from the isotropic solution to the lamella, thereby causing a reverse vesicle. A composition can be obtained.
According to the method for producing an inverse vesicle composition of the present invention, an inverse vesicle composition is produced even in a system in which the bilayer component is difficult to disperse in an oil agent by physical stirring, for example, a system using an oil agent having a large molecular weight. It becomes possible to do.
In particular, an inverse vesicle composition containing fine inverse vesicles can be easily produced.

In one embodiment of the present invention, the isotropic solution may contain water that is not more than 1 times the content of the bilayer component.

In a preferred embodiment of the present invention, the heating is performed to a temperature at which the bilayer membrane component and the oil agent form a one-phase isotropic solution.
In this case, when the oil agent contains two or more oil agents, the heating is performed at a temperature at which the bilayer component forms a one-phase isotropic solution with at least one oil agent. It may be done.

In one embodiment of the present invention, the cooling is performed by diluting the isotropic solution with a cooling solvent having a temperature lower than that of the isotropic solution.
In this embodiment, the cooling solvent preferably contains the oil agent.

The inverse vesicle composition of the present invention has high stability. Moreover, the reverse vesicle composition of the present invention can contain a water-soluble active ingredient in the reverse vesicle of the reverse vesicle composition, and also uses the water pool in the reverse vesicle as a reaction field. It is also possible. In addition, the reverse vesicle composition of the present invention can achieve high safety even when it is assumed to be used for external preparations for skin, foods and the like.
Moreover, the manufacturing method of the reverse vesicle composition of this invention makes it possible to manufacture the said reverse vesicle composition efficiently.

Further, by using the method for producing a reverse vesicle composition of the present invention, it is possible to easily produce a reverse vesicle as compared with a conventional method for producing a reverse vesicle.
In particular, when a reverse vesicle composition is produced using an oil agent having a large molecular weight, it is not necessary to use a physical stirring force as compared with the case of using a conventional method, and productivity is improved in industrial production. It becomes possible. In addition, even when components or the like that have conventionally been difficult to form fine reverse vesicles are used, a reverse vesicle composition containing fine reverse vesicles can be produced relatively easily.

It is a schematic process drawing which shows the manufacturing method of the reverse vesicle composition 1 of this invention. The phase state in each step is also shown. It is a schematic process drawing which shows the manufacturing method of the reverse vesicle composition 2 of this invention. The phase state in each step is also shown. It is a figure showing the small angle X-ray-scattering spectrum of a lecithin / ascorbic acid 2-glucoside aqueous solution. The vertical axis represents the scattering intensity, and the horizontal axis represents the size of the scattering vector. It is a figure showing the small angle X-ray-scattering spectrum of the lecithin / tranexamic acid aqueous solution. The vertical axis represents the scattering intensity, and the horizontal axis represents the size of the scattering vector. It is a figure showing the small angle X-ray-scattering spectrum of a lecithin / dipotassium glycyrrhizinate aqueous solution. The vertical axis represents the scattering intensity, and the horizontal axis represents the size of the scattering vector.

<Reverse vesicle composition containing lecithin>
Hereinafter, the form for implementing this invention which concerns on the reverse vesicle composition containing a lecithin is explained in full detail.
The inverse vesicle composition of the present invention comprises an inverse vesicle containing lecithin and an oil that is liquid at 25 ° C. with a molecular weight of greater than 114 g / mol. Hereinafter, each component which comprises this composition is demonstrated.

(1) Reverse vesicle containing lecithin The reverse vesicle in the reverse vesicle composition of the present invention contains lecithin.
The lecithin forming the inverted vesicle of the present invention may be extracted from living organisms of plants, animals and microorganisms and purified as desired, or may be synthesized. Preferably, plant-derived lecithin such as soybean, corn, peanut, rapeseed, and wheat, or animal-derived lecithin such as egg yolk can be used.
The lecithin in the present invention includes phosphatidylcholine, phosphatidic acid, phosphatidylglycerol, phosphatidylinositol, phosphatidylethanolamine, phosphatidylmethylethanolamine, phosphatidylserine, bisphosphatidic acid, diphosphatidylglycerol (cardiolipin) and the like.
In the present invention, “lecithin” also includes hydrogenated lecithin, enzymatically decomposed lecithin, enzymatically decomposed hydrogenated lecithin, lysolecithin and the like.

The number of carbon atoms of the fatty acid constituting the hydrophobic group portion of lecithin is not particularly limited, and for example, those having 8 to 20 carbon atoms, preferably 16 to 18 carbon atoms can be mainly used. The fatty acid may be saturated or unsaturated. The fatty acid may be linear or branched.
In particular, the inverse vesicle composition of the present invention is advantageous in that lecithin having an unsaturated fatty acid can be used as a main component. As shown in Examples described later, in a conventionally known reverse vesicle composition using cyclohexane as a solvent, it was difficult to use lecithin having an unsaturated fatty acid as a main component.

In the present invention, lecithin can be used in the form of a single kind of the above-mentioned compound or in the form of a mixture of the above-mentioned plural kinds of phospholipids.
The composition of lecithin is preferably composed mainly of phosphatidylcholine, for example, 20% by mass or more, and preferably 50% by mass or more is phosphatidylcholine.

A commercially available lecithin can be used. For example, the following commercially available products can be used.
Resinol S-10, Nikko Chemicals (hydrogenated: ○, PC (phosphatidylcholine) content: 25-30%)
Resinol S-10E, Nikko Chemicals (hydrogenated: ○, PC content: 75-85%)
Resinol S-10EX, Nikko Chemicals (hydrogenated: ○, PC content:> 95%)
Basis LP-20, Nisshin Oillio Co., Ltd. (hydrogenated: x, PC content: 20-30%)
Basis LP-20H, Nisshin Oilio Co., Ltd. (hydrogenated: ○, PC content: unconfirmed)
Basis LS-60HR, Nisshin Oilio Co., Ltd. (hydrogenated: ○, PC content: 60-75%)
Basis LS-60, Nisshin Oillio Co., Ltd. (hydrogenated: x, PC content: unconfirmed)
Phospholipon 85G, H.P. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 85%))
Phospholipon 90G, H.P. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 94%))
Phospholipon 75IP, H.P. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 70%))
Phospholipon 90IP, H.P. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 90%))
Phospholipon 80H, H.P. Holstein GmbH & Co. Company KG ((hydrogenated: ○, PC content:> 70%))
Phospholipon 90H, H.P. Holstein GmbH & Co. KG ((hydrogenated: ○, PC content:> 90%))
Phospholipon 75HIP, H.P. Holstein GmbH & Co. Company KG ((hydrogenated: ○, PC content:> 70%))
Phospholipon 90 HIP, H.P. Holstein GmbH & Co. KG ((hydrogenated: ○, PC content:> 90%))
Lipoid E25, H.I. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 25%))
Lipoid E80, H.I. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 80%))
Lipoid E80S, H.I. Holstein GmbH & Co. KG ((hydrogenated: x, PC content:> 64%))
Lipoid EPCS, H.C. Holstein GmbH & Co. Company KG ((hydrogenated: x, PC content:> 96%))
Epikron 200, Cargill (hydrogenated: x, PC content:> 95%)
Epikron 200SH, Cargill (hydrogenated: ○, PC content: unconfirmed)
Epikron 100P, Cargill (hydrogenated: x, PC content: unconfirmed)
Epikron 100H, Cargill (hydrogenated: ○, PC content: unconfirmed)
PhosphoLipid PCSH70, Nippon Seika Co., Ltd. (hydrogenated: ○, PC content: about 70%)
Egg yolk lecithin PL-100E, Kewpie company (hydrogenated: ○, PC content: about 83%)

The reverse vesicle containing lecithin in the present invention is a vesicle of a bilayer membrane in which the fatty acid chain of lecithin described above is oriented outward.
Moreover, the reverse vesicle in the present invention may contain an auxiliary surfactant (nonionic surfactant, ionic surfactant) other than lecithin as a bilayer constituent.
Here, it is preferable that lecithin accounts for 60% by mass or more, more preferably 80% by mass or more, of the bilayer constituent components forming the reverse vesicle.
The reverse vesicle in the present invention preferably contains water. Water is retained in the bilayer membrane of the reverse vesicle. Thereby, the stability in the composition of a reverse vesicle improves. It is also possible to retain a water-soluble active ingredient in the bilayer membrane. Examples of the active ingredient include ingredients effective for improving skin tissue and promoting health.
When the reverse vesicle contains water, the content of water is preferably 1 mass times or less of the content of the bilayer constituent component containing lecithin. In addition, the content of water is preferably 0.1 to 0.7 times the content of the bilayer membrane component including lecithin. As a result, the reverse vesicle can be stably held without overflowing excessive water from the bilayer membrane of the reverse vesicle.

(2) Liquid oil at 25 ° C. with a molecular weight greater than 114 g / mol The liquid oil at 25 ° C. with a molecular weight greater than 114 g / mol used in the present invention constitutes the external and internal phases of the aforementioned reverse vesicle. .
The oil agent is not particularly limited as long as it has a molecular weight of greater than 114 g / mol and is liquid at 25 ° C.
Here, when an oil agent having a molecular weight of 114 g / mol or less is used, a coexisting phase of a lamellar phase and an oil agent necessary for forming a reverse vesicle cannot be formed. However, by using an oil agent having a molecular weight of greater than 114 g / mol, the solubility of lecithin in the oil agent can be lowered, and a coexisting phase of the lamellar phase and the oil agent can be formed.
The molecular weight of the oil agent is preferably 282 g / mol or more. However, in general, as the molecular weight increases, the viscosity of the oil increases, making it difficult to disperse the lamellar phase. Therefore, it is preferable that the oil agent has a molecular weight or less capable of realizing fluidity at room temperature.

Examples of the oil used in the present invention include silicone oil, hydrocarbon oil, ester oil, natural animal and vegetable oil, and fluorine oil.

Examples of silicone oil include organopolysiloxanes such as dimethylpolysiloxane, methylphenylpolysiloxane, dimethylsiloxane / methylphenylsiloxane copolymer, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane, etc. Examples thereof include cyclic siloxane.
Among these, the cyclic siloxane described above is preferably used.

Hydrocarbon oils include chain and cyclic hydrocarbons such as α-olefin oligomers, light isoparaffins, light liquid isoparaffins, squalane, liquid paraffin, liquid isoparaffins, hydrogenated isobutene, isooctane, decane, isododecane, isohexadecane, Polybutene, decyltetradecanol and the like can be mentioned.

Ester oils include dioctyl succinate, diisobutyl adipate, dioctyl adipate, di (2-heptylundecyl) adipate, diisopropyl sebacate, dioctyl sebacate, dibutyl octyl sebacate, diisostearyl malate, triethyl citrate , Ethylene glycol dioctanoate, neopentyl glycol dioctanoate, propylene glycol dicaprate, neopentyl glycol dicaprate, trimethylolpropane trioctanoate, trimethylolpropane triisostearate, pentaerythritol tetraoleate, ethyl acetate, butyl acetate, amyl acetate Octyldodecyl neopentanoate, cetyl octanoate, isononyl isononanoate, isotridecyl isononanoate, dimethyloctanoate Sildecyl, ethyl laurate, hexyl laurate, isopropyl myristate, myristyl myristate, isocetyl myristate, octyldodecyl myristate, octyl palmitate, octyl palmitate, cetyl palmitate, isocetyl palmitate, isostearyl palmitate, stearic acid Butyl, hexyldecyl stearate, isopropyl isostearate, isocetyl isostearate, decyl oleate, oleyl oleate, octyldodecyl oleate, ethyl linoleate, isopropyl linoleate, cetyl lactate, myristyl lactate, cholesteryl hydroxystearate, dioctyl lauroyl glutamate Dodecyl, lauroyl sarcosine isopropyl, ethyl hexyl methoxycinnamate, tri Caprylic / capric acid) glyceryl, dimerdilinoleic di (isostearyl / phytosteryl), tetra isostearate pentaerythrityl, stearoyloxy stearic acid octyldodecyl, glyceryl trioctanoate, cetyl, and the like ethylhexanoate.

Natural animal and vegetable oils include avocado oil, almond oil, olive oil, wheat germ oil, safflower oil, jojoba oil, macadamia nut oil, cottonseed oil, coconut oil, and the like.

Fluorine oil includes perfluoro oils.

(3) Reverse vesicle composition The reverse vesicle composition of the present invention is obtained by forming the above-described reverse vesicle in the above-described oil agent.
The upper limit of the content of lecithin in the reverse vesicle composition of the present invention is not particularly limited as long as the reverse vesicle composition can be formed, but is usually 10% by mass, preferably 5% by mass, more preferably 2% by mass. More preferably, it is 1% by mass.
Moreover, the lower limit of the content of lecithin in the reverse vesicle composition of the present invention is preferably 0.001% by mass, more preferably 0.01% by mass, and more preferably 0.1% by mass.

The lower limit of the content of the oil agent in the reverse vesicle composition of the present invention is not particularly limited as long as the reverse vesicle composition can be formed, but is preferably 60% by mass, more preferably 80% by mass, and still more preferably 90%. It is 95 mass%, More preferably, it is 95 mass%.

By containing an oil agent in such a range, it becomes easy to form the coexistence phase of a lamella phase and an oil agent, and a reverse vesicle is formed stably and is hold | maintained in a composition.
Moreover, the upper limit of the content of the oil agent in the reverse vesicle composition of the present invention is not particularly limited, but is preferably 99.99% by mass, more preferably 99.90% by mass, and more preferably 99.00% by mass.

The reverse vesicle composition of the present invention may contain water. In this case, as described above, the water is preferably held in the reverse vesicle.
On the other hand, a part of the water in the composition may form an emulsion together with the oil. However, from the viewpoint of the stability of the reverse vesicle, the reverse vesicle composition of the present invention is more preferably not an emulsion type.
From such a viewpoint, the mass of water in the reverse vesicle composition is preferably equal to or less than that of lecithin. By doing in this way, separation of water from the lamellar phase can be suppressed, and most of the water can be held in the reverse vesicle.

The particle size of the reverse vesicle in the reverse vesicle composition of the present invention is preferably 200 μm or less, more preferably 20 μm, and even more preferably 2 μm or less, immediately after preparation. There is an advantage that the smaller the particle diameter is, the more difficult it is to settle in the dispersion. However, the particle size of the inverse vesicle does not particularly affect the stability of the inverse vesicle itself.
The particle size of the inverse vesicle can be measured by a dynamic light scattering method or a laser diffraction method.

The reverse vesicle composition of the present invention may contain other optional components such as preservatives, thickeners, and fragrances as long as they do not interfere with the formation of the reverse vesicles.

(4) Manufacturing method of reverse vesicle composition The reverse vesicle composition mentioned above can be performed by the method similar to manufacture of the conventional vesicle. That is, it can be produced by mixing the above-mentioned lecithin, an oil agent, and optionally water to prepare a mixture, and then shaking or stirring the mixture.
Shaking can be performed using a shaker or the like. Stirring can be performed using an ultrasonic disperser or the like.
Moreover, it is more preferable to manufacture the reverse vesicle composition mentioned above by the manufacturing method of the reverse vesicle composition of this invention mentioned later.
Confirmation that the reverse vesicle is formed can be confirmed, for example, by performing microscopic observation under polarized light.

It is also possible to recover the reverse vesicle from the reverse vesicle composition produced as described above. In addition, the collection | recovery here contains the concept of concentration.
As the method, in the reverse vesicle composition, after the reverse vesicle is precipitated, the supernatant is removed.

<Reverse Vesicle Composition Containing Silicone Surfactant>
Hereinafter, the form for implementing this invention which concerns on a silicone surfactant is explained in full detail.
The reverse vesicle composition of the present invention contains a reverse vesicle containing a silicone surfactant and water, and an oil agent that is liquid at 25 ° C. Hereinafter, each component which comprises this composition is demonstrated.

(1) Reverse vesicle containing silicone surfactant and water The reverse vesicle in the reverse vesicle composition of the present invention contains a silicone surfactant.
The silicone surfactant is a surfactant having a polyorganosiloxane (silicone chain) in a hydrophobic group. The hydrophilic group is preferably selected from polyether or polyglycerin. Preferred examples of the polyether include polyoxyethylene, polyoxypropylene, and oxyethylene / oxypropylene copolymers.
The average degree of polymerization of polyoxyethylene or polyoxypropylene, oxyethylene / oxypropylene copolymer, and polyglycerin is, for example, about 8 to 15.
The polyorganosiloxane may be linear or branched. A plurality of polyorganosiloxane chains may be cross-linked. The silicone chain may be modified with an alkyl group.

The HLB of the silicone surfactant is preferably 3 to 13, more preferably 6 to 10.

It is preferable that the silicone surfactant is soluble or dispersible in the oil agent. Moreover, it is preferable that it is a liquid at room temperature.

In the present invention, the silicone surfactant can be used in the form of a single kind of the above compound, or in the form of a mixture of plural kinds.

These silicone surfactants are known as cosmetic raw materials, and any of them can be used.
Commercially available silicone surfactants can be used. For example, the following commercially available products can be used.
・ SH3772M (PEG-12 dimethicone (polyoxyethylene type), HLB: 6, Toray Dow Corning)
・ SH3773M (PEG-12 dimethicone (polyoxyethylene type), HLB: 8, Toray Dow Corning)
・ FZ2222 (polysilicone-13 (oxyethylene / oxypropylene type), HLB: 6, Toray Dow Corning)
・ KF6013 (PEG-9 dimethicone ((polyoxyethylene type)), HLB: 10, Shin-Etsu Silicone)
・ KF6100 (polyglyceryl 3 disiloxane dimethicone (polyglycerin), Shin-Etsu Silicone)

The reverse vesicle in the present invention is a bilayer vesicle in which the siloxane chain of the above-described silicone surfactant is oriented outward.
Moreover, the reverse vesicle in the present invention may contain a co-surfactant (nonionic surfactant, ionic surfactant) other than the silicone surfactant as a bilayer constituent.
Here, among the bilayer constituent components forming the reverse vesicle, the silicone surfactant preferably accounts for 50% by mass or more, and more preferably 80% by mass or more.

The reverse vesicle in the present invention contains water. Water is retained in the bilayer membrane of the reverse vesicle. It is also possible to retain a water-soluble active ingredient in the bilayer membrane. Examples of the active ingredient include ingredients effective for improving skin tissue and promoting health.
The content of water is preferably 1 mass times or less of the content of the bilayer constituent component including the silicone surfactant. The water content is preferably 0.05 to 0.7 mass times the content of the bilayer constituent component including the silicone surfactant. As a result, the reverse vesicle can be stably held without overflowing excessive water from the bilayer membrane of the reverse vesicle.

(2) Oil agent that is liquid at 25 ° C. The oil agent that is liquid at 25 ° C. used in the present invention constitutes the external and internal phases of the above-described reverse vesicle. The oil agent preferably has a molecular weight or less that can realize fluidity at room temperature.

As the oil used in the present invention, the same oil as described in <Reverse vesicle composition containing lecithin> can be used.

(3) Reverse vesicle composition The reverse vesicle composition of the present invention is obtained by forming the above-described reverse vesicle in the above-described oil agent.
The upper limit of the content of the silicone surfactant in the reverse vesicle composition of the present invention is not particularly limited as long as the reverse vesicle composition can be formed, but is usually 10% by mass, preferably 5% by mass, and more preferably 2% by mass, more preferably 1% by mass.
Moreover, the lower limit of the content of the silicone surfactant in the reverse vesicle composition of the present invention is preferably 0.01% by mass, and more preferably 0.1% by mass.

In the inverse vesicle composition of the present invention, water is included. In this case, as described above, the water is preferably held in the reverse vesicle.
On the other hand, a part of the water in the composition may form an emulsion together with the oil. However, from the viewpoint of the stability of the reverse vesicle, the reverse vesicle composition of the present invention is more preferably not an emulsion type.
From such a viewpoint, the mass of water in the reverse vesicle composition is preferably equal to or less than that of the silicone surfactant. By doing in this way, separation of water from the lamellar phase can be suppressed, and most of the water can be held in the reverse vesicle.

(4) Method for Producing Reverse Vesicle Composition The reverse vesicle composition containing the silicone surfactant described above can be produced in the same manner as the production of conventional vesicles, as is the case with the reverse vesicle composition containing lecithin. it can. Moreover, it is more preferable to manufacture the reverse vesicle composition mentioned above by the manufacturing method of the reverse vesicle composition of this invention mentioned later.
Confirmation that the reverse vesicle is formed can be confirmed by, for example, microscopic observation.

(5) Skin external preparation The reverse vesicle composition containing the lecithin or silicone surfactant of the present invention can be used as a raw material for the skin external preparation. Of course, the reverse vesicle composition containing the lecithin or silicone surfactant of the present invention can be used as it is as a skin external preparation.
The external preparation for skin containing such a reverse vesicle composition can hold a water-soluble active ingredient in the reverse vesicle, and thus can stably hold the active ingredient in the preparation. Examples of such water-soluble active ingredients include tranexamic acid, glycyrrhizic acid and salts thereof, ascorbic acid, ascorbic acid phosphate ester, 3-O-ethylascorbic acid, ascorbic acid glucoside, and ascorbic acids such as salts thereof. Ursolates such as arbutin, potassium ursolate phosphate, vitamin B such as pyridoxine, riboflavin or salts thereof, hyaluronic acid or salts thereof, fucoidan, sulfated trehalose or salts thereof, trehalose, amino acids and amino acid derivatives, Preferred examples include esculetin glycosides, plant extracts (including liquid and solid forms) and the like.
Examples of the external preparation for skin include pharmaceuticals and cosmetics, but the reverse vesicle composition of the present invention is particularly preferably used as a raw material for cosmetics.
For example, the reverse vesicle composition of the present invention can be used as a skin external preparation in the form of lotion or oil as it is. Moreover, the reverse vesicle composition of the present invention can be used as a skin external preparation in the form of a lotion or cream by mixing with other components and emulsifying as necessary. Moreover, it can also be set as powder type cosmetics by mixing the reverse vesicle composition of this invention with the raw material powder of cosmetics.

<The manufacturing method 1 of a reverse vesicle composition>
Hereinafter, the form for implementing this invention which concerns on the manufacturing method of a reverse vesicle composition is explained in full detail, referring FIG.
(1) Step of obtaining first isotropic solution In the production method of the present invention, first, the bilayer membrane component 1 is dissolved in the volatile solvent 2 to obtain the first isotropic solution 3.
The bilayer component indicates a component of the bilayer that constitutes the reverse vesicle.
As a component of such a bilayer membrane, any amphiphilic substance is not particularly limited, and any of an ionic surfactant and a nonionic surfactant can be used. Preferably, lecithin which is an amphoteric surfactant is used. Nonionic surfactants can also be preferably used. For example, silicone surfactants, polyoxyethylene alkyl ethers, sucrose fatty acid esters, sphingosines, fatty acids and the like can be preferably used.
The production method of the present invention is effective when lecithin is used which has a rigid bimolecular film and is difficult to form reverse vesicles by conventional physical agitation. In consideration of using the inverse vesicle composition produced by the production method of the present invention for cosmetics and the like, nonionic surfactants such as lecithin and silicone surfactant are preferably used from the viewpoint of safety.

When producing a reverse vesicle composition comprising lecithin or a silicone surfactant by the production method of the present invention, the lecithin or silicone surfactant comprises <an inverse vesicle composition comprising lecithin> or <a silicone surfactant. Various lecithins or silicone surfactants described in the column “Reverse Vesicle Composition> can be used without limitation.

When lecithin is mainly used, it can be combined with other auxiliary surfactants (nonionic surfactants, ionic surfactants).
In this case, it is preferable that lecithin accounts for 60% by mass or more, more preferably 80% by mass or more, among the bilayer components forming the reverse vesicle.

Examples of the volatile solvent for dissolving the above-described bilayer component include alcohols such as methanol, ethanol, propanol, and isopropanol, hydrocarbons such as pentane, hexane, and cyclopentane, aromatics such as benzene, acetone, and the like. And volatile silicone oils such as ketones, ethers, esters and decamethylpentasiloxane, fluorocarbons, isoparaffins and the like.
Of these, ethanol, propanol, acetone and the like are preferably used.

The content of the bilayer component in the first isotropic solution may be in a range where the bilayer component is sufficiently dissolved. For example, the content of the bilayer component can be 10 to 90% by mass. This is because when the amount is less than 10% by mass, the volatilization time of the volatile solvent may become long, and when it exceeds 90% by mass, the solution becomes viscous and may be difficult to dissolve.

Further, the first isotropic solution may contain water.
Since the production method of the present invention is intended to form an inverted vesicle without relying on conventional physical agitation, the presence of water is not necessary for the purpose of assisting dispersion by physical agitation, but rather there is little water. It can be said that it is useful in the system.
However, in the formation of inverted vesicles by volatilization of the volatile solvent, the presence of water may assist the formation of a bilayer.
From these viewpoints, the present invention may contain water having a mass of 1 or less that of the bilayer membrane component. In this case, the bilayer component can be mixed with water and mixed with a volatile solvent (FIG. 1 (a)). Of course, a bilayer component, water, and a volatile solvent may be mixed.

In the present invention, the bilayer membrane component 1 is dissolved in the volatile solvent 2 to prepare a first isotropic solution 3. This preparation can be performed by ordinary mixing and stirring.
The first isotropic solution 3 obtained by dissolving the bilayer membrane component 1 in the volatile solvent 2 is in a state where the bilayer membrane component 1 is monodispersed in the volatile solvent 2 or in the volatile solvent 2. In this state, aggregates such as reverse micelles of the bilayer membrane component 1 are formed (FIG. 1B).
Such an isotropic solution has a high fluidity and is easy to mix with a subsequent oil agent.

(2) Step of obtaining a second isotropic solution In the production method of the present invention, subsequently, the first isotropic solution 3 obtained above is mixed with an oil agent 4 to obtain a second isotropic solution. Get 5.

As the oil used in the present invention, the same oil as described in <Reverse vesicle composition containing lecithin> can be used. The oil agent is not particularly limited as long as it can be mixed with the first isotropic solution, but a liquid oil agent at 25 ° C. can be preferably used.

The mixing ratio of the first isotropic solution and the oil agent can be set such that the content of the bilayer component in the manufactured reverse vesicle composition is 0.1 to 10% by mass. .

By mixing the first isotropic solution 3 and the oil agent 4, an isotropic solution (second isotropic solution) 5 in which the bilayer membrane component 1 is dispersed in the oil agent 4 can be obtained.
Here, the form of dispersion of the bilayer membrane component in the oil agent varies depending on the solubility of the volatile solvent used in the oil agent.
(1) When the volatile solvent 2 is soluble in the oil agent 4, the first isotropic solution 3 is compatible with the oil agent to form a one-phase solution. That is, the bilayer component 1 contained in the first isotropic solution 3 is present in a monodispersed state or a state in which aggregates such as reverse micelles are formed in the one-

phase solutions

2 and 4. (FIG. 1 (c)).
(2) On the other hand, when the volatile solvent 2 is insoluble or hardly soluble in the oil agent 4, the first isotropic solution 3 is not compatible with the oil agent 4 and forms a two-phase solution. That is, the particles 31 of the first isotropic solution 3 are dispersed in the continuous phase of the oil agent 4 (FIG. 1D). As shown in FIG. 1 (d2), the particles 31 are in a state where the bilayer component 1 is monodispersed in the volatile solvent 2, or an aggregate such as a reverse micelle of the bilayer component 1 in the volatile solvent 2. It is in the state which formed.
This state can be easily formed by a normal shaking or stirring operation in the mixing step.
In addition, when using a combination of a component that is hardly soluble in the oil agent and a component that is soluble in the oil agent as the bilayer component, the component that is insoluble in the oil agent is dissolved in a volatile solvent, and the component that is soluble in the oil agent It is also possible to dissolve these in an oil and mix them.

<3> Step of volatilizing volatile solvent In the production method of the present invention, subsequently, the volatile solvent 2 is volatilized from the second isotropic solution 5 obtained by the above operation.
Volatilization of the volatile solvent can be performed by vaporizing the volatile solvent by reducing the pressure by a conventional method. Moreover, it is possible to carry out by heating a liquid mixture to the temperature which a volatile solvent vaporizes. Volatilization is preferably performed under reduced pressure. Moreover, when heating, it heats below the temperature which can maintain a lamellar phase (reverse vesicle), ie, below the temperature which does not phase-transform.
When the above-mentioned second isotropic solution forms two phases, the first isotropic solution is sufficiently dispersed in the oil by shaking or stirring, and then this step is entered. Is preferred.
It is also preferable to apply a stirring force during volatilization from the viewpoint of forming fine reverse vesicles.

As described above, by volatilizing the volatile solvent 2, the second isotropic solution 5 is phase-transduced, and the inverse vesicle composition 8 in which the inverse vesicle 7 is dispersed in the oil agent 4 can be obtained (FIG. 1). (E)). The state of the formed reverse vesicle may be a single layer or a multilayer. Confirmation that the reverse vesicle is formed can be confirmed, for example, by performing microscopic observation under polarized light.

The particle size of the reverse vesicle in the reverse vesicle composition produced in this manner is, for example, 200 μm or less, 20 μm in a more preferable form, and 2 μm or less in a more preferable form immediately after the production. There is an advantage that the smaller the particle diameter is, the more difficult it is to settle in the dispersion. However, the particle size of the inverse vesicle does not particularly affect the stability of the inverse vesicle itself.
The particle size of the inverse vesicle can be measured by a dynamic light scattering method or a laser diffraction method.

<The manufacturing method 2 of a reverse vesicle composition>
In addition to the method described above, the inverse vesicle composition can be produced by the following method.
Hereinafter, the form for implementing this invention which concerns on the manufacturing method of a reverse vesicle composition is explained in full detail, referring FIG.
(1) Step of obtaining an isotropic solution In the production method of the present invention, first, a mixture obtained by mixing the bilayer membrane component 1 and the oil agent 2 is heated to obtain the isotropic solution 3. In this embodiment, the lamella (Lα) of the bilayer membrane component 1 is dissolved in the oil agent 2 (L1) at this time, thereby forming a one-phase isotropic solution 3 (L1).
The bilayer component indicates a component of the bilayer that constitutes the reverse vesicle.
As a component of such a bilayer membrane, any amphiphilic substance is not particularly limited, and any of an ionic surfactant and a nonionic surfactant can be used. Preferably, lecithin which is an amphoteric surfactant is used. Nonionic surfactants can also be preferably used. For example, silicone surfactants, polyoxyethylene alkyl ethers, sucrose fatty acid esters, sphingosines, fatty acids and the like can be preferably used.

The production method of the present invention is extremely effective in the case of using lecithin in which the bilayer membrane is rigid and it is difficult to form reverse vesicles by conventional physical stirring. In consideration of using the inverse vesicle composition produced by the production method of the present invention for cosmetics and the like, nonionic surfactants such as lecithin and silicone surfactant are preferably used from the viewpoint of safety.

In the present invention, the mixture obtained by mixing the bilayer component with the oil is heated. In addition, the said bilayer membrane component and oil agent can also be mixed, heating.
As the oil agent, an oil agent which is liquid at 25 ° C. can be preferably used. As the oil used in the present invention, the same oil as described in <Reverse vesicle composition containing lecithin> can be used.
Only 1 type may be used for an oil agent, and 2 or more types may be mixed and used for it. Moreover, when mixing 2 or more types, you may combine the oil agent which mutually melt | dissolves and may combine the oil agent which does not melt | dissolve mutually.

The mixing ratio of the bilayer membrane component and the oil agent can be set such that the content of the bilayer membrane component in the manufactured reverse vesicle composition is 0.1 to 10% by mass.

Heating may be performed until the lamella (FIG. 2A) of the bilayer component 1 undergoes phase transition and the mixture becomes an isotropic solution. Whether or not it is an isotropic solution can be determined by observing the solution through a polarizing plate.
Further, the isotropic solution obtained by heating may be one-phase or two-phase, but it is more preferable to heat it until it becomes one-phase (see FIG. 2B, L1). In addition, when the said oil agent contains 2 or more types of oil agents, it is preferable that the said bilayer membrane component is performed to the temperature which forms a one-phase isotropic solution with at least 1 type of the said oil agent.
Whether the isotropic solution is one-phase or two-phase can be distinguished by observing the presence or absence of separation by leaving it at a constant temperature, or by measuring the light transmittance of the solution.
The phase transition temperature of the mixture varies depending on the combination of the bilayer component and the oil used. Therefore, the heating temperature may be adjusted in consideration of the phase transition temperature according to these combinations.
For example, when lecithin is used as a bilayer component and squalane is used as an oil agent, a phase transition from a lamellar phase to a two-phase isotropic solution is observed at around 65 ° C., and a two-phase is observed at around 90 ° C. A phase transition from an isotropic solution to a one-phase isotropic solution is seen. Accordingly, the heating temperature in this case is preferably 65 ° C. or higher, more preferably 90 ° C. or higher.
The isotropic solution 3 obtained by heating the mixture of the bilayer membrane component 1 and the oil agent 2 is in a state where reverse micelles of the bilayer membrane component 1 are formed in the oil agent 2 (FIG. 2 (b)).
In this embodiment, the heating is performed until a one-phase isotropic solution is obtained. However, the heating is performed until the two-phase isotropic solution (L1 + L2) as shown in FIG. 2C is obtained. Form may be sufficient. In the combination of lecithin and squalane, the highly viscous isotropic solution (L2) containing the reverse-like micelles of the bilayer membrane component 1 in the oil agent 2 is phase-separated from the oil agent (L1).
When a two-phase isotropic solution is formed, it is important to stir before cooling and / or during cooling to obtain a dispersed state.

Further, the mixture of the bilayer membrane component and the oil agent may further contain water.
Since the production method of the present invention is intended to form an inverted vesicle without relying on conventional physical agitation, the presence of water is not necessary for the purpose of assisting dispersion by physical agitation, but rather there is little water. It can be said that it is useful in the system.
However, in the formation of inverted vesicles by cooling, which will be described later, the presence of water may assist the formation of a bilayer.
From these viewpoints, the present invention may contain water having a mass of 1 or less that of the bilayer membrane component.
The smaller the water content, the lower the transition temperature to the isotropic solution. Therefore, when the production efficiency in the present invention is taken into consideration, it is advantageous that the water content is small.

(2) Step of cooling isotropic solution In the production method of the present invention, subsequently, the isotropic solution 3 obtained by the above operation is cooled.
The cooling method is not particularly limited, and examples thereof include a method of placing the isotropic solution at a temperature below room temperature and a method of cooling with a refrigerant. Moreover, it can cool by mixing the dilution solvent of temperature lower than the isotropic solution mixed. For example, you may mix the cooled oil agent as a dilution solvent.
The cooling temperature may be equal to or lower than the temperature at which the isotropic solution undergoes phase transition and the coexisting phase of the lamellar liquid crystal and the oil agent is formed. As a guide, cooling to about room temperature can be mentioned.
It is also preferable to apply a stirring force during cooling from the viewpoint of forming fine reverse vesicles.
Moreover, since it becomes possible to form a fine reverse vesicle, so that the rate of cooling becomes large (it quenches rapidly), such a form is also preferable.

As described above, by cooling the isotropic solution 3, a phase transition is performed, and the inverse vesicle composition 5 in which the inverse vesicle 4 is dispersed in the oil agent 2 can be obtained.
In the heated state, the isotropic solution forms an isotropic solution containing reverse micelles (FIG. 2B). When the isotropic solution is cooled, depending on the system, a highly viscous isotropic solution containing reverse string micelles is phase-separated (FIG. 2 (c)), and finally the inverted vesicle 4 is formed. (FIG. 2 (d)).
Confirmation that the reverse vesicle is formed can be confirmed, for example, by performing microscopic observation under polarized light.

The particle size of the reverse vesicle in the reverse vesicle composition produced in this manner is, for example, 200 μm or less, 20 μm in a more preferable form, and 2 μm or less in a more preferable form in a state immediately after preparation. There is an advantage that the smaller the particle diameter is, the more difficult it is to settle in the dispersion. However, the particle size of the inverse vesicle does not particularly affect the stability of the inverse vesicle itself.
The particle size of the inverse vesicle can be measured by a dynamic light scattering method or a laser diffraction method.

The reverse vesicle composition manufactured by the above-described reverse vesicle

composition manufacturing methods

1 and 2 of the present invention can be used as a raw material for an external preparation for skin. Of course, the reverse vesicle composition produced by such a method can be used as a skin external preparation as it is.
Examples of the external preparation for skin include pharmaceuticals and cosmetics, and it is particularly preferable to use cosmetics.
For example, the reverse vesicle composition can be used as a skin external preparation in the form of lotion or oil as it is or with optional components added. Moreover, the reverse vesicle composition can be used as a skin external preparation in the form of a lotion or cream by mixing with other components and emulsifying as necessary. Moreover, it can also be set as a powder type cosmetic by mixing the said reverse vesicle composition with the raw material powder of cosmetics.

<Reverse vesicle composition containing lecithin>
(1) Test example 1
Each component was mixed with the composition shown in Table 1, and the lamellar phase was dispersed in the oil with a chip-type ultrasonic disperser (product name: VCX130 (manufactured by Sonics & Materials)).
Thereafter, formation of reverse vesicles was confirmed using a polarizing microscope. For those in which the formation of reverse vesicles was confirmed, ◯ was entered, and for those in which the formation of reverse vesicles was not confirmed, x was entered.

(Unit:% by mass)
(1) Resinol S-10, manufactured by Nikko Chemicals Co., Ltd. (2) Epikron 200, manufactured by Cargill * Mainly composed of fatty acids having 16 or more carbon atoms, and the molecular weight exceeds 114.

As shown in Table 1, in B and D to J using an oil agent having a molecular weight of greater than 114 g / mol, formation of reverse vesicles was confirmed both when hydrogenated lecithin was used and when lecithin was used. It was.
On the other hand, looking at A and C using an oil agent with a molecular weight of 114 g / mol, formation of reverse vesicles was confirmed in A using hydrogenated lecithin, but formation of reverse vesicles was confirmed in C using lecithin. There wasn't.
From this, it was found that by using an oil agent having a molecular weight larger than 114 g / mol, a reverse vesicle can be formed without being limited by the type of lecithin.

(2) Test example 2
It was confirmed that a reverse vesicle was formed with a combination of lecithin and oil different from those in Test Example 1. Table 2 shows the lecithin and oil used. A mixture containing lecithin 0.8% by mass, water 0.2% by mass, and oil agent 99% by mass was prepared, and the lamellar phase was dispersed in the oil agent using a chip-type ultrasonic disperser. Thereafter, the formation of reverse vesicles was confirmed using a polarizing microscope. For those in which the formation of reverse vesicles was confirmed, ◯ was entered, and for those in which the formation of reverse vesicles was not confirmed, x was entered. The combinations of lecithin and oil that were not tested are blank in Table 2.

(1) Cargill (hydrogenated: x, PC (phosphatidylcholine) content:> 95%)
(2) Nisshin Oilio Co., Ltd. (hydrogenated: ○, PC content: 60-75%)
(3) Nikko Chemicals Co., Ltd. (hydrogenation: ○, PC content: 25-30%)
* It is mainly composed of fatty acids with 16 or more carbon atoms, and the molecular weight exceeds 114.
** It is mainly composed of dimer acid ester having 16 or more carbon atoms, and its molecular weight exceeds 114.
*** Since the degree of polymerization is 2 or more, the molecular weight exceeds 114.

As shown in Table 2, formation of reverse vesicles was confirmed in all the combinations of lecithin and oil tested.
From the results of Test Examples 1 and 2, it was found that by using an oil agent having a molecular weight greater than 114 g / mol, a reverse vesicle can be formed without being limited by the type of lecithin.

(3) Test example 3
We investigated whether crystalline water-soluble active ingredients could inhibit the formation of lamellar phase necessary for the formation of reverse vesicles. In this test example, three types of crystalline water-soluble active ingredients, ascorbic acid 2-glucoside, tranexamic acid, and dipotassium glycyrrhizinate were examined.
First, the solubility of the above three components in water was examined. The results are shown in Table 3.
As shown in Table 3, 40% ascorbic acid 2-glucoside aqueous solution, 10% tranexamic acid aqueous solution, and 10% glycylic salicylic acid aqueous solution are the highest concentration aqueous solutions in which each component dissolves. Went. Lecithin (Epicuron 200) and each aqueous solution were mixed at 8: 2, and the presence of a lamellar phase was observed for this mixture using small-angle X-ray scattering. When a lamellar phase is formed, a scattering spectrum peculiar to the lamellar phase having a peak ratio of 1: 2 is observed. The measurement results of small angle X-ray scattering of each mixture are shown in FIGS.
As shown in FIGS. 3 to 5, a scattering spectrum peculiar to the lamellar phase having a peak ratio of 1: 2 was obtained in all the mixtures. That is, it was confirmed that any water-soluble active ingredient was not contained in the lamellar phase without inhibiting the formation of the lamellar phase.
When a reverse vesicle is formed using the lamellar phase formed as in this test example, a reverse vesicle composition containing a water-soluble active ingredient can be obtained.

(3) Skin external preparation Examples of the skin external preparation (cosmetics) of the present invention are described below. The amount of each component is expressed in terms of mass percent.
Example 1. Treatment oil (A) Lecithin 0.4
(A) Water 0.1
(B) Squalane 69.4
(B) Olive oil 20
(B) Jojoba oil 10
(B) Fragrance 0.1

After the components of (A) group were mixed in advance, the components of (B) group were mixed and dispersed with an ultrasonic disperser.
As a result, a treatment oil containing a reverse vesicle (reverse vesicle solution) was produced.

Example 2 Cream (A) Dimethicone 31.5
(A) Cyclopentasiloxane
(A) (Dimethicone / Vinyl Dimethicone) Crosspolymer 5
(A) Polyether-modified silicone 2
(A) Sorbitan sesquiisostearate 1
(A) Phenoxyethanol 0.5
(B) Water 30
(B) 1,3-butanediol 10
(C) Reverse vesicle solution 10
(C-1) Lecithin 2
(C-2) Squalane 98

A reverse vesicle solution (C) was prepared by previously mixing (C-1 and 2) and dispersing with an ultrasonic disperser. The components of group (A) were mixed uniformly, the components of group (B) were mixed, and an emulsion was formed using a homogenizer. Thereafter, the emulsion and (C) prepared in advance were mixed by hand stirring.
As a result, a cream containing reverse vesicles was produced.

Example 3 Sunscreen cosmetics (A) Cyclopentasiloxane 26.7
(A) Polyether-modified silicone 3
(A) 40% hydrophobized fine particle titanium oxide slurry * 15
(A) 40% hydrophobized fine particle zinc slurry * 10
* Dispersion medium: cyclopentasiloxane (B) water 30
(B) 1,3-BG 5
(B) Methylparaben 0.3
(C) Reverse vesicle solution 10
(C-1) Lecithin 0.7
(C-2) Water 0.3
(C-3) Cyclopentasiloxane 99

A reverse vesicle solution (C) was prepared in the same manner as in Example 1 using (C-1 to 3) in advance. The components of group (A) were uniformly mixed by hand stirring and heated to 80 ° C. What was heated and stirred at 80 degreeC of the component of (B) group was added there, and it emulsified with the homogenizer. When the emulsion was cooled and reached 35 ° C., the emulsion and the previously prepared (C) were mixed by hand stirring.
As a result, a sunscreen cosmetic containing reverse vesicles was produced.

Example 4 Emulsion type foundation (A) Cyclopentasiloxane 24.2
(A) Diphenylsiloxyphenyl trimethicone 10
(A) Polyether-modified silicone 4
(A) Ethylhexyl methoxycinnamate 5
(A) Diethylaminohydroxybenzoyl hexyl benzoate 0.5
(B) Pigment dye (titanium oxide, iron oxide) 10
(C) Organically modified bentonite 1
(D) Water 30
(D) Glycerin 10
(D) Methylparaben 0.3
(E) Reverse vesicle solution 5
(E-1) Lecithin 1.4
(E-2) Water 0.6
(E-3) Cyclopentasiloxane 98

A reverse vesicle solution (E) was prepared in the same manner as in Example 1 using (E-1 to 3) in advance. The components of group (A) were uniformly mixed by hand stirring and heated to 80 ° C. (B) The component of (B) group is disperse | distributed with a disper to the mixture of the component of (A) group, Then, the component for (C) is disperse | distributed with a disper. Using a homogenizer, the obtained oil phase and (D) group uniformly mixed at 80 ° C. are mixed and emulsified. When the emulsion was cooled and reached 35 ° C., the emulsion and (E) prepared in advance were mixed by hand stirring.
As a result, an emulsified foundation containing a reverse vesicle was produced.

Example 5 FIG. Powder foundation (A) Silicone-treated pigment dye (titanium oxide, iron oxide) 15
(A) Talc 29.7
(A) Mica 10
(A) Fluorine-treated sericite 10
(A) Silica 10
(A) Methyl methacrylate cross polymer 10
(A) Mica titanium 5
(A) Methylparaben 0.3
(B) Reverse vesicle solution 10
(B-1) Lecithin 3
(B-2) Water 0.3
(B-3) Polyoxyethylene alkyl ether 0.3
(B-4) Dimethicone 40
(B-5) Jojoba oil 56.4

A reverse vesicle solution (B) was prepared in the same manner as in Example 1 using (B-1 to 5) in advance. After mixing the components of (A) group and coarsely pulverizing with a pulverizer, (B) was added and mixed with a Henschel mixer. Then, it grind | pulverized again with the pulverizer, and it casted into the metal dish.
As a result, a powder foundation containing reverse vesicles was produced.

<Reverse Vesicle Composition Containing Silicone Surfactant>
Each component was mixed with the composition shown in Table 4, and the lamellar phase was dispersed in the oil with a chip-type ultrasonic disperser (product name: VCX130 (manufactured by Sonics & Materials)).
Then, the formation confirmation of the reverse vesicle was confirmed using the optical microscope. For those in which the formation of reverse vesicles was confirmed, ◯ was entered, and for those in which the formation of reverse vesicles was not confirmed, x was entered.

As shown in Table 4, formation of reverse vesicles was confirmed in A to E using a silicone surfactant.
Thus, it was found that a reverse vesicle composition can be obtained by using a silicone surfactant.

Below, the Example of the skin external preparation (cosmetics) of this invention is described. A compounding quantity is shown in the mass percentage.
Example 6 Treatment oil (A) Polyoxyethylene-modified silicone (HLB8) * 0.4
(A) Water 0.1
(B) Squalane 69.4
(B) Olive oil 20
(B) Jojoba oil 10
(B) Fragrance 0.1
* SH3773M, HLB: 8, Toray Dow Corning

After the components of (A) group were mixed in advance, the components of (B) group were mixed and dispersed with an ultrasonic disperser.
As a result, a treatment oil containing reverse vesicles was produced.

Example 7 Cream (A) Dimethicone 31.5
(A) Cyclopentasiloxane
(A) (Dimethicone / Vinyl Dimethicone) Crosspolymer 5
(A) Polyether-modified silicone 2
(A) Sorbitan sesquiisostearate 1
(A) Phenoxyethanol 0.5
(B) Water 30
(B) 1,3-butanediol 10
(C) Reverse vesicle solution 10
(C-1) Polyether-modified silicone (HLB8) * 1.5
(C-2) Water 0.5
(C-3) (Dimethicone / Vinyl Dimethicone) Crosspolymer 10
(C-4) Dimethicone 30
(C-5) Cyclopentasiloxane 58
* SH3773M, HLB: 8, Toray Dow Corning

A reverse vesicle solution (C) was prepared in the same manner as in Example 6 using (C-1 to 5) in advance. The components of group (A) were mixed uniformly, the components of group (B) were mixed, and an emulsion was formed using a homogenizer. Thereafter, the emulsion and (C) prepared in advance were mixed by hand stirring.
As a result, a cream containing reverse vesicles was produced.

Example 8 FIG. Sunscreen cosmetics (A) Cyclopentasiloxane 26.7
(A) Polyether-modified silicone 3
(A) 40% hydrophobized fine particle titanium oxide slurry * 15
(A) 40% hydrophobized fine particle zinc slurry * 10
* Dispersion medium: cyclopentasiloxane (B) water 30
(B) 1,3-BG 5
(B) Methylparaben 0.3
(C) Reverse vesicle solution 10
(C-1) Block copolymer polyether-modified silicone * 0.9
(C-2) Water 0.1
(C-3) Diphenylsiloxyphenyl trimethicone 99
* FZ2222, POE / POP block copolymer type, HLB: 6, Toray Dow Corning

A reverse vesicle solution (C) was prepared in the same manner as in Example 6 using (C-1 to 3) in advance. The components of group (A) were uniformly mixed by hand stirring and heated to 80 ° C. What was heated and stirred at 80 degreeC of the component of (B) group was added there, and it emulsified with the homogenizer. When the emulsion was cooled and reached 35 ° C., the emulsion and the previously prepared (C) were mixed by hand stirring.
As a result, a sunscreen cosmetic containing reverse vesicles was produced.

Example 9 Emulsification foundation Example 9 Emulsion type foundation (A) cyclopentasiloxane 24.2
(A) Diphenylsiloxyphenyl trimethicone 10
(A) Polyether-modified silicone 4
(A) Ethylhexyl methoxycinnamate 5
(A) Diethylaminohydroxybenzoyl hexyl benzoate 0.5
(B) Pigment dye (titanium oxide, iron oxide) 10
(C) Organically modified bentonite 1
(D) Water 30
(D) Glycerin 10
(D) Methylparaben 0.3
(E) Reverse vesicle solution 5
(E-1) Block copolymer polyether-modified silicone (HLB6) *
1.6
(E-2) Block copolymer polyether-modified silicone (HLB3) *
0.1
(E-3) Water 0.3
(E-4) (Dimethicone / Vinyl Dimethicone) Crosspolymer 10
(E-5) Dimethicone 30
(E-6) Cyclopentasiloxane 58
* FZ2222, POE / POP block copolymer type, HLB: 6, Toray Dow Corning * FZ2233, POE / POP block copolymer type, HLB: 3, Toray Dow Corning

A reverse vesicle solution (E) was prepared in the same manner as in Example 6 using (E-1 to 6) in advance. The components of group (A) were uniformly mixed by hand stirring and heated to 80 ° C. (B) The component of (B) group is disperse | distributed with a disper to the mixture of the component of (A) group, Then, the component for (C) is disperse | distributed with a disper. Using a homogenizer, the obtained oil phase and (D) group uniformly mixed at 80 ° C. are mixed and emulsified. When the emulsion was cooled and reached 35 ° C., the emulsion and (E) prepared in advance were mixed by hand stirring.
As a result, an emulsified foundation containing a reverse vesicle was produced.

Example 10 Powder foundation (A) Silicone-treated pigment dye (titanium oxide, iron oxide) 15
(A) Talc 29.7
(A) Mica 10
(A) Fluorine-treated sericite 10
(A) Silica 10
(A) Methyl methacrylate cross polymer 10
(A) Mica titanium 5
(A) Methylparaben 0.3
(B) Reverse vesicle solution 10
(B-1) Polyglycerin-modified silicone * 1.4
(B-2) Water 0.6
(B-3) Dimethicone 98
* KF6100, Shin-Etsu Silicone

A reverse vesicle solution (B) was prepared in the same manner as in Example 6 using (B-1 to 3) in advance. After mixing the components of (A) group and coarsely pulverizing with a pulverizer, (B) was added and mixed with a Henschel mixer. Then, it grind | pulverized again with the pulverizer, and it casted into the metal dish.
As a result, a powder foundation containing reverse vesicles was produced.

<The manufacturing method 1 of a reverse vesicle composition>
With the composition shown in Table 5, an inverse vesicle composition was produced by the following method.
That is, for samples A to D, a mixture of bilayer components and water (lamellar mixture) was dissolved in a volatile solvent to prepare an intermediate solution (first isotropic solution). Subsequently, this intermediate solution was mixed with an oil agent to obtain a mixed solution. This solution formed two phases. Subsequently, this mixed solution was stirred with a vortex mixer for 1 minute to obtain a dispersion (second isotropic solution) in which the intermediate solution was dispersed in the oil, and then heated to 35 ° C. in a reduced pressure oven. Dry until volatile solvent is gone.
For sample E, a mixture of the bilayer component and water was mixed with an oil agent, and the mixed solution was stirred with a vortex mixer under the same conditions as described above.
About the obtained composition, formation of the reverse vesicle was confirmed using the polarization microscope. For those in which the formation of reverse vesicles was confirmed, ◯ was entered, and for those in which the formation of reverse vesicles was not confirmed, x was entered.

As shown in Table 5, formation of reverse vesicles was confirmed in Samples A to D using a method in which the lamella mixture was dissolved in a volatile solvent to prepare an intermediate solution and then mixed with the oil.
On the other hand, in the sample E using the method of directly mixing the lamella mixture with the oil agent as in the conventional case, the formation of the reverse vesicle was not confirmed.
From this, it was found that the reverse vesicle composition can be easily prepared by dissolving the bilayer component in a volatile solvent in advance, mixing it with an oil agent, and then volatilizing the volatile solvent.
In addition, in the prescription of sample E, the present inventors have confirmed that an inverted vesicle composition can be produced by applying a stronger stirring force using an ultrasonic disperser or the like. The production method of the present invention can produce a reverse vesicle composition without requiring a strong stirring force by such an ultrasonic disperser, and is useful in this respect when assuming industrial production. It can be said that there is.
Moreover, when using the oil agent with a larger molecular weight than the oil agent used in the present Example, it is thought that the manufacturing method of this invention becomes very useful.

Below, the manufacture example of skin external preparation (cosmetics) is described. A compounding quantity is shown in the mass percentage.
Example 11 Treatment oil (A) Lecithin 0.4
(A) Water 0.1
(A) Ethanol 0.2
(B) Squalane 69.4
(B) Olive oil 20
(B) Jojoba oil 10
(B) Fragrance 0.1

After the mixture of lecithin and water of group (A) was dissolved in a volatile solvent, these were mixed with the components of group (B), and this mixed solution was stirred with a vortex mixer for 1 minute. Subsequently, the volatile solvent was removed by a conventional method.
As a result, a treatment oil containing a reverse vesicle (reverse vesicle solution) was produced.

Example 12 Cream (A) Dimethicone 31.5
(A) Cyclopentasiloxane
(A) (Dimethicone / Vinyl Dimethicone) Crosspolymer 5
(A) Polyether-modified silicone 2
(A) Sorbitan sesquiisostearate 1
(A) Phenoxyethanol 0.5
(B) Water 30
(B) 1,3-butanediol 10
(C) Reverse vesicle solution 10
(C-1) Lecithin 2
(C-2) Propanol 2
(C-3) Squalane 98

Using (C-1,2,3), a reverse vesicle solution (C) was prepared in the same manner as in Example 11. The components of group (A) were mixed uniformly, the components of group (B) were mixed, and an emulsion was formed using a homogenizer. Thereafter, the emulsion and (C) prepared in advance were mixed by hand stirring.
As a result, a cream containing reverse vesicles was produced.

Example 13 Sunscreen cosmetics (A) Cyclopentasiloxane 26.7
(A) Polyether-modified silicone 3
(A) 40% hydrophobized fine particle titanium oxide slurry * 15
(A) 40% hydrophobized fine particle zinc slurry * 10
* Dispersion medium: cyclopentasiloxane (B) water 30
(B) 1,3-BG 5
(B) Methylparaben 0.3
(C) Reverse vesicle solution 10
(C-1) Lecithin 0.7
(C-2) Water 0.3
(C-3) Ethanol 2.0
(C-4) Cyclopentasiloxane 99

A reverse vesicle solution (C) was prepared in the same manner as in Example 11 using (C-1 to 4) in advance. The components of group (A) were uniformly mixed by hand stirring and heated to 80 ° C. What was heated and stirred at 80 degreeC of the component of (B) group was added there, and it emulsified with the homogenizer. When the emulsion was cooled and reached 35 ° C., the emulsion and the previously prepared (C) were mixed by hand stirring.
As a result, a sunscreen cosmetic containing reverse vesicles was produced.

Example 14 Emulsion type foundation (A) Cyclopentasiloxane 24.2
(A) Diphenylsiloxyphenyl trimethicone 10
(A) Polyether-modified silicone 4
(A) Ethylhexyl methoxycinnamate 5
(A) Diethylaminohydroxybenzoyl hexyl benzoate 0.5
(B) Pigment dye (titanium oxide, iron oxide) 10
(C) Organically modified bentonite 1
(D) Water 30
(D) Glycerin 10
(D) Methylparaben 0.3
(E) Reverse vesicle solution 5
(E-1) Lecithin 1.4
(E-2) Water 0.6
(E-3) Ethanol 3
(E-4) Cyclopentasiloxane 98

A reverse vesicle solution (E) was prepared in the same manner as in Example 11 using (E-1 to 4) in advance. The components of group (A) were uniformly mixed by hand stirring and heated to 80 ° C. (B) The component of (B) group is disperse | distributed with a disper to the mixture of the component of (A) group, Then, the component for (C) is disperse | distributed with a disper. Using a homogenizer, the obtained oil phase and (D) group uniformly mixed at 80 ° C. are mixed and emulsified. When the emulsion was cooled and reached 35 ° C., the emulsion and (E) prepared in advance were mixed by hand stirring.
As a result, an emulsified foundation containing a reverse vesicle was produced.

Example 15. Powder Foundation (A) Silicone-treated pigment dye (titanium oxide, iron oxide) 15
(A) Talc 29.7
(A) Mica 10
(A) Fluorine-treated sericite 10
(A) Silica 10
(A) Methyl methacrylate cross polymer 10
(A) Mica titanium 5
(A) Methylparaben 0.3
(B) Reverse vesicle solution 10
(B-1) Lecithin 3
(B-2) Water 0.3
(B-3) Acetone 1
(B-4) Polyoxyethylene alkyl ether 0.3
(B-5) Dimethicone 40
(B-6) Jojoba oil 56.4

A reverse vesicle solution (B) was prepared in the same manner as in Example 1 using (B-1 to 6) in advance. After mixing the components of (A) group and coarsely pulverizing with a pulverizer, (B) was added and mixed with a Henschel mixer. Then, it grind | pulverized again with the pulverizer, and it casted into the metal dish.
As a result, a powder foundation containing reverse vesicles was produced.

<The manufacturing method 2 of a reverse vesicle composition>
(1) Manufacture of reverse vesicle composition The reverse vesicle composition was manufactured with the composition shown in Table 6 by the following method.
That is, for Samples A to D, the bilayer component, water, and squalane were mixed at the ratio shown in Table 4 and heated to the heating temperature shown in Table 4. It was confirmed through the polarizing plate that all of the obtained solutions were isotropic solutions. The number of phases was determined by allowing the sample to stand for a long time while maintaining a constant temperature to obtain an equilibrium state or observing whether the sample had turbidity. Subsequently, the heated solution was allowed to stand in a cooling chamber having a cooling temperature shown in Table 4 and cooled. Each sample was cooled to a temperature at which it transitioned from the isotropic solution to the lamellar phase.
For sample E, after preparing an isotropic solution in which the concentration of the mixture of lecithin and water was twice that of samples A to D, 0 ° C. squalane was finally mixed to the ratio shown in Table 4 did.
Moreover, about the sample F, the mixture of a bilayer membrane component and water was mixed with the oil agent, and this mixed solution was stirred with the vortex mixer.
About the obtained composition, formation of the reverse vesicle was confirmed using the polarization microscope. For those in which the formation of reverse vesicles was confirmed, ◯ was entered, and for those in which the formation of reverse vesicles was not confirmed, x was entered.

As shown in Table 6, the formation of reverse vesicles was confirmed in Samples A to E using the method of heating the mixture of the bilayer component and the oil to prepare an isotropic solution and then cooling it. .
Moreover, it turned out that any of the method of cooling and the method of mixing the cooled oil agent may be sufficient as the method of cooling.
On the other hand, in the sample F using the method of directly mixing the lamella mixture with the oil agent as in the conventional case, the formation of the reverse vesicle was not confirmed.
From this, it turned out that a reverse vesicle composition can be easily prepared by heating the mixture of a bilayer membrane component and an oil agent to prepare an isotropic solution and then cooling it.
In addition, in the prescription of sample F, the present inventors have confirmed that an inverted vesicle composition can be produced by applying a stronger stirring force using an ultrasonic disperser or the like. The production method of the present invention can produce a reverse vesicle composition without requiring a strong stirring force by such an ultrasonic disperser, and is useful in this respect when assuming industrial production. It can be said that there is.
Moreover, when using the oil agent with a larger molecular weight than the oil agent used in the present Example, it is thought that the manufacturing method of this invention becomes very useful.

(2) Particle size of reverse vesicle For samples A and B produced above, the average particle size (median diameter) was measured by Malvern Zetasizer Nano ZS.
As a result, for sample A, the average particle size immediately after production was about 500 nm, while for sample B, the average particle size immediately after production was about 1000 nm.
From this, it was found that a minute reverse vesicle can be produced by rapidly cooling an isotropic solution. At the same time, it was found that the size of the reverse vesicle can be controlled by changing the cooling rate.
About these samples, when it left to stand for one week or more, sedimentation of particles started to be observed, but it was found that they could be easily dispersed as required.

Below, the manufacture example of skin external preparation (cosmetics) is described. A compounding quantity is shown in the mass percentage.
Example 16 Treatment oil lecithin 0.4
Water 0.1
Squalane 69.4
Olive oil 20
Jojoba oil 10
Fragrance 0.1

Each component was mixed and heated to 90 ° C., and then cooled to about room temperature in a 0 ° C. cooling chamber.
As a result, a treatment oil containing a reverse vesicle (reverse vesicle solution) was produced.

Example 17. Cream (A) Dimethicone 31.5
(A) Cyclopentasiloxane
(A) (Dimethicone / Vinyl Dimethicone) Crosspolymer 5
(A) Polyether-modified silicone 2
(A) Sorbitan sesquiisostearate 1
(A) Phenoxyethanol 0.5
(B) Water 30
(B) 1,3-butanediol 10
(C) Reverse vesicle solution 10
(C-1) Lecithin 2
(C-2) Squalane 98

A reverse vesicle solution (C) was prepared in the same manner as in Example 16 using (C-1, 2). The components of group (A) were mixed uniformly, the components of group (B) were mixed, and an emulsion was formed using a homogenizer. Thereafter, the emulsion and (C) prepared in advance were mixed by hand stirring.
As a result, a cream containing reverse vesicles was produced.

Example 18 Sunscreen cosmetics (A) Cyclopentasiloxane 26.7
(A) Polyether-modified silicone 3
(A) 40% hydrophobized fine particle titanium oxide slurry * 15
(A) 40% hydrophobized fine particle zinc slurry * 10
* Dispersion medium: cyclopentasiloxane (B) water 30
(B) 1,3-BG 5
(B) Methylparaben 0.3
(C) Reverse vesicle solution 10
(C-1) Lecithin 0.7
(C-2) Water 0.3
(C-3) Cyclopentasiloxane 19
(C-4) Diphenylsiloxyphenyl trimethicone 80

A reverse vesicle solution (C) was prepared in the same manner as in Example 16 using (C-1 to 4) in advance. The components of group (A) were uniformly mixed by hand stirring and heated to 80 ° C. What was heated and stirred at 80 degreeC of the component of (B) group was added there, and it emulsified with the homogenizer. When the emulsion was cooled and reached 35 ° C., the emulsion and the previously prepared (C) were mixed by hand stirring.
As a result, a sunscreen cosmetic containing reverse vesicles was produced.

Example 19. Emulsion type foundation (A) Cyclopentasiloxane 24.2
(A) Diphenylsiloxyphenyl trimethicone 10
(A) Polyether-modified silicone 4
(A) Ethylhexyl methoxycinnamate 5
(A) Diethylaminohydroxybenzoyl hexyl benzoate 0.5
(B) Pigment dye (titanium oxide, iron oxide) 10
(C) Organically modified bentonite 1
(D) Water 30
(D) Glycerin 10
(D) Methylparaben 0.3
(E) Reverse vesicle solution 5
(E-1) Lecithin 1.4
(E-2) Water 0.6
(E-3) Cyclopentasiloxane 18
(E-4) Diphenylsiloxyphenyl trimethicone 80

A reverse vesicle solution (E) was prepared in the same manner as in Example 16 using (E-1 to 4) in advance. The components of group (A) were uniformly mixed by hand stirring and heated to 80 ° C. (B) The component of (B) group is disperse | distributed with a disper to the mixture of the component of (A) group, Then, the component for (C) is disperse | distributed with a disper. Using a homogenizer, the obtained oil phase and (D) group uniformly mixed at 80 ° C. are mixed and emulsified. When the emulsion was cooled and reached 35 ° C., the emulsion and (E) prepared in advance were mixed by hand stirring.
As a result, an emulsified foundation containing a reverse vesicle was produced.

Example 20. Powder Foundation (A) Silicone-treated pigment dye (titanium oxide, iron oxide) 15
(A) Talc 29.7
(A) Mica 10
(A) Fluorine-treated sericite 10
(A) Silica 10
(A) Methyl methacrylate cross polymer 10
(A) Mica titanium 5
(A) Methylparaben 0.3
(B) Reverse vesicle solution 10
(B-1) Lecithin 3
(B-2) Water 0.3
(B-3) Polyoxyethylene alkyl ether 0.3
(B-4) Cyclopentasiloxane 40
(B-5) Jojoba oil 56.4

A reverse vesicle solution (B) was prepared in the same manner as in Example 16 using (B-1 to 5) in advance. After mixing the components of (A) group and coarsely pulverizing with a pulverizer, (B) was added and mixed with a Henschel mixer. Then, it grind | pulverized again with the pulverizer, and it casted into the metal dish.
As a result, a powder foundation containing reverse vesicles was produced.

The present invention can be applied to the production of cosmetics and foods.

Claims

A reverse vesicle composition containing a reverse vesicle containing lecithin and an oil agent which has a molecular weight of greater than 114 g / mol at 25 ° C.
The reverse vesicle composition according to claim 1, wherein the oil agent is selected from silicone oil, hydrocarbon oil, ester oil, natural animal and vegetable oil, and fluorine oil.
The reverse vesicle composition according to claim 1 or 2, comprising 40% by mass or more of the oil agent.
The reverse vesicle composition according to any one of claims 1 to 3, wherein the reverse vesicle contains water.
The reverse vesicle composition according to claim 4, wherein the content mass of the water is not more than 1 times the mass content of a bilayer constituent component containing lecithin.
A reverse vesicle composition containing a reverse vesicle containing a silicone surfactant and water, and an oil agent liquid at 25 ° C.
7. The silicone surfactant according to claim 6, wherein the silicone surfactant is selected from polyoxyethylene-modified silicone, polyoxypropylene-modified silicone, polyoxyethylene / polyoxypropylene-modified silicone, and polyglycerin-modified silicone. Reverse vesicle composition.
The reverse vesicle composition according to claim 6 or 7, wherein the silicone surfactant has an HLB of 3 to 13.
The reverse vesicle composition according to any one of claims 6 to 8, wherein the oil agent is selected from silicone oil, hydrocarbon oil, ester oil, natural animal and vegetable oil, and fluorine oil.
The reverse vesicle composition according to any one of claims 6 to 9, comprising 40% by mass or more of the oil agent.
The reverse vesicle composition according to any one of claims 6 to 10, wherein the water-containing mass is not more than 1 times the mass of a bilayer constituent component containing a silicone surfactant.
The reverse vesicle composition according to any one of claims 4 to 11, wherein the reverse vesicle contains a water-soluble active ingredient.
The inverse vesicle composition according to any one of claims 1 to 12, which is a non-emulsifying type.
An external preparation for skin comprising the inverse vesicle composition according to any one of claims 1 to 13.
A method for producing a reverse vesicle composition, comprising preparing a mixture by mixing lecithin and a liquid oil component at 25 ° C. having a molecular weight of greater than 114 g / mol, and then shaking or stirring the mixture.
A method for producing a reverse vesicle composition comprising mixing a silicone surfactant, water, and a liquid oil component at 25 ° C. to prepare a mixture, and then shaking or stirring the mixture.
A method for producing a reverse vesicle, comprising recovering the reverse vesicle from the reverse vesicle composition according to any one of claims 1 to 13.
A skin external preparation containing an inverted vesicle produced by the method of producing an inverted vesicle according to claim 17.
Dissolving a bilayer component in a volatile solvent to obtain a first isotropic solution;
Mixing the first isotropic solution with an oil to obtain a second isotropic solution;
Volatilizing the volatile solvent in the second isotropic solution;
Forming a reverse vesicle of the bilayer component by volatilization of a volatile solvent;
A process for producing a reverse vesicle composition comprising:
The method for producing a reverse vesicle composition according to claim 19, wherein the volatile solvent is selected from alcohols, hydrocarbons, aromatics, ketones, ethers, esters, volatile silicone oil, and isoparaffin.
21. The method for producing an inverted vesicle composition according to claim 19 or 20, wherein the first isotropic solution contains water of not more than 1 times the content of the bilayer component.
The production of the reverse vesicle composition according to any one of claims 19 to 21, wherein the second isotropic solution is a two-phase solution in which particles of the first isotropic solution are dispersed in the oil. Method.
The method for producing a reverse vesicle composition according to any one of claims 19 to 22, wherein the volatile solvent is volatilized under reduced pressure.
The reverse vesicle composition according to any one of claims 19 to 23, which is a method for producing a reverse vesicle composition comprising lecithin and a reverse vesicle composition containing a liquid oil having a molecular weight of greater than 114 g / mol at 25 ° C. Production method.
Mixing the bilayer component and the oil and heating to obtain an isotropic solution;
Cooling the isotropic solution;
Forming a reverse vesicle of the bilayer component by the cooling; and
A process for producing a reverse vesicle composition comprising:
26. The method for producing an inverted vesicle composition according to claim 25, wherein the isotropic solution contains water that is not more than 1 times the content of the bilayer component.
The method for producing an inverted vesicle according to claim 25 or 26, wherein the heating is performed up to a temperature at which the bilayer component and the oil form a one-phase isotropic solution.
28. The reverse of claim 27, wherein the oil agent comprises two or more oil agents, and the heating is performed to a temperature at which the bilayer component forms a one-phase isotropic solution with at least one of the oil agents. Vesicle manufacturing method.
The method for producing an inverted vesicle composition according to any one of claims 25 to 28, wherein the cooling is performed by diluting the isotropic solution with a cooling solvent having a temperature lower than that of the isotropic solution.
The method for producing a reverse vesicle composition according to claim 29, wherein the cooling solvent contains the oil agent.
The reverse vesicle composition according to any one of claims 25 to 30, which is a method for producing a reverse vesicle composition comprising lecithin and a reverse vesicle composition containing a liquid oil having a molecular weight of greater than 114 g / mol at 25 ° C. Production method.
The method for producing a reverse vesicle composition according to any one of claims 19 to 31, wherein the oil agent is selected from silicone oil, hydrocarbon oil, ester oil, natural animal and vegetable oil, and fluorine oil.
The method for producing a reverse vesicle composition according to any one of claims 19 to 32, wherein the bilayer component includes lecithin and / or a nonionic surfactant.
A method for producing an external preparation for skin, comprising a step of mixing the reverse vesicle composition produced by the method for producing a reverse vesicle composition according to any one of claims 19 to 33 with other components.