JP2005145881A - Water-in-oil type emulsified composition - Google Patents
Water-in-oil type emulsified composition Download PDFInfo
- Publication number
- JP2005145881A JP2005145881A JP2003385360A JP2003385360A JP2005145881A JP 2005145881 A JP2005145881 A JP 2005145881A JP 2003385360 A JP2003385360 A JP 2003385360A JP 2003385360 A JP2003385360 A JP 2003385360A JP 2005145881 A JP2005145881 A JP 2005145881A
- Authority
- JP
- Japan
- Prior art keywords
- oil
- powder
- water
- silicone
- zinc oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
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- 239000000843 powder Substances 0.000 claims abstract description 219
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- 239000011787 zinc oxide Substances 0.000 claims abstract description 74
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Abstract
Description
本発明は油中水型乳化組成物、特にシリコーン油相に酸化亜鉛複合粉体を配合する組成物の改良に関する。 The present invention relates to an improvement in a water-in-oil emulsified composition, in particular, a composition in which a zinc oxide composite powder is blended with a silicone oil phase.
従来、油中水型乳化組成物には紫外線防御等の目的で酸化亜鉛、二酸化チタン等の粉体が配合されてきた。これらの無機性粉体は通常その表面が親水性であるため、油性基剤中に分散しづらく、そのまま油相に配合することは困難である。また、乳化化粧料とする際、粉体を含む油相部に分散剤を添加し、水相部を加えて乳化すると、粉体と分散剤、水との相互作用により、凝集を生じることがある。この結果、組成物の安定性に問題を生じるとともに、粉体が本来有している機能の発揮にも支障を生じる。 Conventionally, powders such as zinc oxide and titanium dioxide have been blended in water-in-oil emulsion compositions for the purpose of ultraviolet protection and the like. Since these inorganic powders usually have a hydrophilic surface, they are difficult to disperse in an oily base and are difficult to be blended into an oil phase as they are. When emulsified cosmetics, if a dispersant is added to the oil phase part containing the powder and emulsified by adding the water phase part, agglomeration may occur due to the interaction between the powder, the dispersant and water. is there. As a result, a problem is caused in the stability of the composition, and the function of the powder inherently is hindered.
そこで、分散性の向上を目的として、粉体表面に疎水化処理を施し、親油性を高めた粉体（例えばメタケイ酸アルミン酸マグネシウム（特開平１−３０８８１９号）、フッ素変性シリコーン（特開平７−２７７９１４号）等で酸化亜鉛を被覆した複合粉末）を配合した化粧料、あるいは粉体を特定の分散剤とともに油性分散媒中に分散させた化粧料（特開平９−２０８４３８号）等が各種開発されてきた。 Therefore, for the purpose of improving dispersibility, the powder surface is subjected to a hydrophobization treatment to improve the lipophilicity (for example, magnesium aluminate metasilicate (JP-A-1-308819), fluorine-modified silicone (JP-A-7-7 -277794) and the like, and various kinds of cosmetics (JP-A-9-208438) in which powders are dispersed in an oil-based dispersion medium together with a specific dispersant. Has been developed.
しかしながら、上記組成物においては、粉体の油分散性はある程度向上したものの十分とは言えず、特にシリコーン油中への安定な分散はきわめて困難であり、しかも酸化亜鉛表面が処理されてしまうと該酸化亜鉛自体の各種効果を油相中で十分に発揮させることもまた困難であった。
本発明は、前記従来の課題に鑑みなされたもので、粉体のシリコーン油分散性が良好であり、且つ優れた肌荒れ改善・防止効果を有する油中水型乳化組成物を提供することを目的とする。 The present invention has been made in view of the above-described conventional problems, and an object thereof is to provide a water-in-oil emulsion composition having excellent powder silicone oil dispersibility and having an excellent effect of improving and preventing rough skin. And
前記目的を達成するために本発明者らが鋭意検討を行った結果、酸化亜鉛を親油性基粉体上に部分被覆した複合粉体と、特定の分散剤を用いることにより、該複合粉体をシリコーン油相中に安定に配合しえることを見出し、本発明を完成するに至った。
すなわち、本発明にかかる油中水型乳化組成物は、シリコーン油と、水と、分散剤と、前記シリコーン油中に分散する複合粉体と、を含み、
前記複合粉体は、親油性基粉体と、その表面の少なくとも一部分を被覆する酸化亜鉛とを有し、
前記分散剤はシリコーン油中に水を分散し得る非イオン性分散剤からなり、
前記シリコーン油：複合粉体は質量比で１：１〜９９：１であることを特徴とする。
前記組成物において、親油性基粉体は、シリコーン油により膨潤することが好適である。
As a result of intensive studies by the present inventors in order to achieve the above object, a composite powder obtained by partially coating zinc oxide on a lipophilic base powder and a specific dispersant are used. Has been found to be stably blended in the silicone oil phase, and the present invention has been completed.
That is, the water-in-oil emulsion composition according to the present invention includes a silicone oil, water, a dispersant, and a composite powder dispersed in the silicone oil,
The composite powder has a lipophilic base powder and zinc oxide covering at least a part of the surface thereof,
The dispersant comprises a nonionic dispersant capable of dispersing water in silicone oil,
The silicone oil: composite powder has a mass ratio of 1: 1 to 99: 1.
In the composition, the lipophilic base powder is preferably swollen by silicone oil.
また、前記組成物において、分散剤はポリエーテル変性シリコーン及び／又は架橋型ポリエーテル変性シリコーンを含むことが好適である。
また、前記組成物において、シリコーン油は実質的にイオン性分散剤及び／又はイオン性乳化安定剤を含まないことが好適である。
また、クリーム状油中水型乳化組成物とする場合には、水が組成物中３５〜９０質量％含まれることが好適である。
また、クリーム状油中水型乳化組成物の場合には、シリコーン油：複合粉体は質量比で１：１〜１０：１であることが好適である。
また、乳液状油中水型乳化組成物とする場合には、水が組成物中１５〜３５質量％含まれることが好適である。
In the composition, the dispersant preferably contains a polyether-modified silicone and / or a cross-linked polyether-modified silicone.
In the composition, it is preferable that the silicone oil does not substantially contain an ionic dispersant and / or an ionic emulsion stabilizer.
Moreover, when setting it as a cream-like water-in-oil emulsion composition, it is suitable that 35-90 mass% of water is contained in a composition.
In the case of a creamy water-in-oil emulsion composition, it is preferable that the silicone oil: composite powder has a mass ratio of 1: 1 to 10: 1.
Moreover, when setting it as a water-in-oil emulsion type emulsion composition, it is suitable that 15-35 mass% of water is contained in a composition.
また、前記組成物において、親油性基粉体のζ電位が、皮膚上のｐＨにおいて−１０ｍＶ以下であることが好適である。
また、前記組成物において、親油性基粉体が、有機粉体であることが好適である。
また、前記組成物において、親油性基粉体が、シリコーン樹脂、シリコーンゴム、シリコーン樹脂被覆シリコーンゴム、ポリアミド、ポリメチルメタクリレート、カルバミド酸エチルからなる群より選択される１種又は２種以上で形成されることが好適である。
In the composition, it is preferable that the lipophilic base powder has a ζ potential of −10 mV or less at the pH on the skin.
In the composition, it is preferable that the lipophilic base powder is an organic powder.
In the composition, the lipophilic base powder is formed of one or more selected from the group consisting of silicone resin, silicone rubber, silicone resin-coated silicone rubber, polyamide, polymethyl methacrylate, and ethyl carbamate. It is preferred that
本発明にかかる油中水型乳化組成物は、親油性基粉体の表面に酸化亜鉛を被覆し、特定の分散剤を用いることにより、粉体表面に酸化亜鉛が存在するにもかかわらず安定な系を維持することができる。 The water-in-oil emulsion composition according to the present invention is stable even when zinc oxide is present on the powder surface by coating the surface of the lipophilic base powder with zinc oxide and using a specific dispersant. Can be maintained.
本発明者らはシリコーン油中水型乳化組成物中の外相（シリコーン油）中に酸化亜鉛を有効に配合する技術について検討した。この過程で親油性基粉体に酸化亜鉛を部分被覆した複合粉体が優れたシリコーン油中への分散性を有するとともに、酸化亜鉛の有する各種効果を効率的に発揮しえること、一方で経時安定性には問題を残すことを見出した。
すなわち、酸化亜鉛を親油性基粉体に部分被覆した複合粉体は、後述するように優れた肌荒れ改善・防止効果を奏するが、この複合粉体をシリコーン油相に配合して油中水型乳化組成物を調製すると系の経時安定性が著しく低下する場合があることが明らかになった。
The present inventors examined a technique for effectively blending zinc oxide in the outer phase (silicone oil) in the water-in-silicone emulsion composition. In this process, the composite powder in which zinc oxide is partially coated on the lipophilic base powder has excellent dispersibility in silicone oil and can effectively exhibit various effects of zinc oxide. We have found that stability remains a problem.
That is, a composite powder in which zinc oxide is partially coated on an oleophilic base powder has an excellent effect of improving and preventing rough skin as described later, but this composite powder is blended with a silicone oil phase to form a water-in-oil type. It has been found that when an emulsion composition is prepared, the stability over time of the system may be significantly reduced.
（表１）
試 験 例
１−１ １−２ １−３
シリコーン油（＊１） ２０．０ ２０．０ ２０．０
直鎖型ポリエーテル変性シリコーン ５．０ ２．５ ２．５
有機変性粘土鉱物 − ２．５ ２．５
水 ７０．０ ７０．０ ７０．０
複合粉体（＊２） − − ５．０
親油性基粉体（＊３）のみ ５．０ ５．０ −
評価
調製時 ○ ○ ○
１週間経過時 △ ○ ×
（＊１）：ジメチルポリシロキサン（２０ｃｐ）
（＊２）：酸化亜鉛１７％被覆球状シリコーンゴム
（＊３）：球状シリコーンゴム
(Table 1)
Test example
1-1 1-2 1-3
Silicone oil (* 1) 20.0 20.0 20.0
Linear polyether-modified silicone 5.0 2.5 2.5
Organically modified clay mineral-2.5 2.5
Water 70.0 70.0 70.0
Composite powder (* 2)--5.0
Lipophilic base powder (* 3) only 5.0 5.0-
Evaluation Preparation ○ ○ ○
1 week △ ○ ×
(* 1): Dimethylpolysiloxane (20 cp)
(* 2): Zinc oxide 17% coated spherical silicone rubber (* 3): Spherical silicone rubber
前記表１より明らかなように、通常の球状シリコーンゴムをシリコーン油に配合し油中水型乳化組成物を調製する場合（試験例１−１）、経時安定性が若干悪い。これに対し、有機変性粘土鉱物(乳化安定剤)をシリコーン相に加えた場合（試験例１−２）には、経時安定性が大幅に改善される。
しかしながら、このような安定性が改善された油中水型乳化組成物において、粉末を酸化亜鉛被覆球状シリコーンゴムとすると経時安定性が著しく低下する傾向が認められた。
そこで本発明者らは、分散剤ないし経時安定剤についてさらに検討を行った。
As is apparent from Table 1, when a normal spherical silicone rubber is blended with silicone oil to prepare a water-in-oil emulsion composition (Test Example 1-1), the stability over time is slightly poor. On the other hand, when an organically modified clay mineral (emulsification stabilizer) is added to the silicone phase (Test Example 1-2), the temporal stability is greatly improved.
However, in such a water-in-oil emulsified composition with improved stability, when the powder was made of zinc oxide-coated spherical silicone rubber, a tendency that the stability over time was remarkably lowered was observed.
Therefore, the present inventors have further investigated a dispersant or a aging stabilizer.
（表２）
試 験 例
2-1 2-2 2-3 2-4 2-5 2-6 2-7 2-8
シリコーン油
ジメチルポリシロキサン 20 20 20 20 20 20 20 20
直鎖型ポリエーテル変性シリコーン
5 − − − − − − −
架橋型ポリエーテル変性シリコーン
− 5 − 2.5 2.5 2.5 2.5 2.5
直鎖型：架橋型＝１：１ − − 5 − − − − −
有機変性粘土鉱物 − − − 2.5 − − 1.0 −
脂肪酸石鹸 − − − − 2.5 − − 1.0
グリセリン脂肪酸エステル − − − − − 2.5 1.5 1.5
複合粉体（＊２） 5 5 5 5 5 5 5 5
水 70 70 70 70 70 70 70 70
評価
調製時 ○ ○ ○ ○ ○ ○ ○ ○
１週間経過時 △ ○ ○ × × ○ × ×
(Table 2)
Test example
2-1 2-2 2-3 2-4 2-5 2-6 2-7 2-8
Silicone oil
Dimethylpolysiloxane 20 20 20 20 20 20 20 20
Linear polyether-modified silicone
5-------
Cross-linked polyether-modified silicone
− 5 − 2.5 2.5 2.5 2.5 2.5
Linear type: Cross-linked type = 1: 1 − − 5 − − − − −
Organically modified clay mineral − − − 2.5 − − 1.0 −
Fatty acid soap----2.5--1.0
Glycerin fatty acid ester-----2.5 1.5 1.5
Composite powder (* 2) 5 5 5 5 5 5 5 5
Water 70 70 70 70 70 70 70 70
Evaluation During preparation ○ ○ ○ ○ ○ ○ ○ ○
At the end of a week △ ○ ○ × × ○ × ×
上記表２より明らかなように、親水基を有するポリエーテル変性シリコーンは、他の分散剤を添加しなくても比較的安定な油中水型乳化組成物を調製できるが、直鎖型と架橋型を比較すると架橋型のほうがより安定である（試験例２−１〜２−３）。 As is clear from Table 2 above, the polyether-modified silicone having a hydrophilic group can prepare a relatively stable water-in-oil emulsion composition without adding other dispersant, When the types are compared, the cross-linked type is more stable (Test Examples 2-1 to 2-3).
一方、複合粉体を配合しない場合に、より安定な油中水型乳化組成物の調製に寄与する乳化安定剤（有機変性粘土鉱物、脂肪酸石鹸）の配合は、複合粉体を配合した場合にはむしろ安定性を阻害するものとなる（試験例２−４〜２−５）。この点についてさらに検討したところ、イオン性分散剤ないし乳化安定剤の配合時に著しく安定性が低下する傾向にあり、非イオン性分散剤ないし乳化安定剤（グリセリン脂肪酸エステル）の配合は安定性を阻害することはなく、安定性を改善する傾向にあるものも多いことがわかった。
粉末が非被覆のシリコーン粉体の場合には、このようなイオン性ないし非イオン性に依存した相違は認められず、この場合にはイオン性乳化安定剤でも効果が十分に発揮される。複合粉体において安定性が阻害される原因についてはいまだ不明な点も多いが、複合粉体表面に酸化亜鉛が存在しており、この酸化亜鉛の溶出等により有機変性粘土鉱物、脂肪酸石鹸などの状態に何らかの影響を与えるものと考えられる。
さらに本発明者らは親油性基粉体の膨潤性と乳化安定性について検討を行った。結果を表３に示す。
On the other hand, when the composite powder is not blended, the emulsion stabilizer (organic modified clay mineral, fatty acid soap) that contributes to the preparation of a more stable water-in-oil emulsion composition is blended with the composite powder. Rather, it will inhibit the stability (Test Examples 2-4 to 2-5). Further examination of this point shows that the stability tends to decrease significantly when ionic dispersants or emulsion stabilizers are added, and the addition of nonionic dispersants or emulsion stabilizers (glycerin fatty acid esters) inhibits stability. It has been found that there are many that tend to improve stability.
When the powder is an uncoated silicone powder, such differences depending on ionicity or nonionicity are not observed, and in this case, the effect is sufficiently exhibited even with an ionic emulsion stabilizer. Although there are still many unclear points about the reason why the stability of composite powder is hindered, zinc oxide is present on the surface of the composite powder. Due to elution of this zinc oxide, organically modified clay minerals, fatty acid soaps, etc. It is considered to have some influence on the state.
Furthermore, the present inventors examined the swelling property and emulsion stability of the lipophilic base powder. The results are shown in Table 3.
（表３）
試 験 例
３−１ ３−２
シリコーン油 ２０．０ ２０．０
架橋型ポリエーテル変性シリコーン ５．０ ５．０
水 ７０．０ ７０．０
複合粉体（膨潤性） ５．０ −
複合粉体（非膨潤性） − ５．０
評価
調製時 ○ ○
１週間経過時 ○ △
(Table 3)
Test example
3-1 3-2
Silicone oil 20.0 20.0
Cross-linked polyether-modified silicone 5.0 5.0
Water 70.0 70.0
Composite powder (swellability) 5.0-
Composite powder (non-swelling) -5.0
Evaluation Preparation ○ ○
At the end of one week ○ △
表３より明らかなように、同様のシリコーン粉体を親油性基粉体として用いた場合にも、膨潤性の方が非膨潤性よりも、優れた乳化安定性を示す。これは、外相であるシリコーン相中で複合粉体が膨潤し、一種の増粘安定化剤として機能するためと思われる。
さらに本発明者らは、油中水型乳化組成物の組成と剤型の関係について検討を行った。
この結果を図１に三相図として示す。
As is clear from Table 3, also when the same silicone powder is used as the lipophilic base powder, the swelling property exhibits better emulsion stability than the non-swelling property. This is presumably because the composite powder swells in the silicone phase, which is the outer phase, and functions as a kind of thickening stabilizer.
Furthermore, the present inventors examined the relationship between the composition and dosage form of a water-in-oil emulsion composition.
The result is shown as a three-phase diagram in FIG.
同図より明らかなように、シリコーン油／複合粉体＝１／１以上で安定な乳化系が得られ、複合粉体の肌荒れ防止・改善効果を期待する観点から少なくとも９９／１程度の割合で複合粉体を配合することが好ましい。１／１以下であると複合粉体の基粉体であるシリコーン粉体によりシリコーン油の吸収を生じ、ボソボソとした固形状となり、シリコーン油による連続相(外相)を形成するのが困難となる。
また、内相である水の配合量は１５〜３５質量％／組成物で流動性を有する乳液状となり、３５〜９０質量％／組成物で流動性の低い(５０００ｃｐｓ以上)クリームとなる。
クリーム状油中水型乳化組成物の場合には、シリコーン油：複合粉体は質量比で１：１〜１０：１であることが好適である。
As is clear from the figure, a stable emulsification system can be obtained when silicone oil / composite powder is 1/1 or more, and at a ratio of at least about 99/1 from the viewpoint of expecting the effect of preventing and improving rough skin of the composite powder. It is preferable to blend a composite powder. If it is 1/1 or less, the silicone powder that is the base powder of the composite powder absorbs the silicone oil and becomes a solid solid, making it difficult to form a continuous phase (outer phase) with the silicone oil. .
The amount of water as the inner phase is 15 to 35% by mass / composition of milk having fluidity, and 35 to 90% by mass / composition of cream having low fluidity (5000 cps or more).
In the case of a creamy water-in-oil emulsion composition, the silicone oil: composite powder is preferably 1: 1 to 10: 1 by weight.
＜複合粉体＞
肌荒れ改善・防止効果について
近年肌荒れや角化異常を伴う種々の皮膚疾患の病像形成には、プロテアーゼ、特にプラスミンやプラスミノーゲンアクチベーターといった線溶系酵素の活性変化が深く関与していることが明らかにされつつある。例えば実験的に肌荒れを起こした表皮細胞層ではプラスミンの分布に変化が認められ、肌荒れの防止・改善に抗プラスミン剤が有効であることが報告されている（Kenji kitamura:J.Soc.Cosmet.Chem.Jpn;29(2),1995）。プラスミノーゲンアクチベーターはプラスミンの前駆体であるプラスミノーゲンに特異的に働いて、それを活性なプラスミンに変換するプロテアーゼである。
<Composite powder>
Skin Roughness Improvement / Prevention Effect Changes in the activity of proteases, particularly fibrinolytic enzymes such as plasmin and plasminogen activator, are deeply involved in the pathogenesis of various skin diseases with rough skin and abnormal keratinization in recent years. It is being revealed. For example, in the epidermal cell layer that caused experimental rough skin, changes in the distribution of plasmin were observed, and it has been reported that anti-plasmin agents are effective in preventing and improving rough skin (Kenji kitamura: J. Soc. Cosmet. Chem. Jpn; 29 (2), 1995). Plasminogen activator is a protease that specifically acts on plasminogen, the precursor of plasmin, and converts it to active plasmin.
また、アトピー性皮膚炎においても表皮中に高い線溶活性が認められている（T.Lotti:Department of Dermatology;28(7),1989）。さらに、炎症性異常角化性疾患の代表である乾癬では、その患部表皮の錯角化部位に強いプラスミノーゲンアクチベーター活性が存在すること（Haustein:Arch.Klin.Exp.Dermatol;234,1969）や、乾癬鱗屑から高濃度の塩溶液を用いてプラスミノーゲンアクチベーターを抽出したという報告(Fraki,Hopsu-Havu:Arch.Dermatol.Res;256,1976)がなされている。
本発明において特徴的な複合粉体は、プラスミノーゲンアクチベーターを吸着する親油性基粉体と、該プラスミノーゲンアクチベーターの活性を阻害する亜鉛イオンを溶出する酸化亜鉛との複合粉体であるため、肌荒れ改善・防止効果に優れている。
In addition, high fibrinolytic activity is also observed in the epidermis in atopic dermatitis (T. Lotti: Department of Dermatology; 28 (7), 1989). Furthermore, in psoriasis, which is representative of inflammatory abnormal keratotic diseases, strong plasminogen activator activity exists at the complexed keratinized site of the affected skin (Haustein: Arch.Klin.Exp.Dermatol; 234,1969) There are reports that plasminogen activator was extracted from psoriasis scales using a high-concentration salt solution (Fraki, Hopsu-Havu: Arch. Dermatol. Res; 256, 1976).
The composite powder characteristic in the present invention is a composite powder of a lipophilic base powder that adsorbs plasminogen activator and zinc oxide that elutes zinc ions that inhibit the activity of the plasminogen activator. Therefore, it is excellent in improving and preventing rough skin.
酸化亜鉛
本発明にかかる複合粉体において、酸化亜鉛は亜鉛イオンを溶出し、プラスミノーゲンアクチベーターを不活化する。
下記表４に、イオン濃度１００ｐｐｍにおける各種イオンのウロキナーゼ（ＵＫ）阻害率を示す。ＵＫはプラスミノーゲンアクチベーターの一種である。
Zinc Oxide In the composite powder according to the present invention, zinc oxide elutes zinc ions and inactivates plasminogen activator.
Table 4 below shows urokinase (UK) inhibition rates of various ions at an ion concentration of 100 ppm. UK is a type of plasminogen activator.
（ＵＫ活性阻害率の測定方法）
試料懸濁水２０μLにTris-HCl buffer(ｐＨ７．５)を加えて全量を１８０μＬとし、ここに３００Ｕ／ｍＬの活性型ＵＫ２０μＬを添加して室温に放置する。３０分後、ＵＫの特異的な合成基質であるＳ２４４４（CHROMOGENIX）を２０μＬ添加し、さらに３７℃恒温器に３０分放置する。その後１２％のトリクロロ酢酸水溶液２０μＬを添加して反応を停止させた上で、試料粉末をろ過し、ろ液の４０５ｎｍ吸光度を測定して評価系中のＵＫ活性を求め、さらに試料によるＵＫ活性阻害率を算出する。
(Measurement method of UK activity inhibition rate)
Tris-HCl buffer (pH 7.5) is added to 20 μL of sample suspension to make a total volume of 180 μL, and 20 μL of 300 U / mL active UK is added thereto and left at room temperature. After 30 minutes, 20 μL of UK specific synthetic substrate S2444 (CHROMOGENIX) is added, and further left in a 37 ° C. incubator for 30 minutes. Thereafter, 20 μL of 12% trichloroacetic acid aqueous solution was added to stop the reaction, the sample powder was filtered, the 405 nm absorbance of the filtrate was measured to determine the UK activity in the evaluation system, and the sample inhibited the UK activity. Calculate the rate.
（表４）
試料 UK活性阻害率(%)
Ｚｎ2+ ５２
Ｚｒ4+ ４５
Ｃｕ2+ ３６
Ｎｉ2+ ３０
Ｃｏ2+ ２７
Ａｌ3+ １６
Ｃｅ3+ ５
Ｎａ+、Ｌｉ+、Ｋ+、Ｍｎ2+、Ｂａ2+、Ｍｇ2+、Ｂａ2+、Ｃａ2+ ０
(Table 4)
Sample UK activity inhibition rate (%)
Zn2 + 52
Zr4 + 45
Cu2 + 36
Ni2 + 30
Co2 + 27
Al3 + 16
Ce3 + 5
Na +, Li +, K +, Mn2 +, Ba2 +, Mg2 +, Ba2 +, Ca2 + 0
表４より明らかなように、亜鉛イオンには最も優れたＵＫ阻害作用が認められた。このことから、各イオンの酵素への作用には高い特異性があることが認められる。
本発明において、複合粉体はシリコーン相に分散しているが、化粧料中においては水相と接触するため、酸化亜鉛から亜鉛イオンが溶出し、プラスミノーゲンアクチベーター阻害作用を発揮することができる。
また、本発明において、酸化亜鉛の平均粒子径は特に制限されないが、０．０１〜５００μｍであることが好適である。
As is clear from Table 4, the most excellent UK inhibitory action was observed for zinc ions. From this, it is recognized that the action of each ion on the enzyme has high specificity.
In the present invention, the composite powder is dispersed in the silicone phase, but in cosmetics it comes into contact with the aqueous phase, so that zinc ions are eluted from zinc oxide and exert a plasminogen activator inhibitory action. it can.
In the present invention, the average particle diameter of zinc oxide is not particularly limited, but is preferably 0.01 to 500 μm.
親油性基粉体
本発明にかかる複合粉体において、ζ電位が正の値であるプラスミノーゲンアクチベーターを吸着するために、親油性基粉体のζ電位は、皮膚上のｐＨにおいて負の値、特に−１０ｍＶ以下であることが好適である。
液中で粉体が電荷を持つ時、この電荷を打ち消すため反対の電荷のイオンが静電力で粉体にひきつけられ電気二重層ができる。二重層の最も外側の電位がζ電位である。よって、ζ電位は対象物の表面荷電状態の評価に好適に用いられ、酵素を電気的に吸着する能力の評価を行うことができる。
Lipophilic base powder In the composite powder according to the present invention, in order to adsorb plasminogen activator having a positive ζ potential, the ζ potential of the lipophilic base powder is negative at the pH on the skin. The value, particularly -10 mV or less is preferred.
When the powder has a charge in the liquid, ions of the opposite charge are attracted to the powder by electrostatic force to cancel this charge, and an electric double layer is formed. The outermost potential of the double layer is the ζ potential. Therefore, the ζ potential is suitably used for evaluating the surface charge state of the object, and the ability to electrically adsorb the enzyme can be evaluated.
ζ電位は、通常スモルコフスキーの公式 ζ電位＝４πηＵ／ε（η：溶媒の粘度 Ｕ：電気泳動易動度 ε：溶媒の誘電率）より求められる。
ζ電位を求めるためには、電気泳動法によりコロイド粒子の速度（Ｖ）、及び電気泳動易動度（Ｕ)を求める。帯電しているコロイド粒子に電場（Ｅ）をかけると粒子が移動する。Ｖ＝Ｌ／ｔ（Ｌ：移動距離 ｔ：時間）、Ｕ＝Ｖ／Ｅで得られる。
The ζ potential is usually obtained from the Smolkovsky formula ζ potential = 4πηU / ε (η: viscosity of solvent U: electrophoretic mobility ε: dielectric constant of solvent).
In order to obtain the ζ potential, the velocity (V) and mobility (U) of the colloidal particles are obtained by electrophoresis. When an electric field (E) is applied to the charged colloidal particles, the particles move. V = L / t (L: moving distance t: time), U = V / E.
（ζ電位の測定方法）
ｐＨ７．５のＴｒｉｓ−ＨＣｌ buffer中に試料を分散・超音波処理した後、測定に用いた。ζ電位は大塚電子株式会社製の電気泳動光散乱光度計ＬＥＺＡ−６００を用いて測定する。測定は３回行い、結果はその平均値で表す。
ｐＨ７．５における各物質のζ電位と、濃度１００ｐｐｍにおけるＵＫの吸着率との関係を下記表５に示す。
(Measurement method of zeta potential)
The sample was dispersed and sonicated in pH 7.5 Tris-HCl buffer, and used for measurement. The zeta potential is measured using an electrophoretic light scattering photometer LEZA-600 manufactured by Otsuka Electronics Co., Ltd. The measurement is performed three times, and the result is expressed as an average value.
The relationship between the ζ potential of each substance at pH 7.5 and the adsorption rate of UK at a concentration of 100 ppm is shown in Table 5 below.
（ＵＫ吸着率の測定方法）
試料懸濁水２０μＬにTris-HCl buffer(ｐＨ７．５)を加えて全量を１８０μＬとし、ここに１０μｇ／ｍＬの前駆体型ＵＫ２０μＬを添加して室温で５分間放置する。その後試料粉末をろ過し、ろ液を回収する。さらに一定量のTris-HCl bufferにて粉末を十分に洗浄し、ろ液と洗浄液を合わせ、これを未吸着ＵＫ溶液とした。TintEliza uPA（biopool）を用い、ELISA法にて未吸着ＵＫ溶液中のＵＫ濃度を求め、その値から試料粉末に吸着されたＵＫ量を算出し、ＵＫ吸着率を求める。
(Measurement method of UK adsorption rate)
Tris-HCl buffer (pH 7.5) is added to 20 μL of sample suspension to make the total volume 180 μL, and 20 μL of 10 μg / mL precursor type UK is added thereto and left at room temperature for 5 minutes. Thereafter, the sample powder is filtered and the filtrate is recovered. Further, the powder was sufficiently washed with a fixed amount of Tris-HCl buffer, and the filtrate and the washing solution were combined to make an unadsorbed UK solution. Using TintEliza uPA (biopool), determine the UK concentration in the unadsorbed UK solution by ELISA, calculate the amount of UK adsorbed on the sample powder from that value, and determine the UK adsorption rate.
（表５）
試料 ζ電位（mV） UK吸着率(％)
ポリアミド（ナイロンＳＰ５００ＴＭ） −32.0 34
ポリメチルメタクリレート（ガンツパールＴＭ） −18.0 42
シリコーン樹脂（トスパール１４５ＡＴＭ） −14.0 30
シリコーンゴム（トレフィルＥ５０６ＷＴＭ） −12.0 18
シリコーン樹脂被覆シリコーンゴム（ＫＳＰ１００ＴＭ） −14.0 30
カルバミド酸エチル（プラスチックパウダーＤ４００ＴＭ） −13.0 27
セルロース（セルロフローＣ−２５ＴＭ） − 2.0 21
ポリエチレン（フローセンＵＦ ＴＭ ） ＋ 1.0 10
(Table 5)
Sample ζ potential (mV) UK adsorption rate (%)
Polyamide (Nylon SP500 TM ) −32.0 34
Polymethylmethacrylate (Gantz Pearl TM ) -18.0 42
Silicone resin (Tospearl 145A TM ) -14.0 30
Silicone rubber (Trefill E506W TM ) -12.0 18
Silicone resin coated silicone rubber (KSP100 ™ ) -14.0 30
Ethyl carbamate (plastic powder D400 TM ) -13.0 27
Cellulose (Celluloflow C-25 TM )-2.0 21
Polyethylene (Flocene UF TM ) + 1.0 10
表５より明らかなように、必ずしも比例関係にはならないものの、ζ電位が低いほどＵＫ吸着率が高い傾向があり、ζ電位とＵＫ吸着率には関連性があることが示された。
よって、本発明における親油性基粉体のζ電位は、皮膚上のｐＨにおいて負の値、特に−１０ｍＶ以下を示すことが好適である。好適な親油性基粉体としては、シリコーン樹脂、シリコーンゴム、シリコーン樹脂被覆シリコーンゴム、ポリアミド、ポリメチルメタクリレート、カルバミド酸エチル等が挙げられるが、ζ電位は様々な条件によって変化するものであり、物質により一定なものではない。
As is clear from Table 5, although not necessarily in a proportional relationship, the lower the ζ potential, the higher the UK adsorption rate tends to be, indicating that the ζ potential and the UK adsorption rate are related.
Therefore, the ζ potential of the lipophilic base powder in the present invention is preferably a negative value, particularly −10 mV or less, at the pH on the skin. Suitable lipophilic base powders include silicone resin, silicone rubber, silicone resin-coated silicone rubber, polyamide, polymethyl methacrylate, ethyl carbamate, etc., and the ζ potential varies depending on various conditions, It is not constant depending on the substance.
これらの親油性基粉体の形状は特に制限されるものではなく、一般的には球状、板状又は不定形状であり、また多孔性であっても多孔性でなくてもよい。親油性基粉体が球状である場合には、特に光拡散効果及び使用感に優れたものとなるためより好適である。平均粒子径は特に制限されないが、０．０１〜５００μｍであることが好適である。
本発明にかかる複合粉体においては、酸化亜鉛由来の亜鉛イオンの、プラスミノーゲンアクチベーター活性阻害効果が、該プラスミノーゲンアクチベーターを吸着する親油性基粉体の存在でさらに向上する。
The shape of these lipophilic base powders is not particularly limited, and is generally spherical, plate-like, or indefinite, and may be porous or not porous. In the case where the lipophilic base powder is spherical, it is more preferable because it becomes particularly excellent in light diffusion effect and usability. The average particle size is not particularly limited, but is preferably 0.01 to 500 μm.
In the composite powder according to the present invention, the plasminogen activator activity inhibitory effect of zinc ions derived from zinc oxide is further improved by the presence of the lipophilic base powder that adsorbs the plasminogen activator.
酸化亜鉛のみが存在する場合、特定酵素を十分に阻害するためには、高濃度の亜鉛イオンが必要となり、化粧料に配合するにあたっては、製剤構築上好ましくない場合がある。
しかしながら、酸化亜鉛と親油性基粉体との複合粉体である場合は、基粉体がプラスミノーゲンアクチベーターを吸着するため、亜鉛イオンが該プラスミノーゲンアクチベーターに作用しやすく、亜鉛イオンが低濃度であっても、効果的にプラスミノーゲンアクチベーターの活性阻害効果を発揮することができる。
When only zinc oxide is present, a high concentration of zinc ions is required in order to sufficiently inhibit a specific enzyme, which may be unfavorable for formulation construction when blended into cosmetics.
However, in the case of a composite powder of zinc oxide and lipophilic base powder, since the base powder adsorbs the plasminogen activator, the zinc ion tends to act on the plasminogen activator, and the zinc ion Even at a low concentration, plasminogen activator activity inhibitory effect can be exhibited effectively.
酸化亜鉛と親油性基粉体を別々に化粧料に配合した場合にも、各粉体単独よりもわずかに高い効果を発揮することがあるが、これらの複合粉体を用いた場合に極めて高いプラスミノーゲンアクチベーター阻害効果が認められる。
なお、参考としてプラスミノーゲンアクチベーターと同じセリンプロテアーゼに分類されるトリプシンについても検討したところ、トリプシンは複合粉体に吸着されるものの、活性はほとんど失われなかった。すなわち本発明の複合粉体は非特異的に酵素活性を阻害するものではない。
Even when zinc oxide and lipophilic base powder are blended separately in cosmetics, the effect may be slightly higher than each powder alone, but extremely high when these composite powders are used. A plasminogen activator inhibitory effect is observed.
For reference, trypsin, which is classified into the same serine protease as plasminogen activator, was also examined. Although trypsin was adsorbed to the composite powder, activity was hardly lost. That is, the composite powder of the present invention does not inhibit enzyme activity nonspecifically.
プラスミノーゲンアクチベーターには、ウロキナーゼと組織型プラスミノーゲンアクチベーターと呼ばれる２種類があり、前者は健常な表皮で、後者は主に病的な表皮においてその存在が認められている。
本発明の複合粉体は、この両方のプラスミノーゲンアクチベーターに対し吸着・阻害作用を有するものに代表される。
There are two types of plasminogen activators, called urokinase and tissue-type plasminogen activator, the former being found in healthy epidermis and the latter being found mainly in pathological epidermis.
The composite powder of the present invention is typified by those having an adsorption / inhibition action on both plasminogen activators.
複合化
酸化亜鉛は親水性であるため、酸化亜鉛粉末単独では、油相中に分散しづらく、凝集が起きる。本発明の複合粉体においては、特定の条件で、酸化亜鉛を親油性基粉体に被覆しているため、油相分散性が良好である。以下に具体的な実施形態を説明する。
Since the composite zinc oxide is hydrophilic, the zinc oxide powder alone is difficult to disperse in the oil phase and causes aggregation. In the composite powder of the present invention, the oil phase dispersibility is good because zinc oxide is coated on the lipophilic base powder under specific conditions. Specific embodiments will be described below.
複合化方法１
親油性基粉体（１２）全表面積に対する酸化亜鉛（１４）の被覆率が、１〜９０％である複合粉体（図２（Ａ））。
被覆率が９０％を超えると、親油性が十分でなくなり、油分散性が悪くなることがある。さらに親油性基粉体によるプラスミノーゲンアクチベーター吸着効果が十分でないことがある。
被覆率が１％未満であると、亜鉛イオンによるプラスミノーゲンアクチベーター活性阻害効果が十分発揮されないことがある。
よって、好ましい被覆率は１〜９０％である。
Compounding method 1
Lipophilic base powder (12) Composite powder having a coverage of zinc oxide (14) with respect to the total surface area of 1 to 90% (FIG. 2 (A)).
If the coverage exceeds 90%, the lipophilicity may not be sufficient and the oil dispersibility may deteriorate. Furthermore, the plasminogen activator adsorption effect by the lipophilic base powder may not be sufficient.
If the coverage is less than 1%, the effect of inhibiting plasminogen activator activity by zinc ions may not be sufficiently exhibited.
Therefore, a preferable coverage is 1 to 90%.
複合化方法２
親油性基粉体（１２）が膨潤性であり、油分散時に、膨潤した親油性基粉体（１２）全表面積に対する酸化亜鉛（１４）の被覆率が、１〜９０％である複合粉体（図２（Ｂ））。
粉体乾燥時に、基粉体全表面積に対する酸化亜鉛の被覆率が９０％を超えている場合でも、親油性基粉体が膨潤性である場合、油分散時に、膨潤した状態で、基粉体全表面積に対する酸化亜鉛の被覆率が１〜９０％であれば、良好な油分散性、及び肌荒れ改善・防止効果を示す。
なお、ここでいう被覆率とは表面積に対するものであり、質量に対するものではない。
Compounding method 2
Composite powder in which lipophilic base powder (12) is swellable, and the coverage of zinc oxide (14) with respect to the total surface area of swollen lipophilic base powder (12) during oil dispersion is 1 to 90% (FIG. 2 (B)).
Even when the coverage of zinc oxide with respect to the total surface area of the base powder exceeds 90% when the powder is dried, if the lipophilic base powder is swellable, the base powder is in a swollen state when dispersed in oil. If the coverage of zinc oxide with respect to the total surface area is 1 to 90%, good oil dispersibility and an effect of improving and preventing rough skin are exhibited.
Note that the coverage here refers to the surface area, not the mass.
膨潤性の親油性基粉体としては、シリコーンゴム、シリコーン樹脂被覆シリコーンゴム等が挙げられるが、これらの粉体においても、膨潤性を持つかどうかは架橋度等の条件による。
膨潤性の親油性基粉体は、硬度が１〜８０であることが好ましく、さらに好ましくは１〜５０である。硬度が８０を超えると膨潤性とならない。また、硬度が１未満である粉体は、それ自体製造することができない。
なお本発明において硬度は、スプリング式かたさ試験Ａ形（ＪＩＳ Ｋ６３０１）において測定した値とする。
Examples of the swellable lipophilic base powder include silicone rubber and silicone resin-coated silicone rubber, and these powders also have swelling properties depending on conditions such as the degree of crosslinking.
The swelling lipophilic base powder preferably has a hardness of 1 to 80, more preferably 1 to 50. If the hardness exceeds 80, it does not become swellable. Also, a powder having a hardness of less than 1 cannot be produced by itself.
In the present invention, the hardness is a value measured by a spring type hardness test type A (JIS K6301).
スプリング式かたさ試験（Ａ形）
スプリング式かたさ試験機（Ａ形）を垂直に保ち、押針が試験片（厚さ１２ｍｍ以上）の測定面に垂直になるように加圧面を接触させ、試験片のかたさを求める。
親油性基粉体と酸化亜鉛との平均粒子径の比は、特に制限されないものの、親油性基粉体：酸化亜鉛＝１：１〜１００００：１、特に親油性基粉体：酸化亜鉛＝５：１〜１０００：１であることが好適である。酸化亜鉛が上記比よりも相対的に小さいと、親油性基粉体の表面を完全に被覆してしまう傾向があるため、油分散性、及びプラスミノーゲンアクチベーター吸着効果が悪くなることがある。また、酸化亜鉛が上記比よりも相対的に大きいと、親油性基粉体を被覆しづらくなる。
Spring hardness test (A type)
A spring type hardness tester (type A) is kept vertical, the pressure surface is brought into contact with the measurement surface of the test piece (
The ratio of the average particle diameter of the lipophilic base powder and zinc oxide is not particularly limited, but the lipophilic base powder: zinc oxide = 1: 1 to 10000: 1, particularly the lipophilic base powder: zinc oxide = 5. : It is suitable that it is 1-1000: 1. If the zinc oxide is relatively smaller than the above ratio, the oil dispersibility and the plasminogen activator adsorption effect may be deteriorated because the surface of the lipophilic base powder tends to be completely covered. . Moreover, when zinc oxide is relatively larger than the above ratio, it becomes difficult to coat the lipophilic base powder.
本発明において、酸化亜鉛と親油性基粉体は、単に混合されているのではなく、複合化されていることが必要である。本発明にかかる複合粉体は、酸化亜鉛と親油性基粉体とを乾式あるいは湿式で混合することによって作られる。製造方法は、本発明の効果を損なわない方法であれば、特に限定されないが、例えば、メカノフュージョン処理による方法が挙げられる。 In the present invention, the zinc oxide and the lipophilic base powder need not be simply mixed, but must be combined. The composite powder according to the present invention is produced by mixing zinc oxide and a lipophilic base powder in a dry or wet manner. The production method is not particularly limited as long as it does not impair the effects of the present invention, and examples thereof include a method by mechanofusion treatment.
メカノフュージョンとは、複数の異なる素材粒子にある種の機械的エネルギーを加えて，メカノケミカル的な反応を起こさせ，新しい素材を創造する技術である。図３に示すように、回転容器（２０）内に投入された粉体原料（２２）は，遠心力によりその内壁に押しつけられて固定され，曲率半径の異なるインナーピース（２４）との間で強力な圧縮・剪断力を受ける。この機械的手法は，湿式法等の他の粒子複合化手法に比べて，プロセスがシンプルであり，組合せの幅が格段に広いことが特長である。このメカノフュージョンシステムは表面融合による固体粒子の複合化のみでなく，粒子の形状をコントロールするなど，従来の粉体混合機に比べて混合度の高い粉体融合を実現する。
その他、混合装置としては、各種ボールミル、オングミル、スクリーンミル、ポットミル、乳鉢、アトライター、ハイブリダイザー、ヘンシェルミキサー等が適用される。
Mechanofusion is a technology that creates a new material by adding some kind of mechanical energy to different material particles to cause a mechanochemical reaction. As shown in FIG. 3, the powder raw material (22) put into the rotating container (20) is pressed and fixed to the inner wall by centrifugal force, and between the inner pieces (24) having different curvature radii. Receives strong compression and shear force. This mechanical method is characterized by a simpler process and a wider range of combinations than other particle compositing methods such as the wet method. This mechano-fusion system not only combines the solid particles by surface fusion, but also controls the shape of the particles, enabling powder fusion with a higher degree of mixing than conventional powder mixers.
In addition, various ball mills, ong mills, screen mills, pot mills, mortars, attritors, hybridizers, Henschel mixers, and the like are applied as mixing devices.
本発明の複合粉体は、適度な隠蔽力を有し、これを配合した油中水型乳化組成物は、しみ、そばかす、色むらの隠蔽効果に優れたものとなる。
特に、揮発性油分や水を使用すると、塗布時には肌への塗りのばしやすさや使用性に優れ、塗布後には油分や水が揮発して皮膚上で、光拡散効果に優れる。
また、本発明の複合粉体は光拡散効果に優れているため、これを配合した油中水型乳化組成物は、肌の凹凸ぼかし効果に優れたものとなる。親油性基粉体が球状である場合、特に光拡散効果に優れたものとなる。
The composite powder of the present invention has an appropriate hiding power, and a water-in-oil emulsion composition containing this has an excellent hiding effect on spots, freckles, and uneven color.
In particular, when a volatile oil or water is used, it is easy to spread on the skin and is easy to use at the time of application, and after application, the oil and water are volatilized and the light diffusion effect is excellent on the skin.
Moreover, since the composite powder of this invention is excellent in the light-diffusion effect, the water-in-oil emulsion composition which mix | blended this becomes the thing excellent in the uneven | corrugated blurring effect of skin. When the lipophilic base powder is spherical, it is particularly excellent in light diffusion effect.
本発明の油中水型乳化組成物における複合粉体の含有量は、本発明の効果が得られる範囲であれば別段限定されず、適宜調整して用いることができるが、１〜３０質量％、好ましくは５〜２０質量％である。１質量％未満であると本発明でいう効果が十分に発揮されない場合があり、３０質量％を越えると製剤処方上好ましくない場合がある。 The content of the composite powder in the water-in-oil emulsion composition of the present invention is not particularly limited as long as the effect of the present invention is obtained, and can be appropriately adjusted and used. The amount is preferably 5 to 20% by mass. If the amount is less than 1% by mass, the effect referred to in the present invention may not be sufficiently exhibited.
＜シリコーン油＞
本発明にかかる油中水型乳化組成物において、外相であるシリコーン油相は、シリコーン油を主成分とする。また該シリコーン油は前記複合粉体を膨潤可能であることが好適である。このようなシリコーン油としては、鎖状ポリシロキサン（例えば、ジメチルポリシロキサン、メチルフェニルポリシロキサン、ジフェニルポリシロキサン等）；環状ポリシロキサン（例えば、オクタメチルシクロテトラシロキサン、デカメチルシクロペンタシロキサン、ドデカメチルシクロヘキサシロキサン等）、各種変性ポリシロキサン（アミノ変性ポリシロキサン、ポリエーテル変性ポリシロキサン、アルキル変性ポリシロキサン、フッ素変性ポリシロキサン等）等が例示される。
なお、これらのシリコーン油相には、シリコーン油の機能を損なわない範囲で他の油分を含めることができる。好ましくは、シリコーン油相中の他の油分は５０質量％以下である。
<Silicone oil>
In the water-in-oil emulsified composition according to the present invention, the silicone oil phase that is the outer phase contains silicone oil as a main component. The silicone oil is preferably capable of swelling the composite powder. Such silicone oils include chain polysiloxanes (eg, dimethylpolysiloxane, methylphenylpolysiloxane, diphenylpolysiloxane, etc.); cyclic polysiloxanes (eg, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, dodecamethyl). Cyclohexasiloxane, etc.), various modified polysiloxanes (amino-modified polysiloxane, polyether-modified polysiloxane, alkyl-modified polysiloxane, fluorine-modified polysiloxane, etc.).
These silicone oil phases can contain other oils as long as the function of the silicone oil is not impaired. Preferably, the other oil content in the silicone oil phase is 50% by mass or less.
本発明において用いられる他の油分としては、特に限定されず、アボガド油、ツバキ油、タートル油、マカデミアナッツ油、トウモロコシ油、ミンク油、オリーブ油、ナタネ油、卵黄油、ゴマ油、パーシック油、小麦胚芽油、サザンカ油、ヒマシ油、アマニ油、サフラワー油、綿実油、エノ油、大豆油、落花生油、茶実油、カヤ油、コメヌカ油、シナギリ油、日本キリ油、ホホバ油、胚芽油、トリグリセリン、トリオクタン酸グリセリン、トリイソパルミチン酸グリセリン等の液体油脂；カカオ脂、ヤシ油、馬脂、硬化ヤシ油、パーム油、牛脂、羊脂、硬化牛脂、パーム核油、豚脂、牛骨脂、モクロウ核油、硬化油、牛脚油、モクロウ、硬化ヒマシ油等の固体油脂；ミツロウ、カンデリラロウ、綿ロウ、カルナウバロウ、ベイベリーロウ、イボタロウ、鯨ロウ、モンタンロウ、ヌカロウ、ラノリン、カポックロウ、酢酸ラノリン、液晶ラノリン、サトウキビロウ、ラノリン脂肪酸イソプロピル、ラウリン酸ヘキシル、還元ラノリン、ジョジョバロウ、硬質ラノリン、セラックロウ、POEラノリンアルコールエーテル、POEラノリンアルコールアセテート、POEコレステロールエーテル、ラノリン脂肪酸ポリエチレングリコール、POE水素添加ラノリンアルコールエーテル等のロウ類；流動パラフィン、オゾケライト、スクワレン、プリスタン、パラフィン、セレシン、スクワラン、ワセリン、マイクロクリスタリンワックス等の炭化水素；ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、ベヘン酸、オレイン酸、ウンデシレン酸、トール酸、イソステアリン酸、リノール酸、リノレイン酸、エイコサペンタエン酸（ＥＰＡ）、ドコサヘキサエン酸（ＤＨＡ）等の高級脂肪酸；直鎖アルコール（例えば、ラウリルアルコール、セチルアルコール、ステアリルアルコール、ベヘニルアルコール、ミリスチルアルコール、オレイルアルコール、セトステアリルアルコール等）；分枝鎖アルコール（例えば、モノステアリルグリセリンエーテル(バチルアルコール)、2-デシルテトラデシノール、ラノリンアルコール、コレステロール、フィトステロール、ヘキシルドデカノール、イソステアリルアルコール、オクチルドデカノール等）等の高級アルコール；ミリスチン酸イソプロピル、オクタン酸セチル、ミリスチン酸オクチルドデシル、パルミチン酸イソプロピル、ステアリン酸ブチル、ラウリン酸ヘキシル、ミリスチン酸ミリスチル、オレイン酸デシル、ジメチルオクタン酸ヘキシルデシル、乳酸セチル、乳酸ミリスチル、酢酸ラノリン、ステアリン酸イソセチル、イソステアリン酸イソセチル、 12-ヒドロキシステアリン酸コレステリル、ジ-2-エチルヘキサン酸エチレングリコール、ジペンタエリスリトール脂肪酸エステル、モノイソステアリン酸N-アルキルグリコール、ジカプリン酸ネオペンチルグリコール、リンゴ酸ジイソステアリル、ジ-2-ヘプチルウンデカン酸グリセリン、トリ-2-エチルヘキサン酸トリメチロールプロパン、トリイソステアリン酸トリメチロールプロパン、テトラ-2-エチルヘキサン酸ペンタエリスリトール、トリ-2-エチルヘキサン酸グリセリン、トリオクタン酸グリセリン、トリイソパルミチン酸グリセリン、トリイソステアリン酸トリメチロールプロパン、セチル2-エチルヘキサノエート、2-エチルヘキシルパルミテート、トリミリスチン酸グリセリン、トリ-2-ヘプチルウンデカン酸グリセライド、ヒマシ油脂肪酸メチルエステル、オレイン酸オレイル、アセトグリセライド、パルミチン酸2-ヘプチルウンデシル、アジピン酸ジイソブチル、N-ラウロイル-L-グルタミン酸-2-オクチルドデシルエステル、アジピン酸ジ-2-ヘプチルウンデシル、エチルラウレート、セバシン酸ジ−2-エチルヘキシル、ミリスチン酸2-ヘキシルデシル、パルミチン酸2-ヘキシルデシル、アジピン酸2-ヘキシルデシル、セバシン酸ジイソプロピル、コハク酸2-エチルヘキシル、クエン酸トリエチル等の合成エステル油等が好適に用いられる。 Other oils used in the present invention are not particularly limited, and are avocado oil, camellia oil, turtle oil, macadamia nut oil, corn oil, mink oil, olive oil, rapeseed oil, egg yolk oil, sesame oil, persic oil, wheat germ oil , Sasanqua oil, castor oil, flaxseed oil, safflower oil, cottonseed oil, enoy oil, soybean oil, peanut oil, teaseed oil, kaya oil, rice bran oil, snail oil, Japanese kiri oil, jojoba oil, germ oil, triglycerin Liquid oils such as glycerin trioctanoate and glycerin triisopalmitate; cocoa butter, coconut oil, horse fat, hydrogenated coconut oil, palm oil, beef tallow, sheep fat, hardened beef tallow, palm kernel oil, pork tallow, beef bone fat, Solid fats such as owl kernel oil, hydrogenated oil, cow leg oil, owl, hydrogenated castor oil; beeswax, candelilla wax, cotton wax, carnauba wax, bayberry wax, yellow Tallow, whale wax, montan wax, nukarou, lanolin, kapok wax, lanolin acetate, liquid crystal lanolin, sugarcane wax, lanolin fatty acid isopropyl, hexyl laurate, reduced lanolin, jojoballow, hard lanolin, shellac wax, POE lanolin alcohol ether, POE lanolin alcohol acetate Waxes such as POE cholesterol ether, lanolin fatty acid polyethylene glycol, POE hydrogenated lanolin alcohol ether; hydrocarbons such as liquid paraffin, ozokerite, squalene, pristane, paraffin, ceresin, squalane, petrolatum, microcrystalline wax; lauric acid, myristin Acid, palmitic acid, stearic acid, behenic acid, oleic acid, undecylenic acid, toluic acid, isostearic acid, linoleic acid, lino Higher fatty acids such as inic acid, eicosapentaenoic acid (EPA), docosahexaenoic acid (DHA); linear alcohols (eg, lauryl alcohol, cetyl alcohol, stearyl alcohol, behenyl alcohol, myristyl alcohol, oleyl alcohol, cetostearyl alcohol); Higher alcohols such as branched alcohols (eg monostearyl glycerin ether (batyl alcohol), 2-decyltetradecinol, lanolin alcohol, cholesterol, phytosterol, hexyldodecanol, isostearyl alcohol, octyldodecanol, etc.); isopropyl myristate , Cetyl octanoate, octyldodecyl myristate, isopropyl palmitate, butyl stearate, hexyl laurate, millisyl myristate Til, decyl oleate, hexyldecyl dimethyloctanoate, cetyl lactate, myristyl lactate, lanolin acetate, isocetyl stearate, isocetyl isostearate, cholesteryl 12-hydroxystearate, ethylene glycol di-2-ethylhexanoate, dipentaerythritol fatty acid Esters, N-alkyl glycol monoisostearate, neopentyl glycol dicaprate, diisostearyl malate, glycerin di-2-heptylundecanoate, trimethylolpropane tri-2-ethylhexanoate, trimethylolpropane triisostearate, tetra 2-ethylhexanoic acid pentaerythritol, tri-2-ethylhexanoic acid glycerin, trioctanoic acid glycerin, triisopalmitic acid glycerin, triisostearic acid trimethylo Propane, cetyl 2-ethylhexanoate, 2-ethylhexyl palmitate, glyceryl trimyristate, glyceride tri-2-heptylundecanoate, methyl ester of castor oil fatty acid, oleyl oleate, acetoglyceride, 2-heptylundecyl palmitate , Diisobutyl adipate, N-lauroyl-L-glutamic acid-2-octyldodecyl ester, di-2-heptylundecyl adipate, ethyl laurate, di-2-ethylhexyl sebacate, 2-hexyldecyl myristate, palmitic acid Synthetic ester oils such as 2-hexyldecyl, 2-hexyldecyl adipate, diisopropyl sebacate, 2-ethylhexyl succinate, and triethyl citrate are preferably used.
＜分散剤＞
本発明にかかる乳化組成物において、シリコーン油中に水を分散し得る非イオン性分散剤としては、グリセリン脂肪酸エステル、ソルビタン脂肪酸エステル、ポリオキシアルキレン変性オルガノシロキサン系分散剤などが存在するが、これらの中で好適なものとして下記ポリエーテル変性シリコーン系分散剤が挙げられる。
<Dispersant>
In the emulsified composition according to the present invention, glycerin fatty acid ester, sorbitan fatty acid ester, polyoxyalkylene-modified organosiloxane dispersant, and the like exist as nonionic dispersants capable of dispersing water in silicone oil. Among them, the following polyether-modified silicone dispersant is preferable.
ポリオキシアルキレン基Ｃは、一般式
−Ｃ３Ｈ６Ｏ（Ｃ２Ｈ４Ｏ）ａ（Ｃ３Ｈ６Ｏ）ｂＲ’
（Ｒ’は水素原子、アシル基、または炭素原子数１〜４のアルキル基であり、ａとｂは互いに同一でも異なってもよく、０〜５０の整数である。）
で表されるポリオキシアルキレン基である｝
The polyoxyalkylene group C has the general formula —C 3 H 6 O (C 2 H 4 O) a (C 3 H 6 O) b R ′.
(R ′ is a hydrogen atom, an acyl group, or an alkyl group having 1 to 4 carbon atoms, and a and b may be the same as or different from each other, and are integers of 0 to 50.)
Is a polyoxyalkylene group represented by
前述したように、特に架橋型ポリエーテル変性シリコーンが好適に用いられる。
この架橋型ポリエーテル変性シリコーンは、予めシリコーン油と剪断力下で混練処理されたペースト状ポリエーテル変性シリコーン組成物とされたものを使用するのが好ましいが、ポリエーテル変性シリコーンとシリコーン油等を化粧料成分として配合しても構わない。また、ポリエーテル変性シリコーンとシリコーン油とを、場合によっては更にその他の化粧料成分等と配合した後に混練処理することも可能である。
As described above, a cross-linked polyether-modified silicone is particularly preferably used.
The cross-linked polyether-modified silicone is preferably a pasty polyether-modified silicone composition kneaded with silicone oil under a shearing force, but the polyether-modified silicone and the silicone oil are preferably used. You may mix | blend as a cosmetic ingredient. Further, in some cases, the polyether-modified silicone and silicone oil may be further kneaded after further blending with other cosmetic ingredients.
この架橋型ポリエーテル変性シリコーンを本発明で使用するに当たっては、ｐは３〜２０が好ましい。この範囲を逸脱する３未満では、架橋型ポリエーテル変性シリコーンとシリコーンとを剪断力下で混練処理して得られたペースト状組成物が水の乳化性に乏しく、２０を超えるとシリコーン油への膨潤性が十分でなくなり好ましくない。そして、ｑは１０〜２００が好ましく、１０未満では、シリコーン油に対して十分に膨潤せず、２００を超えるとシリコーン油と剪断力下で混練処理して得られたペースト状組成物が水の乳化性に乏しくなる。 When this crosslinked polyether-modified silicone is used in the present invention, p is preferably 3 to 20. If it is less than 3 that deviates from this range, the paste-like composition obtained by kneading the cross-linked polyether-modified silicone and silicone under shearing force has poor water emulsifying properties. The swelling property is not sufficient, which is not preferable. Further, q is preferably 10 to 200, and if it is less than 10, it does not swell sufficiently with respect to silicone oil, and if it exceeds 200, the paste-like composition obtained by kneading with silicone oil under shearing force is water. Emulsification becomes poor.
また、ｒは１〜１０が好ましく、１より小さいと、３次元構造体の形成ができずシリコーン油と混練処理してもペースト状物とならず、水の乳化性にも劣るものとなる。逆に１０を超えると、３次元構造体の架橋密度が高くなり過ぎるためシリコーン油と混練処理してもシリコーン油を保持できず、安定なペースト状物とならず好ましくない。 In addition, r is preferably 1 to 10, and if it is smaller than 1, a three-dimensional structure cannot be formed, and even if kneaded with silicone oil, it does not become a paste-like product, and the water emulsifiability is poor. Conversely, if it exceeds 10, the crosslinking density of the three-dimensional structure becomes too high, and even if kneaded with silicone oil, the silicone oil cannot be retained, and a stable paste-like product is not preferred.
本発明において、架橋型ポリエーテル変性シリコーンと混練処理するシリコーン油については、特に制限されるものではなく、直鎖状あるいは分岐状のいずれであってもよく、各種のシリコーン油が使用可能であるが、２５℃における粘度が１００ｍＰａ・ｓ以下である低粘度シリコーン油が好ましく使用できる。使用可能な具体的シリコーン油としては、メチルポリシロキサン、メチルフェニルポリシロキサン、エチルポリシロキサン、エチルメチルポリシロキサン、エチルフェニルポリシロキサン、オクタメチルシクロテトラシロキサン、デカメチルシクロペンタシロキサン等の環状のジメチルポリシロキサン等が挙げられ、これらを単独あるいは２種以上混合して使用してもよい。 In the present invention, the silicone oil to be kneaded with the crosslinked polyether-modified silicone is not particularly limited, and may be either linear or branched, and various silicone oils can be used. However, a low-viscosity silicone oil having a viscosity at 25 ° C. of 100 mPa · s or less can be preferably used. Specific silicone oils that can be used include cyclic polydimethylsiloxane such as methylpolysiloxane, methylphenylpolysiloxane, ethylpolysiloxane, ethylmethylpolysiloxane, ethylphenylpolysiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, etc. Siloxane etc. are mentioned, You may use these individually or in mixture of 2 or more types.
架橋型ポリエーテル変性シリコーンとシリコーン油との配合比率については、前記したとおり架橋型ポリエーテル変性シリコーン１００重量部に対してシリコーン油１０〜１０００重量部がよく、好ましくは２０〜５００重量部がよい。架橋型ポリエーテル変性シリコーンの量が前記範囲より少ないと、安定で良好なゲル構造を維持できず、逆に前記範囲を越えると、肌上で重さを感じ使用性、使用感が悪化するため好ましくない。混練処理を剪断力下で行う装置についても、特に制限されるものではなく、通常使用されるものが使用でき、それには例えば３本ロールミル、２本ロールミル、サンドグラインダー、コロイドミル、ガウリンホモジナイザー等が挙げられるが、特に３本ロールミルが好ましく使用できる。 As described above, the blending ratio of the crosslinked polyether-modified silicone and the silicone oil is preferably 10 to 1000 parts by weight, preferably 20 to 500 parts by weight, based on 100 parts by weight of the crosslinked polyether-modified silicone. . If the amount of the cross-linked polyether-modified silicone is less than the above range, a stable and good gel structure cannot be maintained. Conversely, if the amount exceeds the above range, the weight is felt on the skin and the usability and usability are deteriorated. It is not preferable. The apparatus for performing the kneading treatment under a shearing force is not particularly limited, and those that are usually used can be used. For example, a three-roll mill, a two-roll mill, a sand grinder, a colloid mill, and a Gaurin homogenizer can be used. In particular, a three-roll mill can be preferably used.
なお、本発明においてはイオン性分散剤あるいはイオン性分散安定剤の配合は、むしろ系の安定性を損なう結果となり好ましくないが、これらイオン性分散剤などが実質的に機能していない状態、すなわち非イオン性分散剤によりしっかりとした分散状態が形成されている状態で、他のイオン性界面活性剤などが共存していても大きく系の安定性を損なうことにはならない。したがって、本発明において「実質的にイオン性分散剤及び／又はイオン性乳化安定剤を含まない」とは、これらのイオン性物質を抜去しても系の安定性に影響を与えない場合を含むものである。
また、水相中へのイオン性物質の配合は、通常問題とはならない。
In the present invention, the addition of an ionic dispersant or an ionic dispersion stabilizer is not preferable because it results in a loss of stability of the system. However, these ionic dispersants are not substantially functioning, that is, Even when other ionic surfactants and the like coexist in a state where a solid dispersion state is formed by the nonionic dispersant, the stability of the system is not greatly impaired. Therefore, in the present invention, “substantially free of ionic dispersant and / or ionic emulsion stabilizer” includes a case where removal of these ionic substances does not affect the stability of the system. It is a waste.
Also, the incorporation of ionic substances in the aqueous phase is not usually a problem.
＜その他成分＞
本発明の油中水型乳化組成物には上記必須成分の他に通常化粧品や医薬品等に用いられる他の成分、例えば、その他の粉末成分、保湿剤、水溶性高分子、増粘剤、皮膜剤、紫外線吸収剤、金属イオン封鎖剤、低級アルコール、多価アルコール、糖、アミノ酸、有機アミン、高分子エマルジョン、pH調製剤、皮膚栄養剤、ビタミン、酸化防止剤、酸化防止助剤、香料、水等を必要に応じて適宜配合し、常法により製造することが出来る。
<Other ingredients>
In the water-in-oil emulsion composition of the present invention, in addition to the above essential components, other components usually used in cosmetics and pharmaceuticals, for example, other powder components, humectants, water-soluble polymers, thickeners, films Agent, UV absorber, sequestering agent, lower alcohol, polyhydric alcohol, sugar, amino acid, organic amine, polymer emulsion, pH adjuster, skin nutrient, vitamin, antioxidant, antioxidant aid, fragrance, Water or the like can be appropriately blended as necessary, and can be produced by a conventional method.
さらに、エデト酸二ナトリウム、エデト酸三ナトリウム、クエン酸ナトリウム、ポリリン酸ナトリウム、メタリン酸ナトリウム、グルコン酸、リンゴ酸等の金属封鎖剤、カフェイン、タンニン、ベラパミル、トラネキサム酸及びその誘導体、甘草、カリン、イチヤクソウ等の各種生薬抽出物、酢酸トコフェロール、グリチルレジン酸、グリチルリチン酸及びその誘導体又はその塩等の薬剤、ビタミンＣ、アスコルビン酸リン酸マグネシウム、アスコルビン酸グルコシド、アルブチン、コウジ酸等の美白剤、アルギニン、リジン等のアミノ酸及びその誘導体、フルクトース、マンノース、エリスリトール、トレハロース、キシリトール等の糖類等も適宜配合することができる。 Furthermore, edetate disodium, edetate trisodium, sodium citrate, sodium polyphosphate, sodium metaphosphate, gluconic acid, malic acid and other metal sequestering agents, caffeine, tannin, verapamil, tranexamic acid and its derivatives, licorice, Various herbal extracts such as Karin, Ichiyakusou, drugs such as tocopherol acetate, glycyrrhizic acid, glycyrrhizic acid and its derivatives or salts thereof, whitening agents such as vitamin C, magnesium ascorbate phosphate, glucoside ascorbate, arbutin, kojic acid, Amino acids such as arginine and lysine and derivatives thereof, saccharides such as fructose, mannose, erythritol, trehalose and xylitol can also be appropriately blended.
また、本発明の油中水型乳化組成物は、外皮に適用される化粧料、医薬品、及び医薬部外品に広く適用することが可能である。例えば、美白用美容液、乳液、クリーム、パック、ファンデーション、口紅、アイシャドー、アイライナー、マスカラ、洗顔料、ボディー洗浄料、サンスクリーンクリーム、ファンデーション、スプレー、ムース、ジェル、ヘアーリンス、シャンプー、皮膚科用軟膏等、従来化粧料に用いるものであれば何れの形態でも使用することができる。 In addition, the water-in-oil emulsion composition of the present invention can be widely applied to cosmetics, pharmaceuticals, and quasi drugs applied to the outer skin. For example, whitening serum, milk, cream, pack, foundation, lipstick, eye shadow, eyeliner, mascara, face wash, body cleanser, sunscreen cream, foundation, spray, mousse, gel, hair rinse, shampoo, skin Any form can be used as long as it is a conventional ointment such as a medical ointment.
本発明の化粧料は、敏感肌等の従来化粧料の使用が困難であった肌への適用にも優れた効果を示す。
敏感肌とは、刊行物等によれば以下のように言われている。「普段から医薬品外用剤、化粧品、植物、紫外線、金属等、多くの人には何でもない物質に特異的に反応し、皮膚トラブルを起こしやすい肌。バリア機能が低下していてアレルギー性物質（花粉、香料等）や刺激性物質（アルコール等）に体質的に敏感な肌」及び「睡眠不足、過労、生理、季節の変わり目、精神的なストレス等により、肌本来の抵抗力あるいは皮膚の生理機能が弱まるようなときに、刺激物に対して一時的に皮膚トラブルを起こしやすくなる肌。普段使用している化粧品の使用に不安を感じることがある心配肌。」
The cosmetic of the present invention exhibits an excellent effect even when applied to skin where it has been difficult to use conventional cosmetics such as sensitive skin.
Sensitive skin is said as follows according to publications. “Skins that normally react with substances that are not common to many people, such as topical pharmaceuticals, cosmetics, plants, UV rays, metals, etc., and are prone to skin problems. Allergic substances (pollen with reduced barrier function) , Fragrances, etc.) and skin that is physically sensitive to irritants (alcohols, etc.) ”and“ natural resistance to skin or physiological functions of skin due to lack of sleep, overwork, physiology, seasonal changes, mental stress, etc. Skin that is likely to cause temporary skin problems with irritants when it becomes weak.Skin worried that you may feel uneasy about using the cosmetics you normally use. "
このように、肌状態が敏感になる要因としては、皮膚バリア機能の低下、皮膚刺激閾値の低下、皮膚の乾燥、接触皮膚炎の起炎物質、物理化学的刺激、ストレス、体調、季節変化、紫外線、生理等が挙げられる。さらに、誤ったスキンケアにより自ら肌を敏感にしてしまう場合、あるいは単に本人の思い込みで敏感肌に分類される場合も考えられる。 In this way, factors that make the skin condition sensitive include reduced skin barrier function, reduced skin irritation threshold, dry skin, contact dermatitis-causing substances, physicochemical stimulation, stress, physical condition, seasonal changes, Examples include ultraviolet light and physiology. Furthermore, it may be considered that the skin is made sensitive by mistaken skin care, or that the skin is classified as sensitive skin simply by the person's assumption.
本発明において敏感肌対象者とは、下記１〜５のいずれかの処理において異常感覚を覚える者と定義した。
１ ５％クエン酸水溶液１００μＬを頬に塗布し、１０分間置く。
２ ５％乳酸水溶液１００μＬを頬に塗布し、１０分間置く。
３ ５０％エタノール溶液１００μＬを頬に塗布し、１０分間置く。
４ ０．２％メチルパラベン水溶液１００μＬを２×２ｃｍ不織布に含浸し、頬に１０分間静置する。
５ ５％ＳＤＳ水溶液１００μＬを２×２ｃｍ不織布に含浸し、頬に３０分間静置する。
なお異常感覚とは、皮膚領域において感知される、比較的苦痛を伴う感覚、例えばひりひりする痛み、むずむず感、痒み、熱感、不快感、刺すような痛み等を意味する。
以下、本発明の好適な実施例についてさらに詳しく説明する。なお、本発明はこれにより限定されるものではない。
In the present invention, the sensitive skin target person is defined as a person who feels an abnormal sensation in any of the following processes 1 to 5.
15 Apply 100 μL of 5% aqueous citric acid solution on cheek and place for 10 minutes.
2 Apply 100 μL of 5% aqueous lactic acid solution to cheek and place for 10 minutes.
3. Apply 100 μL of 50% ethanol solution to the cheek and place for 10 minutes.
4 100 μL of 0.2% methylparaben aqueous solution is impregnated into a 2 × 2 cm non-woven fabric and left on the cheek for 10 minutes.
5 Impregnate 2 × 2 cm non-woven fabric with 100 μL of 5% SDS aqueous solution and leave on cheek for 30 minutes.
The abnormal sensation means a relatively painful sensation sensed in the skin region, for example, tingling pain, itching sensation, itchiness, heat sensation, discomfort, stinging pain, and the like.
Hereinafter, preferred embodiments of the present invention will be described in more detail. In addition, this invention is not limited by this.
酸化亜鉛被覆シリコーンゴム粉体（膨潤性）
酸化亜鉛（亜鉛華正同：平均粒径０．５μｍ）とシリコーンゴム粉体（トレフィルＥ５０６ＷＴＭ：ζ電位−１２．０ｍＶ：平均粒径５μｍ）とを混合比率を変えて混合し、メカノフュージョン処理（２６００ｒｐｍ、２分間）により複合化し、所望の被覆率の複合粉体を得た（複合粉体１−１〜１−６）。
得られた複合粉体の、膨潤時のシリコーンゴム粉体の全表面積に対する酸化亜鉛の被覆率は電子顕微鏡観察により観察した。
Zinc oxide coated silicone rubber powder (swelling)
Zinc oxide (Zinc Hana: Same particle size: 0.5 μm) and silicone rubber powder (Trefil E506W ™ : ζ potential: 12.0 mV: Average particle size: 5 μm) are mixed at different mixing ratios and mechano-fusion treated. (2600 rpm, 2 minutes) to obtain composite powder having a desired coverage (composite powder 1-1 to 1-6).
The coverage of zinc oxide with respect to the total surface area of the silicone rubber powder during swelling of the obtained composite powder was observed with an electron microscope.
（表６）
複合粉体 1-1 1-2 1-3 1-4 1-5 1-6
膨潤時の被覆率（％） 1 5 10 50 90 100
(Table 6)
Composite powder 1-1 1-2 1-3 1-4 1-5 1-6
Coverage during swelling (%) 1 5 10 50 90 100
比較例１：酸化亜鉛（亜鉛華正同：平均粒径０．５μｍ）と、シリコーンゴム粉体（トレフィルＥ５０６ＷＴＭ）の混合物（質量比１：９）
複合化の確認
初めに本発明の複合粉体が、単に混合されているのではなく、複合化されていることを確認するために、以下の試験を行った。
すなわち、複合粉体１−３ ０．１ｇ、水２０ｇ、シリコーン油（シリコーンオイルＤ５ＴＭ）２０gを混合し、攪拌したところ、油相に良好に分散した。同様に、比較例１の混合粉体０．１ｇ、水２０ｇ、シリコーン油（シリコーンオイルＤ５ＴＭ）２０gを混合し、攪拌したところ、シリコーンゴム粉体は油に、酸化亜鉛は水に、分かれて分散した。このことから、本発明においては、酸化亜鉛と親油性基粉体とが単に混合されているのではなく、確かに複合化されていることが証明された。
Comparative Example 1: Mixture of zinc oxide (Zinc Hana: Same particle size: 0.5 μm) and silicone rubber powder (Trefil E506W ™ ) (mass ratio 1: 9)
Confirmation of compounding First, in order to confirm that the composite powder of the present invention was not simply mixed but compounded, the following test was conducted.
That is, 0.1 g of the composite powder 1-3, 20 g of water, and 20 g of silicone oil (silicone oil D5 TM ) were mixed and stirred. As a result, they were well dispersed in the oil phase. Similarly, when 0.1 g of the mixed powder of Comparative Example 1, 20 g of water, and 20 g of silicone oil (silicone oil D5 TM ) were mixed and stirred, the silicone rubber powder was separated into oil and the zinc oxide was separated into water. Distributed. From this, in the present invention, it was proved that the zinc oxide and the lipophilic base powder were not simply mixed, but were certainly combined.
次に、複合粉体１−３及び比較例１〜３の粉体を用いて、粉体の油分散性及び肌荒れ改善効果との関係について試験した。具体的試験方法ならびにその判定基準は下記のとおりである。
被検粉体の油分散性
（試験方法）
被検粉体とシリコーン油（シリコーンオイルＤ５ＴＭ）とを混合し、攪拌する。
（判定基準）
○：良好に分散した
×：凝集した
Next, the composite powder 1-3 and the powders of Comparative Examples 1 to 3 were tested for the relationship between the oil dispersibility of the powder and the effect of improving skin roughness. The specific test method and its judgment criteria are as follows.
Oil dispersibility of test powder (test method)
The test powder and silicone oil (silicone oil D5 ™ ) are mixed and stirred.
(Criteria)
○: well dispersed ×: agglomerated
肌荒れ改善効果
（試験方法）
下記表７の処方にて油中水型乳化組成物を製造し、パネル２０名の顔面を用い、１日１回以上８週間塗布し、その後の肌の状態を評価した。
著効 ：肌状態が著しく良くなった
有効 ：肌状態が良くなった
やや有効：肌状態がやや良くなった
無効 ：肌状態の変化がない、あるいは悪化した
（判定基準）
◎ ：被験者が著効、有効及びやや有効を示す割合（有効率）が８０％以上
○ ：有効率が５０％以上８０％未満
△ ：有効率が３０％以上５０％未満
× ：有効率が３０％未満
Rough skin improvement effect (test method)
A water-in-oil emulsified composition was produced according to the formulation shown in Table 7 below, applied to the face of 20 panelists at least once a day for 8 weeks, and the skin condition thereafter was evaluated.
Remarkable: Skin condition improved significantly. Effective: Skin condition improved slightly. Effective: Skin condition improved slightly. Invalid: Skin condition did not change or deteriorated.
◎: The ratio (effective rate) at which the subject exhibits remarkable, effective and slightly effective (effective rate) is 80% or more. ○: The effective rate is 50% or more and less than 80%. Δ: The effective rate is 30% or more and less than 50%. %Less than
（表７）
（１）被検粉体 ６．０
（２）ジメチルポリシロキサン ２０．０
（３）架橋型ポリエーテル変性シリコーン ２．０
（４）1，3−ブチレングリコール ５．０
（５）グリセリン ５．０
（６）精製水 残余
（製法）
（１）〜（３）を加熱して７５℃に保つ（油相）。（６）に（４）、（５）を溶解して７５℃に加温する（水相）。水相を油相に添加しホモミキサーで均一に乳化し、よくかきまぜながら３０℃まで冷却する。
(Table 7)
(1) Test powder 6.0
(2) Dimethylpolysiloxane 20.0
(3) Crosslinked polyether-modified silicone 2.0
(4) 1,3-butylene glycol 5.0
(5) Glycerin 5.0
(6) Purified water residue
(Manufacturing method)
(1) to (3) are heated and kept at 75 ° C. (oil phase). (4) and (5) are dissolved in (6) and heated to 75 ° C. (aqueous phase). Add the aqueous phase to the oil phase, uniformly emulsify with a homomixer, and cool to 30 ° C. while stirring well.
複合粉体１−３：10％酸化亜鉛被覆シリコーンゴム粉体
比較例１：酸化亜鉛（亜鉛華正同：平均粒径０．５μｍ）と、シリコーンゴム粉体（トレフィルＥ５０６ＷＴＭ）の混合物（質量比１：９）
比較例２：シリコーンゴム粉体（トレフィルＥ５０６ＷＴＭ）
比較例３：酸化亜鉛（亜鉛華正同：平均粒径０．５μｍ）
結果を表８に示す。
Composite Powder 1-3: 10% Zinc Oxide-Coated Silicone Rubber Powder Comparative Example 1: Mixture (mass) of zinc oxide (Zinc Hana: average particle size 0.5 μm) and silicone rubber powder (Trefil E506W TM ) Ratio 1: 9)
Comparative Example 2: Silicone rubber powder (Trefill E506W ™ )
Comparative Example 3: Zinc oxide (Zinc Hana: Same particle size: 0.5 μm)
The results are shown in Table 8.
（表８）
複合粉体1-3 比較例１ 比較例２ 比較例３
油分散性 ○ × ○ ×
肌荒れ改善効果 ◎ △ × △
(Table 8)
Composite powder 1-3 Comparative example 1 Comparative example 2 Comparative example 3
Oil dispersibility ○ × ○ ×
Rough skin improvement effect ◎ △ × △
酸化亜鉛は親水性であるため、酸化亜鉛単独では油分散性が悪く、肌荒れ改善効果も低かった（比較例３）。シリコーンゴム粉体単独では、油分散性は良いものの、肌荒れ改善効果が見られなかった（比較例２）。また、酸化亜鉛と親油性基粉体を別々に配合した場合（比較例１）は、油分散性が悪く、肌荒れ改善効果も十分ではなかった。これに対し、本発明の複合粉体は、油分散性、肌荒れ改善効果ともに良好であった。
これにより、本発明にかかる複合粉体においては、酸化亜鉛由来の亜鉛イオンのプラスミノーゲンアクチベーター活性阻害効果が、該プラスミノーゲンアクチベーターを吸着する親油性基粉体の存在でさらに向上することが確認された。さらに、酸化亜鉛と親油性基粉体を別々に配合した場合と比較して、これらの複合粉体に極めて高い肌荒れ改善効果が認められることが確認された。
Since zinc oxide is hydrophilic, zinc oxide alone has poor oil dispersibility and low skin roughness improvement effect (Comparative Example 3). Although the silicone rubber powder alone has good oil dispersibility, the effect of improving rough skin was not observed (Comparative Example 2). Moreover, when zinc oxide and lipophilic base powder were blended separately (Comparative Example 1), the oil dispersibility was poor and the effect of improving skin roughness was not sufficient. On the other hand, the composite powder of the present invention was good in both oil dispersibility and rough skin improvement effect.
Thereby, in the composite powder according to the present invention, the plasminogen activator activity inhibitory effect of zinc ions derived from zinc oxide is further improved by the presence of the lipophilic base powder adsorbing the plasminogen activator. It was confirmed. Furthermore, it was confirmed that these composite powders showed an extremely high roughening effect compared to the case where zinc oxide and lipophilic base powder were blended separately.
酸化亜鉛被覆シリコーン樹脂被覆シリコーンゴム粉体（膨潤性）
シリコーンゴム粉体の代わりにシリコーン樹脂被覆シリコーンゴム粉体（ＫＳＰ１００ＴＭ：ζ電位−14.0ｍＶ：平均粒径５μｍ）を用いた以外は実施例１と同様の操作を行い、所望の被覆率の複合粉体を得た。
Zinc oxide coated silicone resin coated silicone rubber powder (swellability)
A composite having a desired coverage was obtained by performing the same operation as in Example 1 except that a silicone resin-coated silicone rubber powder (KSP100 ™ : ζ potential-14.0 mV: average particle size 5 μm) was used instead of the silicone rubber powder. A powder was obtained.
次に上記試験例の粉体配合の油中水型乳化組成物を用い、肌荒れ防止効果を試験した。油中水型乳化組成物の処方は表７の通りである。
肌荒れ防止効果
（試験方法）
５４名の男性パネルの前腕内側部２ヶ所に、５％ＳＤＳ水溶液を浸した脱脂綿（２×２ｃｍ）を当て１５分間固定し、活性剤を洗い落とした後、そこにパネルごとに割り付けた油中水型乳化組成物を塗布した（ｎ＝３）。この操作を７日間繰り返し、８日目に被験部位を十分に洗浄し、６０分放置した後ＳＤＳによって惹起される肌荒れの程度を観察し、以下の判定基準にもとづき評点を付けた。無塗布の部位を対象部位とした。さらにパネルごとに対照部位と化粧料塗布部位の評点差を求め、これを各化粧料ごとに合計し、以下の肌荒れ防止効果基準にもとづき各試料の効果を判定した。
Next, the effect of preventing rough skin was tested using the water-in-oil emulsion composition containing the powder of the above test example. Table 7 shows the formulation of the water-in-oil emulsion composition.
Rough skin prevention effect (test method)
54 male panels were placed on the inner forearm of the 54 male panels with absorbent cotton (2 x 2 cm) soaked in 5% SDS for 15 minutes, washed off the active agent, and then the water in oil assigned to each panel. A mold emulsion composition was applied (n = 3). This operation was repeated for 7 days, and the test site was thoroughly washed on the 8th day. After leaving for 60 minutes, the degree of rough skin caused by SDS was observed, and a score was assigned based on the following criteria. The uncoated part was used as a target part. Further, for each panel, the difference in score between the control part and the cosmetic application part was obtained, and this was summed up for each cosmetic, and the effect of each sample was judged based on the following rough skin prevention effect criteria.
＜肌荒れ評点基準＞
評点４：明らかな紅斑及び/または落屑が認められる。
評点３：中等度の紅斑及び/または僅かに落屑が認められる。
評点２：僅かな紅斑及び/または角層に亀裂が認められる。
評点１：角層表面が白っぽい、または粉を吹いたように見える。
評点０：症状なし。
＜肌荒れ防止効果判定基準＞
◎＝明らかに効果あり ：評点差６以上
○＝やや効果あり ：評点差４または５
△＝防止傾向あり ：評点差２または３
×＝無効 ：評点差１以下。
結果を表９に示す。
<Rough skin score criteria>
Score 4: Clear erythema and / or desquamation is observed.
Score 3: moderate erythema and / or slight desquamation.
Score 2: Slight erythema and / or cracks are observed in the stratum corneum.
Score 1: The stratum corneum surface appears whitish or powdered.
Score 0: No symptoms.
<Criteria for preventing rough skin effect>
◎ = Clearly effective: Grade difference 6 or more ○ = Slightly effective: Grade difference 4 or 5
△ = preventive tendency: Grade difference 2 or 3
× = Invalid: Grade difference of 1 or less.
The results are shown in Table 9.
（表９）
複合粉体2-1 複合粉体2-2 比較例４ 比較例５
肌荒れ防止効果 ◎ ◎ × △
複合粉体２−１：10％酸化亜鉛被覆シリコーン樹脂被覆シリコーンゴム粉体
複合粉体２−２：50％酸化亜鉛被覆シリコーン樹脂被覆シリコーンゴム粉体
比較例４：シリコーン樹脂被覆シリコーンゴム粉体（ＫＳＰ１００ＴＭ）
比較例５：酸化亜鉛（亜鉛華正同：平均粒径０．５μｍ）と、シリコーン樹脂被覆シリコーンゴム粉体（ＫＳＰ１００ＴＭ）の混合物（質量比１：９）
(Table 9)
Composite powder 2-1 Composite powder 2-2 Comparative example 4 Comparative example 5
Rough skin prevention effect ◎ ◎ × △
Composite powder 2-1: 10% zinc oxide coated silicone resin coated silicone rubber powder Composite powder 2-2: 50% zinc oxide coated silicone resin coated silicone rubber powder Comparative Example 4: Silicone resin coated silicone rubber powder ( KSP100 TM )
Comparative Example 5: Mixture of zinc oxide (Zinc Hana: same particle size: 0.5 μm) and silicone resin-coated silicone rubber powder (KSP100 ™ ) (mass ratio 1: 9)
親油性基粉体単独の場合（比較例４）、及び酸化亜鉛と親油性基粉体を複合させずに配合した場合（比較例５）では、無塗布の場合と比較して肌荒れ防止効果はほとんど見られなかった。これに対し、本発明の複合粉体を配合した場合（複合粉体２−１，２−２）は、明らかに効果が見られた。
これにより、本発明にかかる複合粉体においては、酸化亜鉛と親油性基粉体とを複合化することにより、極めて高い肌荒れ防止効果が認められることが確認された。
In the case of the lipophilic base powder alone (Comparative Example 4) and the case where the zinc oxide and the lipophilic base powder are blended without being combined (Comparative Example 5), the effect of preventing rough skin is obtained as compared with the case of no application. It was hardly seen. On the other hand, when the composite powder of the present invention was blended (composite powders 2-1 and 2-2), the effect was clearly seen.
Thereby, in the composite powder concerning this invention, it was confirmed that the extremely high roughening prevention effect is recognized by compounding zinc oxide and lipophilic base powder.
複合粉体３ 酸化亜鉛被覆ポリアミド粉体（非膨潤性）
シリコーンゴム粉体の代わりにポリアミド粉体（ナイロンＳＰ５００ＴＭ：ζ電位−３２．０ｍＶ：平均粒径５μｍ）を用いた以外は実施例１と同様の操作を行い、所望の被覆率の複合粉体を得た。
Composite powder 3 Zinc oxide coated polyamide powder (non-swelling)
A composite powder having a desired coverage was obtained by performing the same operation as in Example 1 except that polyamide powder (nylon SP500 ™ : ζ potential-32.0 mV: average particle size 5 μm) was used instead of the silicone rubber powder. Got.
複合粉体４ 酸化亜鉛被覆ポリエチレン粉体（非膨潤性）
シリコーンゴム粉体の代わりに、ポリエチレン粉体（フローセンＵＦＴＭ：ζ電位+１．０ｍＶ：平均粒径５μｍ）を用いた以外は実施例１と同様の操作を行い、被覆率１０％の複合粉体を得た。
親油性基粉体のζ電位と油分散性及び肌荒れ改善効果との関係
前記試験例の１０％酸化亜鉛被覆親油性基粉体を用いて、親油性基粉体のζ電位と、複合粉体の油分散性及び肌荒れ改善効果との関係について試験した。具体的試験方法ならびにその判定基準は上記のとおりである。
結果を表１０に示す。
Composite powder 4 Zinc oxide-coated polyethylene powder (non-swelling)
A composite powder having a coverage of 10% was prepared in the same manner as in Example 1 except that polyethylene powder (Flocene UF ™ : ζ potential +1.0 mV: average particle size 5 μm) was used instead of the silicone rubber powder. Got the body.
Relationship between ζ Potential of Lipophilic Base Powder and Oil Dispersibility and Skin Roughness Improvement Effect Using the 10% zinc oxide-coated lipophilic base powder of the above test example, ζ potential of lipophilic base powder and composite powder The relationship between the oil dispersibility and the effect of improving skin roughness was tested. The specific test method and its judgment criteria are as described above.
The results are shown in Table 10.
（表１０）
複合粉体1-3 複合粉体2-1 複合粉体3-3 複合粉体４
シリコーン樹脂
親油性基粉体 シリコーンゴム 被覆 ポリアミド ポリエチレン
シリコーンゴム
ζ電位(mv) −12.0 −14.0 −32.0 ＋1.0
被覆率(%) 10 10 10 10
油分散性 ○ ○ ○ ○
肌荒れ改善効果 ◎ ◎ ◎ △
(Table 10)
Composite powder 1-3 Composite powder 2-1 Composite powder 3-3 Composite powder 4
Silicone resin lipophilic base powder Silicone rubber coating Polyamide Polyethylene
silicone rubber
ζ potential (mv) −12.0 −14.0 −32.0 +1.0
Coverage (%) 10 10 10 10
Oil dispersibility ○ ○ ○ ○
Rough skin improvement effect ◎ ◎ ◎ △
どの複合粉体においても、油分散性は良好であったが、ζ電位が正の値であるポリエチレンを用いた場合には、肌荒れ改善効果が十分でなかったのに対し、ζ電位が負の値であるシリコーンゴム、ポリアミド、シリコーンゴム被覆シリコーン樹脂を用いた場合には、肌荒れ改善効果が著しく優れていることが確認された。これは、前述のようにζ電位が負の値である親油性基粉体がプラスミノーゲンアクチベーターを吸着するために、亜鉛イオンが該プラスミノーゲンアクチベーターに作用しやすく、効果的にプラスミノーゲンアクチベーターの活性阻害効果を発揮するからである。よって、親油性基粉体のζ電位は負の値、特に−１０ｍＶ以下であることが好適である。 In any composite powder, the oil dispersibility was good, but when polyethylene with a positive ζ potential was used, the effect of improving the rough skin was not sufficient, whereas the ζ potential was negative. When silicone rubber, polyamide, and silicone rubber-coated silicone resin, which are values, were used, it was confirmed that the effect of improving skin roughness was remarkably excellent. As described above, since the lipophilic base powder having a negative ζ potential adsorbs the plasminogen activator, zinc ions easily act on the plasminogen activator, and effectively This is because it exerts the activity-inhibiting effect of the minogen activator. Therefore, the ζ potential of the lipophilic base powder is preferably a negative value, particularly −10 mV or less.
酸化亜鉛被覆率と油分散性及び肌荒れ改善効果との関係
次に、前記複合粉体１及び３の酸化亜鉛被覆親油性基粉体を用いて、酸化亜鉛被覆率と複合粉体の油分散性及び肌荒れ改善効果との関係について試験した。
結果を表１１，１２に示す。
Relationship Between Zinc Oxide Coverage, Oil Dispersibility, and Skin Roughness Improvement Effect Next, using the zinc oxide-coated lipophilic base powder of the composite powders 1 and 3, the zinc oxide coverage and the oil dispersibility of the composite powder And the relationship with the rough skin improvement effect was tested.
The results are shown in Tables 11 and 12.
（表１１）
酸化亜鉛被覆シリコーンゴム粉体（膨潤性）
複合粉体 1-1 1-2 1-3 1-4 1-5 1-6
被覆率（％） 1 5 10 50 90 100
分散性 ○ ○ ○ ○ ○ ×
肌荒れ改善効果 ○ ◎ ◎ ◎ ○ △
(Table 11)
Zinc oxide coated silicone rubber powder (swelling)
Composite powder 1-1 1-2 1-3 1-4 1-5 1-6
Coverage (%) 1 5 10 50 90 100
Dispersibility ○ ○ ○ ○ ○ ×
Skin roughening effect ○ ◎ ◎ ◎ ○ △
（表１２）
酸化亜鉛被覆ポリアミド粉体（非膨潤性）
複合粉体 3-1 3-2 3-3 3-4 3-5 3-6 3-7
被覆率（％） 1 5 10 20 50 90 100
分散性 ○ ○ ○ ○ ○ ○ ×
肌荒れ改善効果 ○ ◎ ◎ ◎ ◎ ○ △
(Table 12)
Zinc oxide coated polyamide powder (non-swelling)
Composite powder 3-1 3-2 3-3 3-4 3-5 3-6 3-7
Coverage (%) 1 5 10 20 50 90 100
Dispersibility ○ ○ ○ ○ ○ ○ ×
Skin roughening effect ○ ◎ ◎ ◎ ◎ ○ △
表１１，１２に示す結果より、酸化亜鉛被覆率が１〜９０％の時、油分散性、肌荒れ改善効果共に優れていることが確認された。被覆率が９０％を超えると、酸化亜鉛が親油性基粉体を隙間なく被覆するため、親油性面が油分と接触できず油分散性が劣り、また酵素を吸着できないので、肌荒れ改善効果が劣る結果となった。
親油性基粉体がシリコーンゴム（膨潤性）である時は、複合粉体乾燥時の酸化亜鉛被覆率は９０％を超えていてもよい。これは、油分散時にシリコーンゴムが膨潤し、結果的に被覆率が低下するからである。表１１より、膨潤時の被覆率が１〜９０％である時、油分散性、肌荒れ改善効果共に優れていることが確認された。
From the results shown in Tables 11 and 12, it was confirmed that when the zinc oxide coverage was 1 to 90%, both the oil dispersibility and the effect of improving skin roughness were excellent. When the coverage exceeds 90%, the zinc oxide coats the lipophilic base powder without gaps, so the lipophilic surface cannot contact the oil and the oil dispersibility is poor, and the enzyme cannot be adsorbed. The result was inferior.
When the lipophilic base powder is silicone rubber (swelling property), the zinc oxide coverage during drying of the composite powder may exceed 90%. This is because the silicone rubber swells when the oil is dispersed, resulting in a decrease in the coverage. From Table 11, when the coverage at the time of swelling is 1 to 90%, it was confirmed that both the oil dispersibility and the rough skin improvement effect are excellent.
処方例１ プロテクター
配合量
１）シクロメチコン ２７
２）メトキシ桂皮酸オクチル ５
３）ジメチコン ４．５
４）コハク酸ジオクチル １
５）トリメチルシロキシケイ酸 ０．２５
６）架橋型ポリエーテル変性シリコーン ０．５
７）ポリエーテル変性シリコーン ０．５
８）イソステアリン酸 ０．５
９）香料 適量
１０）水 残量
１１）塩化ナトリウム ０．６
１２）エデト酸塩 ０．０５
１３）濃グリセリン ４
１４）エタノール ７
１５）セルロースガム ０．１５
１６）酸化亜鉛被覆ポリアミド粉末 ３
１７）疎水化処理酸化チタン ５
１８）防腐剤 適量
（製法）
１）〜９）の油相混合物中に、あらかじめ１０）〜１５）を溶解混合した水相を、高速攪拌機を用いて攪拌しながら添加し、更に１６）、１７）を高速攪拌機を用いて添加し、目的のプロテクターを得た。
Formulation Example 1 Protector
Compounding amount 1) Cyclomethicone 27
2) Octyl methoxycinnamate 5
3) Dimethicone 4.5
4) Dioctyl succinate 1
5) Trimethylsiloxysilicic acid 0.25
6) Crosslinked polyether-modified silicone 0.5
7) Polyether-modified silicone 0.5
8) Isostearic acid 0.5
9) Perfume appropriate amount 10) Water 11) Sodium chloride 0.6
12) Edetate 0.05
13) Concentrated glycerin 4
14) Ethanol 7
15) Cellulose gum 0.15
16) Zinc oxide coated polyamide powder 3
17) Hydrophobized titanium oxide 5
18) Preservative appropriate amount (production method)
The aqueous phase in which 10) to 15) is dissolved and mixed in advance is added to the oil phase mixture of 1) to 9) with stirring using a high-speed stirrer, and further 16) and 17) are added using a high-speed stirrer. And got the desired protector.
処方例２ ファンデーション
１）シクロメチコン １９
２）メチルフェニルポリシロキサン ３
３）架橋型ポリエーテル変性シリコーン ２
４）ポリエーテル変性シリコーン １
５）スクワラン ２
６）テトラ２−エチルヘキサン酸ペンタエリスリット ０．５
７）酢酸トコフェロール ０．０５
８）パラメトキシ桂皮酸２−エチルヘキシル ２
９）香料 適量
１０）精製水 残部
１１）クエン酸ナトリウム ０．００２
１２）クエン酸 ０．０９８
１３）塩化ナトリウム １
１４）ポリエチレングリコール１０００ １
１５）濃グリセリン ５
１６）キシリトール ２
１７）ジプロピレングリコール ５
１８）酸化防止剤 適量
１９）エタノール ３
２０）防腐剤 適量
２１）酸化亜鉛被覆ポリメチルメタクリレート粉末 １５
２２）調合粉末 ８
（製法）
１）〜９）の油相混合物中に、あらかじめ１０）〜２０）を溶解混合した水相を、高速攪拌機を用いて攪拌しながら添加し、更に２１）、２２）を高速攪拌機を用いて添加し、目的のファンデーションを得た。
Formulation Example 2 Foundation 1) Cyclomethicone 19
2) Methylphenyl polysiloxane 3
3) Crosslinked polyether-modified silicone 2
4) Polyether-modified silicone 1
5) Squalane 2
6) Tetra-2-ethylhexanoic acid pentaerythrit 0.5
7) Tocopherol acetate 0.05
8) 2-Ethylhexyl paramethoxycinnamate 2
9) Perfume appropriate amount 10) Purified water The remaining 11) Sodium citrate 0.002
12) Citric acid 0.098
13) Sodium chloride 1
14) Polyethylene glycol 1000 1
15) Concentrated glycerin 5
16) Xylitol 2
17) Dipropylene glycol 5
18) Antioxidant appropriate amount 19) Ethanol 3
20) Preservative appropriate amount 21) Zinc oxide coated polymethyl methacrylate
22) Mixed powder 8
(Manufacturing method)
The aqueous phase in which 10) to 20) is dissolved and mixed in advance is added to the oil phase mixture of 1) to 9) while stirring using a high-speed stirrer, and 21) and 22) are added using a high-speed stirrer. The target foundation was obtained.
処方例３ スキンクリーム
１）シクロメチコン １６
２）架橋型ポリエーテル変性シリコーン １
３）ポリエーテル変性シリコーン １
４）オレフィンオリゴマー ２
５）２−エチルヘキサン酸セチル ０．５
６）酢酸トコフェロール ０．０５
７）精製水 残部
８）クエン酸ナトリウム ０．０３
９）クエン酸 ０．０７
１０）塩化ナトリウム １
１１）ポリエチレングリコール６０００ １
１２）濃グリセリン ８
１３）ジプロピレングリコール ３
１４）エタノール ３
１５）カルボキシメチルセルロースナトリウム ０．２５
１６）１，３−ブチレングリコール ２
１７）防腐剤 適量
１８）酸化亜鉛被覆シリコーンゴム粉末 ５
（製法）
１）〜６）の油相混合物中に、あらかじめ７）〜１７）を溶解混合した水相を、高速攪拌機を用いて攪拌しながら添加し、更に１８）を高速攪拌機を用いて添加し、目的のスキンクリームを得た。
Formulation Example 3 Skin Cream 1) Cyclomethicone 16
2) Crosslinked polyether-modified silicone 1
3) Polyether-modified silicone 1
4) Olefin oligomer 2
5) Cetyl 2-ethylhexanoate 0.5
6) Tocopherol acetate 0.05
7) Purified water remainder 8) Sodium citrate 0.03
9) Citric acid 0.07
10) Sodium chloride 1
11) Polyethylene glycol 6000 1
12) Concentrated glycerin 8
13) Dipropylene glycol 3
14) Ethanol 3
15) Sodium carboxymethylcellulose 0.25
16) 1,3-butylene glycol 2
17) Preservative appropriate amount 18) Zinc oxide coated silicone rubber powder 5
(Manufacturing method)
The aqueous phase in which 7) to 17) is dissolved and mixed in advance is added to the oil phase mixture of 1) to 6) with stirring using a high-speed stirrer, and 18) is further added using a high-speed stirrer. Obtained skin cream.
１２ 親油性基粉体
１４ 酸化亜鉛
２０ 回転容器
２２ 粉体材料
２４ インナーピース
12
Claims (10)
前記複合粉体は、親油性基粉体と、その表面の少なくとも一部分を被覆する酸化亜鉛とを有し、
前記分散剤はシリコーン油中に水を分散し得る非イオン性分散剤からなり、
前記シリコーン油：複合粉体は質量比で１：１〜９９：１であることを特徴とする油中水型乳化組成物。 A water-in-oil emulsion composition comprising a silicone oil, water, a dispersant, and a composite powder dispersed in the silicone oil,
The composite powder has a lipophilic base powder and zinc oxide covering at least a part of the surface thereof,
The dispersant comprises a nonionic dispersant capable of dispersing water in silicone oil,
The water-in-oil emulsion composition, wherein the silicone oil: composite powder is in a mass ratio of 1: 1 to 99: 1.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010184912A (en) * | 2009-02-13 | 2010-08-26 | Kao Corp | Water-in-oil type emulsion cosmetic |
| WO2021200879A1 (en) * | 2020-03-30 | 2021-10-07 | 積水ポリマテック株式会社 | Silicone composition and method for manufacturing silicone composition |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2010184912A (en) * | 2009-02-13 | 2010-08-26 | Kao Corp | Water-in-oil type emulsion cosmetic |
| WO2021200879A1 (en) * | 2020-03-30 | 2021-10-07 | 積水ポリマテック株式会社 | Silicone composition and method for manufacturing silicone composition |
| CN115052924A (en) * | 2020-03-30 | 2022-09-13 | 积水保力马科技株式会社 | Silicone composition and method for producing silicone composition |
| CN115052924B (en) * | 2020-03-30 | 2024-01-16 | 积水保力马科技株式会社 | Organosilicon composition and method for producing organosilicon composition |
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