JPH09124432A - Production of liquid crystal type emulsion and liquid crystal type emulsion composition obtained thereby - Google Patents
Production of liquid crystal type emulsion and liquid crystal type emulsion composition obtained therebyInfo
- Publication number
- JPH09124432A JPH09124432A JP30347395A JP30347395A JPH09124432A JP H09124432 A JPH09124432 A JP H09124432A JP 30347395 A JP30347395 A JP 30347395A JP 30347395 A JP30347395 A JP 30347395A JP H09124432 A JPH09124432 A JP H09124432A
- Authority
- JP
- Japan
- Prior art keywords
- skin
- liquid crystal
- type emulsion
- phase transition
- component
- 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.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/52—Liquid crystal materials characterised by components which are not liquid crystals, e.g. additives with special physical aspect: solvents, solid particles
- C09K19/54—Additives having no specific mesophase characterised by their chemical composition
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K19/00—Liquid crystal materials
- C09K19/52—Liquid crystal materials characterised by components which are not liquid crystals, e.g. additives with special physical aspect: solvents, solid particles
- C09K2019/528—Surfactants
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Cosmetics (AREA)
Abstract
Description
【0001】[0001]
【発明の属する技術分野】本発明は、医薬部外品、化粧
品等に適用されるエマルションの製造方法および該製造
方法によって得られるエマルション組成物に関する。TECHNICAL FIELD The present invention relates to a method for producing an emulsion applied to quasi drugs, cosmetics and the like, and an emulsion composition obtained by the method.
【0002】[0002]
【従来の技術及び発明が解決しようとする課題】皮膚の
水分は、真皮の基底細胞層から表皮の、さらに角質層へ
と外層に向かうにつれて減少する水分含量の勾配に沿っ
て常に皮膚内部から外層部へ移動し、角質層を通じて外
部へ蒸散しているが、この水分蒸散は主に角質層の緻密
な細胞組織からなる防御機能(バリヤー機能)により制
御されており、該蒸散量(経表皮水分蒸散量(Tran
sepidermal Water Loss)、以下
TWL値と略す)は、例えば健常な皮膚の正常な状態に
おける前腕部皮表では0.2〜0.3mg/cm2/hr、通
常は0.25mg/cm2/hr程度以下に保持されている。BACKGROUND OF THE INVENTION Moisture of the skin is constantly reduced from the inside to the outside of the skin along a gradient of water content decreasing from the basal cell layer of the dermis to the outer layer of the epidermis to the stratum corneum. It moves to the outer part and evaporates to the outside through the stratum corneum, but this water evaporation is mainly controlled by the defense function (barrier function) composed of the dense cellular tissue of the stratum corneum, and the amount of evaporation (transepidermal water content). Transpiration (Tran
sepidermal Water Loss), hereinafter referred to as TWL value), for example, in the forearm skin surface in a normal state of healthy skin 0.2~0.3mg / cm 2 / hr, usually 0.25mg / cm 2 / hr It is kept below the level.
【0003】これに対して、通常にみられる乾燥皮膚
(ドライスキン)あるいは老化皮膚にみられる乾燥皮膚
では、その程度に応じてTWL値は上記の範囲の上限値
もしくはそれよりも大きな値を示し、皮膚の水分保持機
能が低下していることが認められる。これはそれら乾燥
皮膚の場合、角質層の防御機能による通常の制御限界を
越えた状態にあるか、あるいは該防御機能が衰えている
ことに由来するものである。On the other hand, in the case of dry skin which is usually observed or dry skin which is observed in aged skin, the TWL value shows an upper limit value of the above range or a value larger than that depending on the degree. , It is recognized that the water retention function of the skin is lowered. This is because, in the case of those dry skins, the normal control limit of the defense function of the stratum corneum has been exceeded, or the defense function has declined.
【0004】したがって、角質層の細胞組織を緻密化
し、その防御機能を賦活することができれば、これによ
って皮膚の水分保持機能が亢進され、皮膚は健常な状態
に保持されるとともに、さらに乾燥皮膚の改善ないしは
修復が可能となることになる。Therefore, if the cellular tissue of the stratum corneum can be compacted and its defense function can be activated, the water retention function of the skin is enhanced by this, and the skin is kept in a healthy state, and further dry skin It will be possible to improve or repair.
【0005】角質水分含有量の低下を防止し、皮膚機能
を正常に維持する方法としてセラミド(誘導体)や哺乳
動物の脳組織より抽出される成分等、角質層に本来存在
し、水分保持機能を担っている脂質成分を皮膚に適用す
る方法が報告されている(特公平4−57641号公
報、特開昭61−260008号公報、特開昭62−2
9508号公報、特開昭62−56414号公報、特開
昭63−192703号公報)。これらの脂質成分は皮
膚に適用した際、皮膚上で水を含んだ液晶状態を形成
し、皮膚からの水分蒸散を防止するとともに、保水性を
向上させ、皮膚機能を正常に維持するものである。As a method for preventing the decrease in the water content of the keratin and maintaining the normal skin function, ceramide (derivative) and components extracted from the brain tissue of mammals, etc., which are originally present in the horny layer and have a water retaining function. A method of applying a lipid component to the skin has been reported (JP-B-4-57641, JP-A-61-260008, JP-A-62-2).
9508, JP-A-62-56414, JP-A-63-192703). When applied to the skin, these lipid components form a liquid crystal state containing water on the skin, prevent water evaporation from the skin, improve water retention, and maintain normal skin function. .
【0006】これらの脂質成分は若干の界面活性を有し
てはいるものの油剤を乳化するほどの界面活性は有して
いない。したがって、これらの脂質成分を皮膚へ適用す
るためのエマルション製剤へ配合するためには、他の界
面活性剤が必要となる。このような界面活性剤は乳化状
態も安定に維持する。しかし、この界面活性剤によって
これらの脂質成分が形成する液晶が破壊され、目的とす
る皮膚の水分保持機能の亢進・維持や皮膚機能の改善・
修復が阻害されてしまう。このような理由から、現状で
はこれらの脂質を用いた製剤を皮膚へ適用しても、十分
な効果を得ることができなかった。Although these lipid components have some surface activity, they do not have enough surface activity to emulsify an oily agent. Therefore, other surfactants are required to incorporate these lipid components into emulsion formulations for application to the skin. Such a surfactant maintains a stable emulsified state. However, this surfactant destroys the liquid crystals formed by these lipid components, and promotes / maintains the intended water retention function of the skin and improves the skin function.
Repair is hindered. For this reason, at present, even if a preparation using these lipids is applied to the skin, a sufficient effect cannot be obtained.
【0007】[0007]
【課題を解決するための手段】本発明者らは、上記問題
点に鑑み、他の界面活性剤を用いず、皮膚の水分保持機
能の亢進・維持や皮膚機能の改善・修復効果に優れるエ
マルションの製造方法および該製造方法によって得られ
るエマルション組成物について鋭意検討した結果、本発
明を見いだした。すなわち、本発明の請求項1は、セラ
ミド、グルコシルセラミド、ガラクトシルセラミドより
選ばれた少なくとも一種、コレステロールおよび脂肪酸
を油剤中にてその中のセラミド類と脂肪酸の混合系の相
転移温度以上に加熱した後、水溶性多価アルコールを添
加し、得られた組成物を同じ相転移温度以上の水性媒体
と撹拌しながら混合し、相転移温度以下に冷却すること
によって得ることを特徴とする液晶型エマルションの製
造方法である。また、本発明の請求項2は、該製造方法
によって得られた液晶型エマルション組成物である。In view of the above problems, the inventors of the present invention did not use other surfactants, and an emulsion excellent in the effects of promoting and maintaining the water retention function of the skin and improving and repairing the skin function. The present invention has been found as a result of intensive studies on the method for producing the emulsion and the emulsion composition obtained by the method. That is, according to claim 1 of the present invention, at least one selected from ceramide, glucosylceramide, and galactosylceramide, cholesterol and fatty acid are heated in an oil agent to a temperature not lower than the phase transition temperature of the mixed system of ceramides and fatty acid therein. After that, a water-soluble polyhydric alcohol is added, the resulting composition is mixed with an aqueous medium having the same phase transition temperature or higher with stirring, and the liquid crystal emulsion is obtained by cooling to below the phase transition temperature. Is a manufacturing method. A second aspect of the present invention is a liquid crystal emulsion composition obtained by the production method.
【0008】この製造方法にて得られる液晶型エマルシ
ョンは、油滴粒子のまわりにこれらの脂質が液晶状に配
向しており、これらの脂質以外の界面活性剤を用いなく
とも、良好な乳化状態を長期にわたって維持できる。The liquid crystal emulsion obtained by this production method has these lipids oriented in a liquid crystal state around the oil droplet particles, and has a good emulsified state without using a surfactant other than these lipids. Can be maintained for a long time.
【0009】[0009]
【発明の実施の形態】以下、本発明の実施の形態につい
て説明する。本発明に用いるセラミド、グルコシルセラ
ミド、ガラクトシルセラミドは、人、豚、牛、馬、羊な
どの哺乳動物の表皮に微量存在する化合物であって(バ
イオケミストリー、アンド、フィジオロジー、オブ、
ザ、スキン、第363頁〜第381頁(Biochemistry a
nd Physiology of the Skin,Oxford University Press,
Inc.1983 New York)、ジャーナル、オブ、リピッド、
リサーチ第24巻、1983年第131頁〜第140頁
(Journal of Lipid Research Volume 24,1983)等を参
照)、これらの動物表皮より通常の抽出方法にて得るこ
とが可能である。本発明においては、特開昭61−27
1205号公報や生化学実験書(脂質の生化学、生化学
実験講座、第3巻、20〜21頁、1974年、日本生
化学会編、東京化学同人)に記載されている製造方法に
より得られるセラミド、グルコシルセラミド、ガラクト
シルセラミドを用いることができる。BEST MODE FOR CARRYING OUT THE INVENTION Embodiments of the present invention will be described below. Ceramide used in the present invention, glucosyl ceramide, galactosyl ceramide is a compound that is present in a trace amount in the epidermis of mammals such as humans, pigs, cows, horses, and sheep (biochemistry, and, physiology, of,
The Skin, pp. 363-381 (Biochemistry a
nd Physiology of the Skin, Oxford University Press,
Inc.1983 New York), Journal, Of, Lipid,
Research Vol. 24, pp. 131-140, 1983 (Journal of Lipid Research Volume 24, 1983), etc.), and can be obtained from these animal epidermis by a usual extraction method. In the present invention, JP-A-61-27
No. 1205 gazette and biochemistry experiment manual (lipid biochemistry, biochemistry experiment course, Volume 3, 20-21, 1974, edited by the Biochemical Society of Japan, Tokyo Kagaku Dojin). Ceramide, glucosylceramide and galactosylceramide can be used.
【0010】本発明に用いる脂肪酸は一般に化粧料に用
いられるもので、飽和脂肪酸、不飽和脂肪酸あるいは直
鎖脂肪酸、分岐脂肪酸いずれでも良い。炭素数12〜2
4のものが用いられ、さらに好ましくは炭素数14〜2
2のものが用いられる。また、本発明に用いられる油剤
は一般に化粧料に用いられるものであればよく、特に室
温で液状のものが好ましい。例えば、スクワラン、流動
パラフィン等の炭化水素類、オリーブ油、ホホバ油等の
動植物油脂、ミリスチン酸イソプロピル、ミリスチン酸
オクチルドデシル、イソステアリン酸オクチル等のエス
テル類、トリイソステアリン酸グリセリン、トリ2−エ
チルヘキサン酸グリセリン、トリオレイン、トリカプリ
リン等のトリグリセリド類等が挙げられる。The fatty acid used in the present invention is generally used in cosmetics, and may be saturated fatty acid, unsaturated fatty acid, straight chain fatty acid or branched fatty acid. Carbon number 12-2
4 carbon atoms are used, and more preferably 14 to 2 carbon atoms.
2 is used. The oil agent used in the present invention may be any oil agent generally used in cosmetics, and is preferably liquid at room temperature. For example, hydrocarbons such as squalane and liquid paraffin, animal and vegetable oils and fats such as olive oil and jojoba oil, isopropyl myristate, octyldodecyl myristate, octyl isostearate and the like esters, glyceryl triisostearate, glyceryl tri-2-ethylhexanoate. And triglycerides such as triolein and tricaprylin.
【0011】さらに、本発明に用いられる水溶性多価ア
ルコールは分子内に水酸基を2個以上有するもので、一
般に化粧料に用いられるものであればよい。例えば、ジ
プロピレングリコール、1,3−ブチレングリコール、
1,4−ブチレングリコール、グリセリン、ジグリセリ
ン、トリグリセリン、テトラグリセリン、デカグリセリ
ン、マルチトール、ショ糖、フラクトース、キシリトー
ル、ソルビトール、マルトトリオース、ポリエチレング
リコール等が挙げられ、これらのうち1種または2種以
上が用いられる。Further, the water-soluble polyhydric alcohol used in the present invention has two or more hydroxyl groups in the molecule, and may be any one generally used in cosmetics. For example, dipropylene glycol, 1,3-butylene glycol,
1,4-butylene glycol, glycerin, diglycerin, triglycerin, tetraglycerin, decaglycerin, maltitol, sucrose, fructose, xylitol, sorbitol, maltotriose, polyethylene glycol, and the like, and one or more of these may be used. Two or more types are used.
【0012】セラミド、グルコシルセラミド、ガラクト
シルセラミド、コレステロール及び脂肪酸の配合量は、
最終製剤の総量を基準として、各々大略0.01〜5.
0wt%が好ましい。また、油剤は最終製剤の総量を基
準として、大略0.1〜60wt%が好ましく、上記脂
質総量に対して0.1〜100倍の間であれば良い。さ
らに、多価アルコールは最終製剤の総量を基準として、
大略1〜60wt%が好ましく、上記油剤に対して0.
1〜100倍の間であれば良い。配合量がこの範囲より
少ないと効果が十分に達成されない。また、これらが上
記量を越えてもその増加分に見合った効果の向上は望め
ない。The blending amounts of ceramide, glucosylceramide, galactosylceramide, cholesterol and fatty acid are
Based on the total amount of the final preparation, each is approximately 0.01 to 5.
0 wt% is preferred. The oil agent is preferably about 0.1 to 60 wt% based on the total amount of the final preparation, and may be 0.1 to 100 times the total amount of the above lipid. Furthermore, polyhydric alcohol is based on the total amount of the final preparation,
About 1 to 60 wt% is preferable, and it is 0.
It may be between 1 and 100 times. If the blending amount is less than this range, the effect cannot be sufficiently achieved. Further, even if the amount exceeds the above amount, the improvement of the effect commensurate with the increased amount cannot be expected.
【0013】本発明の皮膚化粧料には必要に応じて色
素、香料、防腐剤、界面活性剤、顔料、酸化防止剤等を
本発明の目的を達成する範囲内で適宜配合することがで
きる。本発明の皮膚化粧料は、例えばクリーム類、乳液
類、パック類、美容液等に適用することができる。If necessary, the skin cosmetic of the present invention may be appropriately mixed with a dye, a fragrance, an antiseptic, a surfactant, a pigment, an antioxidant, etc. within a range that achieves the object of the present invention. The skin cosmetic of the present invention can be applied to, for example, creams, emulsions, packs, beauty essences and the like.
【0014】[0014]
【実施例】以下、実施例について説明する。なお、実施
例中で使用したセラミド、グルコシルセラミド、ガラク
トシルセラミドは以下の方法によって得たものを用い
た。Embodiments will be described below. The ceramide, glucosylceramide, and galactosylceramide used in the examples were those obtained by the following method.
【0015】(ガラクトシルセラミドの製造)牛脳を細
切後、アセトンを添加し、ポリトロンにてホモジネート
を調製した。不溶物を濾別後、クロロホルム−メタノー
ル(2:1)を添加、一夜放置後、抽出液を減圧乾固し
た。ついで、冷アセトンに抽出液を懸濁させ、4℃一夜
放置後、沈査を分離した。さらに冷エーテルにて同様の
操作を行い沈査を得た。沈査より、シリカゲルカラムク
ロマトグラフィー(溶媒=クロロホルム:メタノール=
2:1)によりガラクトシルセラミドを分離して得た。(Production of galactosyl ceramide) Bovine brain was cut into small pieces, acetone was added thereto, and a homogenate was prepared with a polytron. The insoluble material was filtered off, chloroform-methanol (2: 1) was added, the mixture was left standing overnight, and the extract was dried under reduced pressure. Then, the extract was suspended in cold acetone, left overnight at 4 ° C., and the precipitate was separated. The same operation was performed with cold ether to obtain a precipitate. From the precipitation, silica gel column chromatography (solvent = chloroform: methanol =
It was obtained by separating galactosylceramide by 2: 1).
【0016】(グルコシルセラミドの製造)上記(ガラ
クトシルセラミドの製造)中、牛脳を牛脾臓に変えるほ
かは全く同様にしてグルコシルセラミドを分離して得
た。(Production of glucosylceramide) In the above (production of galactosylceramide), glucosylceramide was obtained in the same manner except that bovine brain was changed to bovine spleen.
【0017】(セラミドの製造)上記(ガラクトシルセ
ラミドの製造)中、ガラクトシルセラミドを分離後の同
じシリカゲルカラムクロマトグラフィーにて、溶媒をク
ロロホルム:メタノール=1:1にすることによってス
フィンゴミエリンを分離した。これをエーテル−エタノ
ール(98:2)に溶解後、100mMトリス−塩酸緩
衝液(20mM塩化カルシウム含有)及びホスホリパー
ゼC(ウェルシュ菌由来、Sigma社製)を加え、3
0℃3時間振とうさせた。その後、クロロホルム−メタ
ノール(2:1)を添加し撹拌、遠心し、下層を分離し
減圧乾固した。乾固物よりシリカゲルカラムクロマトグ
ラフィー(溶媒=クロロホルム:メタノール=9:1)
によりセラミドを分離した。(Production of ceramide) In the above (Production of galactosylceramide), sphingomyelin was separated by the same silica gel column chromatography after separation of galactosylceramide by changing the solvent to chloroform: methanol = 1: 1. This was dissolved in ether-ethanol (98: 2), 100 mM Tris-hydrochloric acid buffer (containing 20 mM calcium chloride) and phospholipase C (derived from C. perfringens, manufactured by Sigma) were added, and 3
Shake at 0 ° C. for 3 hours. Then, chloroform-methanol (2: 1) was added, and the mixture was stirred and centrifuged, and the lower layer was separated and dried under reduced pressure. Silica gel column chromatography from dry solids (solvent = chloroform: methanol = 9: 1)
To separate the ceramide.
【0018】また、本発明の液晶型エマルションの安定
性を評価するため、以下の実験を行った。The following experiments were conducted to evaluate the stability of the liquid crystal emulsion of the present invention.
【0019】(1)相転移温度の測定 本発明に用いられるセラミド類と脂肪酸の混合系の相転
移温度はDSCにて測定した。すなわち、セラミド類と
脂肪酸の混合物に蒸留水を加えて2wt%の脂質分散液
とし、これを測定用アルミパンにシールして、測定に供
した。測定は0℃〜100℃まで昇温スキャンにて行っ
た。(1) Measurement of Phase Transition Temperature The phase transition temperature of the mixed system of ceramides and fatty acid used in the present invention was measured by DSC. That is, distilled water was added to a mixture of ceramides and fatty acids to prepare a 2 wt% lipid dispersion, which was sealed in an aluminum pan for measurement and used for the measurement. The measurement was performed by a temperature rise scan from 0 ° C to 100 ° C.
【0020】(2)液晶形成の確認 本発明のエマルション組成物の液晶形成は、偏光顕微鏡
観察にて確認した。すなわち、球状のラメラ型液晶に特
有の像である「マルタの十字」の有無によって判断し
た。「マルタの十字」が観察された場合は○、観察され
ない場合は×とした。(2) Confirmation of Liquid Crystal Formation Liquid crystal formation of the emulsion composition of the present invention was confirmed by observation with a polarizing microscope. That is, the judgment was made based on the presence or absence of "Maltese cross" which is an image peculiar to the spherical lamella type liquid crystal. When the "Maltese cross" was observed, it was rated as O, and when it was not observed, it was rated as X.
【0021】(3)エマルションの安定性 本発明のエマルション組成物の安定性は、調製後30℃
にて1週間静置し、その状態を目視にて判定した。安定
な乳化状態を保っている場合は○、分離している場合は
×とした。また、その液晶構造の安定性は偏光顕微鏡に
て判定した。マルタの十字が残存している場合は○、消
失している場合は×とした。また、本発明の液晶型エマ
ルション組成物の皮膚老化防止効果を評価するために用
いた荒れ肌改善効果試験、角質層改善効果試験、保湿効
果試験(TWL値低減率)、美肌効果試験(実用テス
ト)は下記の通りである。(3) Stability of emulsion The stability of the emulsion composition of the present invention is 30 ° C. after preparation.
It was allowed to stand still for 1 week, and the state was visually evaluated. When the stable emulsified state was maintained, it was marked with ◯, and when it was separated, it was marked with x. Further, the stability of the liquid crystal structure was determined by a polarization microscope. When the Maltese cross remained, it was marked with ○, and when it disappeared, it was marked with ×. Also, the rough skin improving effect test, the stratum corneum improving effect test, the moisturizing effect test (TWL value reduction rate), and the skin beautiful effect test (practical test) used to evaluate the skin aging prevention effect of the liquid crystal emulsion composition of the present invention Is as follows.
【0022】(1)荒れ肌改善効果試験 下脚に荒れ肌を有する中高年被験者20名を対象として
4週間連続塗布効果を調べた。被験者の左側下脚試験部
位に1日1回約1gの試料を塗布し、試験開始前及び終
了後の皮膚の状態を下記の判定基準により肉眼判定し
た。右側下脚は試料を塗布せず対照とした。 皮膚乾燥度の判定基準 − :正常 ± :軽微乾燥、落屑なし + :乾燥、落屑軽度 ++ :乾燥、落屑中等度 +++:乾燥、落屑顕著(1) Rough skin improvement effect test The application effect for 20 consecutive weeks was examined for 20 middle-aged and elderly subjects having rough skin on the lower legs. About 1 g of the sample was applied to the left lower leg test site of the test subject once a day, and the condition of the skin before and after the start of the test was visually judged by the following judgment criteria. The lower right leg served as a control without the application of the sample. Criteria for skin dryness −: Normal ±: Minor dryness, no desquamation +: Dry, mild desquamation ++: Moderate, desquamation moderate +++: Dry, remarkable desquamation
【0023】試験前後の試験部位と対照部位の判定結果
を比較し、皮膚乾燥度が2段階以上改善された場合(例
えば、+→−、++→±)を有効、1段階改善された場
合をやや有効、変化がなかった場合を無効とした。試験
結果は有効、やや有効となった被験者の人数で示した。By comparing the judgment results of the test site before and after the test and the control site, the case where the skin dryness is improved by two stages or more (for example, + →-, ++ → ±) is effective, and the case where it is improved by one stage is Somewhat valid, invalid if there was no change. The test results were indicated by the number of subjects who were effective or slightly effective.
【0024】(2)角質層改善効果試験 前述の荒れ肌改善効果試験開始前及び終了後の被験者皮
膚にスコッチテープ(ニチバンメンディングテープ)を
接着し、これを剥離した時テープに付着した角質細胞の
状態を走査型電子顕微鏡によって詳細に調べ、下記の基
準によって皮膚角質細胞抗剥離性を解析し、角質層改善
効果(角質細胞抗剥離性増大効果)を求めた。 (2) Stratum corneum layer improving effect test Scotch tape (Nichiban Mending Tape) was adhered to the skin of the subject before and after the above rough skin improving effect test was started. The condition was examined in detail by a scanning electron microscope, the skin keratinocyte anti-peeling property was analyzed according to the following criteria, and the stratum corneum improving effect (horny cell anti-peeling increasing effect) was determined.
【0025】評価は、4週間連続塗布後の試験部位の評
価点と対照部位のそれとの差が2点以上の場合を有効、
1点の場合をやや有効、0点の場合を無効とした。試験
結果は、20人中有効、やや有効となった被験者の人数
で示した。The evaluation is effective when the difference between the evaluation point of the test site and that of the control site after continuous application for 4 weeks is 2 or more,
The case of 1 point was set to be slightly valid, and the case of 0 point was set to be invalid. The test results are shown by the number of valid subjects in 20 persons, and the number of subjects who became slightly valid.
【0026】(3)保湿効果試験(TWL値低減率) 前述の荒れ肌改善効果試験開始前及び終了後の被験者皮
膚を対照として4週間連続塗布前及び塗布後のTWL値
及びTWL値の低減率(水分保持機能亢進効果)を下記
の如く算出して、保湿効果を調べた。(3) Moisturizing effect test (TWL value reduction rate) The reduction rate of TWL value and TWL value before and after continuous application for 4 weeks using the subject skin before and after the rough skin improving effect test described above as a control ( The water retention function enhancement effect) was calculated as follows, and the moisturizing effect was examined.
【0027】TWL値 密閉した皮表上の空気の一定時間内の温度変化を電気抵
抗にて測定する方法を用いた。即ち、被試験者の皮表を
測定用セルで密閉し、セルに強制乾燥した空気を通気し
てセル内を乾燥空気で充分置換した後、乾燥空気の通気
を停止してその時点でのセル内の相対湿度RHs(%)
を求め、次いで10分間放置して再びセル内の相対湿度
RH10(%)を測定し、この時の湿度変化から下記の
式によりTWL値(mg/cm2 /hr)を算出した。 TWL値=〔(RH10−RHs)×Dt×V×6〕/
S×100 但し、Dt:測定温度下(t℃)での空気中の飽和水蒸
気の密度(mg/l) V :セルの容積(l) S :測定面積(cm2 )TWL Value A method was used in which the temperature change of air on the sealed skin surface within a certain period of time was measured by electric resistance. That is, the skin surface of the test subject is sealed with a measurement cell, and after forcedly drying air through the cell to sufficiently replace the inside of the cell with dry air, the ventilation of the dry air is stopped and the cell at that time is stopped. Relative humidity RHs (%)
Then, the relative humidity RH10 (%) in the cell was measured again after standing for 10 minutes, and the TWL value (mg / cm 2 / hr) was calculated from the change in humidity at this time by the following formula. TWL value = [(RH10−RHs) × Dt × V × 6] /
S × 100 where Dt: density of saturated water vapor in air at measurement temperature (t ° C.) (mg / l) V: cell volume (l) S: measurement area (cm 2 )
【0028】TWL値の低減率 TWL値の低減率は、試料塗布前後のTWL値、TWL
A及びTWLBを下記の式に代入して算出した。 TWL値低減率=(1−TWLB/TWLA)×100
(%) TWLA:試料塗布前のTWL値 TWLB:試料塗布後のTWL値 TWL値の低減率が20%以上の場合を「有効」、低減
率が20%未満の場合を「無効」、とした。試料結果
は、20人中の「有効」であった被験者の人数で表示し
た。Reduction rate of TWL value The reduction rate of the TWL value is the TWL value before and after the sample application, TWL
It calculated by substituting A and TWLB into the following formula. TWL value reduction rate = (1-TWLB / TWLA) × 100
(%) TWLA: TWL value before sample application TWLB: TWL value after sample application TWL value reduction rate of 20% or more was "valid", reduction rate of less than 20% was "invalid" . The sample results were displayed by the number of subjects who were “effective” in 20 persons.
【0029】(4)美肌効果試験(実用テスト) 荒れ肌、小皺、乾燥肌等を訴える女子被験者(35〜5
5才)20人に試料を1日2回(朝・夕)連続3ケ月後
の効果を評価した。試験結果は、皮膚の湿潤性、平滑
性、弾力性の各項目に対して、「皮膚に潤いが生じ
た」、「皮膚が滑らかになった」、「皮膚に張りが生じ
た」と回答した人数で示した。(4) Skin beautification test (practical test) Female subjects (35-5) who complain of rough skin, fine wrinkles, dry skin, etc.
The effect was evaluated on 20 people (5 years old) 20 times twice a day (morning and evening) after 3 consecutive months. In the test results, for each item of skin wettability, smoothness, and elasticity, the respondents answered that "skin was moistened", "skin became smooth", and "skin became taut" Indicated by the number of people.
【0030】実施例1〜4、比較例1〜5 表1の組成にてスキンクリームを調製し、前記諸実験を
行った。 (1) 組成(スキンクリーム)Examples 1 to 4 and Comparative Examples 1 to 5 Skin creams having the compositions shown in Table 1 were prepared and the above-mentioned experiments were conducted. (1) Composition (skin cream)
【0031】[0031]
【表1】 [Table 1]
【0032】スキンクリーム中に配合した本発明の脂質
類を表2に示す。Table 2 shows the lipids of the present invention incorporated into the skin cream.
【0033】[0033]
【表2】 [Table 2]
【0034】(2)相転移温度の測定 組成例1〜3の相転移温度を測定した結果を以下に示
す。 (2) Measurement of phase transition temperature The results of measuring the phase transition temperatures of Composition Examples 1 to 3 are shown below.
【0035】(3)調製法 比較例1 (B)成分(組成例1)を(A)成分に加え、60℃に
加熱した後、(C)成分を添加し、これを、50℃に加
熱した(D)成分に撹拌しながら加え、30℃まで冷却
した。(3) Preparation Method Comparative Example 1 The component (B) (composition example 1) was added to the component (A) and heated to 60 ° C., then the component (C) was added, and this was heated to 50 ° C. The resulting component (D) was added with stirring and cooled to 30 ° C.
【0036】比較例2 (B)成分(組成例2)を(A)成分に加え、50℃に
加熱した後、(C)成分を添加し、これを、50℃に加
熱した(D)成分に撹拌しながら加え、30℃まで冷却
した。Comparative Example 2 The component (B) (composition example 2) was added to the component (A) and heated to 50 ° C., then the component (C) was added, and the component (D) was heated to 50 ° C. It was added to the mixture with stirring and cooled to 30 ° C.
【0037】比較例3 (B)成分(組成例3)を(A)成分に加え、30℃に
加熱した後、(C)成分を添加し、さらに30℃に加熱
した(D)成分を撹拌しながら加え、混合した。Comparative Example 3 The component (B) (composition example 3) was added to the component (A), heated to 30 ° C., the component (C) was added, and the component (D) heated to 30 ° C. was stirred. While adding, mixed.
【0038】比較例4 (B)成分(組成例1)を(A)成分に加え、80℃に
加熱した後、80℃に加熱した(C)成分と(D)成分
の混合物を撹拌しながら加え、30℃まで冷却した。Comparative Example 4 The component (B) (composition example 1) was added to the component (A), heated to 80 ° C., and then the mixture of the components (C) and (D) heated to 80 ° C. was stirred. In addition, it cooled to 30 degreeC.
【0039】比較例5 (B)成分(組成例2)を(A)成分に加え、70℃に
加熱し、これを、80℃に加熱した(C)成分と(D)
成分の混合物に撹拌しながら加え、30℃まで冷却し
た。Comparative Example 5 Component (B) (Composition Example 2) was added to component (A) and heated to 70 ° C., which was heated to 80 ° C. (C) component and (D).
The mixture was added to the mixture of components with stirring and cooled to 30 ° C.
【0040】実施例1 (B)成分(組成例1)を(A)成分に加え、80℃に
加熱した後、(C)成分を添加し、これを、80℃に加
熱した(D)成分に撹拌しながら加え、30℃まで冷却
した。Example 1 Component (B) (composition example 1) was added to component (A) and heated to 80 ° C., then component (C) was added and this was heated to 80 ° C. (D) component It was added to the mixture with stirring and cooled to 30 ° C.
【0041】実施例2 (B)成分(組成例2)を(A)成分に加え、70℃に
加熱した後、(C)成分を添加し、これを、70℃に加
熱した(D)成分に撹拌しながら加え、30℃まで冷却
した。Example 2 Component (B) (composition example 2) was added to component (A) and heated to 70 ° C., then component (C) was added, and component (D) was heated to 70 ° C. It was added to the mixture with stirring and cooled to 30 ° C.
【0042】実施例3 (B)成分(組成例3)を(A)成分に加え、60℃に
加熱した後、(C)成分を添加し、さらに60℃に加熱
した(D)成分を撹拌しながら加えて混合し、30℃ま
で冷却した。Example 3 The component (B) (composition example 3) was added to the component (A), heated to 60 ° C., the component (C) was added, and the component (D) heated to 60 ° C. was stirred. While adding, they were mixed and cooled to 30 ° C.
【0043】実施例4 (B)成分(組成例1)を(A)成分に加え、80℃に
加熱した後、(C)成分を添加し、さらに80℃に加熱
した(D)成分を撹拌しながら加えて混合し、30℃ま
で冷却した。Example 4 Component (B) (composition example 1) was added to component (A) and heated to 80 ° C., then component (C) was added and component (D) heated to 80 ° C. was stirred. While adding, they were mixed and cooled to 30 ° C.
【0044】(4)液晶形成の確認、エマルションの安
定性 比較例1〜5、実施例1〜4について結果を表3に示
す。(4) Confirmation of liquid crystal formation and emulsion stability Table 3 shows the results of Comparative Examples 1 to 5 and Examples 1 to 4.
【0045】[0045]
【表3】 [Table 3]
【0046】(5) 特性 表3に示す如く、本発明の製造方法による実施例1〜4
のスキンクリームは、比較例1〜3の相転移温度以下に
加熱する方法、比較例4〜5の水溶性多アルコールを水
性媒体に加える方法によるスキンクリームと比較して、
液晶が形成されており、また、そのエマルションは安定
であった。(5) Characteristics As shown in Table 3, Examples 1 to 4 according to the manufacturing method of the present invention
Compared with the skin creams of Comparative Examples 1 to 3 and the method of adding the water-soluble polyalcohol of Comparative Examples 4 to 5 to the aqueous medium,
A liquid crystal was formed and the emulsion was stable.
【0047】(6)皮膚老化防止効果 比較例1〜5、実施例1〜4について結果を表4に示
す。(6) Effect of Preventing Skin Aging Table 4 shows the results for Comparative Examples 1-5 and Examples 1-4.
【0048】[0048]
【表4】 [Table 4]
【0049】(7) 特性 表4に示す如く、本発明の製造方法により調製された液
晶型エマルション組成物である実施例1〜4のスキンク
リームは、比較例1〜5の液晶を形成していないスキン
クリームと比較して、諸特性の全てに亘って優れている
ことが認められた。(7) Properties As shown in Table 4, the skin creams of Examples 1 to 4, which are liquid crystal emulsion compositions prepared by the production method of the present invention, form the liquid crystals of Comparative Examples 1 to 5. It was found to be superior in all of its properties as compared to the non-skin cream.
【0050】[0050]
【発明の効果】以上記載の如く、本発明の製造方法によ
れば安定な液晶型エマルションを調製することができ、
また該エマルションは、皮膚が本来備えている水分保持
機能を亢進、維持することによって皮膚を健常な状態に
改善あるいは修復して、かつ美肌作用を有することが明
かである。As described above, according to the production method of the present invention, a stable liquid crystal type emulsion can be prepared,
Further, it is clear that the emulsion improves or restores the skin to a healthy state by enhancing and maintaining the water retention function originally possessed by the skin, and has a skin beautifying action.
Claims (2)
トシルセラミドより選ばれた少なくとも一種、コレステ
ロールおよび脂肪酸を油剤中にてその中のセラミド類と
脂肪酸の混合系の相転移温度以上に加熱した後、水溶性
多価アルコールを添加し、得られた組成物を同じ相転移
温度以上の水性媒体と撹拌しながら混合し、相転移温度
以下に冷却することによって得ることを特徴とする液晶
型エマルションの製造方法。1. At least one selected from ceramides, glucosylceramides and galactosylceramides, cholesterol and fatty acids are heated in an oil solution above the phase transition temperature of a mixed system of ceramides and fatty acids, and then water-soluble A process for producing a liquid crystal emulsion, which comprises adding a polyhydric alcohol, mixing the obtained composition with an aqueous medium having the same phase transition temperature or higher while stirring, and cooling the mixture to the phase transition temperature or lower.
る液晶型エマルション組成物。2. A liquid crystal emulsion composition obtained by the production method according to claim 1.
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ID=17921390
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