JP5840107B2 - ヒアルロン酸ゲル及びその製造方法 - Google Patents
ヒアルロン酸ゲル及びその製造方法 Download PDFInfo
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- JP5840107B2 JP5840107B2 JP2012242203A JP2012242203A JP5840107B2 JP 5840107 B2 JP5840107 B2 JP 5840107B2 JP 2012242203 A JP2012242203 A JP 2012242203A JP 2012242203 A JP2012242203 A JP 2012242203A JP 5840107 B2 JP5840107 B2 JP 5840107B2
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- Prior art keywords
- hyaluronic acid
- acid
- gel
- weight
- skin
- Prior art date
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- KIUKXJAPPMFGSW-DNGZLQJQSA-N (2S,3S,4S,5R,6R)-6-[(2S,3R,4R,5S,6R)-3-Acetamido-2-[(2S,3S,4R,5R,6R)-6-[(2R,3R,4R,5S,6R)-3-acetamido-2,5-dihydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-2-carboxy-4,5-dihydroxyoxan-3-yl]oxy-5-hydroxy-6-(hydroxymethyl)oxan-4-yl]oxy-3,4,5-trihydroxyoxane-2-carboxylic acid Chemical compound CC(=O)N[C@H]1[C@H](O)O[C@H](CO)[C@@H](O)[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@H](O[C@H]2[C@@H]([C@@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@H](O3)C(O)=O)O)[C@H](O)[C@@H](CO)O2)NC(C)=O)[C@@H](C(O)=O)O1 KIUKXJAPPMFGSW-DNGZLQJQSA-N 0.000 title claims description 112
- 229960003160 hyaluronic acid Drugs 0.000 title claims description 112
- 238000004519 manufacturing process Methods 0.000 title claims description 8
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- 150000005846 sugar alcohols Polymers 0.000 claims description 16
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
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- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 2
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 22
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Description
炭酸ガスを皮膚に吸収させて血流を改善する化粧料も知られている(特許文献8)。しかしこの化粧料も、使用時に炭酸塩を含む製剤と酸性成分を含む製剤を混合し炭酸ガスを発生させつつ顔に塗るものであり使用が煩雑である。
さらに本発明が解決しようとする課題は、皮膚に適用し抗シワ効果や美容効果の高い化粧料を提供することである。
速やかに溶解するのは、その様に素材が選択されているためである。
多価カルボン酸若しくはオキシカルボン酸は、ヒアルロン酸100重量部に対して10重量部以上400重量部以下が好ましく、10重量部以上100重量部以下がさらに好ましい。多価アルコールは、ヒアルロン酸100重量部に対して100重量部以上8000重量部以下が好ましい。その中には化粧用有価成分を含有してもよい。
多価カルボン酸若しくはオキシカルボン酸の量は、ヒアルロン酸100重量部に対して10重量部以上が好ましく、20〜100重量部の範囲がより好ましい。10重量部より少ないと、優れた弾性体のゲルを形成できない。一方、ゲル形成には100重量部で十分であり、これ以上はゲルの酸性度が不必要に高くなり好ましくない。
多価アルコールの量は、ヒアルロン酸100重量部に対して100重量部以上あれば好ましく、200〜8000重量部の範囲がより好ましい。多価アルコールの量が100重量部より少ないと、優れた弾性体のゲルを形成できない。一方、8000重量部を超えると柔らかくなり、優れた弾性体のゲルを形成できない。
本発明においては、さらに、ヒドロキシプロピルセルロース、ポリビニルピロリドン、ポリビニルアルコール及びポリエチレングリコールからなる群より選ばれた1種以上の化合物を含んでもよい。
本発明において、ヒアルロン酸ゲルはシート状物であってもよい。
抗シワ成分としては、特に限定されないが、例えば、レチノール、レチノイン酸、酢酸レチノール、パルミチン酸レチノールなどのレチノイド、クエン酸、フルーツ酸、グリコール酸、乳酸などのα−ヒドロキシ酸、α−ヒドロキシ酸コレステロール、ルチン糖誘導体、N−メチルセリン、エラスチン、コラーゲン、セリシン、ツボクサエキス、黄金エキス、等が挙げられる。
抗アレルギー成分としては、特に限定されないが、例えば、グリチルレチン酸、グリチルリチン酸2K,などのグリチルレチン酸誘導体、甘草、クロレラ、コンフリー、ボタンピ、フユボダイジュ、エンメイソウ、セージ、シソ、ヨモギ及びそれらのエキス、チンキ或いはそれらに含まれる成分等が挙げられる。
例えば、ヒアルロン酸、多価カルボン酸若しくはオキシカルボン酸、及び多価アルコールを含む各水溶液をプロペラ式回転型撹拌装置で攪拌し均一化し調製する。この調製した水溶液をポリエチレンテレフタレートフィルム上に均一の厚みになるように塗布し、温風で乾燥することにより、透明で、均一な厚みのシート状ヒアルロン酸ゲルを製造することができる。実使用に当たってはシートを裁断して、円形、楕円形、勾玉状、フェイス状、のシート状化粧料として用いるのが望ましい。
実施例1〜29及び比較例1〜9のヒアルロン酸ゲルシートは、図1及び図2に記載の配合比(重量比)により作成した。図1、2において、ヒアルロン酸の欄の下には用いたヒアルロン酸の分子量を示している。この分子量は、いずれも購入商品に示されている数値である。H200は分子量約200万のヒアルロン酸(HA−LQH、キューピー(株)製)、H80は分子量約80万のヒアルロン酸(FCH−80、キッコーマンバイオケミファ(株)製)、H10は分子量約5〜10万のヒアルロン酸(FCH−SU、キッコーマンバイオケミファ(株)製)、H1は分子量約1万のヒアルロン酸(ヒアオリゴ、キューピー(株)製)、H0.2は分子量約2000のヒアルロン酸(マイクロヒアルロン酸、キッコーマンバイオケミファ(株)製)を表す。
また、グリセリン(濃グリセリン、ミヨシ油脂(株)製)、クエン酸(ナカライテクス(株)製)、ビタミンC誘導体(アプレシエ、昭和電工(株)製)、トコフェノール(ナカライテクス(株)製)、アデノシン(ナカライテクス(株)製)、ポリエチレングリコール(ポリエチレングリコール400、和光純薬(株)製)を用いた。その他の有価成分はいずれも粧原基記載のグレードを使用した。
上述の製造された実施例1〜29、及び比較例1〜9で得られたヒアルロン酸ゲルシートを次の3つの観点から評価した。その評価結果を図3にまとめる。
1.性状観察結果
肉眼及び感触により、柔軟性、弾性、引っ張り強度を観察した結果である。
2.皮膚密着性試験結果
ヒアルロン酸ゲルシート(2cm×2cm)をヒトボランティア前腕内側に適用し 、皮膚への密着性を試験した結果を示す。
3.溶解性試験
ヒトボランティアの前腕部にヒアルロン酸ゲルシート(2cm×2cm)を適用し 10mlの水を滴下して3分間シート上からマッサージし、ヒアルロン酸ゲルの溶 解性を観察した。
性状観察において、Aは柔軟性、弾性及び引張強度がすべて十分であることを、Bは柔軟性及び弾性が不十分であるが引張強度は十分であることを、Cはは柔軟性及び弾性は十分であるが引張強度が不十分であることを、Dは液体であって柔軟性、弾性及び引張強度が全て不可であることを表す。
皮膚密着性試験において、Aはよく密着したことを、Bは部分的に浮いて密着したことを、Cは全く密着せずはがれたことを示す。性状観察の結果がCやDであったものは、そもそもこの試験の対象にならなかった。
溶解性試験において、Aは完全に溶解したことを、Bは部分的に溶解したことを表す。
A*は溶解が速く30秒以内で溶解したことを表す。性状観察の結果がCやDであったものは、そもそもこの試験の対象にもならなかった。
ヒトボランティア5名の前腕の同一部位に朝夜2回、計7日間、以下の4つの被験サンプルを投与し、投与終了1日後(投与開始から8日後)の肌水分量についてキュートメーター(MPA580)を用いて測定した。測定結果を静電容量(単位;a.u.)として表示した。また、コントロールとして、投与前の肌水分量も測定した。投与前と比較した静電容量増加量(=水分増加量)の結果を図4にまとめた。結果は、5名の被験者の結果の平均値とその標準偏差(SD)で表示している。
試験例1: 実施例4のヒアルロン酸ゲルシート(2cm×2cm)を前腕部に30分適用後、ゲルの上に精製水約10mLを少しずつ加えて約3分間マッサージしながら溶かしたのち、精製水で洗い流して、自然乾燥させた。
試験例2: 実施例17のヒアルロン酸ゲルシート(2cm×2cm)を前腕部に30分適用後、ゲルの上に精製水約10mLを少しずつ加えて約3分間マッサージしながら溶かしたのち、精製水で洗い流して、自然乾燥させた。
試験例3: 実施例17のゲルを調製する前の水溶液約1mLを前腕部(約2cm×2cm)に適用して30分後、約3分間マッサージしたのち、精製水で洗い流して、自然乾燥させた。
試験例4: WO 01/57093の実施例6に記載の方法に従い、ヒアルロン酸(HA−LQH:キューピー(株)製)とヒアルロン酸(ヒアロオリゴ:キューピー(株)製)をそれぞれ0.5%含有する水溶液を用いて作製したヒアルロン酸ゲルシート(2cm×2cm)を前腕部に30分投与後、ゲルの上に精製水約10mLを少しずつ加えて約10分間マッサージしたのち、精製水で洗浄して、自然乾燥させた。
実施例30〜36のヒアルロン酸ゲルシートは図5に記載の配合比(重量比)により作成した。各構成成分の水溶液をプロペラ式回転型攪拌装置で攪拌均一化し調製した。調製した水溶液を厚さ26μmのポリエチレンテレフタレートフィルム(DIAFOIL #130−26:三菱樹脂(株)製)上に均一の厚みとなるよう塗布し、ギアオーブンで80℃、30分間乾燥し、厚み約200μmのヒアルロン酸ゲルシートを得た。本ヒアルロン酸ゲルシートを切断して、直径20cmの円形のヒアルロン酸ゲルシートを得、目と口に対応する部分に穴を開けたフェイスマスクを作成した。
比較例10、11のヒアルロン酸ゲルシートも図5に記載の配合比(重量比)により同様に作成した。そのフェイスマスクも同様に作成した。このヒアルロン酸ゲルシートのフィルム上の厚さはそれぞれ15μm及び25μmであった。
次いで試験化粧水をスプレーにより約0.5mLをフェイスマスク全面に吹き付けてマッサージして炭酸ガスの発泡を評価した。本試験において実施例30〜35及び比較例10、11においては化粧水Aを使用し、実施例36においては化粧水Bを使用した。
Claims (7)
- 分子量が5×10 4 〜5×10 6 ダルトンの範囲であるヒアルロン酸100重量部に対し、多価カルボン酸若しくはオキシカルボン酸を10〜100重量部、多価アルコールを100〜8000重量部の割合で含有し、
シートの厚みが30〜1000μmであるヒアルロン酸ゲルシート。 - 前記分子量が5×104〜5×106ダルトンの範囲のヒアルロン酸と、そのヒアルロン酸に対して10重量%以上の分子量が1×104ダルトン以下のヒアルロン酸を含む請求項1に記載のヒアルロン酸ゲルシート。
- 前記多価カルボン酸若しくはオキシカルボン酸が、クエン酸、酒石酸及び乳酸からなる群より選ばれた少なくとも1種以上のカルボン酸であることを特徴とする請求項1又は2に記載のヒアルロン酸ゲルシート。
- 前記多価アルコールが、グリセリンであることを特徴とする請求項1〜3のいずれか1項に記載のヒアルロン酸ゲルシート。
- ヒドロキシプロピルセルロース、ポリビルピロリドン、ポリビニルアルコール、ポリエチレングリコールからなる群より選ばれた1種以上の化合物を含むことを特徴とする請求項1〜4のいずれか1項に記載のヒアルロン酸ゲルシート。
- 化粧品や医薬品に用いられている成分をさらに含むことを特徴とする請求項1〜5のいずれか1項に記載のヒアルロン酸ゲルシート。
- 分子量が5×10 4 〜5×10 6 ダルトンの範囲であるヒアルロン酸100重量部に対し、多価カルボン酸若しくはオキシカルボン酸を10〜100重量部、多価アルコールを100〜8000重量部の割合で含有する水溶液を、ゲルシートの厚みが30〜1000μmとなるようにフィルム上に塗布した後、その水分を乾燥させることを特徴とするヒアルロン酸ゲルシートの製造方法。
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KR20200041343A (ko) * | 2017-09-04 | 2020-04-21 | 다이니치 세이카 고교 가부시키가이샤 | 의료용·미용 재료의 제조 방법 및 의료용·미용 재료 |
KR102322976B1 (ko) | 2017-09-04 | 2021-11-08 | 다이니치 세이카 고교 가부시키가이샤 | 의료용·미용 재료의 제조 방법 및 의료용·미용 재료 |
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