JPH0363209A - Production of sheet-like hyaluronic acid or its salt and its use - Google Patents
Production of sheet-like hyaluronic acid or its salt and its useInfo
- Publication number
- JPH0363209A JPH0363209A JP19654989A JP19654989A JPH0363209A JP H0363209 A JPH0363209 A JP H0363209A JP 19654989 A JP19654989 A JP 19654989A JP 19654989 A JP19654989 A JP 19654989A JP H0363209 A JPH0363209 A JP H0363209A
- Authority
- JP
- Japan
- Prior art keywords
- hyaluronic acid
- salt
- sheet
- skin
- water
- 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.)
- Pending
Links
- 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 abstract description 55
- 229920002674 hyaluronan Polymers 0.000 title claims abstract description 55
- 229960003160 hyaluronic acid Drugs 0.000 title claims abstract description 55
- 150000003839 salts Chemical class 0.000 title claims abstract description 48
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002537 cosmetic Substances 0.000 claims abstract description 22
- 239000006210 lotion Substances 0.000 claims abstract description 17
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 17
- 102000011782 Keratins Human genes 0.000 abstract description 6
- 108010076876 Keratins Proteins 0.000 abstract description 6
- 210000001061 forehead Anatomy 0.000 abstract description 4
- 230000007306 turnover Effects 0.000 abstract description 4
- 230000009759 skin aging Effects 0.000 abstract description 3
- 230000037303 wrinkles Effects 0.000 abstract description 3
- 206010040849 Skin fissures Diseases 0.000 abstract 2
- 230000002401 inhibitory effect Effects 0.000 abstract 1
- 210000003491 skin Anatomy 0.000 description 13
- 229920002385 Sodium hyaluronate Polymers 0.000 description 10
- 229940010747 sodium hyaluronate Drugs 0.000 description 10
- YWIVKILSMZOHHF-QJZPQSOGSA-N sodium;(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- Chemical compound [Na+].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 YWIVKILSMZOHHF-QJZPQSOGSA-N 0.000 description 10
- 238000000034 method Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 238000004108 freeze drying Methods 0.000 description 7
- 239000000706 filtrate Substances 0.000 description 5
- 238000007710 freezing Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 230000008014 freezing Effects 0.000 description 4
- -1 Hyaluronic acid salt Chemical class 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 210000000744 eyelid Anatomy 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 102000008186 Collagen Human genes 0.000 description 2
- 108010035532 Collagen Proteins 0.000 description 2
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 229930195725 Mannitol Natural products 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000003796 beauty Effects 0.000 description 2
- 229920001436 collagen Polymers 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000594 mannitol Substances 0.000 description 2
- 235000010355 mannitol Nutrition 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 210000000434 stratum corneum Anatomy 0.000 description 2
- 210000004127 vitreous body Anatomy 0.000 description 2
- ALSTYHKOOCGGFT-KTKRTIGZSA-N (9Z)-octadecen-1-ol Chemical compound CCCCCCCC\C=C/CCCCCCCCO ALSTYHKOOCGGFT-KTKRTIGZSA-N 0.000 description 1
- 208000036487 Arthropathies Diseases 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000283690 Bos taurus Species 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- 208000012659 Joint disease Diseases 0.000 description 1
- 241001272720 Medialuna californiensis Species 0.000 description 1
- 239000004909 Moisturizer Substances 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 210000000845 cartilage Anatomy 0.000 description 1
- 230000019522 cellular metabolic process Effects 0.000 description 1
- 239000002738 chelating agent Substances 0.000 description 1
- 210000001520 comb Anatomy 0.000 description 1
- 210000002808 connective tissue Anatomy 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000003889 eye drop Substances 0.000 description 1
- 229940012356 eye drops Drugs 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000001333 moisturizer Effects 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 229940055577 oleyl alcohol Drugs 0.000 description 1
- XMLQWXUVTXCDDL-UHFFFAOYSA-N oleyl alcohol Natural products CCCCCCC=CCCCCCCCCCCO XMLQWXUVTXCDDL-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000008213 purified water Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 210000004927 skin cell Anatomy 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、水に対して溶解性の良いシート状のヒアルロ
ン酸またはその塩（以下、ヒアルロン酸（塩）と略記す
る）を得る方法に関するものである。さらに本発明は、
かかる方法で製造されたシート状ヒアルロン酸（塩）の
化粧料への利用に関するものである。Detailed Description of the Invention (Industrial Application Field) The present invention relates to a method for obtaining sheet-like hyaluronic acid or a salt thereof (hereinafter abbreviated as hyaluronic acid (salt)) that is highly soluble in water. It is something. Furthermore, the present invention
The present invention relates to the use of sheet-like hyaluronic acid (salt) produced by such a method in cosmetics.
（従来の技術）
従来、瞼、目尻、額、臼杵、首等の部分に塗布し皮膚に
適度の潤いと「張り」を付与するいわゆるワンポイント
化粧料としては、コラーゲン加水分解物をフィルム状に
底型したものか、或いは不織布にコラーゲン加水分解物
を含浸して乾燥したものが使用されてきた。(Conventional technology) Conventionally, so-called one-point cosmetics that are applied to areas such as the eyelids, outer corners of the eyes, forehead, mortar, neck, etc. to provide appropriate moisture and ``tightness'' to the skin have been made using collagen hydrolyzate in the form of a film. A bottom-shaped one or a nonwoven fabric impregnated with collagen hydrolyzate and dried has been used.
（発明が解決しようとする課題）
ヒアルロン酸く塩）は保湿剤として優れた性質を持って
いるので、皮膚細胞を賦活化し、老化皮膚のターンオー
バーを速め、荒肌改善効果、角質改善効果に著効を呈す
ると共に、皮膚にしっとり感、なめらか感、張り及び艶
を付与し、皮膚を美しくする効果があるとされている。(Problem to be solved by the invention) Hyaluronic acid salt) has excellent properties as a moisturizer, so it activates skin cells, accelerates the turnover of aging skin, and has an effect on improving rough skin and keratin. It is said to have a remarkable effect, and is said to have the effect of making the skin beautiful by giving it a moisturizing, smoothing, firmness, and luster.
かかる効果を持つヒアルロン酸（塩）を瞼、目尻、額、
臼杵、首等の小皺の出やすい部分に塗布し皮膚に適度の
潤いと「張り」を付与するワンポイント化粧料として用
いることが望まれていた。Apply hyaluronic acid (salt) with this effect to the eyelids, outer corners of the eyes, forehead,
It was hoped that the product would be used as a one-point cosmetic that can be applied to areas where fine wrinkles tend to appear, such as the neck and neck, to provide appropriate moisture and ``tightness'' to the skin.
しかし、ヒアルロン酸（塩）の乾燥物は粉末であり、ヒ
アルロン酸（塩）の水溶液を単に乾燥して得られたシー
ト或いはフィルムは、水或いは化粧水に対して溶解性が
非常に悪く、これをワンポイント化粧料として用いるこ
とが出来なかった。However, dried hyaluronic acid (salt) is a powder, and sheets or films obtained by simply drying an aqueous solution of hyaluronic acid (salt) have very poor solubility in water or lotion; could not be used as a one-point cosmetic.
本発明は、上記の如き優れた効果を持つヒアルロン酸（
塩）を水或いは化粧水に対して溶解性の良いシート状或
いはフィルム状に製造する方法を提供することを目的と
する。The present invention provides hyaluronic acid (
It is an object of the present invention to provide a method for manufacturing salt) into a sheet or film having good solubility in water or lotion.
さらに本発明は、荒肌改善効果、角質改善効果、角質層
のターンオーバーを速くする効果、美肌効果等の皮膚老
化防止効果に優れたワンポイント化粧料を提供すること
を目的とする。A further object of the present invention is to provide a one-point cosmetic that is excellent in skin aging prevention effects such as improving rough skin, improving keratin, accelerating the turnover of the stratum corneum, and beautifying the skin.
（課題を解決するための手段）
本発明は、ヒアルロン酸（塩）の水溶液を薄層状に凍ら
せて真空凍結乾燥することを特徴とする、水、特に化粧
水に易溶解性のシート状ヒアルロン酸（塩）の製造法で
ある。また、本発明は、この製造法により製造されたシ
ート状ヒアルロン酸（塩）からなる化粧料、好ましくは
優れた美容効果をもつワンポイント化粧料への応用であ
る。(Means for Solving the Problems) The present invention provides sheet-like hyaluronic acid that is easily soluble in water, especially lotion, and is characterized by freezing an aqueous solution of hyaluronic acid (salt) into a thin layer and vacuum freeze-drying it. This is a method for producing acids (salts). Further, the present invention is applied to cosmetics made of sheet-like hyaluronic acid (salt) produced by this production method, preferably to one-point cosmetics having excellent beauty effects.
本発明に用いるヒアルロン酸は、関節、硝子体、請書、
軟骨、皮膚、鳥類のとさか等の結合組織中にその構成成
分として存在し、組織の柔軟性、構造維持、細胞の代謝
調節等に重要な機能を果たしている。またヒアルロン酸
ナトリウムは、高分子物質であり、その溶液は強い粘弾
性を持ち、保水作用を有するところから、化粧品原料と
して広く使用できるほか、眼科治療薬、目薬、関節症治
療薬としての用途がある。The hyaluronic acid used in the present invention is suitable for joints, vitreous body,
It exists as a component in connective tissues such as cartilage, skin, and bird crests, and plays important functions in maintaining tissue flexibility, structure, and regulating cell metabolism. In addition, sodium hyaluronate is a polymeric substance, and its solution has strong viscoelasticity and water-retaining properties, so it can be widely used as a raw material for cosmetics, as well as ophthalmological drugs, eye drops, and arthropathy drugs. be.
ヒアルロン酸ナトリウムは工業的には、にわとりのとさ
か、牛の目の硝子体、又は調帯等から抽出する抽出法か
、或いはヒアルロン酸を生産する能力を持つ微生物を培
地に培養して製造する方法（！１酵法）が行われている
６本発明に用いられるヒアルロン酸（塩）は抽出法或い
は醗酵法いずれの方法で製造されたものでもよい。Industrially, sodium hyaluronate is manufactured by extraction methods such as extraction from chicken combs, vitreous bodies of cows' eyes, or zona, or by culturing microorganisms capable of producing hyaluronic acid in a medium. The hyaluronic acid (salt) used in the present invention may be produced by either an extraction method or a fermentation method.
現在、工業的に製造されているヒアルロン酸（塩）の分
子量は５万から３００万前後のものまであるが、本発明
に用いるヒアルロン酸（塩）の分子量は、この範囲のも
のであればいずれのものも用いることが出来る。Currently, the molecular weight of industrially produced hyaluronic acid (salt) ranges from 50,000 to around 3,000,000, but the molecular weight of hyaluronic acid (salt) used in the present invention is within this range. can also be used.
本発明のヒアルロン酸く塩〉の水溶液を薄層状に真空凍
結乾燥する方法は次のように行う。先ずヒアルロン酸く
塩〉の０．０５〜２．０％水溶液を作る。The method for vacuum freeze-drying the aqueous solution of the hyaluronic acid salt of the present invention into a thin layer is carried out as follows. First, a 0.05 to 2.0% aqueous solution of hyaluronic acid salt is prepared.
ヒアルロン酸（塩）は水に溶は難く、いわゆるママコに
なり易いので水を良く撹拌しつつ徐々にヒアルロン酸（
塩）を添加して完全に溶解せしめる。Hyaluronic acid (salt) is difficult to dissolve in water and tends to form so-called "mamako", so while stirring the water well, gradually hyaluronic acid (salt)
salt) and dissolve completely.
このようにして得られたヒアルロン酸（塩）水溶液を底
が平らで浅い容器に流し込む、粘稠なヒアルロン酸（塩
）水溶液が水平な表面を形成したところで、冷却し予備
凍結せしめる。これを真空凍結乾燥機の中に入れ、高真
空下で凍結乾燥する。The thus obtained aqueous hyaluronic acid (salt) solution is poured into a shallow container with a flat bottom. Once the viscous aqueous hyaluronic acid (salt) solution forms a horizontal surface, it is cooled and pre-frozen. This is placed in a vacuum freeze dryer and freeze-dried under high vacuum.
乾燥物を容器から取り出すと、白色シート状（薄層状）
のヒアルロン酸（塩）が得られる。予備凍結は真空凍結
乾燥機の中で行うことも出来る。この場合、予備凍結か
ら凍結乾燥までを真空凍結乾燥機の中で連続して操作す
ることが出来る。When you take the dried product out of the container, it will turn into a white sheet (thin layer).
of hyaluronic acid (salt) is obtained. Pre-freezing can also be carried out in a vacuum freeze dryer. In this case, the steps from pre-freezing to freeze-drying can be carried out continuously in a vacuum freeze-dryer.
最近、化粧品は、安全面での配慮から製品の中の雑菌の
数を極力減らす方向にあるが、雑菌数の少ないシート状
ヒアルロン酸（塩）を製造する場合は、ヒアルロン酸（
塩）の水溶液を、０．５Ｉｍ程度のフィルターを用いて
、除菌濾過する。除菌濾過した濾過液を清潔な真空凍結
乾燥機の中で凍結乾燥すると、雑菌数の少ないシート状
ヒアルロン酸（塩）を得ることが出来る。Recently, there has been a trend in cosmetics to reduce the number of germs in products as much as possible due to safety considerations.
The aqueous solution of salt) is sterilized and filtered using a filter of about 0.5 Im. When the sterilized filtrate is freeze-dried in a clean vacuum freeze dryer, sheet-like hyaluronic acid (salt) with a small number of bacteria can be obtained.
ヒアルロン酸（塩）の濃度が薄い水溶液から作成した凍
結乾燥品は、非常に嵩密度の小さなシート状のものとな
るので、物理的強度が非常に弱い。Freeze-dried products made from aqueous solutions with low concentrations of hyaluronic acid (salts) are sheet-like with very low bulk density, and therefore have very low physical strength.
従って、実用的な物理的強度を持つシート状ヒアルロン
酸（塩）を得るには０．１％程度以上のヒアルロン酸（
塩）の水溶液を凍結乾燥することが望ましい、ヒアルロ
ン酸（塩）の濃度が濃い水溶液を凍結乾燥する時は一４
０℃程度の温度で予備凍結を行った方が好ましい結果が
得られるが、予備凍結は必ずしも必要な操作ではない。Therefore, in order to obtain a sheet-like hyaluronic acid (salt) with practical physical strength, the content of hyaluronic acid (salt) of approximately 0.1% or more is required.
When freeze-drying an aqueous solution of hyaluronic acid (salt) with a high concentration, it is desirable to freeze-dry an aqueous solution of hyaluronic acid (salt).
Although preferable results can be obtained by pre-freezing at a temperature of about 0° C., pre-freezing is not necessarily a necessary operation.
本発明の方法で得られるシート状ヒアルロン酸（塩）の
厚さはヒアルロン酸く塩）水溶液の液層の深さを調節す
ることにより、任意の厚みを持ったものを製造すること
が出来る。実用的には０．５〜２ 、５１ｍ程度の厚み
を持ったものが、化粧料として使い易い。The sheet-like hyaluronic acid (salt) obtained by the method of the present invention can be manufactured to have any thickness by adjusting the depth of the liquid layer of the aqueous hyaluronic acid (salt) solution. Practically speaking, one with a thickness of about 0.5 to 2.51 m is easy to use as a cosmetic.
ヒアルロン酸（塩）の水溶液を底が平らで浅い容器に流
し込む場合、シリコン樹脂で表面処理した剥離紙を容器
の底に敷くと、シート状に乾燥したヒアルロン酸〈塩〉
を取り出す操作がスムースに行われる。When pouring an aqueous solution of hyaluronic acid (salt) into a shallow, flat-bottomed container, placing release paper surface-treated with silicone resin on the bottom of the container will release the dried hyaluronic acid (salt) into a sheet.
The operation to take out is performed smoothly.
凍結乾燥は、０．０５ｔｏｒｒ程度の高真空下で行う。Freeze-drying is performed under high vacuum of about 0.05 torr.
本発明のシート状ヒアルロン酸（塩）を作る際、ヒアル
ロン酸（塩）の水溶液に、界面活性剤・増量剤・顔料・
色素・キレート剤・酸化防止剤・紫外線吸収剤・香料等
を加えることが出来る。When making the sheet-like hyaluronic acid (salt) of the present invention, surfactants, fillers, pigments,
Pigments, chelating agents, antioxidants, ultraviolet absorbers, fragrances, etc. can be added.
本発明の方法で得られたシート状ヒアルロン酸（塩）は
、水或いは化粧水に対して非常に溶けやすいという特徴
を持つ。予め、目尻等を化粧水で湿らせた部分に、涙滴
状、半月状、楕円形等適当な形と大きさに切断した本発
明のシート状ヒアルロン酸（塩）を貼ると、シートは急
速に溶解して濃厚なヒアルロン酸（塩）の溶液となる。The sheet-like hyaluronic acid (salt) obtained by the method of the present invention is characterized by being very easily soluble in water or lotion. When a sheet of hyaluronic acid (salt) of the present invention cut into an appropriate shape and size, such as a teardrop shape, a half-moon shape, or an oval shape, is applied to the area moistened with lotion, such as the outer corners of the eyes, the sheet will quickly form. It dissolves into a concentrated hyaluronic acid (salt) solution.
水或いは化粧水が足りなくてシートが完全に溶解しない
場合は、シートの上から水或いは化粧水を適量加えて滲
み込ませて完全に溶解させる。逆に涙滴状に切断し７た
本発明のシート状ヒアルロン酸（塩）を目尻等の部分に
貼り、その上を水或いは化粧水で湿らせても良い。水或
いは化粧水で湿ったシートを指先で軽く押さえると、溶
解は一層完全になる。一定時間経過後、水で洗顔すると
、容易にヒアルロン酸（塩）は水に溶け、皮膚から除く
ことが出来る。If the sheet is not completely dissolved due to insufficient water or lotion, add an appropriate amount of water or lotion to the top of the sheet to allow it to soak in and dissolve completely. Conversely, the sheet-like hyaluronic acid (salt) of the present invention cut into teardrop shapes may be applied to the outer corners of the eyes and the like, and the top may be moistened with water or lotion. If the sheet moistened with water or lotion is lightly pressed with your fingertips, the dissolution will be more complete. When you wash your face with water after a certain period of time, hyaluronic acid (salt) easily dissolves in water and can be removed from your skin.
本発明の方法で得られたシート状ヒアルロン酸（塩）は
、目尻以外に瞼、額、臼杵、首等の小皺の出やすい部分
に化粧料として用いることが出来るが、これ以外の部分
にも勿論用いることが出来る。化粧料として用いた部分
は、ヒアルロン酸く塩）の持つ美容効果で皮膚に適度の
「潤い」と「張り」が付与される。The sheet-like hyaluronic acid (salt) obtained by the method of the present invention can be used as a cosmetic for areas where fine wrinkles tend to appear, such as the eyelids, forehead, mortar, neck, etc., in addition to the outer corners of the eyes, but it can also be used for other areas. Of course you can use it. The part used as a cosmetic has the beauty effect of hyaluronic acid (hyaluronic acid salt), which gives the skin just the right amount of ``moisture'' and ``tightness.''
（発明の効果）
本発明法により、水或いは化粧水に対して非常に溶解性
の良いシート状のヒアルロン酸（塩）を製造することが
出来、これを用いてヒアルロン酸（塩）を主剤とした荒
肌改善効果、角質改善効果、角質層のターンオーバーを
速くする効果、美肌効果等の皮膚老化防止効果等に優れ
たワンポイント化粧料を製造することが出来る。(Effects of the invention) By the method of the present invention, it is possible to produce sheet-like hyaluronic acid (salt) that is highly soluble in water or lotion, and using this, hyaluronic acid (salt) is used as the main ingredient. It is possible to produce a one-point cosmetic that has excellent skin aging prevention effects such as rough skin improvement effect, keratin improvement effect, speeding up the turnover of the stratum corneum, and skin beautification effect.
（実施例）
実施例１
ヒアルロン酸（分子ｉｉ１：１２０万）０．５０ｇを、
純水１０〇−中に溶解させた。この溶液を０．４５−の
フィルターで濾過した。濾液をアル短製のバットに厚さ
２１ｍになるように入れ、−４０℃に冷却した凍結乾燥
庫（ラブコンコ社製、ストッパリングトレイドライヤー
〉で予備凍結した。予備凍結乾燥終了後、２０時間、真
空度： ０．０５ｔｏｒｒで凍結乾燥し、シート状ヒア
ルロン酸０．４２ｇを得た。これを縦３ｃ１１、横４
ｃｍの長方形に切断し、−片９．６■のシート状化粧品
とした。(Example) Example 1 0.50 g of hyaluronic acid (molecule II 1: 1.2 million),
It was dissolved in 100% pure water. This solution was filtered through a 0.45-filter. The filtrate was placed in a short aluminum vat to a thickness of 21 m, and pre-frozen in a freeze-drying oven (manufactured by Loveconco, Stoppering Tray Dryer) cooled to -40°C. After the preliminary freeze-drying was completed, for 20 hours, Degree of vacuum: Lyophilization was carried out at 0.05 torr to obtain 0.42 g of sheet-like hyaluronic acid.
It was cut into rectangles of cm in size to obtain sheet-like cosmetics with a size of 9.6 cm.
このシート状化粧品を、薄く水を張ったシャーレに入れ
たところ、水を吸収して極短時間のうちに熔解した。When this sheet-shaped cosmetic was placed in a Petri dish filled with a thin layer of water, it absorbed the water and melted in a very short time.
比較例１
ヒアルロン酸（分子ｉｔ；１２０万）０．５０ｇを、純
水１００ 、ｄ中に溶解させた。この溶液を０．４５ｍ
ｍのフィルターで濾過した。濾液をアルξ製のバットに
厚さ２Ｈになるように入れ、恒温乾燥機中で温度６０℃
で８時間乾燥した。フィルム状のヒアルロン酸０．４５
ｇを得た。これを縦３ ｃｍ、横４ ｃｔｎの長方形
に切断した。Comparative Example 1 0.50 g of hyaluronic acid (molecular weight: 1.2 million) was dissolved in 100 g of pure water. 0.45m of this solution
It was filtered with a filter of m. Pour the filtrate into a vat made of Al ξ to a thickness of 2H, and heat it in a constant temperature dryer at a temperature of 60°C.
It was dried for 8 hours. Film-like hyaluronic acid 0.45
I got g. This was cut into a rectangle with a length of 3 cm and a width of 4 ctn.
コノフィルムラ、薄＜水を張ったシャーレに入れたとこ
ろ、１０分経っても、膨潤はしたが溶解しなかった。When Conophylluma was placed in a petri dish filled with a thin layer of water, it swelled but did not dissolve even after 10 minutes.
実施例２
醗酵法で製造したヒアルロン酸ナトリウム（分子量：１
２０万） ０．３０ｋｇを精製水１５０１中に溶解させ
た。このヒアルロン酸ナトリウム溶液にマンニトール２
．０ｋｇを添加し、撹拌して完全に溶解せしめた。この
溶液を０．４５−のフィルターで濾過した。Example 2 Sodium hyaluronate (molecular weight: 1
200,000) 0.30 kg was dissolved in purified water 1501. Mannitol 2 is added to this sodium hyaluronate solution.
．． 0 kg was added and stirred to completely dissolve. This solution was filtered through a 0.45-filter.
濾液をアルミ製のバットに厚さ２ｎになるように入れ、
−５０℃に冷却した凍結乾燥機（共和社製、真空凍結乾
燥機ＲＬ−２４１２ＢＳ）内で予備凍結した。Pour the filtrate into an aluminum vat to a thickness of 2 nm.
It was pre-frozen in a freeze dryer (vacuum freeze dryer RL-2412BS, Kyowa Co., Ltd.) cooled to -50°C.
予備凍結乾燥終了後、２日間、真空度： ０．０５ｔｏ
ｒｒで凍結乾燥し、シート状ヒアルロン酸ナトリウム２
．２１ｋｇを得た。これを縦３ｃｍ、横４ＣＩ１１の長
方形に切断し、シート状化粧品とした。Vacuum level: 0.05to for 2 days after preliminary freeze-drying
Freeze-dry with rr, sheet-shaped sodium hyaluronate 2
．． Obtained 21 kg. This was cut into a rectangle with a length of 3 cm and a width of 4 CI11 to obtain a sheet-like cosmetic product.
このシート状化粧品を、薄く水を張ったシャーレに入れ
たところ、水を吸収して極短時間のうちに？容解した。When this sheet-shaped cosmetic was placed in a petri dish filled with a thin layer of water, it absorbed water in a very short period of time. I understand.
比較例２
実施例２で得られたヒアルロン酸ナトリウムとマンニト
ールの混合溶液の濾液をアルミ製のバットに厚さ２ｕに
なるように入れ、恒温減圧乾燥機中で温度６０℃で８時
間乾燥した。フィルム状ヒアルロン酸ナトリウム２．４
０ｋｇを得た。これを縦３Ｃ１１１横４（Ｊの長方形に
切断した。Comparative Example 2 The filtrate of the mixed solution of sodium hyaluronate and mannitol obtained in Example 2 was poured into an aluminum vat to a thickness of 2 μ, and dried in a constant temperature vacuum dryer at a temperature of 60° C. for 8 hours. Film-form sodium hyaluronate 2.4
Obtained 0 kg. This was cut into a rectangle of length 3C111 width 4 (J).
このフィルムを、薄く水を張ったシャーレに入れたとこ
ろ、１０分経っても完全には溶解しなかった。When this film was placed in a petri dish lightly filled with water, it did not completely dissolve even after 10 minutes.
実施例３
本発明のシート状ヒアルロン酸ナトリウムからなる化粧
料の作用効果について、使用テストによって試験を行っ
た。使用テストは１０名の女性をパネルとした。Example 3 The effects of the cosmetic made of the sheet-like sodium hyaluronate of the present invention were tested by use tests. The usage test consisted of a panel of 10 women.
テストは、毎日夜、洗顔後、第１表に示す組成の化粧水
を適量、目尻の部分に塗布し、その上に実施例１で得ら
れたシート状ヒアルロン酸ナトリウムを涙滴状に切断し
たものを貼りつけた。化粧水が足りなくてシートが完全
に溶解出来ないときは、シートの上から化粧水を適量浸
み込まさせ、指先でかるく押さえて溶解させた。１夜、
その状態に保ち、翌朝水で洗顔し、化粧料を洗い落とし
た。In the test, after washing the face every night, an appropriate amount of lotion having the composition shown in Table 1 was applied to the outer corners of the eyes, and the sheet-like sodium hyaluronate obtained in Example 1 was cut into teardrop shapes on top of the lotion. I pasted things. If there was not enough lotion to completely dissolve the sheet, I applied an appropriate amount of lotion on top of the sheet and lightly pressed it with my fingertips to dissolve it. 1 night,
I kept it that way and washed my face with water the next morning to remove the makeup.
テストは３週間にわたって行い、評価は第２表記載の３
項目についてその有効性を判定した。結果は第２表に示
す通りである。The test was conducted for 3 weeks, and the evaluation was 3 as shown in Table 2.
The effectiveness of the items was determined. The results are shown in Table 2.
第１表 化粧水の組成 （重量％）エタノール
８．０％プロピレングリコール
４．０％グリセリン
３．０％ポリオキシエチレンオレイル
アルコールエーテル １．０％
クエン酸ソーダ ０．１％ｐ−オキ
シ安息香酸メチルエステル ０．１％イオン交換水
残量第２表 有効性の判定結果
第２表の結果から明らかなよづに、本発明のシート状ヒ
アルロン酸ナトリウムからなる化粧料は、肌の潤い、肌
の張りが認められた。Table 1 Composition of lotion (wt%) Ethanol
8.0% propylene glycol
4.0% glycerin
3.0% polyoxyethylene oleyl alcohol ether 1.0% sodium citrate 0.1% p-oxybenzoic acid methyl ester 0.1% ion exchange water
Remaining Amount Table 2 Efficacy Judgment Results As is clear from the results in Table 2, the cosmetic composition comprising the sheet-like sodium hyaluronate of the present invention was found to moisturize and tighten the skin.
Claims (3)
空凍結乾燥することを特徴とする、水易溶解性のシート
状ヒアルロン酸またはその塩の製造法。(1) A method for producing easily water-soluble sheet-like hyaluronic acid or a salt thereof, which comprises vacuum freeze-drying an aqueous solution of hyaluronic acid or a salt thereof in a thin layer.
ロン酸またはその塩の製造法。(2) The method for producing a sheet of hyaluronic acid or a salt thereof according to claim 1, wherein the water is a lotion.
ルロン酸またはその塩から成る化粧料。(3) A cosmetic comprising a sheet of hyaluronic acid or a salt thereof produced by the production method according to claim 1.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19654989A JPH0363209A (en) | 1989-07-31 | 1989-07-31 | Production of sheet-like hyaluronic acid or its salt and its use |
| FR9009654A FR2650180B1 (en) | 1989-07-31 | 1990-07-27 | PROCESS FOR PRODUCING AN EASILY WATER-SOLUBLE SHEET BASED ON HYALURONIC ACID OR HYALURONATE AND SHEET THUS OBTAINED |
| DE19904024180 DE4024180A1 (en) | 1989-07-31 | 1990-07-30 | BLAETTER, COMPREHENSIVE HYALURONIC ACID, THEIR MANUFACTURE AND METHOD FOR THEIR USE |
| GB9016817A GB2235204B (en) | 1989-07-31 | 1990-07-31 | Preparation of easily water-soluble sheets comprising hyaluronic acid or hyaluronate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19654989A JPH0363209A (en) | 1989-07-31 | 1989-07-31 | Production of sheet-like hyaluronic acid or its salt and its use |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7120098A Division JPH10212212A (en) | 1998-03-06 | 1998-03-06 | Cosmetic material consisting of sheet-like hyaluronic acid or its salt |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0363209A true JPH0363209A (en) | 1991-03-19 |
Family
ID=16359587
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19654989A Pending JPH0363209A (en) | 1989-07-31 | 1989-07-31 | Production of sheet-like hyaluronic acid or its salt and its use |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0363209A (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09507244A (en) * | 1994-01-10 | 1997-07-22 | ファーマシア アクチボラーグ | Low molecular weight hyaluronic acid with peptides or proteins |
| US7087238B2 (en) | 2000-11-09 | 2006-08-08 | Teikoku Seiyaku Co., Ltd | Sheet-like packs |
| JP2010043022A (en) * | 2008-08-12 | 2010-02-25 | Kao Corp | Sheet-shaped cosmetic product |
| JP2010163386A (en) * | 2009-01-15 | 2010-07-29 | Chisso Corp | Cosmetic sheet |
| JP2013112625A (en) * | 2011-11-25 | 2013-06-10 | Keiwa Inc | Cosmetic sheet for skin and method for producing cosmetic sheet for skin |
| JP2014024828A (en) * | 2012-06-17 | 2014-02-06 | Kosumedei Seiyaku Kk | Hyaluronic acid gel and producing method thereof |
| US20140120144A1 (en) * | 2011-06-14 | 2014-05-01 | Nanotheta CO., LTD. | Thin Film Supporting Hyaluronic Acid Or Derivative Thereof And Thin Film Cosmetic |
| JPWO2016121245A1 (en) * | 2015-01-29 | 2017-12-28 | 株式会社リタファーマ | Water-soluble hyaluronic acid gel and method for producing the same |
| WO2019082922A1 (en) * | 2017-10-27 | 2019-05-02 | 大日精化工業株式会社 | Cosmetic molded article and method for manufacturing same |
| CN112120205A (en) * | 2020-09-25 | 2020-12-25 | 山东华熙海御生物医药有限公司 | Soy sauce and its powder, their preparation method and application |
-
1989
- 1989-07-31 JP JP19654989A patent/JPH0363209A/en active Pending
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09507244A (en) * | 1994-01-10 | 1997-07-22 | ファーマシア アクチボラーグ | Low molecular weight hyaluronic acid with peptides or proteins |
| US7087238B2 (en) | 2000-11-09 | 2006-08-08 | Teikoku Seiyaku Co., Ltd | Sheet-like packs |
| JP2010043022A (en) * | 2008-08-12 | 2010-02-25 | Kao Corp | Sheet-shaped cosmetic product |
| JP2010163386A (en) * | 2009-01-15 | 2010-07-29 | Chisso Corp | Cosmetic sheet |
| US20140120144A1 (en) * | 2011-06-14 | 2014-05-01 | Nanotheta CO., LTD. | Thin Film Supporting Hyaluronic Acid Or Derivative Thereof And Thin Film Cosmetic |
| JP2013112625A (en) * | 2011-11-25 | 2013-06-10 | Keiwa Inc | Cosmetic sheet for skin and method for producing cosmetic sheet for skin |
| JP2014024828A (en) * | 2012-06-17 | 2014-02-06 | Kosumedei Seiyaku Kk | Hyaluronic acid gel and producing method thereof |
| US9855206B2 (en) | 2012-10-17 | 2018-01-02 | Cosmed Pharmaceutical Co., Ltd. | Hyaluronic acid gel and manufacturing method thereof |
| WO2014061332A1 (en) * | 2012-10-17 | 2014-04-24 | コスメディ製薬株式会社 | Hyaluronic acid gel and method for producing same |
| JPWO2016121245A1 (en) * | 2015-01-29 | 2017-12-28 | 株式会社リタファーマ | Water-soluble hyaluronic acid gel and method for producing the same |
| WO2019082922A1 (en) * | 2017-10-27 | 2019-05-02 | 大日精化工業株式会社 | Cosmetic molded article and method for manufacturing same |
| JP2019077665A (en) * | 2017-10-27 | 2019-05-23 | 大日精化工業株式会社 | Molding for cosmetic and method for producing the same |
| CN111278422A (en) * | 2017-10-27 | 2020-06-12 | 大日精化工业株式会社 | Cosmetic molded article and method for producing same |
| AU2018357134B2 (en) * | 2017-10-27 | 2021-11-04 | Dainichiseika Color & Chemicals Mfg. Co., Ltd. | Cosmetic molded article and method for manufacturing same |
| US11458088B2 (en) | 2017-10-27 | 2022-10-04 | Dainichiseika Color & Chemicals Mfg. Co., Ltd. | Cosmetic molded article and method for manufacturing same |
| CN112120205A (en) * | 2020-09-25 | 2020-12-25 | 山东华熙海御生物医药有限公司 | Soy sauce and its powder, their preparation method and application |
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