JP6836820B1 - Water-soluble hyaluronic acid gel and its manufacturing method - Google Patents
Water-soluble hyaluronic acid gel and its manufacturing method Download PDFInfo
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- JP6836820B1 JP6836820B1 JP2020539103A JP2020539103A JP6836820B1 JP 6836820 B1 JP6836820 B1 JP 6836820B1 JP 2020539103 A JP2020539103 A JP 2020539103A JP 2020539103 A JP2020539103 A JP 2020539103A JP 6836820 B1 JP6836820 B1 JP 6836820B1
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- Prior art keywords
- hyaluronic acid
- water
- soluble
- mass
- gel
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- MUPFEKGTMRGPLJ-ZQSKZDJDSA-N raffinose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO[C@@H]2[C@@H]([C@@H](O)[C@@H](O)[C@@H](CO)O2)O)O1 MUPFEKGTMRGPLJ-ZQSKZDJDSA-N 0.000 description 1
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- 230000002195 synergetic effect Effects 0.000 description 1
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- KBPHJBAIARWVSC-XQIHNALSSA-N trans-lutein Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CC(O)CC1(C)C)C=CC=C(/C)C=CC2C(=CC(O)CC2(C)C)C KBPHJBAIARWVSC-XQIHNALSSA-N 0.000 description 1
- 229940074410 trehalose Drugs 0.000 description 1
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- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
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- VBEQCZHXXJYVRD-GACYYNSASA-N uroanthelone Chemical compound C([C@@H](C(=O)N[C@H](C(=O)N[C@@H](CS)C(=O)N[C@@H](CC(N)=O)C(=O)N[C@@H](CS)C(=O)N[C@H](C(=O)N[C@@H]([C@@H](C)CC)C(=O)NCC(=O)N[C@@H](CC=1C=CC(O)=CC=1)C(=O)N[C@@H](CO)C(=O)NCC(=O)N[C@@H](CC(O)=O)C(=O)N[C@@H](CCCNC(N)=N)C(=O)N[C@@H](CS)C(=O)N[C@@H](CCC(N)=O)C(=O)N[C@@H]([C@@H](C)O)C(=O)N[C@@H](CCCNC(N)=N)C(=O)N[C@@H](CC(O)=O)C(=O)N[C@@H](CC(C)C)C(=O)N[C@@H](CCCNC(N)=N)C(=O)N[C@@H](CC=1C2=CC=CC=C2NC=1)C(=O)N[C@@H](CC=1C2=CC=CC=C2NC=1)C(=O)N[C@@H](CCC(O)=O)C(=O)N[C@@H](CC(C)C)C(=O)N[C@@H](CCCNC(N)=N)C(O)=O)C(C)C)[C@@H](C)O)NC(=O)[C@H](CO)NC(=O)[C@H](CC(O)=O)NC(=O)[C@H](CC(C)C)NC(=O)[C@H](CO)NC(=O)[C@H](CCC(O)=O)NC(=O)[C@@H](NC(=O)[C@H](CC=1NC=NC=1)NC(=O)[C@H](CCSC)NC(=O)[C@H](CS)NC(=O)[C@@H](NC(=O)CNC(=O)CNC(=O)[C@H](CC(N)=O)NC(=O)[C@H](CC(C)C)NC(=O)[C@H](CS)NC(=O)[C@H](CC=1C=CC(O)=CC=1)NC(=O)CNC(=O)[C@H](CC(O)=O)NC(=O)[C@H](CC=1C=CC(O)=CC=1)NC(=O)[C@H](CO)NC(=O)[C@H](CO)NC(=O)[C@H]1N(CCC1)C(=O)[C@H](CS)NC(=O)CNC(=O)[C@H]1N(CCC1)C(=O)[C@H](CC=1C=CC(O)=CC=1)NC(=O)[C@H](CO)NC(=O)[C@@H](N)CC(N)=O)C(C)C)[C@@H](C)CC)C1=CC=C(O)C=C1 VBEQCZHXXJYVRD-GACYYNSASA-N 0.000 description 1
- 229940005605 valeric acid Drugs 0.000 description 1
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- 239000000341 volatile oil Substances 0.000 description 1
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- 238000002424 x-ray crystallography Methods 0.000 description 1
- FJHBOVDFOQMZRV-XQIHNALSSA-N xanthophyll Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CC(O)CC1(C)C)C=CC=C(/C)C=CC2C=C(C)C(O)CC2(C)C FJHBOVDFOQMZRV-XQIHNALSSA-N 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/06—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
- A61K47/08—Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
- A61K47/12—Carboxylic acids; Salts or anhydrides thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
- A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/36—Carboxylic acids; Salts or anhydrides thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/06—Ointments; Bases therefor; Other semi-solid forms, e.g. creams, sticks, gels
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/70—Web, sheet or filament bases ; Films; Fibres of the matrix type containing drug
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L15/00—Chemical aspects of, or use of materials for, bandages, dressings or absorbent pads
- A61L15/16—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons
- A61L15/22—Bandages, dressings or absorbent pads for physiological fluids such as urine or blood, e.g. sanitary towels, tampons containing macromolecular materials
- A61L15/28—Polysaccharides or their derivatives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
Abstract
水溶性ヒアルロン酸ゲルの製造において、ヒアルロン酸水溶液から多くの水を蒸発させる工程を設ける必要が無く、高い生産性で製造可能な水溶性ヒアルロン酸ゲルを提供する。ヒアルロン酸、水溶性食物繊維、前記ヒアルロン酸とは異なる酸、及び水を含む水溶性ヒアルロン酸ゲルであって、前記水溶性食物繊維は、グルコースを構成糖とし、1−4結合及び1−6結合以外の結合を有し、環状構造ではない多糖類であり、前記水の含有量が、前記ヒアルロン酸1質量部に対して、1〜300質量部であり、前記水溶性食物繊維の含有量が、前記ヒアルロン酸1質量部に対して、1〜300質量部である、水溶性ヒアルロン酸ゲル。In the production of a water-soluble hyaluronic acid gel, it is not necessary to provide a step of evaporating a large amount of water from the hyaluronic acid aqueous solution, and a water-soluble hyaluronic acid gel that can be produced with high productivity is provided. A water-soluble hyaluronic acid gel containing hyaluronic acid, water-soluble dietary fiber, an acid different from the hyaluronic acid, and water, wherein the water-soluble dietary fiber contains glucose as a constituent sugar, 1-4 bonds and 1-6. It is a polysaccharide having a bond other than the bond and not having a cyclic structure, and the content of the water is 1 to 300 parts by mass with respect to 1 part by mass of the hyaluronic acid, and the content of the water-soluble dietary fiber. However, the water-soluble hyaluronic acid gel is 1 to 300 parts by mass with respect to 1 part by mass of the hyaluronic acid.
Description
本発明は、水溶性ヒアルロン酸ゲル及びその製造方法に関する。 The present invention relates to a water-soluble hyaluronic acid gel and a method for producing the same.
近年、生体適合性に優れ、保湿作用をはじめとする多くの有効作用を示すヒアルロン酸が、美容分野、医療分野、食品分野などにおいて注目されている。ヒアルロン酸は、β−D−N−アセチルグルコサミンとβ−D−グルクロン酸とが交互に結合した、直鎖状の高分子多糖であり、哺乳動物の結合組織に分布するほか、鶏の鶏冠、連鎖球菌の莢膜などにも存在することが知られている。市販されているヒアルロン酸は、一般に、鶏の鶏冠、臍帯等からの単離抽出、ストレプトコッカス属等の微生物を用いた発酵法などにより調製されている。 In recent years, hyaluronic acid, which has excellent biocompatibility and exhibits many effective effects including moisturizing effect, has been attracting attention in the fields of beauty, medical care, food, and the like. Hyaluronic acid is a linear high molecular weight polysaccharide in which β-DN-acetylglucosamine and β-D-glucuronic acid are alternately bound, and is distributed in the connective tissue of mammals. It is known to be present in the capsule of streptococci. Commercially available hyaluronic acid is generally prepared by isolation and extraction from chicken combs, umbilical cords, etc., and fermentation methods using microorganisms such as Streptococcus.
また、従来、高分子材料を含むゲル組成物が、美容分野、医療分野、食品分野などに用いられている。特に、美容分野、医療分野、食品分野などに用いられるゲル組成物は、人体に適用されるため、安全性と生体適合性に優れていることが求められている。このため、このようなゲル組成物に含まれる高分子材料として、天然素材であり、安全性と生体適合性に優れるヒアルロン酸を用いることが検討されている。 Further, conventionally, a gel composition containing a polymer material has been used in the beauty field, the medical field, the food field and the like. In particular, gel compositions used in the fields of beauty, medical care, foods, etc. are required to be excellent in safety and biocompatibility because they are applied to the human body. Therefore, it has been studied to use hyaluronic acid, which is a natural material and has excellent safety and biocompatibility, as the polymer material contained in such a gel composition.
例えば、特許文献1には、0.005〜0.5%のヒアルロン酸及び/又はその塩を配合した酸性透明ゲル状食品において、製品のブリックス(Brix)が20〜40であり、脱アシル型ジェランガム、可溶性カルシウム塩、及び6〜30%の水飴(固形分換算)を配合し、かつ、ヒアルロン酸及び/又はその塩1部に対し60部以上の水飴(固形分換算)を配合することを特徴とする酸性透明ゲル状食品が開示されている。 For example, in Patent Document 1, in an acidic transparent gel-like food containing 0.005 to 0.5% hyaluronic acid and / or a salt thereof, the Brix of the product is 20 to 40, and the product is a deacylated type. Blend gellan gum, soluble calcium salt, and 6 to 30% starch syrup (solid content equivalent), and add 60 or more starch syrup (solid content equivalent) to 1 part of hyaluronic acid and / or its salt. A characteristic acidic transparent gel-like food is disclosed.
特許文献1の酸性透明ゲル状食品は、ヒアルロン酸に加えて、ゲル化剤として、脱アシル型ジェランガム及び可溶性カルシウム塩を併用し、さらにキサンタンガムなどを配合することにより、加熱後も透明感のあるゲル状の物性を維持する技術を開示している。 The acidic transparent gel-like food of Patent Document 1 has a transparent feeling even after heating by using a deacylated gellan gum and a soluble calcium salt as a gelling agent in addition to hyaluronic acid and further adding xanthan gum and the like. It discloses a technique for maintaining gel-like physical properties.
一方、特許文献1とは異なり、ヒアルロン酸を含む水溶性のゲル組成物において、ポリアクリル酸またはその塩、キサンタンガム、グルコマンナン、グアーガム、ローカストビーン、寒天、カラギーナン、ポリビニルアルコールなどの従来使用されているゲル形成成分を用いずに、ヒアルロン酸を単独でゲル形成成分としたヒアルロン酸ゲルの開発が試みられている。 On the other hand, unlike Patent Document 1, in a water-soluble gel composition containing hyaluronic acid, polyacrylic acid or a salt thereof, xanthan gum, glucomannan, guar gum, locust bean, agar, carrageenan, polyvinyl alcohol and the like have been conventionally used. Attempts have been made to develop a hyaluronic acid gel using hyaluronic acid alone as a gel-forming component without using the existing gel-forming component.
例えば、特許文献2には、ヒアルロン酸、糖(但し、25℃において、液体である液性多価アルコールを除く)、及び水を含み、含水量が30質量%超であり、前記ヒアルロン酸以外のゲル形成成分を実質的に含まず、所定の方法によって測定されるpHが1.9〜6.3の範囲にある水溶性ヒアルロン酸ゲルが開示されている。特許文献2に開示された水溶性ヒアルロン酸ゲルは、常温下だけでなく低温下においても安定性に優れたゲルの形態を備えており、化粧料、医療用具用組成物、食品組成物、医薬組成物などとして好適に利用することができる。 For example, Patent Document 2 contains hyaluronic acid, sugar (excluding liquid polyhydric alcohol which is a liquid at 25 ° C.), and water, and has a water content of more than 30% by mass, other than the hyaluronic acid. A water-soluble hyaluronic acid gel is disclosed which is substantially free of the gel-forming component of the above and has a pH in the range of 1.9 to 6.3 as measured by a predetermined method. The water-soluble hyaluronic acid gel disclosed in Patent Document 2 has a gel form that is excellent in stability not only at room temperature but also at low temperature, and is used for cosmetics, medical device compositions, food compositions, and pharmaceuticals. It can be suitably used as a composition or the like.
特許文献2のようなヒアルロン酸をゲル化剤とした水溶性ヒアルロン酸ゲルの製造においては、まず、ヒアルロン酸、ヒアルロン酸とは異なる酸、糖、水などを含むヒアルロン酸水溶液を調製し、次に、ヒアルロン酸水溶液から大部分の水を蒸発させることにより、水溶性ヒアルロン酸ゲルを調製する方法が採用されている。ヒアルロン酸水溶液に含まれる水の含有量は、常温(25℃)程度でヒアルロン酸水溶液がゲル化しない量であり、水溶性ヒアルロン酸ゲルを調製する際には、ヒアルロン酸水溶液から大部分の水を蒸発させる工程が必要である。 In the production of a water-soluble hyaluronic acid gel using hyaluronic acid as a gelling agent as in Patent Document 2, first, an aqueous hyaluronic acid solution containing hyaluronic acid, an acid different from hyaluronic acid, sugar, water, etc. is prepared, and then In addition, a method of preparing a water-soluble hyaluronic acid gel by evaporating most of the water from the hyaluronic acid aqueous solution has been adopted. The content of water contained in the hyaluronic acid aqueous solution is an amount at which the hyaluronic acid aqueous solution does not gel at about room temperature (25 ° C.), and when preparing a water-soluble hyaluronic acid gel, most of the water from the hyaluronic acid aqueous solution is used. A step of evaporating is required.
水溶性ヒアルロン酸ゲルの製造において、ヒアルロン酸水溶液から多くの水を蒸発させる工程が不要となれば、水溶性ヒアルロン酸ゲルの生産性が大きく向上する。 In the production of the water-soluble hyaluronic acid gel, if the step of evaporating a large amount of water from the hyaluronic acid aqueous solution becomes unnecessary, the productivity of the water-soluble hyaluronic acid gel is greatly improved.
本発明は、水溶性ヒアルロン酸ゲルの製造において、ヒアルロン酸水溶液から多くの水を蒸発させる工程を設ける必要が無く、高い生産性で製造可能な水溶性ヒアルロン酸ゲルを提供することを主な目的とする。さらに、本発明は、当該水溶性ヒアルロン酸ゲルの製造方法、当該水溶性ヒアルロン酸ゲルを用いた化粧料、医療用具用組成物、食品組成物、または医薬組成物を提供することも目的とする。 The main object of the present invention is to provide a water-soluble hyaluronic acid gel that can be produced with high productivity without the need to provide a step of evaporating a large amount of water from the hyaluronic acid aqueous solution in the production of the water-soluble hyaluronic acid gel. And. Another object of the present invention is to provide a method for producing the water-soluble hyaluronic acid gel, cosmetics using the water-soluble hyaluronic acid gel, medical device compositions, food compositions, or pharmaceutical compositions. ..
本発明者は、上記のような課題を解決すべく鋭意検討を行った。その結果、ヒアルロン酸、水溶性食物繊維、前記ヒアルロン酸とは異なる酸、及び水を含む水溶性ヒアルロン酸ゲルであって、水溶性食物繊維として、グルコースを構成糖とし、1−4結合及び1−6結合以外の結合を有し、環状構造ではない多糖類を用いた上で、さらに、水及び水溶性食物繊維の含有量を、それぞれ、所定範囲に設定することにより、水溶性ヒアルロン酸ゲルの製造において、ヒアルロン酸水溶液から多くの水を蒸発させる工程を設ける必要が無く、高い生産性で製造可能な水溶性ヒアルロン酸ゲルとなることを見出した。 The present inventor has made diligent studies to solve the above problems. As a result, it is a water-soluble hyaluronic acid gel containing hyaluronic acid, water-soluble dietary fiber, an acid different from the hyaluronic acid, and water, and as the water-soluble dietary fiber, glucose is a constituent sugar, 1-4 bonds and 1 A water-soluble hyaluronic acid gel by using a polysaccharide having a bond other than -6 bond and not having a cyclic structure, and further setting the contents of water and water-soluble dietary fiber within predetermined ranges, respectively. It has been found that a water-soluble hyaluronic acid gel that can be produced with high productivity can be obtained without the need to provide a step of evaporating a large amount of water from the hyaluronic acid aqueous solution.
より具体的には、当該水溶性ヒアルロン酸ゲルの水溶液を加熱しながら調製することで軟化/液状化し、これを冷却すればゲル化する性質を有しており、例えば、水溶性ヒアルロン酸ゲルの組成において、加熱環境で流動性のある均一なヒアルロン酸水溶液を調製することができ、その水溶液のまま容器に充填したり、フィルム上に展延して均一なシート状にすることができ、かつ、室温程度に冷却されると水溶性ヒアルロン酸ゲルを形成する性質を有することを見出した。当該水溶性ヒアルロン酸ゲルは、このような性質を備えていることから、高い生産性で製造できるだけでなく、例えば水溶性ヒアルロン酸ゲルが物流過程で高温環境に置かれて軟化/液状化しても、室温で再びゲル化するため、製品としての安定性に優れている。 More specifically, it has the property of softening / liquefying by preparing an aqueous solution of the water-soluble hyaluronic acid gel while heating, and gelling when cooled, for example, of a water-soluble hyaluronic acid gel. In terms of composition, a uniform hyaluronic acid aqueous solution that is fluid in a heating environment can be prepared, and the aqueous solution can be filled in a container as it is, or spread on a film to form a uniform sheet. , It was found that it has a property of forming a water-soluble hyaluronic acid gel when cooled to about room temperature. Since the water-soluble hyaluronic acid gel has such properties, it can be produced with high productivity, and even if the water-soluble hyaluronic acid gel is placed in a high temperature environment in the distribution process and softened / liquefied, for example. Since it gels again at room temperature, it has excellent stability as a product.
本発明は、これらの知見に基づいて、さらに検討を重ねることにより完成された発明である。 The present invention is an invention completed by further studying based on these findings.
すなわち、本発明は、下記に掲げる態様の発明を提供する。
項1.ヒアルロン酸、水溶性食物繊維、前記ヒアルロン酸とは異なる酸、及び水を含む水溶性ヒアルロン酸ゲルであって、前記水溶性食物繊維は、グルコースを構成糖とし、1−4結合及び1−6結合以外の結合を有し、環状構造ではない多糖類であり、前記水の含有量が、前記ヒアルロン酸1質量部に対して、1〜300質量部であり、前記水溶性食物繊維の含有量が、前記ヒアルロン酸1質量部に対して、1〜300質量部である、水溶性ヒアルロン酸ゲル。
項2.以下の測定方法によって測定される水溶液のpHが、1.9〜6.3の範囲にある、項1に記載の水溶性ヒアルロン酸ゲル。
(pHの測定方法)ヒアルロン酸1gを含む分量の前記水溶性ヒアルロン酸ゲルに含まれる成分のうち、水を除く全てのイオン性成分を水に溶解して200mLとなるように水溶液を調製し、得られた水溶液のpHを測定する。
項3.前記水溶性食物繊維が、イソマルトデキストリン、難消化性デキストリン、難消化性グルカン、及びポリデキストロースからなる群より選択される少なくとも1種である、項1又は2に記載の水溶性ヒアルロン酸ゲル。
項4.前記ヒアルロン酸、前記水溶性食物繊維、前記ヒアルロン酸とは異なる酸、及び前記水の合計含有率が、前記水溶性ヒアルロン酸ゲル100質量%中、30質量%以上である、項1〜3のいずれか1項に記載の水溶性ヒアルロン酸ゲル。
項5.糖(但し、25℃において、液体である液性多価アルコールを除く)をさらに含む、項1〜4のいずれか1項に記載の水溶性ヒアルロン酸ゲル。
項6.シート状である、項1〜5のいずれかに記載の水溶性ヒアルロン酸ゲル。
項7.粒状である、項1〜5のいずれかに記載の水溶性ヒアルロン酸ゲル。
項8.塊状である、項1〜5のいずれかに記載の水溶性ヒアルロン酸ゲル。
項9.項1〜8のいずれかに記載の水溶性ヒアルロン酸ゲルを用いた化粧料。
項10.項1〜8のいずれかに記載の水溶性ヒアルロン酸ゲルを用いた食品組成物。
項11.項1〜8のいずれかに記載の水溶性ヒアルロン酸ゲルを用いた医薬組成物。
項12.項1〜8のいずれかに記載の水溶性ヒアルロン酸ゲルを用いた医療用具用組成物。
項13.項1〜8のいずれかに記載の水溶性ヒアルロン酸ゲルの製造方法であって、前記ヒアルロン酸と、前記ヒアルロン酸1質量部に対して1〜300質量部の前記水溶性食物繊維と、前記ヒアルロン酸とは異なる酸と、前記ヒアルロン酸1質量部に対して1〜300質量部の水を含み、40℃以上の温度に加熱されたヒアルロン酸水溶液を調製する工程1と、前記加熱されたヒアルロン酸水溶液を40℃未満の温度に冷却する工程2と、を備える、水溶性ヒアルロン酸ゲルの製造方法。
項14.前記工程1から前記工程2の間における、前記水溶性ヒアルロン酸水溶液からの水の減少率が、50質量%以下である、項13に記載の水溶性ヒアルロン酸ゲルの製造方法。That is, the present invention provides the inventions of the following aspects.
Item 1. A water-soluble hyaluronic acid gel containing hyaluronic acid, water-soluble dietary fiber, an acid different from the hyaluronic acid, and water, wherein the water-soluble dietary fiber contains glucose as a constituent sugar, 1-4 bonds and 1-6. It is a polysaccharide having a bond other than the bond and not having a cyclic structure, and the content of the water is 1 to 300 parts by mass with respect to 1 part by mass of the hyaluronic acid, and the content of the water-soluble dietary fiber. However, the water-soluble hyaluronic acid gel is 1 to 300 parts by mass with respect to 1 part by mass of the hyaluronic acid.
Item 2. Item 2. The water-soluble hyaluronic acid gel according to Item 1, wherein the pH of the aqueous solution measured by the following measuring method is in the range of 1.9 to 6.3.
(Method for measuring pH) Of the components contained in the water-soluble hyaluronic acid gel in an amount containing 1 g of hyaluronic acid, all ionic components except water were dissolved in water to prepare an aqueous solution so as to have a concentration of 200 mL. The pH of the obtained aqueous solution is measured.
Item 3. Item 2. The water-soluble hyaluronic acid gel according to Item 1 or 2, wherein the water-soluble dietary fiber is at least one selected from the group consisting of isomaltodextrin, indigestible dextrin, indigestible glucan, and polydextrose.
Item 4. Item 1 to 3, wherein the total content of the hyaluronic acid, the water-soluble dietary fiber, an acid different from the hyaluronic acid, and the water is 30% by mass or more in 100% by mass of the water-soluble hyaluronic acid gel. The water-soluble hyaluronic acid gel according to any one of the following items.
Item 5. Item 2. The water-soluble hyaluronic acid gel according to any one of Items 1 to 4, further comprising a sugar (excluding a liquid polyhydric alcohol which is a liquid at 25 ° C.).
Item 6. Item 2. The water-soluble hyaluronic acid gel according to any one of Items 1 to 5, which is in the form of a sheet.
Item 7. Item 2. The water-soluble hyaluronic acid gel according to any one of Items 1 to 5, which is granular.
Item 8. Item 2. The water-soluble hyaluronic acid gel according to any one of Items 1 to 5, which is lumpy.
Item 9. A cosmetic using the water-soluble hyaluronic acid gel according to any one of Items 1 to 8.
Item 10. A food composition using the water-soluble hyaluronic acid gel according to any one of Items 1 to 8.
Item 11. A pharmaceutical composition using the water-soluble hyaluronic acid gel according to any one of Items 1 to 8.
Item 12. A composition for a medical device using the water-soluble hyaluronic acid gel according to any one of Items 1 to 8.
Item 13. Item 2. The method for producing a water-soluble hyaluronic acid gel according to any one of Items 1 to 8, wherein the hyaluronic acid, 1 to 300 parts by mass of the water-soluble dietary fiber with respect to 1 part by mass of the hyaluronic acid, and the above. Step 1 of preparing an aqueous hyaluronic acid solution containing an acid different from hyaluronic acid and 1 to 300 parts by mass of water with respect to 1 part by mass of the hyaluronic acid and heated to a temperature of 40 ° C. or higher, and the heating A method for producing a water-soluble hyaluronic acid gel, comprising the step 2 of cooling the hyaluronic acid aqueous solution to a temperature of less than 40 ° C.
Item 14. Item 3. The method for producing a water-soluble hyaluronic acid gel according to Item 13, wherein the reduction rate of water from the water-soluble hyaluronic acid aqueous solution between the steps 1 and 2 is 50% by mass or less.
本発明によれば、水溶性ヒアルロン酸ゲルの製造において、ヒアルロン酸水溶液から多くの水を蒸発させる工程を設ける必要が無く、高い生産性で製造可能な水溶性ヒアルロン酸ゲルを提供することができる。本発明によれば、当該水溶性ヒアルロン酸ゲルの製造方法、当該水溶性ヒアルロン酸ゲルを用いた化粧料、医療用具用組成物、食品組成物、または医薬組成物を提供することができる。 According to the present invention, in the production of a water-soluble hyaluronic acid gel, it is not necessary to provide a step of evaporating a large amount of water from the hyaluronic acid aqueous solution, and it is possible to provide a water-soluble hyaluronic acid gel that can be produced with high productivity. .. According to the present invention, it is possible to provide a method for producing the water-soluble hyaluronic acid gel, cosmetics using the water-soluble hyaluronic acid gel, a composition for medical devices, a food composition, or a pharmaceutical composition.
本発明の水溶性ヒアルロン酸ゲルは、ヒアルロン酸、水溶性食物繊維、前記ヒアルロン酸とは異なる酸、及び水を含む水溶性ヒアルロン酸ゲルであって、水溶性食物繊維は、グルコースを構成糖とし、1−4結合及び1−6結合以外の結合を有し、環状構造ではない多糖類であり、水の含有量が、前記ヒアルロン酸1質量部に対して、1〜300質量部であり、水溶性食物繊維の含有量が、前記ヒアルロン酸1質量部に対して、1〜300質量部であることを特徴とする。 The water-soluble hyaluronic acid gel of the present invention is a water-soluble hyaluronic acid gel containing hyaluronic acid, water-soluble dietary fiber, an acid different from the hyaluronic acid, and water, and the water-soluble dietary fiber contains glucose as a constituent sugar. It is a polysaccharide having bonds other than 1-4 bonds and 1-6 bonds and not having a cyclic structure, and the content of water is 1 to 300 parts by mass with respect to 1 part by mass of the hyaluronic acid. The content of the water-soluble dietary fiber is 1 to 300 parts by mass with respect to 1 part by mass of the hyaluronic acid.
本発明の水溶性ヒアルロン酸ゲルは、このような構成を備えていることにより、水溶性ヒアルロン酸ゲルの製造において、ヒアルロン酸水溶液から多くの水を蒸発させる工程を設ける必要が無く、高い生産性で製造可能である。より具体的には、本発明の水溶性ヒアルロン酸ゲルの水溶液を加熱しながら調製することで軟化/液状化し、これを冷却すればゲル化する性質を有しており、例えば、水溶性ヒアルロン酸ゲルの組成において、加熱環境で流動性のある均一なヒアルロン酸水溶液を調製することができ、その水溶液のまま容器に充填したり、フィルム上に展延して均一なシート状にすることができ、かつ、室温程度に冷却されると水溶性ヒアルロン酸ゲルを形成する性質を有する。本発明の水溶性ヒアルロン酸ゲルは、このような性質を備えていることから、高い生産性で製造できるだけでなく、例えば水溶性ヒアルロン酸ゲルが物流過程で高温環境に置かれて軟化/液状化しても、室温で再びゲル化するため、製品としての安定性に優れている。以下、本発明の水溶性ヒアルロン酸ゲル、当該水溶性ヒアルロン酸ゲルの製造方法、当該水溶性ヒアルロン酸ゲルを用いた化粧料、医療用具用組成物、食品組成物、または医薬組成物(外用、経口など)について詳述する。 Since the water-soluble hyaluronic acid gel of the present invention has such a structure, it is not necessary to provide a step of evaporating a large amount of water from the hyaluronic acid aqueous solution in the production of the water-soluble hyaluronic acid gel, and the productivity is high. Can be manufactured at. More specifically, it has the property of softening / liquefying by preparing an aqueous solution of the water-soluble hyaluronic acid gel of the present invention while heating, and gelling when cooled, for example, water-soluble hyaluronic acid. In the composition of the gel, a uniform hyaluronic acid aqueous solution that is fluid in a heating environment can be prepared, and the aqueous solution can be filled in a container as it is or spread on a film to form a uniform sheet. Moreover, it has the property of forming a water-soluble hyaluronic acid gel when cooled to about room temperature. Since the water-soluble hyaluronic acid gel of the present invention has such properties, it can be produced with high productivity, and for example, the water-soluble hyaluronic acid gel is softened / liquefied by being placed in a high temperature environment in the distribution process. However, since it gels again at room temperature, it has excellent stability as a product. Hereinafter, the water-soluble hyaluronic acid gel of the present invention, the method for producing the water-soluble hyaluronic acid gel, cosmetics using the water-soluble hyaluronic acid gel, medical device compositions, food compositions, or pharmaceutical compositions (external use, Oral, etc.) will be described in detail.
本発明の水溶性ヒアルロン酸ゲルは、ヒアルロン酸、水溶性食物繊維、前記ヒアルロン酸とは異なる酸、及び水を含む。後述の通り、本発明の水溶性ヒアルロン酸ゲルは、例えば、ヒアルロン酸と、ヒアルロン酸1質量部に対して1〜300質量部の水溶性食物繊維と、ヒアルロン酸とは異なる酸と、ヒアルロン酸1質量部に対して1〜300質量部の水を含み、40℃以上の温度に加熱されたヒアルロン酸水溶液を調製する工程1と、加熱されたヒアルロン酸水溶液を40℃未満の温度に冷却する工程2とを備える製造方法によって、好適に製造することができ、当該製造方法において、水を多量に蒸発させる工程を備える必要はない。すなわち、加熱されたヒアルロン酸水溶液を室温程度に冷却すれば、ヒアルロン酸水溶液と実質的に同じ組成を有する本発明の水溶性ヒアルロン酸ゲルが得られる。後述の通り、工程1から工程2の間における、水溶性ヒアルロン酸水溶液からの水の減少率は、50質量%以下(すなわち、ヒアルロン酸水溶液に含まれる水の含有量を100質量%(基準)とした場合に、水溶性ヒアルロン酸ゲルに含まれる水の含有量は、50質量%以上である。)とすることができる。 The water-soluble hyaluronic acid gel of the present invention contains hyaluronic acid, water-soluble dietary fiber, an acid different from the hyaluronic acid, and water. As will be described later, the water-soluble hyaluronic acid gel of the present invention contains, for example, hyaluronic acid, 1 to 300 parts by mass of water-soluble dietary fiber with respect to 1 part by mass of hyaluronic acid, an acid different from hyaluronic acid, and hyaluronic acid. Step 1 of preparing a hyaluronic acid aqueous solution containing 1 to 300 parts by mass of water with respect to 1 part by mass and heated to a temperature of 40 ° C. or higher, and cooling the heated hyaluronic acid aqueous solution to a temperature of less than 40 ° C. It can be suitably produced by the production method including step 2, and it is not necessary to include a step of evaporating a large amount of water in the production method. That is, when the heated hyaluronic acid aqueous solution is cooled to about room temperature, the water-soluble hyaluronic acid gel of the present invention having substantially the same composition as the hyaluronic acid aqueous solution can be obtained. As will be described later, the reduction rate of water from the water-soluble hyaluronic acid aqueous solution between steps 1 and 2 is 50% by mass or less (that is, the content of water contained in the hyaluronic acid aqueous solution is 100% by mass (reference)). The content of water contained in the water-soluble hyaluronic acid gel is 50% by mass or more).
本発明の水溶性ヒアルロン酸ゲルにおいては、ヒアルロン酸が、ゲル形成成分として含まれている。本発明の水溶性ヒアルロン酸ゲル中においては、ヒアルロン酸が実質的に単独でゲル形成成分として含まれており、他のゲル形成成分が実質的に含まれない。なお、本発明の効果を阻害しないことを限度として、本発明の水溶性ヒアルロン酸ゲルは、ヒアルロン酸に加えて、他のゲル形成成分を僅かに含んでいてもよい。他のゲル形成成分としては、特に制限されないが、例えば、ポリアクリル酸またはその塩、キサンタンガム、ゲランガム、グルコマンナン、グアーガム、ローカストビーンガム、寒天、ゼラチン、ペクチン、カゼンイン、アラビアゴム、カラギーナン、アガロース、アルギン酸、アルギン酸プロピレングリコール、カルボキシメチルセルロースNa、ヒドロキシプロピルセルロース、ポリビニルアルコール、カルボキシビニルポリマー、デンプン/アクリル酸塩グラフト共重合体、メチルビニルエーテル/無水マレイン酸共重合体等の公知のゲル形成成分が挙げられる。ただし、他のゲル形成成分を含む場合、本発明の水溶性ヒアルロン酸ゲルの特性を生かす観点から、他のゲル形成成分の含有量は、本発明の水溶性ヒアルロン酸ゲルの組成において、ヒアルロン酸を配合しない場合にはゲルが形成されない量以下であることが好ましい。たとえば、他のゲル形成成分の含有量は、他のゲル形成成分の種類によっても異なるが、本発明の水溶性ヒアルロン酸ゲル中、5質量%以下、好ましくは2.5質量%以下、より好ましくは1質量%以下、さらに好ましくは0.5質量%以下、より一層好ましくは0.1質量%以下であることが挙げられる。 In the water-soluble hyaluronic acid gel of the present invention, hyaluronic acid is contained as a gel-forming component. In the water-soluble hyaluronic acid gel of the present invention, hyaluronic acid is substantially alone as a gel-forming component, and other gel-forming components are not substantially contained. The water-soluble hyaluronic acid gel of the present invention may contain a small amount of other gel-forming components in addition to hyaluronic acid, as long as the effects of the present invention are not impaired. Other gel-forming components are not particularly limited, but are, for example, polyacrylic acid or a salt thereof, xanthan gum, gellan gum, glucomannan, guar gum, locust bean gum, agar, gelatin, pectin, cazenine, arabic rubber, carrageenan, agarose, etc. Known gel-forming components such as alginic acid, propylene glycol alginate, sodium carboxymethyl cellulose, hydroxypropyl cellulose, polyvinyl alcohol, carboxyvinyl polymer, starch / acrylate graft copolymer, methyl vinyl ether / maleic anhydride copolymer and the like can be mentioned. .. However, when other gel-forming components are included, the content of the other gel-forming components is determined by the composition of the water-soluble hyaluronic acid gel of the present invention from the viewpoint of utilizing the characteristics of the water-soluble hyaluronic acid gel of the present invention. When is not blended, the amount is preferably less than the amount at which gel is not formed. For example, the content of other gel-forming components varies depending on the type of other gel-forming components, but is 5% by mass or less, preferably 2.5% by mass or less, more preferably in the water-soluble hyaluronic acid gel of the present invention. Is 1% by mass or less, more preferably 0.5% by mass or less, and even more preferably 0.1% by mass or less.
また、本発明の水溶性ヒアルロン酸ゲルには、特許文献1に開示された、脱アシル型ジェランガム及び可溶性カルシウム塩の少なくとも一方が実質的に含まれていないことが好ましい。脱アシル型ジェランガムが実質的に含まれないとは、例えば、脱アシル型ジェランガムの含有率が0.05質量%未満、より好ましくは0.03質量%以下、さらに好ましくは0.01質量%以下であることを意味する。また、可溶性カルシウム塩が実質的に含まれないとは、例えば、可溶性カルシウム塩の含有率が0.01質量%未満、より好ましくは0.005質量%以下、さらに好ましくは0.003質量%以下であることを意味する。 Further, it is preferable that the water-soluble hyaluronic acid gel of the present invention does not substantially contain at least one of the deacylated gellan gum and the soluble calcium salt disclosed in Patent Document 1. Substantially free of deacylated gellan gum means, for example, that the content of deacylated gellan gum is less than 0.05% by mass, more preferably 0.03% by mass or less, still more preferably 0.01% by mass or less. Means that Further, the fact that the soluble calcium salt is substantially not contained means, for example, that the content of the soluble calcium salt is less than 0.01% by mass, more preferably 0.005% by mass or less, still more preferably 0.003% by mass or less. Means that
なお、特許文献1に記載のとおり、脱アシル型ジェランガムとは、スフィンゴモナス・エロデア(Sphingomonaselodea)が産出する微生物多糖類の脱アシル化体である。また、可溶性カルシウム塩とは、ゲル化助剤として機能するカルシウム塩であり、例えば乳酸カルシウム、塩化カルシウム、酢酸カルシウム、グルコン酸カルシウム、第一リン酸カルシウム、フマル酸カルシウム、リンゴ酸カルシウム、コハク酸カルシウム、クエン酸カルシウムなどである。 As described in Patent Document 1, the deacylated gellan gum is a deacylated product of a microbial polysaccharide produced by Sphingomonas elodea. The soluble calcium salt is a calcium salt that functions as a gelling aid, for example, calcium lactate, calcium chloride, calcium acetate, calcium gluconate, calcium monophosphate, calcium fumarate, calcium malate, calcium succinate, etc. For example, calcium citrate.
本発明において、「ヒアルロン酸」は、ヒアルロン酸及びその塩を含む概念で使用される。従って、特に「ヒアルロン酸の塩」などと明示しない限り、本発明においては、「ヒアルロン酸及び/又はその塩」を、単に「ヒアルロン酸」と表記する。ヒアルロン酸の塩としては、特に制限されないが、例えば、ヒアルロン酸ナトリウム、ヒアルロン酸カリウム、ヒアルロン酸マグネシウム、ヒアルロン酸カルシウムなどが挙げられる。本発明において、ヒアルロン酸は、1種類単独で使用してもよいし、2種類以上を組み合わせて使用してもよい。 In the present invention, "hyaluronic acid" is used in a concept including hyaluronic acid and a salt thereof. Therefore, in the present invention, "hyaluronic acid and / or a salt thereof" is simply referred to as "hyaluronic acid" unless otherwise specified as "a salt of hyaluronic acid". The salt of hyaluronic acid is not particularly limited, and examples thereof include sodium hyaluronate, potassium hyaluronate, magnesium hyaluronate, calcium hyaluronate, and the like. In the present invention, one type of hyaluronic acid may be used alone, or two or more types may be used in combination.
ヒアルロン酸の分子量としては、ヒアルロン酸を単独でゲル形成成分とした場合にも、ゲルを形成することができれば特に制限されないが、前述のように高い生産性で製造可能な水溶性ヒアルロン酸ゲルをより一層好適に提供する観点からは、好ましくは5.0×104〜5.0×106ダルトン程度、より好ましくは1.0×105〜2.3×106ダルトン程度、さらに好ましくは3.5×105〜1.6×106が挙げられる。ヒアルロン酸としては、単一分子量のものを用いてもよいし、複数種類の分子量のものを混合して用いてもよい。The molecular weight of hyaluronic acid is not particularly limited as long as it can form a gel even when hyaluronic acid is used alone as a gel-forming component, but as described above, a water-soluble hyaluronic acid gel that can be produced with high productivity can be obtained. From the viewpoint of providing more preferably, it is preferably about 5.0 × 10 4 to 5.0 × 10 6 daltons, more preferably about 1.0 × 10 5 to 2.3 × 10 6 daltons, and even more preferably about 1.0 × 10 5 to 2.3 × 10 6 daltons. Examples thereof include 3.5 × 10 5 to 1.6 × 10 6 . As the hyaluronic acid, one having a single molecular weight may be used, or one having a plurality of types of molecular weights may be mixed and used.
ヒアルロン酸の由来は特に制限されず、例えば、鶏の鶏冠、臍帯等から単離抽出されたものや、ストレプトコッカス属等の微生物を用いた発酵法などにより調製されたものなどが好適に使用できる。本発明において、ヒアルロン酸としては、市販品を使用することができる。本発明の水溶性ヒアルロン酸ゲルは、ヒアルロン酸として化学修飾したものを用いる必要がないため、生体適合性に優れ、天然のヒアルロン酸が有する特徴を発揮することができる。すなわち、本発明の水溶性ヒアルロン酸ゲルにおいて、ヒアルロン酸としては、実質的に化学修飾されていないヒアルロン酸のみを用いてよい。なお、本発明の水溶性ヒアルロン酸ゲルは、本発明の効果を阻害しないことを限度として、化学修飾されたヒアルロン酸をさらに含んでいてもよい。 The origin of hyaluronic acid is not particularly limited, and for example, those isolated and extracted from chicken combs, umbilical cords, etc., and those prepared by a fermentation method using microorganisms such as Streptococcus can be preferably used. In the present invention, a commercially available product can be used as the hyaluronic acid. Since the water-soluble hyaluronic acid gel of the present invention does not need to be chemically modified as hyaluronic acid, it has excellent biocompatibility and can exhibit the characteristics of natural hyaluronic acid. That is, in the water-soluble hyaluronic acid gel of the present invention, only hyaluronic acid that is not substantially chemically modified may be used as the hyaluronic acid. The water-soluble hyaluronic acid gel of the present invention may further contain chemically modified hyaluronic acid as long as it does not inhibit the effect of the present invention.
化学修飾されたヒアルロン酸の具体例としては、ヒアルロン酸ヒドロキシプロピルトリモニウム、加水分解ヒアルロン酸アルキル(C12−13)グリセリル、ヒアルロン酸プロピレングリコール、アセチル化ヒアルロン酸ナトリウムなどが挙げられる。化学修飾されたヒアルロン酸は、1種類単独で使用してもよいし、2種類以上を組み合わせて使用してもよい。 Specific examples of chemically modified hyaluronic acid include hydroxypropyltrimonium hyaluronate, hydrolyzed alkyl hyaluronate (C12-13) glyceryl, propylene glycol hyaluronate, and acetylated sodium hyaluronate. The chemically modified hyaluronic acid may be used alone or in combination of two or more.
本発明の水溶性ヒアルロン酸ゲルにおいて、ヒアルロン酸の含有量としては、ゲルを形成することができれば特に制限されないが、前述のように高い生産性で製造可能な水溶性ヒアルロン酸ゲルをより一層好適に提供する観点からは、例えば0.2〜50質量%程度、好ましくは0.3〜30質量%程度、より好ましくは0.4〜10質量%程度が挙げられる。水溶性ヒアルロン酸ゲルにおけるヒアルロン酸の含有量が0.2質量%未満となる場合、ヒアルロン酸水溶液からゲルが形成されない場合がある。また、水溶性ヒアルロン酸ゲルにおけるヒアルロン酸の含有量が50質量%を超える場合、水溶性ヒアルロン酸ゲルが固くなり過ぎて、後述の化粧料、食品組成物、医薬組成物、または医療用具用組成物などとして利用し難くなる場合がある。 In the water-soluble hyaluronic acid gel of the present invention, the content of hyaluronic acid is not particularly limited as long as the gel can be formed, but as described above, the water-soluble hyaluronic acid gel that can be produced with high productivity is more preferable. From the viewpoint of providing the above, for example, about 0.2 to 50% by mass, preferably about 0.3 to 30% by mass, and more preferably about 0.4 to 10% by mass. When the content of hyaluronic acid in the water-soluble hyaluronic acid gel is less than 0.2% by mass, the gel may not be formed from the aqueous hyaluronic acid solution. When the content of hyaluronic acid in the water-soluble hyaluronic acid gel exceeds 50% by mass, the water-soluble hyaluronic acid gel becomes too hard, and the cosmetics, food compositions, pharmaceutical compositions, or medical device compositions described below are used. It may be difficult to use it as an object.
本発明において、水溶性食物繊維は、グルコースを構成糖とし、1−4結合及び1−6結合以外の結合を有し、環状構造ではない多糖類である。従って、例えば、環状構造である難消化性シクロデキストリンなどは、当該水溶性食物繊維には含まれない。当該多糖類は、グルコアミラーゼによって加水分解されない成分が、好ましくは30質量%以上、より好ましくは50質量%以上、さらに好ましくは70質量%以上、さらに好ましくは80質量%以上、特に好ましくは90質量%以上である。当該水溶性食物繊維の好ましい具体例としては、イソマルトデキストリン、難消化性デキストリン、難消化性グルカン、及びポリデキストロースなどが挙げられ、好ましくは加熱による着色の少ないイソマルトデキストリン、還元難消化性デキストリン、及び還元ポリデキストロースなどが挙げられる。これらの水溶性食物繊維についても、グルコアミラーゼによって加水分解されない成分が、好ましくは30質量%以上、より好ましくは50質量%以上、さらに好ましくは70質量%以上、さらに好ましくは80質量%以上、特に好ましくは90質量%以上である。本発明の水溶性ヒアルロン酸ゲルに含まれる水溶性食物繊維は、1種類であってもよいし、2種類以上であってもよい。 In the present invention, the water-soluble dietary fiber is a polysaccharide having glucose as a constituent sugar, having bonds other than 1-4 bonds and 1-6 bonds, and not having a cyclic structure. Therefore, for example, indigestible cyclodextrin having a cyclic structure is not included in the water-soluble dietary fiber. In the polysaccharide, the component that is not hydrolyzed by glucoamylase is preferably 30% by mass or more, more preferably 50% by mass or more, still more preferably 70% by mass or more, still more preferably 80% by mass or more, and particularly preferably 90% by mass. % Or more. Preferred specific examples of the water-soluble dietary fiber include isomaltodextrin, indigestible dextrin, indigestible glucan, polydextrose and the like, and preferably isomaltodextrin and reduced indigestible dextrin, which are less colored by heating. , And reduced polydextrose and the like. Regarding these water-soluble dietary fibers, the component that is not hydrolyzed by glucoamylase is preferably 30% by mass or more, more preferably 50% by mass or more, still more preferably 70% by mass or more, still more preferably 80% by mass or more, particularly. It is preferably 90% by mass or more. The water-soluble dietary fiber contained in the water-soluble hyaluronic acid gel of the present invention may be one kind or two or more kinds.
イソマルトデキストリンとは、コーンスターチなどのでん粉に酵素を作用させることによりα結合のグルコースのみから構成される高度に分岐した多分岐α−グルカンであり、必要に応じて脱塩、脱色した水溶性食物繊維であり、難消化性の特徴を持つものをいう。イソマルトデキストリンの市販品としては、例えば、ファイバリクサ(林原株式会社製)等が挙げられる。 Isomaltodextrin is a highly branched multi-branched α-glucan composed only of α-linked glucose by allowing an enzyme to act on starch such as cornstarch, and is a water-soluble food that has been desalted and decolorized as necessary. A fiber that has indigestible characteristics. Examples of commercially available isomaltodextrin products include Fiberlixa (manufactured by Hayashibara Co., Ltd.) and the like.
また、難消化性デキストリンとは、とうもろこし、小麦、米、豆類、イモ類、タピオカなどの植物由来の澱粉を加酸(例えば塩酸を添加)及び/又は加熱して得た焙焼デキストリンを、必要に応じてαアミラーゼ及び/又はグルコアミラーゼで酵素処理した後、必要に応じて脱塩、脱色した水溶性食物繊維であり、難消化性の特徴を持つものをいう。難消化性デキストリンには、水素添加により製造される、難消化性デキストリンの還元物も含まれるものとする。難消化性デキストリンの市販品としては、例えば、ファイバーソル2(松谷化学工業株式会社製)、アミレッツC−7099M(王子コーンスターチ株式会社製)、ニュートリオース(ロケット・フルーレ社製)、プロミター85(テイト&ライル社製)等が挙げられる。難消化性デキストリンの還元物(還元難消化性デキストリン)の市販品としては、ファイバーソル2H(松谷化学工業株式会社製)が挙げられる。 Indigestible dextrin requires roasted dextrin obtained by acidifying (for example, adding hydrochloric acid) and / or heating starch derived from plants such as corn, wheat, rice, beans, potatoes, and tapioca. A water-soluble dietary fiber that has been subjected to enzymatic treatment with α-amylase and / or glucoamylase, and then desalted and decolorized as necessary, and has indigestible characteristics. The indigestible dextrin shall also include a reduced product of the indigestible dextrin produced by hydrogenation. Commercially available products of indigestible dextrin include, for example, Fibersol 2 (manufactured by Matsutani Chemical Industry Co., Ltd.), Amirets C-70099M (manufactured by Oji Corn Starch Co., Ltd.), Nutriose (manufactured by Rocket Foil Co., Ltd.), Promiter 85 (Tate) & Made by Lyle), etc. As a commercially available product of a reduced product of indigestible dextrin (reduced indigestible dextrin), Fibersol 2H (manufactured by Matsutani Chemical Industry Co., Ltd.) can be mentioned.
また、難消化性グルカンとは、澱粉分解物(好ましくは、デキストロース当量(DE)が70〜100の澱粉分解物)を加熱重合させて得られる水溶性食物繊維であり、難消化性の特徴を持つものをいう。この際、原料には、グルコース以外の単糖又はこれらの単糖を含むオリゴ糖等が含まれていてもよい。なお、「難消化性グルカン」は、難消化性グルカンそのものであってよく、難消化性グルカンを糖質分解酵素で処理した難消化性グルカン酵素処理物であってもよく、難消化性グルカン酵素処理物を分画処理した難消化性グルカン分画処理物であってもよく、難消化性グルカンにおける還元末端のアルデヒド基を水酸基に還元した難消化性グルカン還元処理物であってもよい。難消化性グルカンの市販品としては、例えば、フィットファイバー#80(日本食品化工株式会社製)等が挙げられる。 The indigestible glucan is a water-soluble dietary fiber obtained by heat-polymerizing a starch decomposition product (preferably a starch decomposition product having a dextrose equivalent (DE) of 70 to 100), and is characterized by being indigestible. It means what you have. At this time, the raw material may contain monosaccharides other than glucose, oligosaccharides containing these monosaccharides, and the like. The "indigestible glucan" may be the indigestible glucan itself, or may be an indigestible glucan enzyme-treated product obtained by treating the indigestible glucan with a glycolytic enzyme, and the indigestible glucan enzyme. It may be an indigestible glucan fractionated product obtained by fractionating the treated product, or may be an indigestible glucan reduced product obtained by reducing the aldehyde group at the reducing end of the indigestible glucan to a hydroxyl group. Examples of commercially available products of indigestible glucan include Fit Fiber # 80 (manufactured by Nihon Shokuhin Kako Co., Ltd.).
ポリデキストロースとは、ソルビトールと酸(例えば、クエン酸、リン酸)の存在下で、D−グルコースを高温で重合させて得られる、高度に分岐しランダムに結合した水溶性食物繊維であり、難消化性の特徴を持つものをいう。ポリデキストロースには、ポリデキストロースの還元物も含まれるものとする。ポリデキストロースの市販品としては、例えば、スターライトIII(株式会社光洋商会製)、ライテス(ファイザー株式会社製)、ライテスII(ダニスコ社製)等が挙げられる。ポリデキストロースの還元物(還元ポリデキストロース)の市販品としては、スターライトエリート(株式会社光洋商会製)が挙げられる。 Polydextrose is a highly branched and randomly bound water-soluble dietary fiber obtained by polymerizing D-glucose at a high temperature in the presence of sorbitol and an acid (for example, citric acid or phosphoric acid). Those with digestible characteristics. Polydextrose shall also include a reduced product of polydextrose. Examples of commercially available polydextrose products include Starlight III (manufactured by Koyo Shokai Co., Ltd.), Lites (manufactured by Pfizer Japan Inc.), Lites II (manufactured by Danisco Inc.), and the like. Examples of commercially available products of reduced polydextrose (reduced polydextrose) include Starlight Elite (manufactured by Koyo Shokai Co., Ltd.).
本発明の水溶性ヒアルロン酸ゲルにおいて、当該水溶性食物繊維の含有量は、ヒアルロン酸1質量部に対して、1〜300質量部である。前述のように高い生産性で製造可能な水溶性ヒアルロン酸ゲルをより一層好適に提供する観点からは、当該水溶性食物繊維の含有量は、ヒアルロン酸1質量部に対して、好ましくは2〜200質量部程度、より好ましくは3〜200質量部程度、さらに好ましくは5〜200質量部程度、さらに好ましくは3〜100質量部程度、さらに好ましくは5〜100質量部程度、さらに好ましくは8〜150質量部程度、さらに好ましくは8〜100質量部程度である。また、本発明の水溶性ヒアルロン酸ゲルにおける水溶性食物繊維の含有量は、「内閣府令食品表示基準」に示されている「食物繊維を含む」との表現が可能となることから、水溶性ヒアルロン酸ゲル100質量%中、3質量%以上が好ましく、さらに「高濃度の水溶性食物繊維を含む」との表現が可能となることから、水溶性ヒアルロン酸ゲル100質量%中、6質量%以上がより好ましい。 In the water-soluble hyaluronic acid gel of the present invention, the content of the water-soluble dietary fiber is 1 to 300 parts by mass with respect to 1 part by mass of hyaluronic acid. From the viewpoint of more preferably providing a water-soluble hyaluronic acid gel that can be produced with high productivity as described above, the content of the water-soluble dietary fiber is preferably 2 to 2 parts by mass with respect to 1 part by mass of hyaluronic acid. About 200 parts by mass, more preferably about 3 to 200 parts by mass, still more preferably about 5 to 200 parts by mass, still more preferably about 3 to 100 parts by mass, still more preferably about 5 to 100 parts by mass, still more preferably about 8 to 8 to 100 parts by mass. It is about 150 parts by mass, more preferably about 8 to 100 parts by mass. In addition, the content of water-soluble dietary fiber in the water-soluble hyaluronic acid gel of the present invention can be expressed as "containing dietary fiber" as shown in "Cabinet Office Ordinance Food Labeling Standards". 3% by mass or more is preferable in 100% by mass of the hyaluronic acid gel, and since it is possible to express that "containing a high concentration of water-soluble dietary fiber", 6% by mass in 100% by mass of the water-soluble hyaluronic acid gel. % Or more is more preferable.
ヒアルロン酸とは異なる酸としては、水と混合して酸性を示すものであれば、特に制限されず、無機酸、有機酸のいずれを使用することもできる。無機酸としては、例えば、リン酸、塩酸、硫酸、硝酸、過塩素酸、炭酸などが挙げられ、好ましくはリン酸、塩酸、硫酸が挙げられる。また、有機酸としては、ギ酸、酢酸、プロピオン酸、酪酸、イソ酪酸、吉草酸、リポ酸等のモノカルボン酸;コハク酸、フタル酸、フマル酸、シュウ酸、マロン酸、グルタル酸等のジカルボン酸;グリコール酸、クエン酸、乳酸、ピルビン酸、リンゴ酸、酒石酸、アジピン酸、サリチル酸等のオキシカルボン酸;グルコノ−δ−ラクトン、ラクトピオン酸等のポリヒドロキシ酸;グルタミン酸、アスパラギン酸等の酸性アミノ酸;ナールスゲン(登録商標、カルボキシメチルフェニルアミノカルボキシプロピルホスホン酸メチル)等のアミノ酸誘導体;アスコルビン酸、アスコルビン酸エチル、アスコルビン酸グルコシド等のアスコルビン酸またはその誘導体が挙げられ、好ましくは酢酸、アスコルビン酸、クエン酸、グリコール酸、乳酸、リンゴ酸、酒石酸、サリチル酸、アスコルビン酸エチル、アスコルビン酸グルコシド、グルコノ−δ−ラクトン、ラクトピオン酸などが挙げられる。また、経口摂取する用途の場合の酸は、好ましくは良好な酸味料でもあるクエン酸、酒石酸、アスコルビン酸、アスコルビン酸誘導体、リンゴ酸、フマル酸、コハク酸、アジピン酸、乳酸などが挙げられる。酸は、1種類単独で使用してもよいし、2種類以上を組み合わせて使用してもよい。 The acid different from hyaluronic acid is not particularly limited as long as it is mixed with water and exhibits acidity, and either an inorganic acid or an organic acid can be used. Examples of the inorganic acid include phosphoric acid, hydrochloric acid, sulfuric acid, nitric acid, perchloric acid, carbonic acid and the like, and preferably phosphoric acid, hydrochloric acid and sulfuric acid. Examples of organic acids include monocarboxylic acids such as formic acid, acetic acid, propionic acid, butyric acid, isobutyric acid, valeric acid and lipoic acid; and dicarboxylic acids such as succinic acid, phthalic acid, fumaric acid, oxalic acid, malonic acid and glutaric acid. Acids; oxycarboxylic acids such as glycolic acid, citric acid, lactic acid, pyruvate, malic acid, tartaric acid, adipic acid, salicylic acid; polyhydroxy acids such as glucono-δ-lactone and lactopionic acid; acidic amino acids such as glutamate and aspartic acid Amino acid derivatives such as Narsgen (registered trademark, methyl carboxymethylphenylaminocarboxypropylphosphonate); Ascorbic acid such as ascorbic acid, ethyl ascorbate, ascorbic acid glucoside or derivatives thereof, preferably acetic acid, ascorbic acid, citrus Examples thereof include acids, glycolic acids, lactic acid, malic acid, tartaric acid, salicylic acid, ethyl ascorbate, ascorbic acid glucoside, glucono-δ-lactone and lactopionic acid. In addition, examples of the acid for oral ingestion include citric acid, tartaric acid, ascorbic acid, ascorbic acid derivative, malic acid, fumaric acid, succinic acid, adipic acid, and lactic acid, which are also good acidulants. One type of acid may be used alone, or two or more types may be used in combination.
水溶性ヒアルロン酸ゲルは、以下の測定方法によって測定される水溶液のpHが、1.9〜6.3の範囲にあることが好ましく、2.0〜5.2の範囲にあることがより好ましく、2.0〜4.6の範囲にあることがさらに好ましい。pHは、ヒアルロン酸とは異なる酸の配合量などによって調整することができる。 In the water-soluble hyaluronic acid gel, the pH of the aqueous solution measured by the following measuring method is preferably in the range of 1.9 to 6.3, more preferably in the range of 2.0 to 5.2. , 2.0 to 4.6 is more preferred. The pH can be adjusted by adjusting the amount of an acid different from hyaluronic acid.
(pHの測定方法)
ヒアルロン酸1gを含む分量の前記水溶性ヒアルロン酸ゲルに含まれる成分のうち、水を除く全てのイオン性成分を水に溶解して200mLとなるように水溶液を調製し、得られた水溶液のpHを測定する。(Method of measuring pH)
Of the components contained in the water-soluble hyaluronic acid gel in an amount containing 1 g of hyaluronic acid, all the ionic components except water were dissolved in water to prepare an aqueous solution so as to have 200 mL, and the pH of the obtained aqueous solution was prepared. To measure.
水溶性ヒアルロン酸ゲルをそのまま水に溶解させてpHを測定すると、水溶性ヒアルロン酸ゲルに含まれる非イオン性成分の種類や量などによっては、本発明において好適なpHを測定することが困難になる場合があるため、上記のような測定方法によって調製した水溶液のpHを測定する。例えば、水溶性ヒアルロン酸ゲル中に、非イオン性である水溶性食物繊維や糖などが多量に含まれている場合、pHが正確に測定し難くなる。このため、本発明においては、水溶性ヒアルロン酸ゲルに配合する成分のうち、水を除く全てのイオン性成分のみを水に溶解し、得られた水溶液のpHを測定する方法を用いる。 When the water-soluble hyaluronic acid gel is dissolved in water as it is and the pH is measured, it becomes difficult to measure the pH suitable for the present invention depending on the type and amount of nonionic components contained in the water-soluble hyaluronic acid gel. Therefore, the pH of the aqueous solution prepared by the above-mentioned measuring method is measured. For example, when the water-soluble hyaluronic acid gel contains a large amount of nonionic water-soluble dietary fiber, sugar, etc., it becomes difficult to accurately measure the pH. Therefore, in the present invention, among the components to be blended in the water-soluble hyaluronic acid gel, only all the ionic components except water are dissolved in water, and the pH of the obtained aqueous solution is measured.
本発明の水溶性ヒアルロン酸ゲルにおいて、水の含有量が、前記ヒアルロン酸1質量部に対して、1〜300質量部である。前述のように高い生産性で製造可能な水溶性ヒアルロン酸ゲルをより一層好適に提供する観点からは、水の含有量は、ヒアルロン酸1質量部に対して、好ましくは2〜200質量部程度、より好ましくは5〜200質量部程度、さらに好ましくは5〜150質量部程度、さらに好ましくは8〜150質量部程度、さらに好ましくは2〜100質量部程度、3〜100質量部程度、さらに好ましくは5〜100質量部程度、さらに好ましくは8〜100質量部程度である。また、本発明の水溶性ヒアルロン酸ゲルにおける水の含有量は、水溶性ヒアルロン酸ゲル100質量%中、好ましくは15〜90質量%、より好ましくは15〜70質量%、さらに好ましくは15〜60質量%が挙げられる。 In the water-soluble hyaluronic acid gel of the present invention, the content of water is 1 to 300 parts by mass with respect to 1 part by mass of the hyaluronic acid. From the viewpoint of more preferably providing a water-soluble hyaluronic acid gel that can be produced with high productivity as described above, the content of water is preferably about 2 to 200 parts by mass with respect to 1 part by mass of hyaluronic acid. , More preferably about 5 to 200 parts by mass, still more preferably about 5 to 150 parts by mass, still more preferably about 8 to 150 parts by mass, still more preferably about 2 to 100 parts by mass, still more preferably about 3 to 100 parts by mass. Is about 5 to 100 parts by mass, more preferably about 8 to 100 parts by mass. The water content of the water-soluble hyaluronic acid gel of the present invention is preferably 15 to 90% by mass, more preferably 15 to 70% by mass, and further preferably 15 to 60% by mass in 100% by mass of the water-soluble hyaluronic acid gel. Mass% is mentioned.
また、本発明の水溶性ヒアルロン酸ゲルにおいて、前記水溶性食物繊維と水との配合割合(水溶性食物繊維:水)としては、質量基準で、好ましくは1:0.2〜15程度、より好ましくは1:0.3〜10程度、さらに好ましくは1:0.4〜5程度、1:0.5〜2程度が挙げられる。 Further, in the water-soluble hyaluronic acid gel of the present invention, the mixing ratio of the water-soluble dietary fiber and water (water-soluble dietary fiber: water) is preferably about 1: 0.2 to 15 on a mass basis. It is preferably about 1: 0.3 to 10, more preferably about 1: 0.4 to 5, and more preferably about 1: 0.5 to 2.
また、本発明の水溶性ヒアルロン酸ゲルにおいて、ヒアルロン酸、水溶性食物繊維、ヒアルロン酸とは異なる酸、及び水の合計含有率は、水溶性ヒアルロン酸ゲル100質量%中、30質量%以上であることが好ましく、40質量%以上がより好ましく、50質量%以上がより好ましく、60質量%以上がさらに好ましい。なお、当該合計含有率は、70質量%以上であってもよいし、75質量%以上であってもよいし、85質量%以上であってもよいし、90質量%以上であってもよいし、95質量%以上であってもよいし、100質量%であってもよい。なお、ヒアルロン酸、水溶性食物繊維、ヒアルロン酸とは異なる酸、及び水以外の他の成分が含まれる場合、他の成分としては、後述する糖(但し、25℃において、液体である液性多価アルコールを除く)が含まれることが好ましい。当該他の成分の含有量としては、例えば5〜70質量%程度、5〜60質量%程度、5〜50質量%程度、5〜40質量%程度、5〜30質量%程度、5〜20質量%程度、5〜10質量%などが挙げられる。 Further, in the water-soluble hyaluronic acid gel of the present invention, the total content of hyaluronic acid, water-soluble dietary fiber, an acid different from hyaluronic acid, and water is 30% by mass or more in 100% by mass of the water-soluble hyaluronic acid gel. It is preferably 40% by mass or more, more preferably 50% by mass or more, and further preferably 60% by mass or more. The total content may be 70% by mass or more, 75% by mass or more, 85% by mass or more, or 90% by mass or more. However, it may be 95% by mass or more, or 100% by mass. When hyaluronic acid, water-soluble dietary fiber, an acid different from hyaluronic acid, and other components other than water are contained, the other components include sugars described later (however, liquid properties that are liquid at 25 ° C.). (Excluding polyhydric alcohol) is preferably contained. The contents of the other components are, for example, about 5 to 70% by mass, about 5 to 60% by mass, about 5 to 50% by mass, about 5 to 40% by mass, about 5 to 30% by mass, and 5 to 20% by mass. %, 5 to 10% by mass, and the like.
糖(但し、25℃において、液体である液性多価アルコールを除く)としては、特に限定されず、単糖、二糖〜十糖程度までの糖を用いることができる。糖の具体例としては、グルコース、フルクトース、キシリトール、ソルビトール、マルチトール、エリスリトール、ラクチトール、マンニトール、トレハロース、ラクトース、マルトース、スクロース、ラフィノース、還元イソマルツノース、オリゴ糖(フラクトオリゴ糖、ガラクトオリゴ糖、マンナンオリゴ糖、乳糖果糖オリゴ糖、イソマルトオリゴ糖、乳糖オリゴ糖、マルトオリゴ糖、大豆オリゴ糖、キシロオリゴ糖など)、α−シクロデキストリン、β−シクロデキストリン、γ−シクロデキストリン、デキストリン、水飴、還元水飴、高糖化還元水飴、直鎖オリゴ糖アルコール、分岐オリゴ糖アルコール、ハチミツなどが挙げられる。また、腸内のビフィズス菌や乳酸菌などの善玉菌の養分となるオリゴ糖を配合することにより、腸内環境を整える水溶性食物繊維との相乗効果が期待できることから、本発明の水溶性ヒアルロン酸ゲルにオリゴ糖を配合することが好ましい。糖は、1種類単独で使用してもよいし、2種類以上を組み合わせて使用してもよい。 The sugar (excluding the liquid polyhydric alcohol which is a liquid at 25 ° C.) is not particularly limited, and a monosaccharide or a sugar up to about disaccharide to ten sugar can be used. Specific examples of sugars include glucose, fructose, xylitol, sorbitol, martitol, erythritol, lactitol, mannitol, trehalose, lactose, maltose, sucrose, raffinose, reduced isomaltose, oligosaccharides (fructo-oligosaccharides, galactooligosaccharides, mannan oligosaccharides). Sugar, lactose-fructose oligosaccharide, isomaltooligosaccharide, lactose oligosaccharide, maltooligosaccharide, soybean oligosaccharide, xylooligosaccharide, etc.), α-cyclodextrin, β-cyclodextrin, γ-cyclodextrin, dextrin, water candy, reduced water candy, high Examples include saccharified and reduced lactose, linear oligosaccharide alcohol, branched oligosaccharide alcohol, and honey. In addition, the water-soluble hyaluronic acid of the present invention can be expected to have a synergistic effect with the water-soluble dietary fiber that regulates the intestinal environment by blending oligosaccharides that serve as nutrients for good bacteria such as bifidobacteria and lactic acid bacteria in the intestine. It is preferable to add oligosaccharide to the gel. One type of sugar may be used alone, or two or more types may be used in combination.
本発明において、水溶性ヒアルロン酸ゲルに含まれる前記糖の含有率としては、特に制限されないが、前記の他の成分の含有量として記載した通り、例えば5〜70質量%程度、5〜60質量%程度、5〜50質量%程度、5〜40質量%程度、5〜30質量%程度、5〜20質量%程度、5〜10質量%などが挙げられる。なお、水溶性ヒアルロン酸ゲルに糖が複数種類含まれる場合は、糖の含有量は、全ての糖の合計量を意味する。 In the present invention, the content of the sugar contained in the water-soluble hyaluronic acid gel is not particularly limited, but as described as the content of the other components, for example, about 5 to 70% by mass, 5 to 60% by mass. %, About 5 to 50% by mass, about 5 to 40% by mass, about 5 to 30% by mass, about 5 to 20% by mass, about 5 to 10% by mass, and the like. When the water-soluble hyaluronic acid gel contains a plurality of types of sugars, the sugar content means the total amount of all the sugars.
なお、本発明の水溶性ヒアルロン酸ゲルは、1気圧下、25℃において液体である液性多価アルコールをさらに含んでいてもよい。このような液性多価アルコールとしては、特に制限されないが、好ましくはグリセリン、ジグリセリン等のグリセリン類;プロピレングリコール、ジプロピレングリコール等のプロピレングリコール類;1,3−プロパンジオール、ブタンジオール(1,3−ブタンジオール、1,4−ブタンジオールなど)、1,2−ペンタンジオール、1,2−ヘキサンジオール、1,2−オクタンジオール;エチレングリコール、ジエチレングリコール、トリエチレングリコール、ポリエチレングリコール等のエチレングリコール類などが挙げられ、より好ましくはグリセリン、ジグリセリン、プロピレングリコール、1,3−ブタンジオール、ポリエチレングリコール200、ポリエチレングリコール400、ポリエチレングリコール600、1,3−プロパンジオール、1,2−ペンタンジオール、1,2−ヘキサンジオールなどが挙げられる。これらの中でも、グリセリン、ジグリセリン、ブタンジオールなどが特に好ましい。多価アルコールは、1種類単独で使用してもよいし、2種類以上を組み合わせて使用してもよい。 The water-soluble hyaluronic acid gel of the present invention may further contain a liquid polyhydric alcohol that is liquid at 25 ° C. under 1 atm. Such a liquid polyhydric alcohol is not particularly limited, but is preferably glycerin such as glycerin and diglycerin; propylene glycol such as propylene glycol and dipropylene glycol; 1,3-propanediol and butanediol (1). , 3-Butandiol, 1,4-Butanediol, etc.), 1,2-Pentanediol, 1,2-hexanediol, 1,2-octanediol; ethylene such as ethylene glycol, diethylene glycol, triethylene glycol, polyethylene glycol, etc. Examples thereof include glycols, and more preferably glycerin, diglycerin, propylene glycol, 1,3-butanediol, polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600, 1,3-propanediol, and 1,2-pentanediol. , 1,2-Hexanediol and the like. Among these, glycerin, diglycerin, butanediol and the like are particularly preferable. One type of polyhydric alcohol may be used alone, or two or more types may be used in combination.
本発明の水溶性ヒアルロン酸ゲルにおける前記液性多価アルコールの含有率としては、特に制限されないが、前記の他の成分の含有量として記載した通り、例えば5〜50質量%程度、5〜40質量%程度、5〜30質量%程度、5〜20質量%程度、5〜10質量%程度などが挙げられる。なお、水溶性ヒアルロン酸ゲルに液性多価アルコールが複数種類含まれる場合は、液性多価アルコールの含有量は、全ての液性多価アルコールの合計量を意味する。 The content of the liquid polyhydric alcohol in the water-soluble hyaluronic acid gel of the present invention is not particularly limited, but as described as the content of the other components, for example, about 5 to 50% by mass, 5 to 40. Examples thereof include about mass%, about 5 to 30% by mass, about 5 to 20% by mass, and about 5 to 10% by mass. When the water-soluble hyaluronic acid gel contains a plurality of types of liquid polyhydric alcohols, the content of the liquid polyhydric alcohols means the total amount of all the liquid polyhydric alcohols.
なお、本発明の水溶性ヒアルロン酸ゲルは、液性多価アルコールを含まなくても、好適にゲル化している。すなわち、本発明の水溶性ヒアルロン酸ゲルは、実質的に液性多価アルコールを含まなくてもよい。例えば、本発明の水溶性ヒアルロン酸ゲル中における液性多価アルコールの含有量としては、1質量%以下、さらには0.1質量%以下、0質量%であってよい。 The water-soluble hyaluronic acid gel of the present invention is suitably gelled even if it does not contain a liquid polyhydric alcohol. That is, the water-soluble hyaluronic acid gel of the present invention does not have to contain substantially a liquid polyhydric alcohol. For example, the content of the liquid polyhydric alcohol in the water-soluble hyaluronic acid gel of the present invention may be 1% by mass or less, further 0.1% by mass or less, or 0% by mass.
本発明の水溶性ヒアルロン酸ゲルは、水溶性有機溶媒(前述の液性多価アルコールを除く)を含んでいてもよい。本発明の水溶性ヒアルロン酸ゲルが水溶性有機溶媒を含む場合、その含有量としては、10質量%以下、好ましくは5質量%以下、さらに好ましくは2質量%以下、1質量%以下、0質量%が挙げられる。水溶性有機溶媒としては、特に制限されず、例えば、エタノール、メタノール、イソプロパノール、アセトンなどが挙げられる。水溶性有機溶媒は、1種類単独で使用してもよいし、2種類以上を組み合わせて使用してもよい。本発明の水溶性ヒアルロン酸ゲルは、後述の通り、美容分野、医療分野、食品分野において、好適に使用される。このような観点からは、本発明の水溶性ヒアルロン酸ゲルは、水溶性有機溶媒を実質的に含まないことが好ましい。また、水溶性有機溶媒を用いると、ヒアルロン酸水溶液の粘度が高くなりやすいため、ヒアルロン酸水溶液を基板上などに薄く拡げることが困難になる場合がある。このため、水溶性有機溶媒を用いると、例えばキャスト法などの簡便な方法によって、水溶性ヒアルロン酸ゲルをシート状に形成することが困難となる場合がある。このような観点からも、本発明の水溶性ヒアルロン酸ゲルは、水溶性有機溶媒を実質的に含まないことが好ましい。 The water-soluble hyaluronic acid gel of the present invention may contain a water-soluble organic solvent (excluding the above-mentioned liquid polyhydric alcohol). When the water-soluble hyaluronic acid gel of the present invention contains a water-soluble organic solvent, the content thereof is 10% by mass or less, preferably 5% by mass or less, more preferably 2% by mass or less, 1% by mass or less, and 0% by mass. % Can be mentioned. The water-soluble organic solvent is not particularly limited, and examples thereof include ethanol, methanol, isopropanol, and acetone. The water-soluble organic solvent may be used alone or in combination of two or more. The water-soluble hyaluronic acid gel of the present invention is suitably used in the fields of beauty, medicine, and food as described later. From this point of view, it is preferable that the water-soluble hyaluronic acid gel of the present invention contains substantially no water-soluble organic solvent. Further, when a water-soluble organic solvent is used, the viscosity of the hyaluronic acid aqueous solution tends to be high, so that it may be difficult to spread the hyaluronic acid aqueous solution thinly on a substrate or the like. Therefore, when a water-soluble organic solvent is used, it may be difficult to form the water-soluble hyaluronic acid gel in the form of a sheet by a simple method such as a casting method. From this point of view, it is preferable that the water-soluble hyaluronic acid gel of the present invention substantially does not contain a water-soluble organic solvent.
本発明の水溶性ヒアルロン酸ゲルの弾性、機械的強度、形状維持性などは、水溶性ヒアルロン酸ゲル中の各成分の含有量、ヒアルロン酸の分子量、または前述のpHの測定方法における水溶液のpHの範囲を所定範囲に設定することにより、調整することができる。例えば、水溶性ヒアルロン酸ゲル中のヒアルロン酸の含有量を多くする(割合を大きくする)と、水溶性ヒアルロン酸ゲルが固くなり、水溶性ヒアルロン酸ゲルの弾性、機械的強度、形状維持性が高くなる傾向がある。また、例えば、水溶性ヒアルロン酸ゲル中のヒアルロン酸の分子量を大きくすると、水溶性ヒアルロン酸ゲルが固くなり、水溶性ヒアルロン酸ゲルの弾性、機械的強度、形状維持性が高くなる傾向がある。 The elasticity, mechanical strength, shape retention, etc. of the water-soluble hyaluronic acid gel of the present invention are the content of each component in the water-soluble hyaluronic acid gel, the molecular weight of hyaluronic acid, or the pH of the aqueous solution in the above-mentioned pH measuring method. It can be adjusted by setting the range of. For example, when the content of hyaluronic acid in the water-soluble hyaluronic acid gel is increased (the ratio is increased), the water-soluble hyaluronic acid gel becomes hard, and the elasticity, mechanical strength, and shape retention of the water-soluble hyaluronic acid gel are improved. It tends to be higher. Further, for example, when the molecular weight of hyaluronic acid in the water-soluble hyaluronic acid gel is increased, the water-soluble hyaluronic acid gel tends to become hard, and the elasticity, mechanical strength, and shape retention of the water-soluble hyaluronic acid gel tend to increase.
本発明の水溶性ヒアルロン酸ゲルは、水溶性である。本発明の水溶性ヒアルロン酸ゲルの水溶性とは、厚さ100μm、縦4cm、横4cmのシート状とした水溶性ヒアルロン酸ゲルをpH7.4のリン酸緩衝液100mL中に入れ、37℃で撹拌子を用いて120rpmで撹拌した場合に、4時間以内に完全に溶解することをいう。 The water-soluble hyaluronic acid gel of the present invention is water-soluble. The water solubility of the water-soluble hyaluronic acid gel of the present invention means that a sheet-shaped water-soluble hyaluronic acid gel having a thickness of 100 μm, a length of 4 cm, and a width of 4 cm is placed in 100 mL of a phosphate buffer solution having a pH of 7.4 and at 37 ° C. It means that when the mixture is stirred at 120 rpm using a stirrer, it is completely dissolved within 4 hours.
本発明の水溶性ヒアルロン酸ゲルの形状は、特に制限されず、用途に応じて適宜設定することができる。本発明の水溶性ヒアルロン酸ゲルの形状としては、例えば、シート状、粒状、塊状などが挙げられる。 The shape of the water-soluble hyaluronic acid gel of the present invention is not particularly limited and can be appropriately set according to the intended use. Examples of the shape of the water-soluble hyaluronic acid gel of the present invention include a sheet shape, a granular shape, and a lump shape.
例えば、水溶性ヒアルロン酸ゲルがシート状(水溶性ヒアルロン酸ゲルシート)である場合、後述の通り、例えば、本発明の水溶性ヒアルロン酸ゲルを皮膚や口腔内などに貼り付けて、化粧料、医薬組成物、または医療用具用組成物などとして好適に使用することができる。また、シート状の水溶性ヒアルロン酸ゲルを、口腔衛生改善フィルム等の食品組成物や口腔内徐放フィルム等の経口医薬組成物などとしてもよい。水溶性ヒアルロン酸ゲルシートの厚みとしては、特に制限されず、例えば0.01〜10mm程度、好ましくは0.05〜5mm程度が挙げられる。また、例えば水溶性ヒアルロン酸ゲルが塊状である場合には、スティック状やカップの容器に入った栄養補助食品等の食品組成物や顔や身体をマッサージする化粧料などとして好適に使用することができる。また、ゼリー飲料等の食品組成物や嚥下補助飲料等の経口医薬組成物などとしても好適に使用することができる。水溶性ヒアルロン酸ゲルが粒状である場合には、グミタイプの栄養補助食品等の食品組成物や経口医薬組成物などとして好適に使用することができる。 For example, when the water-soluble hyaluronic acid gel is in the form of a sheet (water-soluble hyaluronic acid gel sheet), as described later, for example, the water-soluble hyaluronic acid gel of the present invention may be attached to the skin, oral cavity, etc. It can be suitably used as a composition, a composition for medical devices, and the like. Further, the sheet-shaped water-soluble hyaluronic acid gel may be used as a food composition such as an oral hygiene improving film or an oral pharmaceutical composition such as an oral sustained-release film. The thickness of the water-soluble hyaluronic acid gel sheet is not particularly limited, and examples thereof include about 0.01 to 10 mm, preferably about 0.05 to 5 mm. Further, for example, when the water-soluble hyaluronic acid gel is in the form of a lump, it can be suitably used as a food composition such as a dietary supplement in a stick shape or a cup container, or as a cosmetic for massaging the face or body. it can. It can also be suitably used as a food composition such as a jelly beverage or an oral pharmaceutical composition such as a swallowing aid beverage. When the water-soluble hyaluronic acid gel is granular, it can be suitably used as a food composition such as a gummy-type dietary supplement or an oral pharmaceutical composition.
本発明の水溶性ヒアルロン酸ゲルは、保湿作用などを有するヒアルロン酸を含むため、美容分野、医療分野などにおいて、皮膚などに適用することができる。また、ヒアルロン酸や糖など、食用や医薬用として使用できる成分のみによって構成することもできるため、口腔内などにも好適に適用することができる。すなわち、本発明の水溶性ヒアルロン酸ゲルは、化粧料、食品組成物、医薬組成物、または医療用具用組成物などとして好適に使用することができる。 Since the water-soluble hyaluronic acid gel of the present invention contains hyaluronic acid having a moisturizing effect and the like, it can be applied to the skin and the like in the fields of beauty, medical treatment and the like. Further, since it can be composed only of ingredients that can be used for food or medicine such as hyaluronic acid and sugar, it can be suitably applied to the oral cavity and the like. That is, the water-soluble hyaluronic acid gel of the present invention can be suitably used as a cosmetic, a food composition, a pharmaceutical composition, a composition for a medical device, or the like.
本発明の水溶性ヒアルロン酸ゲルを化粧料、医薬組成物、または医療用具用組成物として使用する場合、化粧料、医薬部外品、医薬品、医療用具に配合される公知の成分(添加剤)をさらに配合することができる。このような成分としては、例えば、美白成分、抗老化成分、オイル成分、各種ビタミン及びその誘導体、各種動植物エキス、抗炎症剤、抗酸化剤、色素、香料(アロマ成分)、防腐剤などが挙げられる。また、本発明の水溶性ヒアルロン酸ゲルに脂溶性成分(添加剤)を添加する場合、脂溶性成分をリポソーム、エマルジョン、ナノエマルジョンなどの状態にして添加することもできる。これらの成分は、1種類単独で使用してもよいし、2種類以上を組み合わせて使用してもよい。 When the water-soluble hyaluronic acid gel of the present invention is used as a cosmetic, pharmaceutical composition, or medical device composition, known components (additives) to be blended in cosmetics, quasi-drugs, pharmaceuticals, and medical devices. Can be further blended. Examples of such components include whitening components, anti-aging components, oil components, various vitamins and their derivatives, various animal and plant extracts, anti-inflammatory agents, antioxidants, pigments, fragrances (aroma components), preservatives and the like. Be done. Further, when a fat-soluble component (additive) is added to the water-soluble hyaluronic acid gel of the present invention, the fat-soluble component can be added in the state of liposome, emulsion, nanoemulsion or the like. These components may be used alone or in combination of two or more.
美白成分の具体例としては、ビタミンCまたはその誘導体、アスタキサンチンなどが挙げられる。抗老化成分の具体例としては、ナールスゲン(登録商標、カルボキシメチルフェニルアミノカルボキシプロピルホスホン酸メチル)、ピロロキノリンキノン、LR2412(登録商標、テトラハイドロジャスモン酸ナトリウム)、グリーンピール(登録商標、植物性精油)などが挙げられる。オイル成分の具体例としては、スクワラン、ホホバオイル、オリーブオイルなどが挙げられる。 Specific examples of the whitening ingredient include vitamin C or a derivative thereof, astaxanthin and the like. Specific examples of the anti-aging component include Narsgen (registered trademark, methyl carboxymethylphenylaminocarboxypropylphosphonate), pyrroloquinoline quinone, LR2412 (registered trademark, sodium tetrahydrojasmonate), and green peel (registered trademark, vegetable essential oil). ) And so on. Specific examples of the oil component include squalane, jojoba oil, olive oil and the like.
また、本発明の水溶性ヒアルロン酸ゲルには、コラーゲン、ポリフィリン、プロテオグリカン、アセチルグルコサミン、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、リピジュア(登録商標、2−メタクリロイルオキシエチルホスホリルコリンのホモポリマーまたはコポリマー)、分子量が1万以下の低分子量のヒアルロン酸またはその塩などの水溶性高分子(添加剤)を配合してもよい。水溶性高分子は、1種類単独で使用してもよいし、2種類以上を組み合わせて使用してもよい。 In addition, the water-soluble hyaluronic acid gel of the present invention includes collagen, polyphyllin, proteoglycan, acetylglucosamine, hydroxypropyl cellulose, polyvinylpyrrolidone, polyvinyl alcohol, Lipidure (registered trademark, homopolymer or copolymer of 2-methacryloyloxyethyl phosphorylcholine). A water-soluble polymer (additive) such as hyaluronic acid having a molecular weight of 10,000 or less or a salt thereof may be blended. One type of water-soluble polymer may be used alone, or two or more types may be used in combination.
本発明の水溶性ヒアルロン酸ゲルには、適度な弾性、適度な機械的強度、及び適度な形状維持性を付与することができるため、本発明の水溶性ヒアルロン酸ゲルをそのまま化粧料のパック剤として使用することもできる。本発明の水溶性ヒアルロン酸ゲルをパック剤として使用する場合、本発明の水溶性ヒアルロン酸ゲルはシート状であることが好ましい。パック剤として使用する場合、本発明の水溶性ヒアルロン酸ゲルシートを直接皮膚に貼り付け、一定期間保持することにより、ヒアルロン酸による保湿効果などを皮膚に付与することができる。また、本発明の水溶性ヒアルロン酸ゲルが上記のような化粧料、医薬部外品、医薬品、医療用具に配合される公知の成分(添加剤)を含む場合、本発明の水溶性ヒアルロン酸ゲルシートを直接皮膚に貼り付けることにより、これらの成分を経皮吸収させることができる。 Since the water-soluble hyaluronic acid gel of the present invention can be imparted with appropriate elasticity, appropriate mechanical strength, and appropriate shape retention, the water-soluble hyaluronic acid gel of the present invention can be used as it is as a pack for cosmetics. Can also be used as. When the water-soluble hyaluronic acid gel of the present invention is used as a packing agent, the water-soluble hyaluronic acid gel of the present invention is preferably in the form of a sheet. When used as a pack, the water-soluble hyaluronic acid gel sheet of the present invention is directly attached to the skin and held for a certain period of time to impart a moisturizing effect of hyaluronic acid to the skin. Further, when the water-soluble hyaluronic acid gel of the present invention contains a known component (additive) to be blended in cosmetics, quasi-drugs, pharmaceuticals, and medical devices as described above, the water-soluble hyaluronic acid gel sheet of the present invention These components can be percutaneously absorbed by directly adhering to the skin.
また、本発明の水溶性ヒアルロン酸ゲルは、水溶性を有するため、水分中にヒアルロン酸が溶け出しやすい。このため、本発明の水溶性ヒアルロン酸ゲルは、皮膚などに適用された場合に、ヒアルロン酸による皮膚への潤いやハリを与える効果が高く、美容分野などへの使用に適している。例えば、本発明の水溶性ヒアルロン酸ゲルシートを皮膚に貼り付けた後、該シートに水をかけて徐々に溶解させながら皮膚をマッサージすることにより、水中に溶け出したヒアルロン酸による保湿効果をより高めることができる。 Further, since the water-soluble hyaluronic acid gel of the present invention has water solubility, hyaluronic acid easily dissolves in water. Therefore, the water-soluble hyaluronic acid gel of the present invention has a high effect of moisturizing and firming the skin by hyaluronic acid when applied to the skin and the like, and is suitable for use in the beauty field and the like. For example, after the water-soluble hyaluronic acid gel sheet of the present invention is attached to the skin, the moisturizing effect of the hyaluronic acid dissolved in water is further enhanced by massaging the skin while sprinkling water on the sheet and gradually dissolving the sheet. be able to.
さらに、本発明の水溶性ヒアルロン酸ゲルは、安全性と生体適合性に優れ、吸水性/保水性も高いことから、創傷部位、褥瘡部位を保護する医療用具などへの使用に適している。例えば、本発明の水溶性ヒアルロン酸ゲルは、安全性と生体適合性に優れ、吸水性/保水性も高いことから、救急絆創膏のパットや褥瘡部位の被覆保護材などとして好適に使用することができる。また、このような用途に使用する場合、水溶性ヒアルロン酸ゲル中に上皮成長因子等の治癒促進成分や抗菌成分(添加剤)を配合することもできる。 Further, the water-soluble hyaluronic acid gel of the present invention is excellent in safety and biocompatibility, and has high water absorption / water retention, so that it is suitable for use in a medical device for protecting a wound site and a pressure ulcer site. For example, the water-soluble hyaluronic acid gel of the present invention is excellent in safety and biocompatibility, and has high water absorption / water retention. Therefore, it can be suitably used as a pad for an emergency adhesive plaster or a covering protective material for a pressure ulcer site. it can. Further, when used for such an application, a healing promoting component such as epidermal growth factor or an antibacterial component (additive) can be blended in the water-soluble hyaluronic acid gel.
本発明の水溶性ヒアルロン酸ゲルは、支持体上に載せて用いてもよい。水溶性ヒアルロン酸ゲルを支持体上に形成することにより、好適に水溶性ヒアルロン酸ゲルシートとすることができる。支持体としては、特に制限されず、例えば、不織布、織布、織物、紙、高分子フィルム(ポリエチレンテレフタレート、ポリエチレンなどのポリオレフィン、塩化ビニル、ポリウレタン等のフィルム)などが挙げられ、より好ましくは、水溶性ヒアルロン酸ゲルと支持体との接着強度の観点から、不織布/高分子フィルムからなるラミネートフィルムや不織布などが挙げられる。また、支持体上の水溶性ヒアルロン酸ゲルを、皮膚に保持させる目的で、粘着テープ、ハイドロゲルテープ、サポーター、包帯、マスク、アイマスクなどで固定してもよい。 The water-soluble hyaluronic acid gel of the present invention may be used by being placed on a support. By forming the water-soluble hyaluronic acid gel on the support, a water-soluble hyaluronic acid gel sheet can be preferably obtained. The support is not particularly limited, and examples thereof include non-woven fabrics, woven fabrics, textiles, papers, polymer films (polyethylene terephthalate, polyolefins such as polyethylene, vinyl chloride, films such as polyurethane), and more preferably. From the viewpoint of the adhesive strength between the water-soluble hyaluronic acid gel and the support, a laminated film made of a non-woven fabric / polymer film, a non-woven fabric, and the like can be mentioned. Further, the water-soluble hyaluronic acid gel on the support may be fixed with an adhesive tape, a hydrogel tape, a supporter, a bandage, a mask, an eye mask, or the like for the purpose of holding the water-soluble hyaluronic acid gel on the skin.
本発明の水溶性ヒアルロン酸ゲルは、そのまま製品として単独で使用することができる。また、当該ゲルと粘着テープや支持体などとを一体化したものを製品とすることもできるし、水溶性ヒアルロン酸ゲルを製品とし、粘着テープ、ハイドロゲルテープ、サポーター、包帯、マスク、アイマスクなどで当該ゲルを固定して使用するものとしてもよい。 The water-soluble hyaluronic acid gel of the present invention can be used alone as a product as it is. In addition, a product in which the gel is integrated with an adhesive tape or a support can be used as a product, or a water-soluble hyaluronic acid gel is used as a product, and an adhesive tape, hydrogel tape, supporter, bandage, mask, eye mask, etc. can be used as a product. The gel may be fixed and used for use.
また、前述の通り、本発明の水溶性ヒアルロン酸ゲルは、ヒアルロン酸や糖など、食用または医薬用として使用できる成分のみによって構成することができるため、水溶性ヒアルロン酸ゲルを含む食品組成物、経口医薬組成物などとしても好適に使用することができる。 Further, as described above, since the water-soluble hyaluronic acid gel of the present invention can be composed only of ingredients that can be used for food or medicine such as hyaluronic acid and sugar, a food composition containing the water-soluble hyaluronic acid gel, It can also be suitably used as an oral pharmaceutical composition or the like.
本発明の水溶性ヒアルロン酸ゲルを食品組成物として使用する場合、食品組成物に配合される公知の成分(添加剤)をさらに配合することができる。このような成分としては、例えば、甘味料、高糖味度甘味料(アスパラテーム、スクラロース、グリチルリチン、サッカリン、ステビア、ズルチン、トリクロロシュークロース、ソーマチン、アセスルファムカリウムなど)、香料、着色料、酸味料、抗酸化剤、乳化剤、防腐剤、安定剤などが挙げられる。更に、栄養補助食品組成物とする場合、栄養補助食品組成物に配合される公知の有効成分(添加剤)をさらに配合することができる。このような有効成分としては、例えば、ビタミン、ミネラル、アミノ酸、ペプチド、プロテイン、グルコサミン、コンドロイチン、コラーゲン、メチルサルフォニルメタン、カルニチン、クルクミン、α−リポ酸、アスタキサンチン、ルテイン、ドコサヘキサエン酸、エイコサペンタエン酸、コエンザイムQ10、大豆イソフラボン、動植物エキス、ラクトフェリン、ビフィズス菌、乳酸菌、緑茶抽出物などが挙げられる。また、本発明の水溶性ヒアルロン酸ゲルを経口医薬組成物として使用する場合、経口医薬組成物に配合される公知の成分(添加剤)をさらに配合することができる。このような成分としては、例えば、薬効成分、香料、着色料、酸味料、抗酸化剤、乳化剤、防腐剤、安定剤などが挙げられる。食品組成物または経口医薬組成物において、これらの成分は、1種類単独で使用してもよいし、2種類以上を組み合わせて使用してもよい。 When the water-soluble hyaluronic acid gel of the present invention is used as a food composition, known components (additives) to be blended in the food composition can be further blended. Such ingredients include, for example, sweeteners, high-sugar sweeteners (aspartame, sucralose, glycyrrhizin, saccharin, stevia, dulcin, trichlorosucrose, thaumatin, acesulfame potassium, etc.), flavors, colorants, acidulants, etc. , Antioxidants, emulsifiers, preservatives, stabilizers and the like. Further, in the case of a dietary supplement composition, a known active ingredient (additive) to be blended in the dietary supplement composition can be further blended. Examples of such active ingredients include vitamins, minerals, amino acids, peptides, proteins, glucosamine, chondroitin, collagen, methylsulfonylmethane, carnitine, curcumin, α-lipoic acid, astaxanthin, lutein, docosahexaenoic acid, and eicosapentaenoic acid. Examples thereof include acid, coenzyme Q10, soybean isoflavone, animal and plant extracts, lactoferrin, bifidus bacteria, lactic acid bacteria, and green tea extract. Further, when the water-soluble hyaluronic acid gel of the present invention is used as an oral pharmaceutical composition, known components (additives) to be blended in the oral pharmaceutical composition can be further blended. Examples of such ingredients include medicinal ingredients, fragrances, colorants, acidulants, antioxidants, emulsifiers, preservatives, stabilizers and the like. In the food composition or the oral pharmaceutical composition, these components may be used alone or in combination of two or more.
本発明の水溶性ヒアルロン酸ゲルを用いた栄養補助食品組成物または経口医薬組成物は、ヒアルロン酸を含有しているため、当該栄養補助食品組成物または経口医薬組成物を経口摂取することによって、例えば、皮膚の含水量を増加させ、皮膚の保湿効果を高め得る効果などが期待できる。さらに、当該栄養補助食品組成物や経口医薬組成物は水溶性食物繊維を含有しているため、糖の吸収スピードの遅延作用(食後血糖の上昇抑制作用)、整腸作用、脂肪の吸収スピードの遅延作用(食後中性脂肪の上昇抑制作用)、内臓脂肪の低減作用、ミネラルの吸収促進作用、などの効果が期待できる。また、前述のような公知の成分(添加剤)を含む場合には、これらの成分による効果も発揮することができる。 Since the dietary supplement composition or oral pharmaceutical composition using the water-soluble hyaluronic acid gel of the present invention contains hyaluronic acid, by ingesting the dietary supplement composition or oral pharmaceutical composition orally, For example, it can be expected to have an effect of increasing the water content of the skin and enhancing the moisturizing effect of the skin. Furthermore, since the dietary supplement composition and the oral pharmaceutical composition contain water-soluble dietary fiber, the effect of delaying the absorption speed of sugar (the effect of suppressing the increase in postprandial blood glucose), the effect of intestinal regulation, and the effect of absorbing fat are reduced. It can be expected to have effects such as delaying action (suppressing the rise of triglyceride after meals), reducing visceral fat, and promoting absorption of minerals. Further, when the above-mentioned known components (additives) are contained, the effects of these components can also be exhibited.
本発明の水溶性ヒアルロン酸ゲルを食品組成物または経口医薬組成物とする場合、これらの形状としては特に限定されないが、例えば、口腔衛生改善フィルムのようなシート状、グミタイプのような粒状、スティック状やカップの容器に入った栄養補助食品組成物や嚥下補助飲料/ゼリー飲料のような塊状などとすることができる。特に、近年、健康食品や栄養補助食品をおいしく手軽に摂取できる剤型としてグミが注目されており、グミタイプの粒状は好適な形状である。すなわち、本発明の水溶性ヒアルロン酸ゲルは、粒状のグミ組成物であることも好ましい。 When the water-soluble hyaluronic acid gel of the present invention is used as a food composition or an oral pharmaceutical composition, the shapes thereof are not particularly limited, but for example, a sheet such as an oral hygiene improving film, a granule such as a gummy type, or a stick. It can be in the form of a dietary supplement composition in a cup container or in the form of a lump such as a swallowing supplement / jelly drink. In particular, in recent years, gummy candies have been attracting attention as a dosage form that allows delicious and easy ingestion of health foods and dietary supplements, and gummy type granules have a suitable shape. That is, the water-soluble hyaluronic acid gel of the present invention is preferably a granular gummy composition.
本発明の水溶性ヒアルロン酸ゲルは、X線結晶解析に用いる蛋白質を固相で結晶化させるためのハイドロゲルとしても好適に使用することができる。 The water-soluble hyaluronic acid gel of the present invention can also be suitably used as a hydrogel for crystallizing a protein used for X-ray crystallography in a solid phase.
本発明の水溶性ヒアルロン酸ゲルの製造方法は、特に制限されないが、例えば、ヒアルロン酸と、ヒアルロン酸1質量部に対して1〜300質量部の水溶性食物繊維と、ヒアルロン酸とは異なる酸と、ヒアルロン酸1質量部に対して1〜300質量部の水を含み、40℃以上の温度に加熱されたヒアルロン酸水溶液を調製する工程1と、加熱されたヒアルロン酸水溶液を40℃未満の温度に冷却する工程2とを備える方法によって、好適に製造することができる。 The method for producing the water-soluble hyaluronic acid gel of the present invention is not particularly limited, but for example, hyaluronic acid, 1 to 300 parts by mass of water-soluble dietary fiber with respect to 1 part by mass of hyaluronic acid, and an acid different from hyaluronic acid. Step 1 of preparing a hyaluronic acid aqueous solution containing 1 to 300 parts by mass of water with respect to 1 part by mass of hyaluronic acid and heated to a temperature of 40 ° C. or higher, and the heated hyaluronic acid aqueous solution having a temperature of less than 40 ° C. It can be suitably produced by a method including the step 2 of cooling to a temperature.
工程1における加熱温度としては、ヒアルロン酸水溶液に含まれる各成分を均一に溶解・分散させる観点から、好ましくは50℃以上、より好ましくは60℃以上、さらに好ましくは70℃以上であり、上限としては、100℃以下が挙げられる。また、工程2における冷却温度としては、ヒアルロン酸水溶液がゲル化して水溶性ヒアルロン酸ゲルが形成される温度であれば、特に制限されず、40℃未満、35℃以下、30℃以下、25℃以下などが挙げられ、下限については例えば0℃が挙げられる。 The heating temperature in step 1 is preferably 50 ° C. or higher, more preferably 60 ° C. or higher, still more preferably 70 ° C. or higher, as an upper limit, from the viewpoint of uniformly dissolving and dispersing each component contained in the hyaluronic acid aqueous solution. Is 100 ° C. or lower. The cooling temperature in step 2 is not particularly limited as long as it is a temperature at which the hyaluronic acid aqueous solution gels to form a water-soluble hyaluronic acid gel, and is less than 40 ° C., 35 ° C. or lower, 30 ° C. or lower, 25 ° C. The following can be mentioned, and the lower limit is, for example, 0 ° C.
本発明の水溶性ヒアルロン酸ゲルの製造方法において、水を多量に蒸発させる工程を行う必要はない。すなわち、加熱されたヒアルロン酸水溶液がゲル化する温度に冷却すれば、ヒアルロン酸水溶液と実質的に同じ組成を有する本発明の水溶性ヒアルロン酸ゲルが得られる。工程1から工程2の間における、水溶性ヒアルロン酸水溶液からの水の減少率は、好ましくは50質量%以下、より好ましくは30質量%以下、さらに好ましくは20質量%以下、特に好ましくは10質量%以下である(すなわち、ヒアルロン酸水溶液に含まれる水の含有量を100質量%(基準)とした場合に、水溶性ヒアルロン酸ゲルに含まれる水の含有量は、好ましくは50質量%以上、より好ましくは70質量%以上、さらに好ましくは80質量%以上、特に好ましくは90質量%以上である。)。 In the method for producing a water-soluble hyaluronic acid gel of the present invention, it is not necessary to carry out a step of evaporating a large amount of water. That is, when the heated hyaluronic acid aqueous solution is cooled to a gelling temperature, the water-soluble hyaluronic acid gel of the present invention having substantially the same composition as the hyaluronic acid aqueous solution can be obtained. The reduction rate of water from the water-soluble hyaluronic acid aqueous solution between steps 1 and 2 is preferably 50% by mass or less, more preferably 30% by mass or less, still more preferably 20% by mass or less, and particularly preferably 10% by mass. % Or less (that is, when the content of water contained in the aqueous hyaluronic acid solution is 100% by mass (reference), the content of water contained in the water-soluble hyaluronic acid gel is preferably 50% by mass or more. More preferably 70% by mass or more, further preferably 80% by mass or more, and particularly preferably 90% by mass or more).
本発明の水溶性ヒアルロン酸ゲルの製造方法において、各成分の混合順序は、特に制限されないが、ヒアルロン酸、水溶性食物繊維、及び水が含まれる溶液を加熱し、ヒアルロン酸とは異なる酸を添加することで、ヒアルロン酸水溶液から均質なゲルが形成されやすい。また、各成分の混合方法も特に制限されず、例えば攪拌機などを用いて攪拌すればよい。 In the method for producing a water-soluble hyaluronic acid gel of the present invention, the mixing order of each component is not particularly limited, but a solution containing hyaluronic acid, water-soluble dietary fiber, and water is heated to obtain an acid different from hyaluronic acid. By adding, a homogeneous gel is easily formed from the hyaluronic acid aqueous solution. Further, the mixing method of each component is not particularly limited, and for example, stirring may be performed using a stirrer or the like.
また、本発明の水溶性ヒアルロン酸ゲルの製造方法において、水溶性食物繊維や糖を飽和溶解度以上の濃度とするため、加熱しながら水に水溶性食物繊維や糖を飽和溶解度となるように溶解させた後、この水溶液を加熱濃縮する工程を備えてもよい。 Further, in the method for producing a water-soluble hyaluronic acid gel of the present invention, in order to make the water-soluble dietary fiber and sugar have a concentration equal to or higher than the saturated solubility, the water-soluble dietary fiber and sugar are dissolved in water so as to have a saturated solubility while heating. After that, a step of heating and concentrating this aqueous solution may be provided.
水溶性ヒアルロン酸ゲルシートの製造方法において、ゲルが所定の厚みとなるようにトレーやバット等の容器にヒアルロン酸水溶液を入れ、ゲル化させることによって、水溶性ヒアルロン酸ゲルシートを容易に製造することができる。すなわち、加熱されたヒアルロン酸水溶液を容器に入れて冷却することにより、例えば、容器内に形成された水溶性ヒアルロン酸ゲルシートを、容器ごとそのまま最終製品とすることもでき、水溶性ヒアルロン酸ゲルシートを切断するなどの加工工程を省略することができる。 In the method for producing a water-soluble hyaluronic acid gel sheet, a water-soluble hyaluronic acid gel sheet can be easily produced by putting an aqueous hyaluronic acid solution in a container such as a tray or a bat so that the gel has a predetermined thickness and gelling the gel. it can. That is, by putting a heated hyaluronic acid aqueous solution in a container and cooling it, for example, the water-soluble hyaluronic acid gel sheet formed in the container can be used as a final product as it is, and the water-soluble hyaluronic acid gel sheet can be obtained. Processing steps such as cutting can be omitted.
また、塊状のヒアルロン酸ゲルの製造方法において、加熱されたヒアルロン酸水溶液を容器に入れて冷却することにより、例えば、容器内に形成された水溶性ヒアルロン酸ゲルを、スティック状やカップの容器に入った栄養補助食品、ゼリー飲料等の食品や嚥下補助飲料等の医薬品として、容器ごとそのまま最終製品にすることができる。 Further, in the method for producing a massive hyaluronic acid gel, a heated hyaluronic acid aqueous solution is placed in a container and cooled, so that, for example, the water-soluble hyaluronic acid gel formed in the container is put into a stick-shaped or cup container. It can be used as a final product as it is as a food such as a nutritional supplement, a jelly drink, or a pharmaceutical product such as a swallowing supplement.
また、グミタイプのような粒状のヒアルロン酸ゲルの製造方法(すなわち粒状のグミ組成物の製造方法)において、スターチに形成された型やシリコーン等の型の中に加熱されたヒアルロン酸水溶液を充填して冷却することにより、粒状の水溶性ヒアルロン酸ゲルとすることができる。更に、この粒状の水溶性ヒアルロン酸ゲルを乾燥させることで、より弾力性のあるグミ食感の水溶性ヒアルロン酸ゲルとすることができる。必要に応じて、光沢剤、離型剤等をグミの表面に付着させてもよい。 Further, in a method for producing a granular hyaluronic acid gel such as a gummy type (that is, a method for producing a granular gummy composition), a heated hyaluronic acid aqueous solution is filled in a mold formed on a starch or a mold such as silicone. By cooling the gel, a granular water-soluble hyaluronic acid gel can be obtained. Further, by drying the granular water-soluble hyaluronic acid gel, a more elastic water-soluble hyaluronic acid gel having a gummy texture can be obtained. If necessary, a brightener, a mold release agent, or the like may be attached to the surface of the gummy.
グミタイプのような粒状のヒアルロン酸ゲルの製造方法(すなわち粒状のグミ組成物の製造方法)において、一般的なグミの製造方法と同様にして、加熱濃縮しながら混錬可能なヒアルロン酸水溶液を調製し、そのヒアルロン酸水溶液をスターチに形成された型やシリコーン等の型の中に充填することにより、粒状の水溶性ヒアルロン酸ゲルとすることができる。更に、この粒状の水溶性ヒアルロン酸ゲルを乾燥させることで、より弾力性のあるグミ食感の水溶性ヒアルロン酸ゲル(グミ組成物)とすることができる。必要に応じて、光沢剤、離型剤等をグミの表面に付着させてもよい。 In a method for producing a granular hyaluronic acid gel such as a gummy type (that is, a method for producing a granular gummy composition), an aqueous hyaluronic acid solution that can be kneaded while being heat-concentrated is prepared in the same manner as a general gummy production method. Then, by filling the hyaluronic acid aqueous solution into a mold formed in starch or a mold such as silicone, a granular water-soluble hyaluronic acid gel can be obtained. Further, by drying the granular water-soluble hyaluronic acid gel, a water-soluble hyaluronic acid gel (gummy composition) having a more elastic gummy texture can be obtained. If necessary, a brightener, a mold release agent, or the like may be attached to the surface of the gummy.
また、本発明の水溶性ヒアルロン酸ゲルの製造方法において、ヒアルロン酸水溶液をゲル化した後、例えば、化粧料、食品、医薬部外品、医薬品、医療用具等に配合される上記各種成分(添加剤)を添加する工程をさらに備えていてもよい。例えば、前述の工程2の後、上記各種成分(添加剤)を添加することもできる。 Further, in the method for producing a water-soluble hyaluronic acid gel of the present invention, after gelling an aqueous hyaluronic acid solution, for example, the above-mentioned various components (additions) to be blended in cosmetics, foods, quasi-drugs, pharmaceuticals, medical devices, etc. The agent) may be further provided. For example, after the above-mentioned step 2, the above-mentioned various components (additives) can be added.
以下に、実施例及び比較例を示して本発明を詳細に説明する。ただし、本発明は、実施例に限定されない。なお、以下の実施例及び比較例で用いた試薬は、以下の通りである。各表中の組成の単位は、質量部である。 Hereinafter, the present invention will be described in detail with reference to Examples and Comparative Examples. However, the present invention is not limited to the examples. The reagents used in the following examples and comparative examples are as follows. The unit of composition in each table is parts by mass.
<試薬>
ヒアルロン酸(230万):ヒアルロン酸ナトリウム、キューピー株式会社製の商品名「HYALURONSANHA−LQSH」(製品表示:分子量160万〜290万、平均分子量230万)
ヒアルロン酸(160万):ヒアルロン酸ナトリウム、キューピー株式会社製の商品名「HYALURONSANHA−LQH」(製品表示:分子量120万〜220万、平均分子量160万)
ヒアルロン酸(80万):ヒアルロン酸ナトリウム、キューピー株式会社製の商品名「ヒアベスト(J)」(製品表示:分子量60万〜120万、平均分子量80万)
ヒアルロン酸(35万):ヒアルロン酸、キューピー株式会社製の商品名「ヒアルロン酸HA−LF−P」(製品表示:分子量20万〜50万、平均分子量35万)
ヒアルロン酸(10万):ヒアルロン酸ナトリウム、キッコーマンバイオケミファ株式会社製の商品名「ヒアルロン酸FCH−SU」(製品表示:平均分子量5万〜11万)イソマルトデキストリン:株式会社林原製の商品名「ファイバリクサ」
難消化性デキストリン:松谷化学工業株式会社製の商品名「ファイバーソル2」
還元難消化性デキストリン:松谷化学工業株式会社製の商品名「ファイバーソル2H」
難消化性グルカン:日本食品化工株式会社製の商品名「フィットファイバー#80」固形分約72%
ポリデキストロース:株式会社光洋商会製の商品名「スターライトIII」
還元ポリデキストロース:株式会社光洋商会製の商品名「スターライトエリート」固形分70%
イソマルトオリゴ糖:株式会社林原製の商品名「パノラップ」固形分約75質量%
フラクトオリゴ糖:株式会社明治フードマテリアル製の商品名「メイオリゴP(粉末)」
乳糖果糖オリゴ糖;株式会社林原製の商品名「乳果オリゴ700」固形分約75質量%
デキストリン:松谷化学工業株式会社製の商品名「パインデックス#2」
キシリトール:和光純薬工業株式会社製のキシリトール(特級)
ソルビトール;富士フィルム和光純薬工業株式会社製のソルビトール(特級)
ハチミツ:アピ株式会社製の精製蜂蜜固形分約80質量%
グルコース:和光純薬工業株式会社製のD(+)−グルコース(特級)
マルトース:和光純薬工業株式会社製のD(+)−マルトース一水和物(特級)
スクロース:和光純薬工業株式会社製のスクロース(特級)
フルクトース:和光純薬工業株式会社製のD(−)−フルクトース(特級)
還元イソマルツノース;三井製糖株式会社製の商品名「パラチニット」
グリセリン;富士フィルム和光純薬株式会社製のグリセリン(特急)
クエン酸:和光純薬工業株式会社製のクエン酸(特級)
酢酸:和光純薬工業株式会社製の酢酸(特級)
乳酸:和光純薬工業株式会社製のDL−乳酸(特級)
酒石酸:和光純薬工業株式会社製のD(−)−酒石酸(一級)
アスコルビン酸(ビタミンC):和光純薬工業株式会社製のL(+)−アスコルビン酸(特級)
アスコルビン酸グルコシド;株式会社林原製の商品名「アスコフレッシュ」
アスパラギン酸:和光純薬株式会社製のDL−アスパラギン酸(特級)
リン酸:和光純薬工業株式会社製のリン酸(特級)
硫酸:和光純薬工業株式会社製の硫酸(特級)<Reagent>
Hyaluronic acid (2.3 million): Sodium hyaluronate, trade name "HYALURONSANHA-LQSH" manufactured by Kewpie Corp. (Product label: molecular weight 1.6 million to 2.9 million, average molecular weight 2.3 million)
Hyaluronic acid (1.6 million): Sodium hyaluronate, trade name "HYALURONSANHA-LQH" manufactured by Kewpie Corp. (Product label: molecular weight 1.2 million to 2.2 million, average molecular weight 1.6 million)
Hyaluronic acid (800,000): Sodium hyaluronate, trade name "Hiabest (J)" manufactured by Kewpie Corp. (Product label: molecular weight 600,000-1.2 million, average molecular weight 800,000)
Hyaluronic acid (350,000): Hyaluronic acid, trade name "Hyaluronic acid HA-LF-P" manufactured by Kewpie Corp. (Product label: molecular weight 200,000-500,000, average molecular weight 350,000)
Hyaluronic acid (100,000): Sodium hyaluronate, product name "Hyaluronic acid FCH-SU" manufactured by Kikkoman Biochemifa Co., Ltd. (Product label: average molecular weight 50,000 to 110,000) Isomaltodextrin: Product name manufactured by Hayashibara Co., Ltd. "Fiberlixer"
Indigestible dextrin: Product name "Fiber Sol 2" manufactured by Matsutani Chemical Industry Co., Ltd.
Reduced indigestible dextrin: Product name "Fibersol 2H" manufactured by Matsutani Chemical Industry Co., Ltd.
Indigestible glucan: Brand name "Fit Fiber # 80" manufactured by Nihon Shokuhin Kako Co., Ltd. Solid content about 72%
Polydextrose: Product name "Starlight III" manufactured by Koyo Shokai Co., Ltd.
Reduced polydextrose: Product name "Starlight Elite" manufactured by Koyo Shokai Co., Ltd. Solid content 70%
Isomaltooligosaccharide: Product name "Panowrap" manufactured by Hayashibara Co., Ltd. Solid content approx. 75% by mass
Fructooligosaccharide: Product name "Meioligo P (powder)" manufactured by Meiji Food Material Co., Ltd.
Lactose-fructose oligosaccharide; brand name "milk-fructose oligo 700" manufactured by Hayashibara Co., Ltd. Solid content approx. 75% by mass
Dextrin: Product name "Paindex # 2" manufactured by Matsutani Chemical Industry Co., Ltd.
Xylitol: Xylitol (special grade) manufactured by Wako Pure Chemical Industries, Ltd.
Sorbitol; Sorbitol (special grade) manufactured by Fuji Film Wako Pure Chemical Industries, Ltd.
Honey: Approximately 80% by mass of refined honey solids manufactured by Api Co., Ltd.
Glucose: D (+)-glucose (special grade) manufactured by Wako Pure Chemical Industries, Ltd.
Maltose: D (+)-maltose monohydrate (special grade) manufactured by Wako Pure Chemical Industries, Ltd.
Sucrose: Sucrose (special grade) manufactured by Wako Pure Chemical Industries, Ltd.
Fructose: D (-)-fructose (special grade) manufactured by Wako Pure Chemical Industries, Ltd.
Reduced Isomalz North; Brand name "Palatinit" manufactured by Mitsui Sugar Co., Ltd.
Glycerin; Glycerin manufactured by Fuji Film Wako Pure Chemical Industries, Ltd. (Limited Express)
Citric acid: Citric acid (special grade) manufactured by Wako Pure Chemical Industries, Ltd.
Acetic acid: Acetic acid manufactured by Wako Pure Chemical Industries, Ltd. (special grade)
Lactic acid: DL-lactic acid (special grade) manufactured by Wako Pure Chemical Industries, Ltd.
Tartaric acid: D (-)-tartaric acid (first grade) manufactured by Wako Pure Chemical Industries, Ltd.
Ascorbic acid (vitamin C): L (+)-ascorbic acid (special grade) manufactured by Wako Pure Chemical Industries, Ltd.
Ascorbic acid glucoside; trade name "Asco Fresh" manufactured by Hayashibara Co., Ltd.
Aspartic acid: DL-aspartic acid (special grade) manufactured by Wako Pure Chemical Industries, Ltd.
Phosphoric acid: Phosphoric acid (special grade) manufactured by Wako Pure Chemical Industries, Ltd.
Sulfuric acid: Sulfuric acid manufactured by Wako Pure Chemical Industries, Ltd. (special grade)
[実施例1〜4及び比較例1〜9]
室温環境(25℃)において、表1に記載の配合比(質量部)となるように、ヒアルロン酸(ヒアルロン酸ナトリウム)を蒸留水に均一に溶解した後、さらにクエン酸以外の成分(水溶性食物繊維又は糖)を添加して50℃で24時間加熱してヒアルロン酸水溶液を調製した。このヒアルロン酸水溶液を室温に戻した後、プロペラ式回転型撹拌装置を用いて撹拌しながら少しずつクエン酸を添加して溶解した後、室温で24時間保管し、表1の加熱前の性状(25℃)を有するゲル状物を得た。次に、得られたゲル状物約10gをプラスチックチューブに入れて密栓し、80℃で12時間加熱して、表1の加熱時の性状(80℃)を有する液状物を得た。その後、室温で3日保管し、プラスチックチューブの内容物の性状を観察した。その結果、それぞれ、内容物は表1に記載の冷却後の性状(25℃)を有していた。[Examples 1 to 4 and Comparative Examples 1 to 9]
In a room temperature environment (25 ° C.), hyaluronic acid (sodium hyaluronate) is uniformly dissolved in distilled water so that the compounding ratio (parts by mass) shown in Table 1 is obtained, and then components other than citric acid (water-soluble) are further dissolved. (Distilled fiber or sugar) was added and heated at 50 ° C. for 24 hours to prepare an aqueous hyaluronic acid solution. After returning this aqueous hyaluronic acid solution to room temperature, citric acid was gradually added and dissolved while stirring using a propeller-type rotary stirrer, and then stored at room temperature for 24 hours. A gel having a temperature of 25 ° C.) was obtained. Next, about 10 g of the obtained gel-like substance was placed in a plastic tube, sealed tightly, and heated at 80 ° C. for 12 hours to obtain a liquid substance having the properties at the time of heating (80 ° C.) in Table 1. Then, it was stored at room temperature for 3 days, and the properties of the contents of the plastic tube were observed. As a result, each of the contents had the properties after cooling (25 ° C.) shown in Table 1.
※1:固形分約72質量%
※2:固形分約75質量%
※3:固形分約80質量%* 1: Solid content approx. 72% by mass
* 2: Solid content approx. 75% by mass
* 3: Solid content of about 80% by mass
なお、表1において、「不均質ゲル」とは、硬い部分と柔らかい部分とが混在したゲルを意味している。実施例1〜4及び比較例1〜9においては、室温において、水溶性ヒアルロン酸水溶液にクエン酸を加えることで、迅速にゲル化したため、加熱前の性状(25℃)においては、クエン酸が均一に分散しておらず、このような不均質なゲルが形成された。また、表1において、「均質ゲル」とは、ゲル全体の硬さが均質であるものを意味している。実施例1〜4の水溶性ヒアルロン酸ゲルは、不均質ゲルを80℃に加熱することによって、クエン酸が均一に分散した均質な液状物が生成し、これを室温に冷却することで、均質ゲルが形成された。 In Table 1, the "inhomogeneous gel" means a gel in which a hard portion and a soft portion are mixed. In Examples 1 to 4 and Comparative Examples 1 to 9, citric acid was rapidly gelled by adding citric acid to a water-soluble hyaluronic acid aqueous solution at room temperature, so that citric acid was present in the properties before heating (25 ° C.). It was not uniformly dispersed and such an inhomogeneous gel was formed. Further, in Table 1, the “homogeneous gel” means a gel in which the hardness of the entire gel is homogeneous. In the water-soluble hyaluronic acid gels of Examples 1 to 4, a homogeneous liquid substance in which citric acid is uniformly dispersed is produced by heating the heterogeneous gel to 80 ° C., and this is cooled to room temperature to be homogeneous. A gel was formed.
表1に示されるとおり、実施例1〜4の水溶性ヒアルロン酸ゲルは、ヒアルロン酸、水溶性食物繊維、ヒアルロン酸とは異なる酸、及び水を含む水溶性ヒアルロン酸ゲルであって、水溶性食物繊維は、グルコースを構成糖とし、1−4結合及び1−6結合以外の結合を有し、環状構造ではない多糖類であり、水の含有量がヒアルロン酸1質量部に対して1〜300質量部であり、水溶性食物繊維の含有量がヒアルロン酸1質量部に対して1〜300質量部である。実施例1〜4の水溶性ヒアルロン酸ゲルは、水溶性ヒアルロン酸ゲルの製造において、ヒアルロン酸水溶液から多くの水を蒸発させる工程を設ける必要が無く、高い生産性で製造可能である。また、実施例1〜4の水溶性ヒアルロン酸ゲルは、加熱すれば液状化し、冷却すればゲル化する性質を有しており、水溶性ヒアルロン酸ゲルの組成において、加熱環境で流動性のある均一なヒアルロン酸水溶液を調製することができ、その水溶液のまま容器に充填することができ、かつ、室温程度に冷却されると水溶性ヒアルロン酸ゲルを形成する性質を有することが分かる。当該水溶性ヒアルロン酸ゲルは、このような性質を備えていることから、高い生産性で製造できるだけでなく、例えば水溶性ヒアルロン酸ゲルが物流過程で高温環境に置かれて液状化しても、室温で再びゲル化するため、製品としての安定性に優れている。 As shown in Table 1, the water-soluble hyaluronic acid gels of Examples 1 to 4 are water-soluble hyaluronic acid gels containing hyaluronic acid, water-soluble dietary fiber, an acid different from hyaluronic acid, and water, and are water-soluble. Dietary fiber is a polysaccharide having glucose as a constituent sugar, having bonds other than 1-4 bonds and 1-6 bonds, and not having a cyclic structure, and has a water content of 1 to 1 part by mass of hyaluronic acid. It is 300 parts by mass, and the content of water-soluble dietary fiber is 1 to 300 parts by mass with respect to 1 part by mass of hyaluronic acid. The water-soluble hyaluronic acid gels of Examples 1 to 4 can be produced with high productivity without the need to provide a step of evaporating a large amount of water from the hyaluronic acid aqueous solution in the production of the water-soluble hyaluronic acid gel. Further, the water-soluble hyaluronic acid gels of Examples 1 to 4 have a property of liquefying when heated and gelling when cooled, and the composition of the water-soluble hyaluronic acid gel is fluid in a heating environment. It can be seen that a uniform hyaluronic acid aqueous solution can be prepared, the aqueous solution can be filled in a container as it is, and it has a property of forming a water-soluble hyaluronic acid gel when cooled to about room temperature. Since the water-soluble hyaluronic acid gel has such properties, it can be produced with high productivity, and for example, even if the water-soluble hyaluronic acid gel is placed in a high temperature environment in the distribution process and liquefied, it is at room temperature. Because it gels again in, it has excellent stability as a product.
一方、比較例1〜9の水溶性ヒアルロン酸ゲルには、前記所定の水溶性食物繊維が所定量含まれていない。比較例1〜9の水溶性ヒアルロン酸ゲルは、水溶性ヒアルロン酸ゲルの組成において、加熱環境でヒアルロン酸水溶液を調製することができるが、冷却してもゲル化する性質を有しないことから、高い生産性で製造されるものではなかった。 On the other hand, the water-soluble hyaluronic acid gels of Comparative Examples 1 to 9 do not contain the predetermined amount of the predetermined water-soluble dietary fiber. The water-soluble hyaluronic acid gels of Comparative Examples 1 to 9 can prepare an aqueous hyaluronic acid solution in a heating environment in the composition of the water-soluble hyaluronic acid gel, but do not have the property of gelling even when cooled. It was not manufactured with high productivity.
[実施例5〜19]
水溶性ヒアルロン酸ゲルの組成が表2に記載の配合比(質量部)となるように、密閉できるガラス瓶中でヒアルロン酸(ヒアルロン酸ナトリウム)を蒸留水に均一に溶解した後、イソマルトデキストリンを添加して50℃で24時間加熱してヒアルロン酸水溶液を調製した。このヒアルロン酸水溶液を80℃に加熱した状態で、プロペラ式回転型撹拌装置を用いて撹拌しながらクエン酸を添加して溶解した後、密閉した状態で、80℃で12時間加熱し、均一な液状物を得た。その後、室温で3日保管した。その結果、それぞれ、表2に記載の冷却後の性状(25℃)のゲル(すなわち、均質ゲル)が得られた。[Examples 5 to 19]
Hyaluronic acid (sodium hyaluronate) is uniformly dissolved in distilled water in a sealable glass bottle so that the composition of the water-soluble hyaluronic acid gel has the compounding ratio (parts by mass) shown in Table 2, and then isomaltodextrin is added. It was added and heated at 50 ° C. for 24 hours to prepare an aqueous hyaluronic acid solution. In a state where this aqueous hyaluronic acid solution is heated to 80 ° C., citric acid is added and dissolved while stirring using a propeller type rotary stirrer, and then the hyaluronic acid aqueous solution is heated at 80 ° C. for 12 hours in a sealed state to make it uniform. A liquid material was obtained. Then, it was stored at room temperature for 3 days. As a result, gels having the properties (25 ° C.) after cooling shown in Table 2 (that is, homogeneous gels) were obtained.
[実施例20〜30]
水溶性ヒアルロン酸ゲルの組成が表3に記載の配合比(質量部)となるように、密閉できるガラス瓶中でヒアルロン酸(ヒアルロン酸ナトリウム)を蒸留水に均一に溶解した後、イソマルトデキストリンを添加して50℃で24時間加熱してヒアルロン酸水溶液を調製した。このヒアルロン酸水溶液を80℃に加熱した状態で、プロペラ式回転型撹拌装置を用いて撹拌しながらクエン酸を添加して溶解した後、密閉した状態で、80℃で12時間加熱し、均一な液状物を得た。その後、室温で3日保管し、ゲル状物を得た。その結果、それぞれ、表3に記載の冷却後の性状(25℃)のゲル(すなわち、均質ゲル)が得られた。[Examples 20 to 30]
Hyaluronic acid (sodium hyaluronate) is uniformly dissolved in distilled water in a sealable glass bottle so that the composition of the water-soluble hyaluronic acid gel has the compounding ratio (parts by mass) shown in Table 3, and then isomaltodextrin is added. It was added and heated at 50 ° C. for 24 hours to prepare an aqueous hyaluronic acid solution. In a state where this aqueous hyaluronic acid solution is heated to 80 ° C., citric acid is added and dissolved while stirring using a propeller type rotary stirrer, and then the hyaluronic acid aqueous solution is heated at 80 ° C. for 12 hours in a sealed state to make it uniform. A liquid material was obtained. Then, it was stored at room temperature for 3 days to obtain a gel-like substance. As a result, gels having the properties (25 ° C.) after cooling shown in Table 3 (that is, homogeneous gels) were obtained.
[実施例31〜43]
水溶性ヒアルロン酸ゲルの組成が表4に記載の配合比(質量部)となるように、密閉できるガラス瓶中でヒアルロン酸(ヒアルロン酸ナトリウム)を蒸留水に均一に溶解した後、糖(イソマルトデキストリン)を添加して50℃で24時間加熱してヒアルロン酸水溶液を調製した。このヒアルロン酸水溶液を80℃に加熱した状態で、プロペラ式回転型撹拌装置を用いて撹拌しながらクエン酸を添加して溶解した後、密閉した状態で、80℃で12時間加熱し、均一な液状物を得た。その後、室温で3日保管し、ゲル状物を得た。その結果、それぞれ、表4に記載の冷却後の性状(25℃)のゲル(すなわち、均質ゲル)が得られた。[Examples 31 to 43]
Hyaluronic acid (sodium hyaluronate) is uniformly dissolved in distilled water in a sealable glass bottle so that the composition of the water-soluble hyaluronic acid gel has the compounding ratio (parts by mass) shown in Table 4, and then sugar (isomaltodextrin). Dextrin) was added and heated at 50 ° C. for 24 hours to prepare an aqueous hyaluronic acid solution. In a state where this aqueous hyaluronic acid solution is heated to 80 ° C., citric acid is added and dissolved while stirring using a propeller type rotary stirrer, and then the hyaluronic acid aqueous solution is heated at 80 ° C. for 12 hours in a sealed state to make it uniform. A liquid material was obtained. Then, it was stored at room temperature for 3 days to obtain a gel-like substance. As a result, gels having the properties (25 ° C.) after cooling shown in Table 4 (that is, homogeneous gels) were obtained.
[実施例44〜50]
水溶性ヒアルロン酸ゲルの組成が表5に記載の配合比(質量部)となるように、密閉できるガラス瓶中でヒアルロン酸(ヒアルロン酸ナトリウム)を蒸留水に均一に溶解した後、糖(イソマルトデキストリン)を添加して50℃で24時間加熱してヒアルロン酸水溶液を調製した。このヒアルロン酸水溶液を80℃に加熱した状態で、プロペラ式回転型撹拌装置を用いて撹拌しながら酸を添加して溶解した後、密閉した状態で、80℃で12時間加熱し、均一な液状物を得た。その後、室温で3日保管し、ゲル状物を得た。その結果、それぞれ、表5に記載の冷却後の性状(25℃)のゲル(すなわち、均質ゲル)が得られた。[Examples 44 to 50]
Hyaluronic acid (sodium hyaluronate) is uniformly dissolved in distilled water in a sealable glass bottle so that the composition of the water-soluble hyaluronic acid gel has the compounding ratio (parts by mass) shown in Table 5, and then sugar (isomalto). Dextrin) was added and heated at 50 ° C. for 24 hours to prepare an aqueous hyaluronic acid solution. This hyaluronic acid aqueous solution is heated to 80 ° C., and the acid is added and dissolved while stirring using a propeller-type rotary stirrer, and then the hyaluronic acid aqueous solution is heated at 80 ° C. for 12 hours in a closed state to form a uniform liquid. I got something. Then, it was stored at room temperature for 3 days to obtain a gel-like substance. As a result, gels having the properties (25 ° C.) after cooling shown in Table 5 (that is, homogeneous gels) were obtained.
[実施例51〜58]
水溶性ヒアルロン酸ゲルの組成が表6に記載の配合比(質量部)となるように、密閉できるガラス瓶中でヒアルロン酸(ヒアルロン酸ナトリウム)を蒸留水に均一に溶解した後、イソマルトデキストリン、ハチミツ、キシリトール、又はイソマルトオリゴ糖を添加して50℃で24時間加熱してヒアルロン酸水溶液を調製した。このヒアルロン酸水溶液を80℃に加熱した状態で、プロペラ式回転型撹拌装置を用いて撹拌しながらクエン酸を添加して溶解した後、密閉した状態で、80℃で12時間加熱し、均一な液状物を得た。それぞれ、表6記載の冷却後の性状(25℃)のゲル(すなわち、均質ゲル)が得られた。[Examples 51 to 58]
After uniformly dissolving hyaluronic acid (sodium hyaluronate) in distilled water in a sealable glass bottle so that the composition of the water-soluble hyaluronic acid gel has the compounding ratio (parts by mass) shown in Table 6, isomaltodextrin, An aqueous hyaluronic acid solution was prepared by adding honey, xylitol, or isomalto-oligosaccharide and heating at 50 ° C. for 24 hours. In a state where this aqueous hyaluronic acid solution is heated to 80 ° C., citric acid is added and dissolved while stirring using a propeller type rotary stirrer, and then the hyaluronic acid aqueous solution is heated at 80 ° C. for 12 hours in a sealed state to make it uniform. A liquid material was obtained. Gels having the properties (25 ° C.) after cooling shown in Table 6 (that is, homogeneous gels) were obtained.
※2:固形分約75質量%
※3:固形分約80質量%* 2: Solid content approx. 75% by mass
* 3: Solid content of about 80% by mass
[実施例59〜62]
実施例53、54、57、及び、58で得られたゲル状物約5gを、それぞれ、シャーレに入れ、室温で自然乾燥させて、表7に記載の水分量となるように調整したゲル状物を得た。実施例53が実施例59に対応し、実施例54が実施例60に対応し、実施例57が実施例61に対応し、実施例58が実施例62に対応する。これらのゲル状物は、いずれも高い弾性を示し、食感は硬いグミと同等であった。[Examples 59 to 62]
Approximately 5 g of the gel-like products obtained in Examples 53, 54, 57, and 58 were placed in a petri dish, air-dried at room temperature, and adjusted to have the water content shown in Table 7. I got something. Example 53 corresponds to Example 59, Example 54 corresponds to Example 60, Example 57 corresponds to Example 61, and Example 58 corresponds to Example 62. All of these gel-like substances showed high elasticity, and the texture was equivalent to that of hard gummies.
※2:固形分約75質量%
※3:固形分約80質量%* 2: Solid content approx. 75% by mass
* 3: Solid content of about 80% by mass
[実施例63〜66]
水溶性ヒアルロン酸ゲルの組成が表8に記載の配合比(質量部)となるように、密閉できるガラス瓶中でヒアルロン酸(ヒアルロン酸ナトリウム)を蒸留水に均一に溶解した後、表8に記載の各種糖(イソマルトデキストリンなど)を添加して90℃で2時間加熱してヒアルロン酸水溶液を調製した。このヒアルロン酸水溶液を90℃に加熱した状態で、プロペラ式回転型撹拌装置を用いて撹拌しながらクエン酸を添加して溶解した後、密閉した状態で、90℃で1時間加熱し、均一な液状物を得た。その後、室温で1日保管し、ゲル状物を得た。その結果、それぞれ、表8に記載の冷却後の性状(25℃)のゲル(すなわち、均質ゲル)が得られた。[Examples 63 to 66]
Hyaluronic acid (sodium hyaluronate) is uniformly dissolved in distilled water in a sealable glass bottle so that the composition of the water-soluble hyaluronic acid gel has the blending ratio (parts by mass) shown in Table 8, and then shown in Table 8. Various sugars (isomaltodextrin, etc.) were added and heated at 90 ° C. for 2 hours to prepare an aqueous hyaluronic acid solution. In a state where this aqueous hyaluronic acid solution is heated to 90 ° C., citric acid is added and dissolved while stirring using a propeller type rotary stirrer, and then the hyaluronic acid aqueous solution is heated at 90 ° C. for 1 hour in a sealed state to make it uniform. A liquid material was obtained. Then, it was stored at room temperature for 1 day to obtain a gel-like substance. As a result, gels having the properties (25 ° C.) after cooling shown in Table 8 (that is, homogeneous gels) were obtained.
※2:固形分約75質量% * 2: Solid content approx. 75% by mass
[実施例67〜70]
実施例63、64、65、及び、66で得られたゲル状物約5gを、それぞれ、シャーレに入れ、室温で自然乾燥させて、表9に記載の水分量となるように調整したゲル状物を得た。実施例63が実施例67に対応し、実施例64が実施例68に対応し、実施例65が実施例69に対応し、実施例66が実施例70に対応する。これらのゲル状物は、いずれも高い弾性を示し、食感は硬いグミと同等であった。[Examples 67 to 70]
Approximately 5 g of the gel-like products obtained in Examples 63, 64, 65, and 66 were placed in a petri dish, air-dried at room temperature, and adjusted to have the water content shown in Table 9. I got something. Example 63 corresponds to Example 67, Example 64 corresponds to Example 68, Example 65 corresponds to Example 69, and Example 66 corresponds to Example 70. All of these gel-like substances showed high elasticity, and the texture was equivalent to that of hard gummies.
※2:固形分約75質量% * 2: Solid content approx. 75% by mass
[実施例71〜77]
水溶性ヒアルロン酸ゲルの組成が表10に記載の配合比(質量部)となるように、密閉できるガラス瓶中でヒアルロン酸(ヒアルロン酸ナトリウム)を蒸留水に均一に溶解した後、表10に記載の各種糖(イソマルトデキストリンなど)を添加して90℃で2時間加熱してヒアルロン酸水溶液を調製した。このヒアルロン酸水溶液を90℃に加熱した状態で、プロペラ式回転型撹拌装置を用いて撹拌しながらクエン酸を添加して溶解した後、密閉した状態で、90℃で1時間加熱し、均一な液状物を得た。その後、室温で1日保管し、ゲル状物を得た。その結果、それぞれ、表10に記載の冷却後の性状(25℃)のゲル(すなわち、均質ゲル)が得られた。[Examples 71-77]
Hyaluronic acid (sodium hyaluronate) is uniformly dissolved in distilled water in a sealable glass bottle so that the composition of the water-soluble hyaluronic acid gel has the blending ratio (parts by mass) shown in Table 10, and then shown in Table 10. Various sugars (isomaltodextrin, etc.) were added and heated at 90 ° C. for 2 hours to prepare an aqueous hyaluronic acid solution. In a state where this aqueous hyaluronic acid solution is heated to 90 ° C., citric acid is added and dissolved while stirring using a propeller type rotary stirrer, and then the hyaluronic acid aqueous solution is heated at 90 ° C. for 1 hour in a sealed state to make it uniform. A liquid material was obtained. Then, it was stored at room temperature for 1 day to obtain a gel-like substance. As a result, gels having the properties (25 ° C.) after cooling shown in Table 10 (that is, homogeneous gels) were obtained.
※2:固形分約75質量% * 2: Solid content approx. 75% by mass
[実施例78〜84]
実施例71、72、73、74、75、76、及び、77で得られたゲル状物約5gを、それぞれ、シャーレに入れ、室温で自然乾燥させて、表11に記載の水分量となるように調整したゲル状物を得た。実施例71が実施例78に対応し、実施例72が実施例79に対応し、実施例73が実施例80に対応し、実施例74が実施例81に対応し、実施例75が実施例82に対応し、実施例76が実施例83に対応し、実施例77が実施例84に対応する。これらのゲル状物は、いずれも高い弾性を示し、食感は硬いグミと同等であった。[Examples 78 to 84]
Approximately 5 g of the gel-like products obtained in Examples 71, 72, 73, 74, 75, 76, and 77 are placed in a petri dish and air-dried at room temperature to obtain the water content shown in Table 11. A gel-like product prepared as described above was obtained. Example 71 corresponds to Example 78, Example 72 corresponds to Example 79, Example 73 corresponds to Example 80, Example 74 corresponds to Example 81, and Example 75 corresponds to Example 75. Corresponding to 82, Example 76 corresponds to Example 83, and Example 77 corresponds to Example 84. All of these gel-like substances showed high elasticity, and the texture was equivalent to that of hard gummies.
※2:固形分約75質量% * 2: Solid content approx. 75% by mass
[実施例85〜87]
水溶性ヒアルロン酸ゲルの組成が表12に記載の配合比(質量部)となるように、密閉できるガラス瓶中でヒアルロン酸(ヒアルロン酸ナトリウム)を蒸留水に均一に溶解した後、表12に記載の各種糖(還元難消化性デキストリンなど)を添加して90℃で2時間加熱してヒアルロン酸水溶液を調製した。このヒアルロン酸水溶液を90℃に加熱した状態で、プロペラ式回転型撹拌装置を用いて撹拌しながらクエン酸を添加して溶解した後、密閉した状態で、90℃で1時間加熱し、均一な液状物を得た。その後、室温で1日保管し、ゲル状物を得た。その結果、それぞれ、表12に記載の冷却後の性状(25℃)のゲル(すなわち、均質ゲル)が得られた。[Examples 85-87]
Hyaluronic acid (sodium hyaluronate) is uniformly dissolved in distilled water in a sealable glass bottle so that the composition of the water-soluble hyaluronic acid gel has the blending ratio (parts by mass) shown in Table 12, and then shown in Table 12. Various sugars (reducing indigestible dextrin, etc.) were added and heated at 90 ° C. for 2 hours to prepare an aqueous hyaluronic acid solution. In a state where this aqueous hyaluronic acid solution is heated to 90 ° C., citric acid is added and dissolved while stirring using a propeller type rotary stirrer, and then the hyaluronic acid aqueous solution is heated at 90 ° C. for 1 hour in a sealed state to make it uniform. A liquid material was obtained. Then, it was stored at room temperature for 1 day to obtain a gel-like substance. As a result, gels having the properties (25 ° C.) after cooling shown in Table 12 (that is, homogeneous gels) were obtained.
※2:固形分約75質量%
※4:固形分約70質量%* 2: Solid content approx. 75% by mass
* 4: Solid content approx. 70% by mass
[実施例88〜90]
実施例85、86、及び、87で得られたゲル状物約5gを、それぞれ、シャーレに入れ、室温で自然乾燥させて、表13に記載の水分量となるように調整したゲル状物を得た。実施例85が実施例88に対応し、実施例86が実施例89に対応し、実施例87が実施例90に対応する。これらのゲル状物は、いずれも高い弾性を示し、食感は硬いグミと同等であった。[Examples 88 to 90]
Approximately 5 g of the gel-like products obtained in Examples 85, 86, and 87 were placed in a petri dish and air-dried at room temperature to prepare a gel-like product adjusted to have the water content shown in Table 13. Obtained. Example 85 corresponds to Example 88, Example 86 corresponds to Example 89, and Example 87 corresponds to Example 90. All of these gel-like substances showed high elasticity, and the texture was equivalent to that of hard gummies.
※2:固形分約75質量%
※4:固形分約70質量%* 2: Solid content approx. 75% by mass
* 4: Solid content approx. 70% by mass
[実施例91〜93]
水溶性ヒアルロン酸ゲルの組成が表14に記載の配合比(質量部)となるように、密閉できるガラス瓶中でヒアルロン酸(ヒアルロン酸ナトリウム)を蒸留水に均一に溶解した後、表14に記載の各種糖(イソマルトデキストリンなど)を添加して90℃で2時間加熱してヒアルロン酸水溶液を調製した。このヒアルロン酸水溶液を90℃に加熱した状態で、プロペラ式回転型撹拌装置を用いて撹拌しながらクエン酸を添加して溶解した後、密閉した状態で、90℃で1時間加熱し、均一な液状物を得た。その後、室温で1日保管し、ゲル状物を得た。その結果、それぞれ、表14に記載の冷却後の性状(25℃)のゲル(すなわち、均質ゲル)が得られた。[Examples 91-93]
Hyaluronic acid (sodium hyaluronate) is uniformly dissolved in distilled water in a sealable glass bottle so that the composition of the water-soluble hyaluronic acid gel has the blending ratio (parts by mass) shown in Table 14, and then shown in Table 14. Various sugars (isomaltodextrin, etc.) were added and heated at 90 ° C. for 2 hours to prepare an aqueous hyaluronic acid solution. In a state where this aqueous hyaluronic acid solution is heated to 90 ° C., citric acid is added and dissolved while stirring using a propeller type rotary stirrer, and then the hyaluronic acid aqueous solution is heated at 90 ° C. for 1 hour in a sealed state to make it uniform. A liquid material was obtained. Then, it was stored at room temperature for 1 day to obtain a gel-like substance. As a result, gels having the properties (25 ° C.) after cooling shown in Table 14 (that is, homogeneous gels) were obtained.
※2:固形分約75質量% * 2: Solid content approx. 75% by mass
[実施例94〜96]
実施例91、92、及び、93で得られたゲル状物約5gを、それぞれ、シャーレに入れ、室温で自然乾燥させて、表15に記載の水分量となるように調整したゲル状物を得た。実施例91が実施例94に対応し、実施例92が実施例95に対応し、実施例93が実施例96に対応する。これらのゲル状物は、いずれも高い弾性を示し、食感は硬いグミと同等であった。[Examples 94 to 96]
Approximately 5 g of the gel-like products obtained in Examples 91, 92, and 93 were placed in a petri dish and air-dried at room temperature to prepare a gel-like product adjusted to have the water content shown in Table 15. Obtained. Example 91 corresponds to Example 94, Example 92 corresponds to Example 95, and Example 93 corresponds to Example 96. All of these gel-like substances showed high elasticity, and the texture was equivalent to that of hard gummies.
※2:固形分約75質量% * 2: Solid content approx. 75% by mass
[実施例97〜99]
水溶性ヒアルロン酸ゲルの組成が表16に記載の配合比(質量部)となるように、密閉できるガラス瓶中でヒアルロン酸(ヒアルロン酸ナトリウム)を蒸留水に均一に溶解した後、表16に記載の各種糖(イソマルトデキストリンなど)を添加して90℃で2時間加熱してヒアルロン酸水溶液を調製した。このヒアルロン酸水溶液を90℃に加熱した状態で、プロペラ式回転型撹拌装置を用いて撹拌しながら各種酸を添加して溶解した後、密閉した状態で、90℃で1時間加熱し、均一な液状物を得た。その後、室温で1日保管し、ゲル状物を得た。その結果、それぞれ、表16に記載の冷却後の性状(25℃)のゲル(すなわち、均質ゲル)が得られた。[Examples 97 to 99]
Hyaluronic acid (sodium hyaluronate) is uniformly dissolved in distilled water in a sealable glass bottle so that the composition of the water-soluble hyaluronic acid gel has the blending ratio (parts by mass) shown in Table 16, and then shown in Table 16. Various sugars (isomaltodextrin, etc.) were added and heated at 90 ° C. for 2 hours to prepare an aqueous hyaluronic acid solution. In a state where this aqueous hyaluronic acid solution is heated to 90 ° C., various acids are added and dissolved while stirring using a propeller type rotary stirrer, and then the hyaluronic acid aqueous solution is heated at 90 ° C. for 1 hour in a sealed state to make it uniform. A liquid material was obtained. Then, it was stored at room temperature for 1 day to obtain a gel-like substance. As a result, gels having the properties (25 ° C.) after cooling shown in Table 16 (that is, homogeneous gels) were obtained.
※2:固形分約75質量% * 2: Solid content approx. 75% by mass
[実施例100〜102]
実施例97、98、及び、99で得られたゲル状物約5gを、それぞれ、シャーレに入れ、室温で自然乾燥させて、表17に記載の水分量となるように調整したゲル状物を得た。実施例97が実施例100に対応し、実施例98が実施例101に対応し、実施例99が実施例102に対応する。これらのゲル状物は、いずれも高い弾性を示し、食感は硬いグミと同等であった。[Examples 100 to 102]
Approximately 5 g of the gel-like products obtained in Examples 97, 98, and 99 were placed in a petri dish and air-dried at room temperature to prepare a gel-like product adjusted to have the water content shown in Table 17. Obtained. Example 97 corresponds to Example 100, Example 98 corresponds to Example 101, and Example 99 corresponds to Example 102. All of these gel-like substances showed high elasticity, and the texture was equivalent to that of hard gummies.
※2:固形分約75質量% * 2: Solid content approx. 75% by mass
[実施例103〜109]
水溶性ヒアルロン酸ゲルの組成が表18に記載の配合比(質量部)となるように、密閉できるガラス瓶中でヒアルロン酸(ヒアルロン酸ナトリウム)を蒸留水に均一に溶解した後、表18に記載の各種糖(イソマルトデキストリンなど)を添加して90℃で2時間加熱してヒアルロン酸水溶液を調製した。このヒアルロン酸水溶液を90℃に加熱した状態で、プロペラ式回転型撹拌装置を用いて撹拌しながらクエン酸を添加して溶解した後、密閉した状態で、90℃で1時間加熱し、均一な液状物を得た。その後、室温で1日保管し、ゲル状物を得た。その結果、それぞれ、表18に記載の冷却後の性状(25℃)のゲル(すなわち、均質ゲル)が得られた。[Examples 103 to 109]
Hyaluronic acid (sodium hyaluronate) is uniformly dissolved in distilled water in a sealable glass bottle so that the composition of the water-soluble hyaluronic acid gel has the blending ratio (parts by mass) shown in Table 18, and then shown in Table 18. Various sugars (isomaltodextrin, etc.) were added and heated at 90 ° C. for 2 hours to prepare an aqueous hyaluronic acid solution. In a state where this aqueous hyaluronic acid solution is heated to 90 ° C., citric acid is added and dissolved while stirring using a propeller type rotary stirrer, and then the hyaluronic acid aqueous solution is heated at 90 ° C. for 1 hour in a sealed state to make it uniform. A liquid material was obtained. Then, it was stored at room temperature for 1 day to obtain a gel-like substance. As a result, gels having the properties (25 ° C.) after cooling shown in Table 18 (that is, homogeneous gels) were obtained.
※2:固形分約75質量%
※3:固形分約80質量%
※5:固形分約75質量%* 2: Solid content approx. 75% by mass
* 3: Solid content of about 80% by mass
* 5: Solid content approx. 75% by mass
[実施例110〜116]
実施例103、104、105、106、107、108、及び、109で得られたゲル状物約5gを、それぞれ、シャーレに入れ、室温で自然乾燥させて、表19に記載の水分量となるように調整したゲル状物を得た。実施例103が実施例110に対応し、実施例104が実施例111に対応し、実施例105が実施例112に対応し、実施例106が実施例113に対応し、実施例107が実施例114に対応し、実施例108が実施例115に対応し、実施例109が実施例116に対応する。これらのゲル状物は、いずれも高い弾性を示し、食感は硬いグミと同等であった。[Examples 110 to 116]
Approximately 5 g of the gel-like products obtained in Examples 103, 104, 105, 106, 107, 108, and 109 are placed in a petri dish and air-dried at room temperature to obtain the water content shown in Table 19. A gel-like product prepared as described above was obtained. Example 103 corresponds to Example 110, Example 104 corresponds to Example 111, Example 105 corresponds to Example 112, Example 106 corresponds to Example 113, and Example 107 corresponds to Example. Corresponding to 114, Example 108 corresponds to Example 115, and Example 109 corresponds to Example 116. All of these gel-like substances showed high elasticity, and the texture was equivalent to that of hard gummies.
※2:固形分約75質量%
※3:固形分約80質量%
※5:固形分約75質量%* 2: Solid content approx. 75% by mass
* 3: Solid content of about 80% by mass
* 5: Solid content approx. 75% by mass
[実施例117〜119]
表20に記載の配合比(質量部)の蒸留水の2倍の質量部に、広口瓶中でヒアルロン酸(ヒアルロン酸ナトリウム)を均一に溶解した後、90℃で加熱した状態でプロペラ式回転型撹拌装置を用いて撹拌しながら表20に記載の各種糖(イソマルトデキストリンなど)を添加して均一に溶解し、更に、クエン酸を添加して均一に溶解した後、水分を蒸散させて濃縮して、水溶性ヒアルロン酸ゲルの組成が表20に記載の配合比(質量部)となる均一な高粘度グミ組成物を得た。この高粘度グミ組成物約5gをシャーレに入れ、密閉した状態で、室温で1日保管した。その結果、それぞれ、表20に記載の冷却後の性状(25℃)のゲル(すなわち、均質ゲル)が得られた。これらのゲル状物は、いずれも高い弾性を示し、食感はグミと同等であった。[Examples 117 to 119]
Hyaluronic acid (sodium hyaluronate) is uniformly dissolved in a wide-mouthed bottle in twice the mass of distilled water having the compounding ratio (parts by mass) shown in Table 20, and then propeller-type rotation while heating at 90 ° C. While stirring using a mold stirrer, various sugars (isomaltodextrin, etc.) shown in Table 20 are added to uniformly dissolve the sugar, and citric acid is further added to uniformly dissolve the sugar, and then the water is evaporated. By concentrating, a uniform high-viscosity gummy composition having a composition of the water-soluble hyaluronic acid gel having the compounding ratio (part by mass) shown in Table 20 was obtained. About 5 g of this high-viscosity gummy composition was placed in a petri dish and stored in a closed state at room temperature for 1 day. As a result, gels having the properties (25 ° C.) after cooling shown in Table 20 (that is, homogeneous gels) were obtained. All of these gel-like substances showed high elasticity, and the texture was equivalent to that of gummy candies.
※2:固形分約75質量%
※5:固形分約75質量%* 2: Solid content approx. 75% by mass
* 5: Solid content approx. 75% by mass
[実施例120〜122]
実施例117、118、及び、119で得られたシャーレに入ったゲル状物約5gを、室温で自然乾燥させて、表21に記載の水分量となるように調整したゲル状物を得た。実施例117が実施例120に対応し、実施例118が実施例121に対応し、実施例119が実施例122に対応する。これらのゲル状物は、いずれも高い弾性を示し、食感は硬いグミと同等であった。[Examples 120 to 122]
Approximately 5 g of the gel-like product contained in the petri dish obtained in Examples 117, 118, and 119 was air-dried at room temperature to obtain a gel-like product adjusted to have the water content shown in Table 21. .. Example 117 corresponds to Example 120, Example 118 corresponds to Example 121, and Example 119 corresponds to Example 122. All of these gel-like substances showed high elasticity, and the texture was equivalent to that of hard gummies.
※2:固形分約75質量%
※5:固形分約75質量%* 2: Solid content approx. 75% by mass
* 5: Solid content approx. 75% by mass
[実施例123〜127]
水溶性ヒアルロン酸ゲルの組成が表22に記載の配合比(質量部)となるように、密閉できるガラス瓶中でヒアルロン酸(ヒアルロン酸ナトリウム)を蒸留水に均一に溶解した後、表22に記載の各種糖(イソマルトデキストリンなど)を添加して90℃で2時間加熱してヒアルロン酸水溶液を調製した。このヒアルロン酸水溶液を90℃に加熱した状態で、プロペラ式回転型撹拌装置を用いて撹拌しながらクエン酸を添加して溶解した後、密閉した状態で、90℃で1時間加熱し、均一な液状物を得た。その後、室温で1日保管し、ゲル状物を得た。その結果、それぞれ、表22に記載の冷却後の性状(25℃)のゲル(すなわち、均質ゲル)が得られた。[Examples 123 to 127]
Hyaluronic acid (sodium hyaluronate) is uniformly dissolved in distilled water in a sealable glass bottle so that the composition of the water-soluble hyaluronic acid gel has the blending ratio (parts by mass) shown in Table 22, and then shown in Table 22. Various sugars (isomaltodextrin, etc.) were added and heated at 90 ° C. for 2 hours to prepare an aqueous hyaluronic acid solution. In a state where this aqueous hyaluronic acid solution is heated to 90 ° C., citric acid is added and dissolved while stirring using a propeller type rotary stirrer, and then the hyaluronic acid aqueous solution is heated at 90 ° C. for 1 hour in a sealed state to make it uniform. A liquid material was obtained. Then, it was stored at room temperature for 1 day to obtain a gel-like substance. As a result, gels having the properties (25 ° C.) after cooling shown in Table 22 (that is, homogeneous gels) were obtained.
※2:固形分約75質量%
※3:固形分約80質量%
※5:固形分約75質量%* 2: Solid content approx. 75% by mass
* 3: Solid content of about 80% by mass
* 5: Solid content approx. 75% by mass
<pHの測定>
別途、ヒアルロン酸(ヒアルロン酸ナトリウム)は1g、酸はヒアルロン酸1gに対して各表1〜22に記載の配合比(質量部)となるように、ヒアルロン酸と酸を蒸留水200mLにプロペラ式回転型撹拌装置を用いて均一に混合して、pH測定用ヒアルロン酸水溶液を得た。この得られたヒアルロン酸水溶液のpHを、メトラー・トレド株式会社製のFiveEasy(登録商標)pHメータを用いて測定した。<Measurement of pH>
Separately, hyaluronic acid and acid are added to 200 mL of distilled water using a propeller formula so that the blending ratio (parts by mass) shown in Tables 1 to 22 is obtained with respect to 1 g of hyaluronic acid (sodium hyaluronate) and 1 g of acid. The mixture was uniformly mixed using a rotary stirrer to obtain an aqueous hyaluronic acid solution for pH measurement. The pH of the obtained aqueous hyaluronic acid solution was measured using a FiveEasy (registered trademark) pH meter manufactured by METTLER TOLEDO Co., Ltd.
Claims (14)
前記水溶性食物繊維は、グルコースを構成糖とし、1−4結合及び1−6結合以外の結合を有し、環状構造ではない多糖類であり、
前記水の含有量が、前記ヒアルロン酸1質量部に対して、1〜300質量部であり、
前記水溶性食物繊維の含有量が、前記ヒアルロン酸1質量部に対して、1〜300質量部であり、
前記水溶性ヒアルロン酸ゲル100質量%中、前記ヒアルロン酸の含有率が0.2〜50質量%であり、
ゲル形成成分として、前記ヒアルロン酸とは異なる他のゲル形成成分が実質的に含まれない、水溶性ヒアルロン酸ゲル。 A water-soluble hyaluronic acid gel containing hyaluronic acid, water-soluble dietary fiber, an acid different from the hyaluronic acid, and water.
The water-soluble dietary fiber is a polysaccharide having glucose as a constituent sugar, having bonds other than 1-4 bonds and 1-6 bonds, and not having a cyclic structure.
The content of the water is 1 to 300 parts by mass with respect to 1 part by mass of the hyaluronic acid.
The content of the water-soluble dietary fiber, with respect to the 1 part by weight of hyaluronic acid, Ri 1 to 300 parts by mass der,
The hyaluronic acid content is 0.2 to 50% by mass in 100% by mass of the water-soluble hyaluronic acid gel.
A water-soluble hyaluronic acid gel that does not substantially contain other gel-forming components different from the hyaluronic acid as gel-forming components.
(pHの測定方法)
ヒアルロン酸1gを含む分量の前記水溶性ヒアルロン酸ゲルに含まれる成分のうち、水を除く全てのイオン性成分を水に溶解して200mLとなるように水溶液を調製し、得られた水溶液のpHを測定する。 The water-soluble hyaluronic acid gel according to claim 1, wherein the pH of the aqueous solution measured by the following measuring method is in the range of 1.9 to 6.3.
(Method of measuring pH)
Of the components contained in the water-soluble hyaluronic acid gel in an amount containing 1 g of hyaluronic acid, all ionic components except water were dissolved in water to prepare an aqueous solution so as to have 200 mL, and the pH of the obtained aqueous solution was prepared. To measure.
前記ヒアルロン酸と、前記ヒアルロン酸1質量部に対して1〜300質量部の前記水溶性食物繊維と、前記ヒアルロン酸とは異なる酸と、前記ヒアルロン酸1質量部に対して1〜300質量部の水を含み、40℃以上の温度に加熱されたヒアルロン酸水溶液を調製する工程1と、
前記加熱されたヒアルロン酸水溶液を40℃未満の温度に冷却する工程2と、
を備える、水溶性ヒアルロン酸ゲルの製造方法。 The method for producing a water-soluble hyaluronic acid gel according to any one of claims 1 to 8.
The hyaluronic acid, 1 to 300 parts by mass of the water-soluble dietary fiber with respect to 1 part by mass of the hyaluronic acid, an acid different from the hyaluronic acid, and 1 to 300 parts by mass with respect to 1 part by mass of the hyaluronic acid. Step 1 to prepare an aqueous hyaluronic acid solution containing the water of 40 ° C. or higher and heated to a temperature of 40 ° C. or higher.
Step 2 of cooling the heated hyaluronic acid aqueous solution to a temperature of less than 40 ° C.
A method for producing a water-soluble hyaluronic acid gel.
The method for producing a water-soluble hyaluronic acid gel according to claim 13, wherein the reduction rate of water from the water-soluble hyaluronic acid aqueous solution between the steps 1 and 2 is 50% by mass or less.
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