JPH0767687A - Production of water-soluble silk fibroin - Google Patents
Production of water-soluble silk fibroinInfo
- Publication number
- JPH0767687A JPH0767687A JP5234312A JP23431293A JPH0767687A JP H0767687 A JPH0767687 A JP H0767687A JP 5234312 A JP5234312 A JP 5234312A JP 23431293 A JP23431293 A JP 23431293A JP H0767687 A JPH0767687 A JP H0767687A
- Authority
- JP
- Japan
- Prior art keywords
- silk fibroin
- water
- silk
- soluble
- production
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 108010022355 Fibroins Proteins 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 6
- 239000003513 alkali Substances 0.000 claims abstract description 12
- 230000007062 hydrolysis Effects 0.000 claims abstract description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 8
- 108091005804 Peptidases Proteins 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- 239000004365 Protease Substances 0.000 claims description 4
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims description 4
- 230000003301 hydrolyzing effect Effects 0.000 claims description 4
- 239000002537 cosmetic Substances 0.000 abstract description 4
- 235000013305 food Nutrition 0.000 abstract description 4
- 102000035195 Peptidases Human genes 0.000 abstract description 2
- 235000019833 protease Nutrition 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 229940034586 silk sericin Drugs 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229940088598 enzyme Drugs 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 244000146553 Ceiba pentandra Species 0.000 description 1
- 240000000249 Morus alba Species 0.000 description 1
- 235000008708 Morus alba Nutrition 0.000 description 1
- 108010013296 Sericins Proteins 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 235000019621 digestibility Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000015243 ice cream Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 229940024999 proteolytic enzymes for treatment of wounds and ulcers Drugs 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- 210000000813 small intestine Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
Landscapes
- Confectionery (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Cosmetics (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】絹から水溶性絹フィブロインの製
造法及び該ペプチドは食品、化粧品素材等に使用され
る。BACKGROUND OF THE INVENTION Industrial field: A method for producing water-soluble silk fibroin from silk and the peptide are used for foods, cosmetic materials and the like.
【０００２】[0002]
発明の背景 従来から繭或いは絹糸等の絹は微細粉砕して化粧品、食
品素材に使用されている。又、それら絹をアルカリで加
水分解してフィブロイン水溶液及び又はセリシン水溶液
を得、この水溶液を食品として使用することが提案され
ている（特許出願公開 平１─２５６３５１）。BACKGROUND OF THE INVENTION Silk such as cocoon or silk thread has been finely pulverized and used for cosmetics and food materials. Further, it has been proposed that the silk is hydrolyzed with an alkali to obtain an aqueous solution of fibroin and / or an aqueous solution of sericin, and the aqueous solution is used as a food (Patent Application Publication No. 1-256351).
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、従来の
方法では、加水分解の進行の制御が難しい。又、鉱酸で
加水分解した場合、使用する鉱酸の量が多くその中和に
要するアルカリの量が多くなり、従って、生成する塩の
量が多くなり、着色或いは分解終了後の酸の除去などが
煩雑となる欠点がある。However, it is difficult to control the progress of hydrolysis by the conventional methods. Also, when hydrolyzed with a mineral acid, the amount of mineral acid used is large and the amount of alkali required for its neutralization is large, so the amount of salt produced is large and the removal of acid after coloring or decomposition is complete. There is a drawback that it becomes complicated.
【０００４】[0004]
【発明を解決するための手段】本発明は、絹を稀アルカ
リで加水分解し、更に蛋白分解酵素により加水分解する
ことを特徴とする水溶性絹フィブロインの製造法であ
る。The present invention is a method for producing water-soluble silk fibroin, which comprises hydrolyzing silk with a dilute alkali and further hydrolyzing it with a protease.
【０００５】本発明を詳細に説明する。本発明の絹と
は、繭、絹綿、絹糸或いは屑絹糸など絹製品のいずれで
も使用できるが、経済的には繭或いは屑絹糸が適してお
り、桑類の蛋白質或いは糖類等を除去した高純度の絹が
最適である。アルカリとは、水溶液状態でｐＨ８乃至１
４のアルカリ物質が使用でき、具体的には、Ｎａ2 ＣＯ
3 、ＮａＯＨ、ＫＯＨがある。The present invention will be described in detail. The silk of the present invention can be used in any of silk products such as cocoon, silk cotton, silk thread or scrap silk thread. However, cocoon or scrap silk thread is economically suitable, and high purity obtained by removing proteins or sugars of mulberry and the like. Silk is the best. Alkali means a pH of 8 to 1 in an aqueous solution.
Alkali substances of 4 can be used. Specifically, Na2 CO
There are 3, NaOH and KOH.
【０００６】更に具体的に本発明を説明する。絹は中心
の絹フィブロインが強固な絹セリシンで覆われており、
よって先ず、絹を水に浸漬状態で、ｐＨ８〜１４で加水
分解処理を行い絹セリシンを分解する。分解は、使用す
るアルカリの種類及び処理条件で異なるが、稀アルカリ
（ｐＨ８〜１３．５）で２〜６時間、好ましくはｐＨ９
〜１２で３〜５時間で加熱処理して行う。例えば、Ｎａ
ＯＨの２〜５％水溶液で３〜４時間加熱処理する。強ア
ルカリを使用した場合は必要に応じ酸にて中和する。該
処理後、絹セリシンは加水分解されガム状乃至樹脂状と
なり、フィブロインはゾル状乃至水溶性となる。よっ
て、絹セリシン及びその分解物は容易に分離することが
できる。分離は通常の個液分離処理が採用でき、例えば
濾過、遠心分離等により行うことができる。The present invention will be described more specifically. As for silk, the central silk fibroin is covered with strong silk sericin,
Therefore, first, the silk is immersed in water and hydrolyzed at pH 8 to 14 to decompose the silk sericin. Decomposition varies depending on the type of alkali used and treatment conditions, but is 2 to 6 hours with dilute alkali (pH 8 to 13.5), preferably pH 9
It heat-processes for 3 to 5 hours by -12. For example, Na
Heat treatment with a 2-5% aqueous solution of OH for 3-4 hours. If a strong alkali is used, neutralize with acid as necessary. After the treatment, silk sericin is hydrolyzed to be gum-like or resin-like, and fibroin is sol-like or water-soluble. Therefore, silk sericin and its decomposition products can be easily separated. The separation can be carried out by an ordinary individual liquid separation treatment, for example, filtration, centrifugation or the like.
【０００７】濾液として得られたゾル状乃至水溶性の絹
フィブロインは、更に、蛋白分解酵素により３５℃乃至
６０℃にて２４乃至７２時間好ましくは４０℃乃至５５
℃で３６乃至４８時間醗酵させて加水分解させ、絹フィ
ブロイン水溶液を得る。条件により異なるが、絹フィブ
ロインは、分子量１０００乃至５０００程度に保持され
る。絹フィブロイン水溶液はこのままでも種々の用途に
使用できるが、必要により、活性炭処理して精製し、
又、水分を除去して粉末とすることも可能である。例え
ば、絹フィブロイン水溶液を冷凍乾燥し、又は、噴霧乾
燥して粉末状の水溶性絹フィブロインを得る。The sol or water-soluble silk fibroin obtained as the filtrate is further subjected to proteolytic enzymes at 35 ° C to 60 ° C for 24 to 72 hours, preferably 40 ° C to 55 ° C.
Fermentation is carried out at 36 ° C. for 36 to 48 hours for hydrolysis to obtain an aqueous silk fibroin solution. Depending on the conditions, silk fibroin is retained at a molecular weight of about 1000 to 5000. The silk fibroin aqueous solution can be used for various purposes as it is, but if necessary, it is treated with activated carbon for purification,
It is also possible to remove water to obtain powder. For example, an aqueous silk fibroin solution is freeze-dried or spray-dried to obtain powdery water-soluble silk fibroin.
【０００８】得られた水溶性絹フィブロインは、分子量
１０００乃至５０００程度であり、無味・無臭であり保
湿性、分解性、水溶性に優れ、特に小腸に於ける吸収・
消化性の良い優れた機能性食品となる。又、アイスクリ
ームやドリンク等に用いた場合、起泡性、滑らかさ、保
香性が優れている。化粧品やシャンプーに用いられた場
合、保水性、親水性が優れている。本発明のアルカリと
酵素による二段階による加水分解では、反応の進行の制
御、調整が容易であり、得られる水溶性絹フィブロイン
の分子量を任意に調整でき、よって、製品の性質が優れ
ている。The obtained water-soluble silk fibroin has a molecular weight of about 1,000 to 5,000, is tasteless and odorless, and has excellent moisturizing properties, degradability and water solubility, and is particularly absorbed in the small intestine.
It becomes an excellent functional food with good digestibility. When used for ice cream, drinks, etc., it has excellent foaming properties, smoothness, and aroma retention. When used in cosmetics and shampoo, it has excellent water retention and hydrophilicity. In the two-step hydrolysis with alkali and enzyme of the present invention, the progress of the reaction can be easily controlled and adjusted, and the molecular weight of the resulting water-soluble silk fibroin can be arbitrarily adjusted, and thus the product has excellent properties.
【０００９】実施例 １ リフラックス冷却管の付いた丸底フラスコに屑繭４００
グラム及び苛性ソーダ２．５％水溶液３００ｍｌを加え
沸騰させ、固形分が消失するまで（３時間３０分）加熱
した。次いで、４％の塩酸約５０ｍｌを加えてほぼｐＨ
７に中和し、濾過した。濾過残渣は固形樹脂物であり、
絹セリシンであった。濾液を、１５０ｍｌまで濃縮し粘
稠な絹フィブロイン水溶液を得た。これに蛋白分解酵素
３グラムを加え４５乃至５０℃で４８時間保持し醗酵さ
せ、加水分解した。次いで、８５℃３０分加熱し、酵素
を失活させ、限界濾過膜を通し脱塩処理して、透明な絹
フィブロイン水溶液（水溶性絹フィブロインの水溶液）
を得た。得られた絹フィブロイン水溶液を更に冷凍乾燥
し、燐片状の水溶性絹フィブロイン粉末を得た。Example 1 A scrap cocoon 400 was placed in a round bottom flask equipped with a reflux condenser.
Grams and 300 ml of a 2.5% aqueous solution of caustic soda were added and the mixture was boiled and heated until the solid content disappeared (3 hours 30 minutes). Next, add about 50 ml of 4% hydrochloric acid to adjust the pH to about
Neutralized to 7 and filtered. The filtration residue is a solid resin material,
It was silk sericin. The filtrate was concentrated to 150 ml to obtain a viscous silk fibroin aqueous solution. To this, 3 g of a protease was added, and the mixture was kept at 45 to 50 ° C. for 48 hours for fermentation and hydrolysis. Then, the mixture is heated at 85 ° C. for 30 minutes to inactivate the enzyme and desalted through an ultrafiltration membrane to obtain a transparent silk fibroin aqueous solution (water-soluble silk fibroin aqueous solution).
Got The obtained silk fibroin aqueous solution was further freeze-dried to obtain flaky water-soluble silk fibroin powder.
【００１０】[0010]
【発明の効果】加水分解の進行、制御が容易であり、得
られる水溶性絹フィブロインの性質が優れている。EFFECTS OF THE INVENTION The progress and control of hydrolysis are easy, and the water-soluble silk fibroin obtained has excellent properties.
フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ａ６１Ｋ 7/00 Ｊ Continuation of front page (51) Int.Cl. 6 Identification code Office reference number FI technical display area A61K 7/00 J
Claims (4)
解酵素により加水分解することを特徴とする水溶性絹フ
ィブロインの製造法1. A method for producing water-soluble silk fibroin, which comprises hydrolyzing silk with a dilute alkali and further hydrolyzing it with a protease.
をｐＨ１０から１３．５で３０分から３時間行う方法2. The method according to claim 1, wherein the hydrolysis is carried out with a dilute alkali at pH 10 to 13.5 for 30 minutes to 3 hours.
フィブロインの平均分子量が１，０００乃至５，０００
となるまで加水分解する方法3. The average molecular weight of silk fibroin according to claim 2, which is 1,000 to 5,000 by the protease.
To hydrolyze until
ロインの製造4. Production of water-soluble silk fibroin obtained by the method of claim 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5234312A JPH0767687A (en) | 1993-08-27 | 1993-08-27 | Production of water-soluble silk fibroin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5234312A JPH0767687A (en) | 1993-08-27 | 1993-08-27 | Production of water-soluble silk fibroin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0767687A true JPH0767687A (en) | 1995-03-14 |
Family
ID=16969037
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5234312A Pending JPH0767687A (en) | 1993-08-27 | 1993-08-27 | Production of water-soluble silk fibroin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0767687A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001226242A (en) * | 2000-02-17 | 2001-08-21 | Lion Corp | Oral composition |
| KR20020073621A (en) * | 2001-03-15 | 2002-09-28 | 김영호 | The functional bread making by the supplementation with silkpeptide and process for preparation thereof |
| KR100407764B1 (en) * | 2001-04-02 | 2003-12-01 | 유한회사한풍제약 | Method for Production of Silk Peptides |
| KR100420824B1 (en) * | 2001-06-21 | 2004-03-02 | 배도규 | Silk peptide and silk fibroin powder materials made by silk and manufacturing method for those materials |
| US7060260B2 (en) | 2003-02-20 | 2006-06-13 | E.I. Du Pont De Nemours And Company | Water-soluble silk proteins in compositions for skin care, hair care or hair coloring |
| KR100754276B1 (en) * | 2007-02-22 | 2007-09-03 | 김재현 | Health supplements containing silk peptides and calcium |
| KR100789405B1 (en) * | 2007-07-03 | 2007-12-28 | 월드웨이(주) | Method for preparing silk tyrosine |
| JP2014525265A (en) * | 2011-08-26 | 2014-09-29 | アグリカルチュアル リサーチ ディベロプメント エージェンシー（パブリック オーガナイゼーション） | Silk-based bioactive oligopeptide composition and process for its production |
| KR20220083389A (en) * | 2020-12-11 | 2022-06-20 | 동의대학교 산학협력단 | Skin anti-pollution composition comprising cocoon extract |
-
1993
- 1993-08-27 JP JP5234312A patent/JPH0767687A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001226242A (en) * | 2000-02-17 | 2001-08-21 | Lion Corp | Oral composition |
| KR20020073621A (en) * | 2001-03-15 | 2002-09-28 | 김영호 | The functional bread making by the supplementation with silkpeptide and process for preparation thereof |
| KR100407764B1 (en) * | 2001-04-02 | 2003-12-01 | 유한회사한풍제약 | Method for Production of Silk Peptides |
| KR100420824B1 (en) * | 2001-06-21 | 2004-03-02 | 배도규 | Silk peptide and silk fibroin powder materials made by silk and manufacturing method for those materials |
| US7060260B2 (en) | 2003-02-20 | 2006-06-13 | E.I. Du Pont De Nemours And Company | Water-soluble silk proteins in compositions for skin care, hair care or hair coloring |
| KR100754276B1 (en) * | 2007-02-22 | 2007-09-03 | 김재현 | Health supplements containing silk peptides and calcium |
| KR100789405B1 (en) * | 2007-07-03 | 2007-12-28 | 월드웨이(주) | Method for preparing silk tyrosine |
| JP2014525265A (en) * | 2011-08-26 | 2014-09-29 | アグリカルチュアル リサーチ ディベロプメント エージェンシー（パブリック オーガナイゼーション） | Silk-based bioactive oligopeptide composition and process for its production |
| EP2748177A4 (en) * | 2011-08-26 | 2015-04-08 | Agricultural Res Dev Agency Public Organization | Silk-based bioactive oligopeptide compositions and manufacturing process therefor |
| KR20220083389A (en) * | 2020-12-11 | 2022-06-20 | 동의대학교 산학협력단 | Skin anti-pollution composition comprising cocoon extract |
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