CN101781672A - Process for preparing hydrolyzed II-type collagen - Google Patents
Process for preparing hydrolyzed II-type collagen Download PDFInfo
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- CN101781672A CN101781672A CN200910250112A CN200910250112A CN101781672A CN 101781672 A CN101781672 A CN 101781672A CN 200910250112 A CN200910250112 A CN 200910250112A CN 200910250112 A CN200910250112 A CN 200910250112A CN 101781672 A CN101781672 A CN 101781672A
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Abstract
The invention discloses a process for preparing hydrolyzed II-type collagen, which comprises the following steps: adding clean livestock gristles serving as raw materials into water to boil the clean livestock gristles; adding biological complex enzymes into boiled livestock gristle solution for hydrolysis; and filtering the livestock gristle solution obtained after the hydrolysis to obtain clear solution of the hydrolyzed II-type collagen. The process for preparing the hydrolyzed II-type collagen effectively improves the absorptivity of the product by changing insoluble collagen intor water-soluble collagen with a complex enzyme hydrolysis technique and reducing the molecular weight of the product. In the preparation process, no inorganic acid and alkalis, which can increase the ash content of the solution, are added. The preparation process has the advantages of simple steps, easy operation and control and low cost.
Description
Technical field
The invention belongs to the preparation technology of collagen protein, be specifically related to the preparation technology of the hydrolyzed II-type collagen of low grey matter.
Background technology
Joint cartilage mainly is to be made of compound mucopolysaccharide (GAG), II collagen type (CollagenII) and water.Its mechanism is: under chondrocyte's effect, form the electronegative proteoglycan aggregate (PG) of macromole long-chain of spatial grid structure by compound mucopolysaccharide (GAG) and II collagen type (Collagen II), attract the form of II collagen type, be wound in proteoglycan aggregate (PG) and become cartilaginous tissue gradually with the three-dimensional spiral structure.Joint cartilage can absorb synovia and expand, because the squeezing action of joint motion, joint cartilage just can constantly be upgraded, thereby makes joint cartilage have good elasticity and vitality.The major function of synovial tissue is the secretion synovia in the joint cavity.And synovia is the basic substance of joint cartilage existence, is to be formed under synovial cell's effect by compound mucopolysaccharide (GAG) and II collagen type (CollagenII).Joint cavity is to contain compound mucopolysaccharide (GAG) and the abundantest place of II collagen type (CollagenII), can be described as " storage vault " of compound mucopolysaccharide (GAG) and II collagen type (CollagenII).Because being closely connected of each organ of body, constitute a big recycle system, if other tissue lacks compound mucopolysaccharide (GAG) and II collagen type (Collagen II), the poising action of body will make the concentration of interior compound mucopolysaccharide (GAG) of joint cavity and II collagen type (CollagenII) reduce, thereby cause articular cartilage degeneration, the various joint diseases of secondary.Rheumatoid arthritis (RA) be a kind of common serve as the autoimmune disorder of main performance with joint tissue chronic inflammation pathology.In most crowds, the morbidity of quasi-wind gateway is 0.3～1.5%.
Osteoarthritis is one of main illness that causes because the organic matter of bone lacks, and also claims degenerative osteoarthritis.Form reason and mainly be human body with age, functions of biological organs is degenerated, generate the scarce capacity of compound mucopolysaccharide (GAG) and II collagen type (CollagenII), cause the organic shortage of joint tissue, cause joint cartilage sclerosis and follow the string, the hardened cartilage damages because of the phase mutual friction, and the fragment that damage comes off falls into and causes inflammation in the joint cavity, thereby causes arthralgia and dyskinesia.In recent years, very active abroad to the research of oral administration of soluble II collagen type treatment experimental animal models arthritis model and people's rheumatoid arthritis, propose this therapy and have conveniently, advantage such as nontoxic and antigen-specific, can use simultaneously with other products.Oral Ji Yuan and ox source II collagen type can obviously alleviate suffers from mouse swollen joint expansibility, reduces the sickness rate of rheumatoid arthritis, adjuvant-induced arthritis.Its market application surface will be all similar rheumatism patients.The market potential of therefore being somebody's turn to do product is very big.Therefore, if product is carried out the good market development, will produce huge economic benefit.
II collagen protein in the market mainly is directly to be ground after boiling by cartilage to form, and molecular weight product is big, and the nutritive ingredient in the cartilage does not discharge fully, and product is not water-soluble, and color is darker, and human body is not easy to absorb.Form after the fresh cartilage hydrolysis of fundamentally different with these products is hydrolyzed II-type collagen adopts animal, the ratio of various effective constituents such as II collagen type, mucopolysaccharide, hyaluronic acid keeps pure natural constant in the starting material, and molecular weight diminishes, make the nutritive ingredient in the framework dissociate out fully, be easy to human consumption and absorb, effectively improved utilization ratio of raw materials.Simultaneously, because starting material adopt the fresh cartilage of healthy animal, be the whole food nutritious supplementary, security of products is also given and guarantee.Testing data shows, by oral can absorbed hydrolyzed II-type collagen, to skin, all kinds of joint diseases are had tangible effect, skin and joint problem that the collagen protein that alleviation causes because of age growth runs off and produces, effectively help skin care, promote bony articulation health and improve bone joint pain and the swelling that causes owing to sacroiliitis.
Summary of the invention
The invention provides a kind of preparation technology of hydrolyzed II-type collagen of low grey matter, this preparation technology adopts the combinative enzyme hydrolysis technology that insoluble collagen protein is become water miscible collagen protein, the molecular weight of product is diminished, effectively improved the specific absorption of product.Do not add mineral acid, the alkaloids of any increase solution ash content in its preparation process, this preparation technology's method steps is simple, it is easy, with low cost to operate and control.
The technical solution adopted in the present invention is as follows:
A kind of preparation technology of hydrolyzed II-type collagen is characterized in that described preparation technology comprises the steps:
Adopting clean livestock and poultry cartilage is raw material, is added to the water and carries out boiling;
Be hydrolyzed adding compound bio-enzyme in the livestock and poultry cartilage solution after the boiling;
Livestock and poultry cartilage solution after the filtration hydrolysis obtains the hydrolyzed II-type collagen settled solution.
Concretely, described livestock and poultry cartilage comprises the cartilage of healthy livestock and poultry chicken, ox, pig, duck, sheep.
Described compound bio-enzyme is by two or more prozyme formed in papain, neutral enzymatic, Traumanase, trypsinase, stomach en-, the food flavor enzyme.
The add-on of every kind of enzyme is 0.4%～1.0% of a cartilage total amount in the described prozyme, and described water is purified water or deionized water.
A kind of preparation technology of hydrolyzed II-type collagen is characterized in that described preparation technology's concrete steps are:
Adopting clean livestock and poultry cartilage is raw material, and the livestock and poultry cartilage is pulverized, and is added to the water then to carry out boiling to softening fully in 100～120 ℃;
Livestock and poultry cartilage solution after the boiling is cooled to the biological enzyme hydrolysis temperature, and the adding compound bio-enzyme is hydrolyzed;
Solution after the hydrolysis enzyme that goes out is handled;
Filter this solution to clarification, and concentrate and spraying drying, obtain the hydrolyzed II-type collagen powder.
Concretely, described compound bio-enzyme is by two or more prozyme formed in papain, neutral enzymatic, Traumanase, trypsinase, stomach en-, the food flavor enzyme.
Described hydrolysis comprises: the livestock and poultry cartilage solution after the boiling is cooled to 50～70 ℃, adopts compound bio-enzyme hydrolysis 2～5 hours, every kind of enzyme add-on in the described prozyme is 0.4～1% of a livestock and poultry cartilage weight, and described water is purified water or deionized water.
The described enzyme that goes out is handled and is comprised:
Add activated carbon, be warming up to 90～100 ℃, keep 20～30 minutes enzymes that go out.
Described preparation technology specifically comprises and adopts flame filter press to filter or whizzer centrifuging is gone out solution behind the enzyme to clarification; Being concentrated into concentration with thickener then is 2～3 times of stoste; At last with spray-drier ejection hydrolysis II collagen polypeptide powder.
In the hydrolyzed II-type collagen powder that described this preparation industry obtains, the II collagen content is 60～70%, and mucopolysaccharide content is 20%～30%, and hyaluronic acid contents is 8～12%, fat≤2%; Ash content≤10%, pH5.0～6.5.
The preparation technology of this hydrolyzed II-type collagen is a raw material with healthy, fresh livestock and poultry animal cartilage, by carrying out the compound bio-enzyme hydrolysis after the boiling, collagen hydrolysate is become micromolecule polypeptide, and can discharge materials such as chondroitin sulfate in the cartilage, hyaluronic acid; Mineral acid, the alkaloids that need not add any increase solution ash content in the whole preparation process, the hydrolyzed II-type collagen purity height that obtains at last, its composition is easier is absorbed by human body.
Beneficial effect of the present invention is that the preparation technology of this hydrolyzed II-type collagen adopts combinative enzyme hydrolysis
Technology becomes water miscible collagen protein with insoluble collagen protein, and the molecular weight of product is diminished, and has effectively improved the specific absorption of product.Do not add mineral acid, the alkaloids of any increase solution ash content in its preparation process, this preparation technology's method steps is simple, it is easy, with low cost to operate and control.
The invention will be further elaborated below in conjunction with the drawings and specific embodiments.
Fig. 1 is the step skeleton diagram of the specific embodiment of the invention;
Fig. 2 is the GPC gel chromatography figure of the hydrolyzed II-type collagen that obtains according to the embodiment of the invention 1.
Embodiment 1 as shown in Figure 1, at first the pigeon breast cartilage with health is that the feedstock production hydrolyzed II-type collagen is an example, carries out the operation of following processing step successively:
Description of drawings
Step 1 cartilage cleans: select healthy pigeon breast cartilage for use, clean with warm water, remove surface impurity;
Step 2: pulverize: the Cartilage powder after will cleaning is broken into the block of big grain of rice size;
Embodiment
Step 3: boiling: the cartilage 500g after will pulverizing drops in the reactor of 500g purified water, and boiling is 20 minutes under 100～120 ℃ of temperature, bumps promptly mashed to pigeon breast cartilage one;
Step 4: compound bio enzymic hydrolysis: the cartilage solution after the boiling is reduced to 60 ℃, add papain 3g, food flavor enzyme 2g, opening stirring arm simultaneously stirs at a slow speed, keep 60 ℃ of constant temperature hydrolysis 4 hours, the cartilage fritter of solution the inside becomes solution fully after the hydrolysis, and discharges the materials such as polysaccharide in the cartilage;
Step 5: add the 5g gac, be warming up to 90～100 ℃ and kept 20 minutes, the enzyme that goes out is handled;
Step 6: filter: clarify to solution with the flame filter press direct filtration or with supercentrifuge is centrifugal;
Step 7: concentrate: be concentrated into 2 times of original liquid concentration with the economic benefits and social benefits thickener;
Step 8: spraying drying: with spray-drier ejection hydrolyzed II-type collagen powder.
The hydrolyzed II-type collagen powder that above-mentioned preparation technology is obtained detects, II collagen content 〉=60% wherein, and mucopolysaccharide content is 〉=20%, and hyaluronic acid contents 〉=8%, pH are 5.0～6.5, and its each component is easier to be absorption of human body.The amino acid that it contained and other compound mensuration result such as following table 1.
The amino acid of table 1 hydrolyzed II-type collagen and other compound mensuration result
As shown in Table 1, fat and ash oontent all are lower than the prepared hydrolyzed II-type collagen of prior art in the hydrolyzed II-type collagen that obtains of this preparation technology.
It (promptly is stationary phase with the porous filler that the hydrolyzed II-type collagen that this preparation technology is obtained carries out that the GPC gel chromatography detects, difference according to sample component molecular volume size is separated, under the uv-absorbing wavelength 220nm of peptide bond condition, detect, the exclusive data process software (being GPC software) that uses the gel chromatography determining molecular weight to distribute, color atlas and data thereof are handled, calculated the relative molecular weight size and the distribution range of collagen hydrolysate).The GPC gel chromatography figure that obtains as shown in Figure 2.
Embodiment 2 is that raw material prepares hydrolyzed II-type collagen as follows with the cartilage of the ox of health, sheep, duck:
Step 1 cartilage cleans: select the cartilage of healthy and fresh ox, sheep and duck for use, clean with warm water, remove surface impurity;
Step 2: pulverize: the Cartilage powder after will cleaning is broken into the block of big grain of rice size;
Step 3: boiling: the cartilage 1000g after will pulverizing drops in the reactor of 1200g purified water, and boiling is 30 minutes under 100～110 ℃ of temperature, till the softening not variable color of cartilage boiling;
Step 4: compound bio enzymic hydrolysis: the cartilage solution after the boiling is reduced to 50 ℃, add Traumanase, each 10g of trypsinase, stomach en-4g, opening stirring arm simultaneously stirs, keep 50 ℃ of constant temperature hydrolysis 3 hours, the cartilage fritter of solution the inside becomes solution fully after the hydrolysis, and discharges the materials such as polysaccharide in the cartilage;
Step 5: add the 10g gac, be warming up to 90 ℃ and kept 30 minutes, the enzyme that goes out is handled;
Step 6: filter: clarify to solution with supercentrifuge is centrifugal;
Step 7: concentrate: be concentrated into 3 times of original liquid concentration with the economic benefits and social benefits thickener;
Step 8: spraying drying: with spray-drier ejection hydrolyzed II-type collagen powder.
The hydrolyzed II-type collagen powder that above-mentioned preparation technology is obtained detects, II collagen content 〉=60% wherein, and mucopolysaccharide content is 〉=20%, and hyaluronic acid contents 〉=8%, pH are 5.0～6.5, and its each component is easier to be absorption of human body.
Embodiment 3 is that raw material prepares hydrolyzed II-type collagen as follows with the pig cartilage of health:
Step 1 cartilage cleans: select healthy and fresh pig cartilage for use, clean with warm water, remove surface impurity;
Step 2: pulverize: the Cartilage powder after will cleaning is broken into the block of big grain of rice size;
Step 3: boiling: the cartilage 800g after will pulverizing drops in the reactor of 1200g purified water, and boiling is 30 minutes under 100～120 ℃ of temperature, till the softening not variable color of cartilage boiling;
Step 4: compound bio enzymic hydrolysis: the cartilage solution after the boiling is reduced to 65 ℃, add 4 of papains, 6 of food flavor enzymes, opening stirring arm simultaneously stirs, keep 65 ℃ of constant temperature hydrolysis 3 hours, the cartilage fritter of solution the inside becomes solution fully after the hydrolysis, and discharges the materials such as polysaccharide in the cartilage;
Step 5: add the 10g gac, be warming up to 90 ℃ and kept 30 minutes, the enzyme that goes out is handled;
Step 6: filter: clarify to solution with supercentrifuge is centrifugal;
Step 7: concentrate: be concentrated into 2 times of original liquid concentration with the economic benefits and social benefits thickener;
Step 8: spraying drying: with spray-drier ejection hydrolyzed II-type collagen powder.
The hydrolyzed II-type collagen powder that above-mentioned preparation technology is obtained detects, II collagen content 〉=60% wherein, and mucopolysaccharide content is 〉=20%, and hyaluronic acid contents 〉=8%, pH are 5.0～6.5, and its each component is easier to be absorption of human body.
Claims (10)
1. the preparation technology of a hydrolyzed II-type collagen is characterized in that described preparation technology comprises the steps:
Adopting clean livestock and poultry cartilage is raw material, is added to the water and carries out boiling;
Be hydrolyzed adding compound bio-enzyme in the livestock and poultry cartilage solution after the boiling;
Livestock and poultry cartilage solution after the filtration hydrolysis obtains the hydrolyzed II-type collagen settled solution.
2. the preparation technology of hydrolyzed II-type collagen according to claim 1 is characterized in that described livestock and poultry cartilage comprises the cartilage of healthy livestock and poultry chicken, ox, pig, duck, sheep.
3. the preparation technology of hydrolyzed II-type collagen according to claim 1 is characterized in that described compound bio-enzyme is by two or more prozyme formed in papain, neutral enzymatic, Traumanase, trypsinase, stomach en-, the food flavor enzyme.
4. the preparation technology of hydrolyzed II-type collagen according to claim 3, the add-on that it is characterized in that every kind of enzyme in the described prozyme is 0.4%～1.0% of a cartilage total amount, described water is purified water or deionized water.
5. the preparation technology of a hydrolyzed II-type collagen is characterized in that described preparation technology's concrete steps are:
Adopting clean livestock and poultry cartilage is raw material, and the livestock and poultry cartilage is pulverized, and is added to the water then to carry out boiling to softening fully in 100～120 ℃;
Livestock and poultry cartilage solution after the boiling is cooled to the biological enzyme hydrolysis temperature, and the adding compound bio-enzyme is hydrolyzed;
Solution after the hydrolysis enzyme that goes out is handled;
Filter this solution to clarification, and concentrate and spraying drying, obtain the hydrolyzed II-type collagen powder.
6. the preparation technology of hydrolyzed II-type collagen according to claim 5 is characterized in that described compound bio-enzyme is by two or more prozyme formed in papain, neutral enzymatic, Traumanase, trypsinase, stomach en-, the food flavor enzyme.
7. the preparation technology of hydrolyzed II-type collagen according to claim 6, it is characterized in that described hydrolysis comprises: the livestock and poultry cartilage solution after the boiling is cooled to 50～70 ℃, adopt compound bio-enzyme hydrolysis 2～5 hours, every kind of enzyme add-on in the described prozyme is 0.4～1% of a livestock and poultry cartilage weight, and described water is purified water or deionized water.
8. the preparation technology of hydrolyzed II-type collagen according to claim 5 is characterized in that the described enzyme that goes out is handled to comprise:
Add activated carbon, be warming up to 90～100 ℃, keep 20～30 minutes enzymes that go out.
9. the preparation technology of hydrolyzed II-type collagen according to claim 5 is characterized in that described preparation technology specifically comprises to adopt flame filter press to filter or whizzer centrifuging is gone out solution behind the enzyme to clarification; Being concentrated into concentration with thickener then is 2～3 times of stoste; At last with spray-drier ejection hydrolysis II collagen polypeptide powder.
10. the preparation technology of hydrolyzed II-type collagen according to claim 5, it is characterized in that in the industrial hydrolyzed II-type collagen powder that obtains of described this preparation, the II collagen content is 60～70%, mucopolysaccharide content is 20%～30%, hyaluronic acid contents is 8～12%, fat≤2%; Ash content≤10%, pH5.0～6.5.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101986859A (en) * | 2010-10-19 | 2011-03-23 | 河南双汇投资发展股份有限公司 | Method for preparing II type collagen mixtures by using poultry chest cartilage as raw materials |
| CN102146428A (en) * | 2010-12-22 | 2011-08-10 | 烟台东诚生化股份有限公司 | Method for extracting collagen II |
| CN102453108A (en) * | 2010-10-19 | 2012-05-16 | 河南双汇投资发展股份有限公司 | Combined production method for processing chondroitin sulfate and protein powder with bird skeletons as raw material |
| CN103060406A (en) * | 2011-10-18 | 2013-04-24 | 中国科学院理化技术研究所 | Method for extracting low molecular weight collagen from cattle bone |
| CN103356993A (en) * | 2012-04-06 | 2013-10-23 | 中国科学院大连化学物理研究所 | Application of collagen peptide in preparation of blood lipid lowering medicaments and health-care products |
| CN104621338A (en) * | 2015-03-03 | 2015-05-20 | 浙江小二黑食品有限公司 | Method for preparing novel silkie bone polypeptides |
| CN108378374A (en) * | 2018-02-08 | 2018-08-10 | 湖南易能生物医药有限公司 | A kind of pre- preventing bone rarefaction, the composition for promoting bone health |
| CN112544778A (en) * | 2020-12-09 | 2021-03-26 | 美泰科技（青岛）股份有限公司 | Preparation method of high-quality cartilage extract with high purity and good taste and application of prepared cartilage extract |
| EP4084868A4 (en) * | 2019-12-27 | 2024-01-31 | Suntory Holdings Ltd | Food or beverage composition containing peptide and/or salt thereof, production method thereof, use of hydrolyzed collagen type ii, composition for inhibiting bone resorption, and use of chicken extract |
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| CN1687441A (en) * | 2005-04-22 | 2005-10-26 | 黄磊 | III type proteinic small peptide and preparation technique thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101986859A (en) * | 2010-10-19 | 2011-03-23 | 河南双汇投资发展股份有限公司 | Method for preparing II type collagen mixtures by using poultry chest cartilage as raw materials |
| CN102453108A (en) * | 2010-10-19 | 2012-05-16 | 河南双汇投资发展股份有限公司 | Combined production method for processing chondroitin sulfate and protein powder with bird skeletons as raw material |
| CN102146428A (en) * | 2010-12-22 | 2011-08-10 | 烟台东诚生化股份有限公司 | Method for extracting collagen II |
| CN103060406A (en) * | 2011-10-18 | 2013-04-24 | 中国科学院理化技术研究所 | Method for extracting low molecular weight collagen from cattle bone |
| CN103060406B (en) * | 2011-10-18 | 2015-02-18 | 中国科学院理化技术研究所 | Method for extracting low molecular weight collagen from cattle bone |
| CN103356993A (en) * | 2012-04-06 | 2013-10-23 | 中国科学院大连化学物理研究所 | Application of collagen peptide in preparation of blood lipid lowering medicaments and health-care products |
| CN104621338A (en) * | 2015-03-03 | 2015-05-20 | 浙江小二黑食品有限公司 | Method for preparing novel silkie bone polypeptides |
| CN108378374A (en) * | 2018-02-08 | 2018-08-10 | 湖南易能生物医药有限公司 | A kind of pre- preventing bone rarefaction, the composition for promoting bone health |
| EP4084868A4 (en) * | 2019-12-27 | 2024-01-31 | Suntory Holdings Ltd | Food or beverage composition containing peptide and/or salt thereof, production method thereof, use of hydrolyzed collagen type ii, composition for inhibiting bone resorption, and use of chicken extract |
| CN112544778A (en) * | 2020-12-09 | 2021-03-26 | 美泰科技（青岛）股份有限公司 | Preparation method of high-quality cartilage extract with high purity and good taste and application of prepared cartilage extract |
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Application publication date: 20100721 |