CN107177658A - A kind of preparation method of Cartilage collagen peptide - Google Patents
A kind of preparation method of Cartilage collagen peptide Download PDFInfo
- Publication number
- CN107177658A CN107177658A CN201710630817.0A CN201710630817A CN107177658A CN 107177658 A CN107177658 A CN 107177658A CN 201710630817 A CN201710630817 A CN 201710630817A CN 107177658 A CN107177658 A CN 107177658A
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- Prior art keywords
- cartilage
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- collagen peptide
- feed liquid
- desugar
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P21/00—Preparation of peptides or proteins
- C12P21/06—Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K14/00—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof
- C07K14/435—Peptides having more than 20 amino acids; Gastrins; Somatostatins; Melanotropins; Derivatives thereof from animals; from humans
- C07K14/78—Connective tissue peptides, e.g. collagen, elastin, laminin, fibronectin, vitronectin, cold insoluble globulin [CIG]
Abstract
The present invention relates to technical field of bioengineering, more particularly to a kind of preparation method of Cartilage collagen peptide.Comprise the following steps：Cartilage is pre-processed, desugar, purified treatment, composite hydrolysis, and go out enzyme, filtering, adsorbs desugar, is concentrated by ultrafiltration, and is sterilized and is spray-dried.The present invention has carried out two step desugars in the preparation process of Cartilage collagen peptide, salt and alkali method is first passed through to remove substantial amounts of polysaccharide in cartilage, cartilage is hydrolyzed again extraction collagen peptide, then Adsorption is carried out to polysaccharide a small amount of in peptide liquid via macroreticular resin again, whole technical process is more convenient, and operation is relatively easy, quality of finished is higher.The present invention is removed the polysaccharide in cartilage by salt and alkali method, and during follow-up composite hydrolysis is carried out, the cartilage composite hydrolysis after desugar only needs to 1 2h, greatly shortens the composite hydrolysis time.After desugar, follow-up filtration step is also more smooth, shortens filtration time, improves the efficiency of integrated artistic.
Description
Technical field
The present invention relates to technical field of bioengineering, more particularly to a kind of preparation method of Cartilage collagen peptide.
Background technology
Animal Husbandry in China high speed development since the nineties in last century, main poultry kind especially live pig breeding stock growth is strong
Strength, 4.5 hundred million are up to by 2016 year end live pig breeding stocks.As common people's meat intake demand is improved, cartilage is slaughtered in livestock
Largely individually rejected during government official.Cartilaginous tissue is without vascular distribution, no lesion risk, rich in abundant collagen and many
Sugar, is the high-quality cartilage source for producing high-quality collagen peptide.Contain what is enriched in cartilage in distinctive Type Ⅱ collagen albumen
Hydroxyproline, proline and glycine, are the important supplements of amino acid needed for health.Cartilage is rarely used on the market now
Collagen peptide product is prepared, polysaccharide can not be mainly efficiently separated in technique, the collagen peptide purity produced is relatively low not
Beneficial to digesting and assimilating for human body.
The content of the invention
To solve the deficiency that prior art is present, the present invention provides a kind of preparation method of Cartilage collagen peptide, we
Collagen peptide purity prepared by method is high, is conducive to digesting and assimilating for human body.
The technical scheme is that：
A kind of preparation method of Cartilage collagen peptide, comprises the following steps：
1) cartilage is pre-processed：Cartilage is put into water, 1-2h is stirred, cartilage surface attachment impurity is removed, the removal of impurity will be gone
Cartilage be crushed to particle diameter for 8-20mm；
2) desugar：Compare 1 according to feed liquid weight:4-12 adds water into the cartilage after crushing, then adds cartilage weight 1-5%
Alkali and cartilage weight 1-6% salt, stirring immersion 12-16h, soaked rear separation of solid and liquid；
3) purified treatment：Compare 1 according to feed liquid weight:5-8 adds water, soaking and washing 1-2h, leaching into the cartilage after separation
Bubble has cleaned rear separation of solid and liquid；
4) composite hydrolysis：Compare 1 according to feed liquid weight:3-6 adds water into the cartilage after separation, is heated to while stirring
45-60 DEG C, pH to 7.5-9.5 is adjusted, cartilage weight 1-5 ‰ enzyme preparation is added, 1-2h is reacted；
5) go out enzyme：After hydrolysis terminates, pH is to 5.0-7.0 for regulation, is heated to 75-85 DEG C, holds warm 10-20min；
6) filter：By the feed liquid after the enzyme that goes out through filter circulating filtration；
7) desugar is adsorbed：Clarification feed liquid after filtering is cooled to 30-50 DEG C through heat exchanger, the feed liquid after cooling is with 2-
3m/h flow velocity is through macroporous resin adsorption desugar；
8) it is concentrated by ultrafiltration：Feed liquid after desugar enters ultrafiltration apparatus, and the feed liquid after desugar is concentrated into the 15- of original volume
35%；
9) sterilize：Drying process will be entered after the sterilized machine sterilizing of feed liquid after concentration；
10) it is spray-dried：Concentrate is cooled to 40-55 DEG C, and drying tower is delivered to through high-pressure pump, controls the EAT to be
160-190 DEG C, temperature of outgoing air is 85-100 DEG C, is dried to sieve after powder, packs.
Further, the cartilage is cartilage in mammals.
Further, the step 2) in alkali be sodium hydroxide or calcium hydroxide or potassium hydroxide；The step 2) in
Salt be sodium chloride.
Further, the step 4) in enzyme preparation be complex enzyme formulation, mixed by protease, lipase and cellulase
Conjunction is formed.
Further, the protease, lipase and cellulase are in the proportion shared by complex enzyme formulation：80%th,
15%th, 5%.
Further, the step 7) in the type of macroreticular resin be：D290 resin anion (R.A.)s.
Further, the step 8) in, pressure≤5bar of the ultrafiltration apparatus.
Further, the step 9) in, the temperature of the sterilizing is 135 DEG C, and the time is 15s.
The beneficial effects of the invention are as follows：
The present invention has carried out two step desugars in the preparation process of Cartilage collagen peptide, first passes through salt and alkali method by cartilage
Substantial amounts of polysaccharide is removed, then cartilage is hydrolyzed, and extracts collagen peptide, then again via macroreticular resin to a small amount of in peptide liquid
Polysaccharide carry out Adsorption, whole technical process is more convenient, and operates relatively easy, and quality of finished is higher.
The present invention is removed the polysaccharide in cartilage by salt and alkali method, during follow-up composite hydrolysis is carried out, after desugar
Cartilage composite hydrolysis only need to 1-2h, greatly shorten composite hydrolysis time, and filtration step follow-up after desugar
It is more smooth, filtration time is shortened, the efficiency of integrated artistic is improved.
The present invention is by independent separation of polysaccharides step, then the small molecule glue that composite hydrolysis obtains high content is carried out to cartilage
Former protein peptides, are conducive to lifting product purity and absorption of human body level.
Embodiment
The present invention is described in more details below.
Embodiment 1
Cartilage employed in the present embodiment is pig cartilage.
Drinking water is added in cartilage, did not had cartilage surface 20cm, 1h is stirred, cartilage surface is removed and adheres to miscellaneous dirt.Weigh and remove
Cartilage 100Kg after miscellaneous dirt is ground into particle diameter for 8mm into pulverizer.400Kg purified waters are added into the cartilage after crushing, then
Add separation of solid and liquid after 1Kg sodium hydroxide and 1Kg sodium chloride, stirring immersion 12h.Feed liquid after separation can individually reclaim many
Sugar, cartilage particles then enter cleaning procedure.Cartilage after separation is added into separation of solid and liquid after 500Kg purified waters, soaking and washing 2h, returned
Rinse water is received to lower batch cleaning procedure, cartilage particles enter hydrolyzing process.Cartilage after separation is added into 300Kg purified waters, side
Stirring side is heated to 45 DEG C, adds salt acid for adjusting pH and is added to 7.5, then by complex enzyme formulation, the addition of complex enzyme formulation is
0.1Kg, wherein proteinase-10 .08Kg, lipase 0.015Kg and cellulase 0.005Kg, the lower reaction 2h of stirring.Hydrolysis terminates
Afterwards, salt acid for adjusting pH is added to 7.0, is warming up to 75 DEG C, is held warm 10min.Feed liquid is through filter circulating filtration to clarification.After filtering
Feed liquid be cooled to 30 DEG C through heat exchanger, the feed liquid after cooling with 2-3m/h speed through D290 resin anion (R.A.)s adsorb desugar.
Feed liquid after desugar enters ultrafiltration apparatus, is concentrated into the 15% of remaining material liquid volume under≤5bar pressure, feed liquid is sterilized
Enter drying process after the 15s that kept steady at 135 DEG C of machine sterilizations.When feed temperature is down to 40 DEG C, drying tower tower is delivered to through high-pressure pump
Top, controls 160 DEG C of EAT, and 85 DEG C of temperature of outgoing air is dried to sieve after powder, packed.The weight of the collagen peptide of preparation
For：46Kg, purity is：97.5%.
Embodiment 2
Cartilage employed in the present embodiment is ox cartilage.
Drinking water is added in cartilage, did not had cartilage surface 30cm, 2h is stirred, cartilage surface is removed and adheres to miscellaneous dirt.Weigh and remove
Cartilage 100Kg after miscellaneous dirt is ground into particle diameter for 20mm into pulverizer.1200Kg purified waters are added into the cartilage after crushing,
Add separation of solid and liquid after 5Kg potassium hydroxide and 6Kg sodium chloride, stirring immersion 16h.Feed liquid after separation can be reclaimed individually
Polysaccharide, cartilage particles then enter cleaning procedure.Cartilage after separation is added into separation of solid and liquid after 600Kg purified waters, soaking and washing 2h,
Recovery and rinsing water to lower batch cleaning procedure, cartilage particles enter hydrolyzing process.Cartilage after separation is added into 600Kg purified waters,
60 DEG C are heated to while stirring, are added salt acid for adjusting pH and are added to 9.5, then by complex enzyme formulation, the addition of complex enzyme formulation
For 0.5Kg, wherein proteinase-10 .4Kg, lipase 0.075Kg and cellulase 0.025Kg, the lower reaction 2h of stirring.Hydrolysis terminates
Afterwards, salt acid for adjusting pH is added to 6.0, is warming up to 85 DEG C, is held warm 20min.Feed liquid is through filter circulating filtration to clarification.After filtering
Feed liquid be cooled to 50 DEG C through heat exchanger, the feed liquid after cooling with 2-3m/h speed through D290 resin anion (R.A.)s adsorb desugar.
Feed liquid after desugar enters ultrafiltration apparatus, is concentrated into the 35% of remaining material liquid volume under≤5bar pressure, feed liquid is sterilized
Enter drying process after the 15s that kept steady at 135 DEG C of machine sterilizations.When feed temperature is down to 55 DEG C, drying tower tower is delivered to through high-pressure pump
Top, controls 190 DEG C of EAT, and 100 DEG C of temperature of outgoing air is dried to sieve after powder, packed.The weight of the collagen peptide of preparation
For：52Kg purity is：96.8%.
Embodiment 3
Cartilage employed in the present embodiment is sheep cartilage.
Drinking water is added in cartilage, did not had cartilage surface 20cm, 1h is stirred, cartilage surface is removed and adheres to miscellaneous dirt.Weigh and remove
Cartilage 100Kg after miscellaneous dirt is ground into particle diameter for 10mm into pulverizer.600Kg purified waters are added into the cartilage after crushing,
Add separation of solid and liquid after 3Kg sodium hydroxide and 4Kg sodium chloride, stirring immersion 15h.Feed liquid after separation can be reclaimed individually
Polysaccharide, cartilage particles then enter cleaning procedure.Cartilage after separation is added into solid-liquid point after 800Kg purified waters, soaking and washing 1.5h
From recovery and rinsing water to lower batch cleaning procedure, cartilage particles enters hydrolyzing process.400Kg is added to purify the cartilage after separation
Water, is heated to 50 DEG C while stirring, adds salt acid for adjusting pH and is added to 8.5, then by complex enzyme formulation, the addition of complex enzyme formulation
Measure as 0.4Kg, wherein proteinase-10 .32Kg, lipase 0.06Kg and cellulase 0.02Kg, the lower reaction 1h of stirring.Hydrolysis terminates
Afterwards, salt acid for adjusting pH is added to 5.0, is warming up to 85 DEG C, is held warm 15min.Feed liquid is through filter circulating filtration to clarification.After filtering
Feed liquid be cooled to 40 DEG C through heat exchanger, the feed liquid after cooling with 2-3m/h speed through D290 resin anion (R.A.)s adsorb desugar.
Feed liquid after desugar enters ultrafiltration apparatus, is concentrated into the 20% of remaining material liquid volume under≤5bar pressure, feed liquid is sterilized
Enter drying process after the 15s that kept steady at 135 DEG C of machine sterilizations.When feed temperature is down to 30 DEG C, drying tower tower is delivered to through high-pressure pump
Top, controls 180 DEG C of EAT, and 90 DEG C of temperature of outgoing air is dried to sieve after powder, packed.The weight of the collagen peptide of preparation
For：55Kg purity is：97.2%.
The embodiments of the present invention described above are not intended to limit the scope of the present invention.It is any in the present invention
Spirit and principle within the modifications, equivalent substitutions and improvements made etc., should be included in the claim protection model of the present invention
Within enclosing.
Claims (8)
1. a kind of preparation method of Cartilage collagen peptide, it is characterised in that comprise the following steps：
1) cartilage is pre-processed：Cartilage is put into water, 1-2h is stirred, cartilage surface attachment impurity is removed, will go deimpurity soft
Bone meal is broken to particle diameter for 8-20mm；
2) desugar：Compare 1 according to feed liquid weight:4-12 adds water into the cartilage after crushing, then adds cartilage weight 1-5% alkali
With cartilage weight 1-6% salt, stirring immersion 12-16h has soaked rear separation of solid and liquid；
3) purified treatment：Compare 1 according to feed liquid weight:5-8 adds water into the cartilage after separation, and soaking and washing 1-2h, immersion is clear
Wash rear separation of solid and liquid；
4) composite hydrolysis：Compare 1 according to feed liquid weight:3-6 adds water into the cartilage after separation, and 45-60 is heated to while stirring
DEG C, pH to 7.5-9.5 is adjusted, cartilage weight 1-5 ‰ enzyme preparation is added, 1-2h is reacted；
5) go out enzyme：After hydrolysis terminates, pH is to 5.0-7.0 for regulation, is heated to 75-85 DEG C, holds warm 10-20min；
6) filter：By the feed liquid after the enzyme that goes out through filter circulating filtration；
7) desugar is adsorbed：Clarification feed liquid after filtering is cooled to 30-50 DEG C through heat exchanger, the feed liquid after cooling is with 2-3m/h's
Flow velocity is through macroporous resin adsorption desugar；
8) it is concentrated by ultrafiltration：Feed liquid after desugar enters ultrafiltration apparatus, and the feed liquid after desugar is concentrated into the 15-35% of original volume；
9) sterilize：Drying process will be entered after the sterilized machine sterilizing of feed liquid after concentration；
10) it is spray-dried：Concentrate is cooled to 40-55 DEG C, and drying tower is delivered to through high-pressure pump, and it is 160- to control EAT
190 DEG C, temperature of outgoing air is 85-100 DEG C, is dried to sieve after powder, packs.
2. a kind of preparation method of Cartilage collagen peptide according to claim 1, it is characterised in that：The cartilage is the food in one's mouth
Newborn animal cartilage.
3. a kind of preparation method of Cartilage collagen peptide according to claim 1, it is characterised in that：The step 2) in
Alkali be sodium hydroxide or calcium hydroxide or potassium hydroxide；The step 2) in salt be sodium chloride.
4. a kind of preparation method of Cartilage collagen peptide according to claim 1, it is characterised in that：The step 4) in
Enzyme preparation be complex enzyme formulation, mixed by protease, lipase and cellulase.
5. a kind of preparation method of Cartilage collagen peptide according to claim 4, it is characterised in that：The protease,
Lipase and cellulase are in the proportion shared by complex enzyme formulation：80%th, 15%, 5%.
6. a kind of preparation method of Cartilage collagen peptide according to claim 1, it is characterised in that：The step 7) in
The type of macroreticular resin be：D290 resin anion (R.A.)s.
7. a kind of preparation method of Cartilage collagen peptide according to claim 1, it is characterised in that：The step 8)
In, pressure≤5bar of the ultrafiltration apparatus.
8. a kind of preparation method of Cartilage collagen peptide according to claim 1, it is characterised in that：The step 9)
In, the temperature of the sterilizing is 135 DEG C, and the time is 15s.
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| CN201710630817.0A CN107177658A (en) | 2017-07-28 | 2017-07-28 | A kind of preparation method of Cartilage collagen peptide |
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| CN201710630817.0A CN107177658A (en) | 2017-07-28 | 2017-07-28 | A kind of preparation method of Cartilage collagen peptide |
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| CN108048514A (en) * | 2017-12-20 | 2018-05-18 | 安达市旭朗生物科技有限公司 | The method of fresh bone extraction chondroitin sulfate, collagen peptide and albumen fatty powder |
| CN109384842A (en) * | 2018-12-25 | 2019-02-26 | 美泰科技（青岛）股份有限公司 | A kind of preparation method of non denatured II collagen of industrialization |
| CN111773375A (en) * | 2020-07-10 | 2020-10-16 | 河北智同生物制药股份有限公司 | Bone polypeptide composition and oral liquid for promoting bone growth and maintaining bone health |
| CN111808185A (en) * | 2020-07-08 | 2020-10-23 | 威海市宇王集团海洋生物工程有限公司 | Method for extracting elastin peptide from bovine cartilage |
| CN112813127A (en) * | 2021-04-08 | 2021-05-18 | 日照岚山生化制品有限公司 | Method for preparing collagen peptide from chondroitin sulfate ultrafiltration waste liquid |
| CN114457138A (en) * | 2022-02-25 | 2022-05-10 | 浙江工业大学 | Method for removing type II collagen peptide polysaccharide |
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| CN109384842A (en) * | 2018-12-25 | 2019-02-26 | 美泰科技（青岛）股份有限公司 | A kind of preparation method of non denatured II collagen of industrialization |
| CN111808185A (en) * | 2020-07-08 | 2020-10-23 | 威海市宇王集团海洋生物工程有限公司 | Method for extracting elastin peptide from bovine cartilage |
| CN111773375A (en) * | 2020-07-10 | 2020-10-16 | 河北智同生物制药股份有限公司 | Bone polypeptide composition and oral liquid for promoting bone growth and maintaining bone health |
| CN111773375B (en) * | 2020-07-10 | 2023-09-12 | 河北智同生物制药股份有限公司 | Bone polypeptide composition and oral liquid for promoting bone growth and maintaining bone health |
| CN112813127A (en) * | 2021-04-08 | 2021-05-18 | 日照岚山生化制品有限公司 | Method for preparing collagen peptide from chondroitin sulfate ultrafiltration waste liquid |
| CN114457138A (en) * | 2022-02-25 | 2022-05-10 | 浙江工业大学 | Method for removing type II collagen peptide polysaccharide |
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