CN103172729A - Method for rapidly preparing fish collagen - Google Patents

Method for rapidly preparing fish collagen Download PDF

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Publication number
CN103172729A
CN103172729A CN2013100768825A CN201310076882A CN103172729A CN 103172729 A CN103172729 A CN 103172729A CN 2013100768825 A CN2013100768825 A CN 2013100768825A CN 201310076882 A CN201310076882 A CN 201310076882A CN 103172729 A CN103172729 A CN 103172729A
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China
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collagen
fish
protein
fish scale
isin glue
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Pending
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CN2013100768825A
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Chinese (zh)
Inventor
周钢
樊瑜波
侯永昭
阿茹罕
徐奕
祖力胡玛尔
刘文勇
刘海峰
牛旭锋
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Beihang University
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Beihang University
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Abstract

The invention discloses a method for rapidly preparing fish collagen. An apparatus adopts a flash extraction way against the physiological and biochemical properties of fish collagen in order to rapidly prepare the fish collagen. The method is characterized in that the method treats fish skins or fish scales as a raw material and utilizes the flash extraction way to rapidly remove water-soluble pigments, other proteins and fat in order to obtain crude collagen, and the crude collagen is refined through utilizing salt-out and dialysis ways. Less loss, small denaturation, high yield and high purity of the collagen are realized in the whole preparation process. The prepared collagen has a high viscosity, a high gel strength and good application performances.

Description

A kind of quick method for preparing Isin glue collagen
Technical field
The present invention relates to a kind ofly for Isin glue collagen extractive technique method field, specifically, is to be raw material for fish-skin or fish scale, adopts sudden strain of a muscle formula extraction method to prepare fast the method for Isin glue collagen.
Background technology
Along with developing rapidly of culture fishery and processing industry, a large amount of fish-skins, fish scale the like waste produce thereupon, if can be taken full advantage of, and not only can environmental contamination reduction, the added value of fish be can also improve, thereby good economic benefit and social benefit obtained.
At present, acidleach formulation, alkali method, hot water extraction and enzyme extraction are the common methods of Isin glue collagen preparation.Acidleach formulation and alkali method are respectively to make fish-skin (squama) collagen protein generation Partial digestion with certain density acid solution or alkali lye, then are discharged in extraction agent.But when adopting acid/alkaline process to extract, collagen protein can produce decomposition to a certain degree, and this will cause biological activity to be lost, and the acidity or the alkaline waste liquor that meanwhile produce can cause secondary pollution to environment again.Hot water lixiviate collagen protein, extraction time is long, and temperature is high, and the collagen protein sex change is serious.Collagen Extraction with Enzyme albumen, reaction time consumption is long, and yield is low, and production cost is high, uses relatively limitation.Therefore, in the urgent need to developing a kind of simple and easy, method of effectively extracting the high-quality collagen protein.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, the employing working method is simple, the extracting method of applied range obtains collagen protein.It can satisfy the needs that collagen protein is produced, and dodges and invented the method that the formula extraction method prepares Isin glue collagen fast.
The present invention is a kind of method that the formula extraction method prepares Isin glue collagen fast of dodging, and comprises following processing step: (1) fish scale pre-treatment: remove the fish-skin of fish scale adhesion, fish scale is cleaned, dry.With the pending fish scale of pulverizer chopping; (2) add distilled water, the sudden strain of a muscle formula is extracted 2 times; (3) collagen protein extracts: add low-concentration acetic acid solution with swelling ratio 1:15-30, mix, place 4h, with the centrifugal 5-30min of 3500-5500r/min rotating speed, remove impurity afterwards, get supernatant liquor, and standby; (4) except foreigh protein removing: crude extract and NaCl solution are mixed by weight ratio, with the centrifugal 5-30min of 3500-5500r/min rotating speed, abandoning supernatant, precipitation is with the acetic acid dissolving of the 0.5mol/L of 10 times of volumes, with the centrifugal 5-30min of 3500-5500r/min rotating speed.Repeat this step 3 left and right; (5) deacidification and salt: the supernatant liquor that obtains later of saltouing was several times dialysed three days, changed first water per half a day.The dialysis tubing aperture is 7000; (6) dry sample: the collagen solution later of dialysing carries out drying with vacuum freeze drier, gets final product to get collagen product;
Fish scale pre-treatment in the present invention, acid are carried, the technological temperature of deacidification and salt is normal temperature, except the foreigh protein removing temperature is 4 ℃.The concentration of low-concentration acetic acid solution is 0.1-1mol/L, and it can remove fribrillin, makes fish-skin softening, and collagen protein is stable than foreign protein.In addition, the acetum of lower concentration can't cause collagen to degrade in a large number when foreign protein is removed in hydrolysis.Low-concentration acetic acid is collaborative to be extracted, and the collagen protein that obtains can keep its triple helix structure to greatest extent, is applicable to biomedical material and raw material thereof.The concentration of NaCl solution is 0.1-1mol/L, and certain density NaCl can make the foreign protein in fish-skin separate out, and assists in removing foreign protein collagen purification albumen.
Compared with prior art, the method that the present invention adopts the sudden strain of a muscle formula to extract is broken cell, has improved the productive rate of collagen.And adopt sudden strain of a muscle formula extraction method, with short production cycle, cost is low, and output is high, and the collagen protein sex change is few, and easily realizes industrialization.The collagen protein relative molecular mass that makes is large, and viscosity is high, and gel-strength is good, applied range.
Description of drawings
Fig. 1 is the pictorial diagram that adopts the collagen of the inventive method preparation
Fig. 2 is the pictorial diagram that adopts the collagen gel of the inventive method preparation
Fig. 3 adopts the atom of the collagen of the inventive method preparation to try hard to
Fig. 4 is the infared spectrum that adopts the collagen of the inventive method preparation
Embodiment
The present invention is further elaborated by following instance, but does not limit the scope of the invention.The production technique of this manufacturing technology is easily to implement for these professional personnel.
It is raw material that example 1 is chosen the tilapia fish scale, removes other materials of fish-skin and adhesion on fish scale, cleans and shred stand-by.With distilled water with fish scale by weight ratio for 15-30:1 mixes, dodge and to carry twice, each 1.5 minutes.Be the acetic acid solution that 1:15-30 adds 0.5mol/L by swelling ratio, with the centrifugal 5-30min of 3500-5500r/min rotating speed, get supernatant liquor afterwards, standby.Crude extract and NaCl solution are mixed by weight ratio, with the centrifugal 5-30min of 3500-5500r/min rotating speed, abandoning supernatant, precipitation is with the acetic acid dissolving of the 0.5mol/L of 10 times of volumes, with the centrifugal 5-30min of 3500-5500r/min rotating speed.Repeat this step 3 left and right.First water is changed in the supernatant liquor dialysis that obtains later saltouing several times three days per half a day.The dialysis tubing aperture is 7000.Dialysis collagen solution is later carried out drying with vacuum freeze drier, get final product to get the collagen protein raw product.
The collagen protein that adopts above method to make, relative molecular weight is high, and viscosity is high, and gel-strength is large, and its increase with concentration increases, square almost proportional with concentration.Collagen product after purifying colloidal form exists, easily preserves, and volatility not, applied range has good retentiveness.
It is raw material that example 2 is chosen tilapia fishskin, removes other materials of adhesion on fish scale and fish-skin, cleans and shred stand-by.With distilled water with fish-skin by weight ratio for 15-30:1 mixes, dodge and to carry twice, each 1.5 minutes.Be the acetic acid solution that 1:15-30 adds 0.5mol/L by swelling ratio, with the centrifugal 5-30min of 3500-5500r/min rotating speed, get supernatant liquor afterwards, standby.Crude extract and NaCl solution are mixed by weight ratio, with the centrifugal 5-30min of 3500-5500r/min rotating speed, abandoning supernatant, precipitation is with the acetic acid dissolving of the 0.5mol/L of 10 times of volumes, with the centrifugal 5-30min of 3500-5500r/min rotating speed.Repeat this step 3 left and right.First water is changed in the supernatant liquor dialysis that obtains later saltouing several times three days per half a day.The dialysis tubing aperture is 7000.Dialysis collagen solution is later carried out drying with vacuum freeze drier, get final product to get the collagen protein raw product.
It is raw material that example 3 is chosen the carp fish scale, removes other materials of fish-skin and adhesion on fish scale, cleans and shred stand-by.With distilled water with fish scale by weight ratio for 15-30:1 mixes, dodge and to carry twice, each 1.5 minutes.Be the acetic acid solution that 1:15-30 adds 0.5mol/L by swelling ratio, with the centrifugal 5-30min of 3500-5500r/min rotating speed, get supernatant liquor afterwards, standby.Crude extract and NaCl solution are mixed by weight ratio, with the centrifugal 5-30min of 3500-5500r/min rotating speed, abandoning supernatant, precipitation is with the acetic acid dissolving of the 0.5mol/L of 10 times of volumes, with the centrifugal 5-30min of 3500-5500r/min rotating speed.Repeat this step 3 left and right.First water is changed in the supernatant liquor dialysis that obtains later saltouing several times three days per half a day.The dialysis tubing aperture is 7000.Dialysis collagen solution is later carried out drying with vacuum freeze drier, get final product to get the collagen protein raw product.
It is raw material that example 2 is chosen common carp skin, removes other materials of adhesion on fish scale and fish-skin, cleans and shred stand-by.With distilled water with fish-skin by weight ratio for 15-30:1 mixes, dodge and to carry twice, each 1.5 minutes.Be the acetic acid solution that 1:15-30 adds 0.5mol/L by swelling ratio, with the centrifugal 5-30min of 3500-5500r/min rotating speed, get supernatant liquor afterwards, standby.Crude extract and NaCl solution are mixed by weight ratio, with the centrifugal 5-30min of 3500-5500r/min rotating speed, abandoning supernatant, precipitation is with the acetic acid dissolving of the 0.5mol/L of 10 times of volumes, with the centrifugal 5-30min of 3500-5500r/min rotating speed.Repeat this step 3 left and right.First water is changed in the supernatant liquor dialysis that obtains later saltouing several times three days per half a day.The dialysis tubing aperture is 7000.Dialysis collagen solution is later carried out drying with vacuum freeze drier, get final product to get the collagen protein raw product.

Claims (7)

1. a method for preparing fast Isin glue collagen, is characterized in that: adopt sudden strain of a muscle formula extraction method.Isin glue collagen extracting method of the present invention can from the starting material of fish scale and fish-skin, adopt sudden strain of a muscle formula extraction method to prepare fast the method for Isin glue collagen.
2. extracting method according to claim 1, is characterized in that, described fish scale and fish-skin starting material specifically derive from carp, crucian, black carp, grass carp, silver carp, bighead, tilapia etc.
3. a kind of quick method for preparing Isin glue collagen according to claim 1, is characterized in that, described method is to overcome the deficiencies in the prior art, adopts that working method is simple, the extracting method of applied range obtains Isin glue collagen.It can satisfy the needs that Isin glue collagen is produced, and dodges and invented the method that the formula extraction method prepares Isin glue collagen fast.
4. method for preparing fast Isin glue collagen is characterized in that comprising following steps: comprise following processing step:
(1) fish scale pre-treatment: remove the fish-skin of fish scale adhesion, fish scale is cleaned, dry.With the pending fish scale of pulverizer chopping;
(2) add distilled water, the sudden strain of a muscle formula is extracted 2 times;
(3) collagen protein extracts: add low-concentration acetic acid solution with swelling ratio 1:15-30, mix, place 4h, with the centrifugal 5-30min of 3500-5500r/min rotating speed, remove impurity afterwards, get supernatant liquor, and standby;
(4) except foreigh protein removing: crude extract and NaCl solution are mixed by weight ratio, with the centrifugal 5-30min of 3500-5500r/min rotating speed, abandoning supernatant, precipitation is with the acetic acid dissolving of the 0.5mol/L of 10 times of volumes, with the centrifugal 5-30min of 3500-5500r/min rotating speed.Repeat this step 3 left and right;
(5) deacidification and salt: the supernatant liquor that obtains later of saltouing was several times dialysed three days, changed first water per half a day.The dialysis tubing aperture is 7000;
(6) dry sample: the collagen solution later of dialysing carries out drying with vacuum freeze drier, gets final product to get collagen product.
5. the service temperature of extraction step according to claim 4, is characterized in that, described fish scale pre-treatment, acid are carried, the technological temperature of deacidification and salt is normal temperature, except the foreigh protein removing temperature is 4 ℃.
6. acetum according to claim 4, is characterized in that, described low-concentration acetic acid solution, and its concentration is the 0.1-1mol/L left and right.Acetic acid can be removed fribrillin, makes fish-skin softening, and collagen protein is stable than foreign protein, and the acetum of lower concentration can't cause collagen to degrade in a large number when foreign protein is removed in hydrolysis.Low-concentration acetic acid is collaborative to be extracted, and the collagen protein that obtains can keep its triple helix structure to greatest extent, is applicable to biomedical material and raw material thereof.
7. salts solution according to claim 4, is characterized in that, described salts solution refers to NaCl solution, and its concentration is 0.1-1mol/L, and certain density NaCl can make the foreign protein in fish-skin separate out, and assists in removing foreign protein collagen purification albumen.
CN2013100768825A 2013-03-11 2013-03-11 Method for rapidly preparing fish collagen Pending CN103172729A (en)

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Cited By (6)

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Publication number Priority date Publication date Assignee Title
CN104892750A (en) * 2015-05-27 2015-09-09 深圳先进技术研究院 Preparation method of acid-soluble fish scale collagen
CN105131109A (en) * 2015-09-30 2015-12-09 陕西艾尔肤组织工程有限公司 Collagen extracting method
CN105420324A (en) * 2015-12-23 2016-03-23 武汉梁子湖水产品加工有限公司 Preparation method of high-molecular-weight silver carp skin collagen peptide
CN108314726A (en) * 2018-04-28 2018-07-24 贵阳学院 A kind of giant salamander collagen extracting method and the collagen product extracted by this method
CN108523032A (en) * 2018-04-13 2018-09-14 北京同仁堂健康(大连)海洋食品有限公司 A kind of preparation method of fish glue dried product
CN110386976A (en) * 2019-06-25 2019-10-29 浙江省农业科学院 A kind of grass carp air bladder collagen self-assembling method and collagen biomaterial

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CN101886106A (en) * 2010-07-02 2010-11-17 湖北远成药业有限公司 Method for extracting collagen peptide from fish scales
CN102925421A (en) * 2012-11-27 2013-02-13 天津蚓福生物科技开发有限公司 Preparation method of lumbrukinase

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104892750A (en) * 2015-05-27 2015-09-09 深圳先进技术研究院 Preparation method of acid-soluble fish scale collagen
CN105131109A (en) * 2015-09-30 2015-12-09 陕西艾尔肤组织工程有限公司 Collagen extracting method
CN105420324A (en) * 2015-12-23 2016-03-23 武汉梁子湖水产品加工有限公司 Preparation method of high-molecular-weight silver carp skin collagen peptide
CN105420324B (en) * 2015-12-23 2019-02-15 武汉梁子湖水产品加工有限公司 A kind of preparation method of high molecular weight silver carp collagen peptide
CN108523032A (en) * 2018-04-13 2018-09-14 北京同仁堂健康(大连)海洋食品有限公司 A kind of preparation method of fish glue dried product
CN108314726A (en) * 2018-04-28 2018-07-24 贵阳学院 A kind of giant salamander collagen extracting method and the collagen product extracted by this method
CN108314726B (en) * 2018-04-28 2020-10-30 贵阳学院 Giant salamander skin collagen extraction method and collagen product extracted by same
CN110386976A (en) * 2019-06-25 2019-10-29 浙江省农业科学院 A kind of grass carp air bladder collagen self-assembling method and collagen biomaterial
CN110386976B (en) * 2019-06-25 2020-12-25 浙江省农业科学院 Grass carp swim bladder collagen self-assembly method and collagen biological raw material

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Application publication date: 20130626