CN101643766B - Method for preparing hydrolyzed collagen protein by fresh animal skin - Google Patents
Method for preparing hydrolyzed collagen protein by fresh animal skin Download PDFInfo
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- CN101643766B CN101643766B CN2009100183196A CN200910018319A CN101643766B CN 101643766 B CN101643766 B CN 101643766B CN 2009100183196 A CN2009100183196 A CN 2009100183196A CN 200910018319 A CN200910018319 A CN 200910018319A CN 101643766 B CN101643766 B CN 101643766B
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Abstract
The invention relates to a method for preparing hydrolyzed collagen protein by fresh animal skin, which mainly comprises the following steps: animal skin processing; enzymolysis; solid particulate matter elimination; enzymolysis reaction-separation and coupling; nanofiltration concentration; spray drying; and the like. The invention has high finished product yield; in addition, the average molecular weight of a product is about 2000, the product is easier to absorb by human bodies and has no bitter taste.
Description
(1) technical field the present invention relates to a kind of preparation method of Collagen Hydrolysate, mainly produces from the fresh animal skin.
(2), the background technology Collagen Hydrolysate claims collagen peptide again, is that Collagen Hydrolysate has identical chemical constitution with collagen protein by the soluble small molecular albumen of collagen protein through the hydrolysis preparation.Because the reduction of molecular weight, Collagen Hydrolysate solvability in water improves, thereby easier in absorptions such as the skin of human body, hairs, its trophic function is further brought into play.The main raw material of producing collagen protein at present has pigskin, the skin of the rawhide of animals such as ox-hide, bone key and fish (eel, filefish etc.).
Scientific research shows, molecular-weight average (approximately contains 30 amino acid) about 2000, Collagen Hydrolysate the easiest be absorbed by the body of polypeptide length about the 30-50 nanometer, the Collagen Hydrolysate of molecular-weight average excessive (for example molecular-weight average is greater than 5000) is difficult for being absorbed by the body, and molecular-weight average too small (for example molecular-weight average is less than 500) easily drains with moisture and also is difficult for being absorbed by the body.
The method for hydrolysis of domestic and foreign current mainly contains strong acid, and highly basic, single enzyme are handled, and mode such as prozyme processing, and wherein using maximum is that prozyme is handled.
Wherein, the main drawback of existing enzymolysis process method is, the enzymolysis degree is restive, the molecular weight of the Collagen Hydrolysate of preparation is difficult to meet above-mentioned standard and product has bitter taste, and because enzyme digestion reaction is reversible reaction, existing enzymolysis process can not change the enzymolysis balance, thereby the transformation efficiency of substrate can be subjected to the restriction of the enzyme digestion reaction equilibrium constant, cause the transformation efficiency of substrate low slow with the product generating rate, the yield of product is low.After finishing, enzymolysis also need carry out the technology of high temperature (90 ℃) enzyme that goes out, not only consumes energy but also waste raw material.
The producer that has also adopts the collagen peptide of ultrafiltration means control macromolecule to produce, and with the ultrafiltrate evaporation concentration.Evaporation is to make the solution boiling vaporization that contains the non-volatility solute and remove steam, thereby makes the unit operation that solute concentration improves in the solution, to reach the purpose of liquid concentration.Evaporation concentration needs continuous heat supply, adopts not only energy consumption height of this method, and does not reach the purpose that removes micromolecular Collagen Hydrolysate.
(3) summary of the invention technical problem to be solved by this invention provides a kind of method of preparing hydrolyzed collagen protein by fresh animal skin, to overcome existing Collagen Hydrolysate preparation method's aforesaid drawbacks.Optimize enzymolysis process by enzyme digestion reaction-separation coupling, improve the transformation efficiency of substrate and the generating rate of product, improve the product yield; And ultrafiltration and nanofiltration technique cut the Collagen Hydrolysate of macromolecule and small molecular weight, makes the product molecular-weight average meet the requirement that human body is easy to absorb; Product does not have bitter taste; Process energy consumption is low.
For above-mentioned technical problem, the present invention adopts following technical scheme:
A kind of method of preparing hydrolyzed collagen protein by fresh animal skin is characterized in that: mainly comprise following processing step:
(1), animal skin pre-treatment: will be through the fresh food level animal skin chopping after the depilation degreasing, length * wide≤1 * 1cm without storage;
(2), enzymolysis: adding 1.5 tons of water and weight in wet base in reactor is the animal skin of 100～120kg chopping, is steam heated to 40～65 ℃ under stirring, and adds 0.3～1.2Kg Sumizyme MP, insulated and stirred reaction 3～5 hours;
(3), remove the solid particles thing: the reaction solution of (2) step reaction was left standstill 0.5～1 hour, remove the solid particles thing;
(4), enzyme digestion reaction-separation coupling: the reaction solution that will remove behind the solid particles thing is got in the ultrafiltration jar that is placed with 2 tons of softening waters, stirs employing molecular weight cut-off after 15～20 minutes greater than 5000 filter membrane ultra-filtration and separation; The filtrate that sees through ultra-filtration membrane enters in the nanofiltration jar by pipeline, and the solution that sees through filter membrane is got back to and continued loop ultrafiltration behind the enzymolysis in the ultrafiltration jar;
(5), nanofiltration concentrates: the ultrafiltrate weight that flows in the nanofiltration jar reaches 1.8～2.2 ton hours and adopts molecular weight cut-off less than 500 filter membrane nanofiltration; The filtrate that sees through nanofiltration membrane by in the pipeline input ultrafiltration jar as the diluent of ultrafiltration; Irritate total amount of liquid when ultrafiltration and reach 2.5 ton hours, nanofiltration filtrate is directly drained; The liquid that sees through nanofiltration membrane is not got back to the nanofiltration that circulates in the nanofiltration jar by pipeline; The ultra-filtration and separation process reaches terminal point when ultrafiltration pot liquid volume is 300～500L, stops ultrafiltration; The nanofiltration separation process reaches terminal point when nanofiltration pot liquid volume is 150～300 liters, stops nanofiltration;
(6), spraying drying: with the liquid spray drying in the nanofiltration jar.
The processing condition of described (6) one step spray-drying: 150～180 ℃ of inlet temperatures, 60～90 ℃ of temperature outs.
Advantage of the present invention is:
(1), select for use Sumizyme MP also by enzyme digestion reaction-separation coupling optimization order enzymolysis process, to adopt ultra-filtration membrane to remove the enzyme digestion reaction product be molecular weight less than 5000 Collagen Hydrolysate, change the enzymolysis balance, make enzyme digestion reaction more help carrying out to the hydrolysis direction, improve the transformation efficiency of substrate and the generating rate of product, enzyme digestion reaction is more abundant, product yield height.Save the go out technology of enzyme of high temperature, save the energy and raw material, and product do not had bitter taste.
(2), ultrafiltration removes molecular weight greater than 5000 the macromolecule Collagen Hydrolysate that is not easy to be absorbed by the body, reach the purpose of control molecular weight.
(3), adopt nanofiltration to concentrate and substitute the evaporating and concentrating process that generally adopts at present, not only molecular weight is removed at the small molecules Collagen Hydrolysate below 500, collagen peptide products molecule weight range is more met the requirements, and will comprise the diluent of molecular weight filtrate in the Collagen Hydrolysate solution below 500 is squeezed in the ultrafiltration jar as the ultrafiltration jar by pipeline, reach the purpose of recycling waste liquid, the conserve water resource reduces energy consumption and production costs.Further solved product bitter taste problem because of removing the small molecules Collagen Hydrolysate simultaneously.
(4), by this handling 100 kilograms of fresh pig skins technology pilot scale day, can produce 15 kilograms of hydrolytic collagen protein powders, product yield is at (pigskin is with dry weight basis) more than 60%.Year working days is by 200 days, 3 tons of annual production.Remarkable in economical benefits.And process using physical method and biologic treating technique, there are not any chemical additive and insalubrious material, guarantee product quality.And cut the Collagen Hydrolysate of macromolecule and small molecular weight by ultrafiltration and nanofiltration technique, and make the product molecular-weight average about 2000, more help absorption by human body.
The invention will be further described below in conjunction with embodiment for embodiment.
Embodiment 1
It is as follows with the pigskin to be that raw material is produced the technology of Collagen Hydrolysate:
(1), preparation work: with container and flushing of pipeline clean after, with softening water container and pipeline sky are walked one time.
(2), will to rectificate * wide≤1 * 1cm through the fresh food level pigskin chopping after the depilation degreasing without storage.
(3), enzymolysis: adding 1.5 tons of water and weight in wet base in reactor is the pigskin that 110kg shreds, and is steam heated to 60 ℃ under stirring, and adds 0.6Kg2709 proteolytic enzyme, and this moment, pH value was 8.0, and insulated and stirred reaction 4 hours has not had block cladding in the reactor at this moment.
(4), remove the solid particles thing: the reaction solution of (3) step reaction was left standstill 0.7 hour, and solid particles thing and oil layer are removed in the complete sedimentation of solid particles thing this moment;
(5), enzyme digestion reaction-separation coupling: the reaction solution that will remove behind solid particles thing and the oil layer is got in the ultrafiltration jar that is placed with 2 tons of softening waters, stir 17 minutes afterreaction liquid and flow into ultrafiltration in the ultrafiltration apparatus by the road, ultrafiltration apparatus adopts molecular weight cut-off greater than 5000 filter membrane ultra-filtration and separation; The filtrate that sees through ultra-filtration membrane enters in the nanofiltration jar by pipeline, gets back to through the solution of filter membrane and continues in the ultrafiltration jar to enter loop ultrafiltration in the ultrafiltration apparatus once more behind the enzymolysis;
(6), nanofiltration concentrates: the ultrafiltrate weight that flows in the nanofiltration jar reaches 2 ton hours, and ultrafiltrate flows in the nanofiltration equipment by the road, and nanofiltration equipment adopts molecular weight cut-off less than 500 filter membrane nanofiltration; The filtrate that sees through nanofiltration membrane by in the pipeline input ultrafiltration jar as the diluent of ultrafiltration; Irritate total amount of liquid when ultrafiltration and reach 2.5 ton hours, nanofiltration filtrate is directly drained; The liquid that sees through nanofiltration membrane is not got back to the nanofiltration that circulates in the nanofiltration jar by pipeline; The ultra-filtration and separation process reaches terminal point when ultrafiltration pot liquid volume is 400L, and this moment, ultrafiltration apparatus did not almost have flow, stopped ultrafiltration; The nanofiltration separation process reaches terminal point when nanofiltration pot liquid volume is 225L, and the flow of nanofiltration this moment equipment reduces half, stops nanofiltration;
(7), spraying drying: with the liquid spray drying in the nanofiltration jar, 170 ℃ of inlet temperatures, 80 ℃ of temperature outs.
(8), packing: the ultraviolet lamp sterilization packs.
Product is detected sense environmental conditions: 25 ℃ of temperature, humidity 60%, assay such as table one:
Table one
Embodiment 2
It is as follows with the sheepskin to be that raw material is produced the technology of Collagen Hydrolysate:
(1), preparation work: with container and flushing of pipeline clean after, with softening water container and pipeline sky are walked one time.
(2), will to rectificate * wide≤1 * 1cm through the fresh food level sheepskin chopping after the depilation degreasing without storage;
(3), enzymolysis: adding 1.5 tons of water and weight in wet base in reactor is the sheepskin that 100kg shreds, and is steam heated to 40 ℃ under stirring, and adds 0.3Kg1398 proteolytic enzyme, and this moment, pH value was 8.2, and insulated and stirred reaction 5 hours has not had block cladding in the reactor at this moment.
(4), remove the solid particles thing: the reaction solution of (3) step reaction was left standstill 0.5 hour, and solid particles thing and oil layer are removed in the complete sedimentation of solid particles thing this moment;
(5), enzyme digestion reaction-separation coupling: the reaction solution that will remove behind solid particles thing and the oil layer is got in the ultrafiltration jar that is placed with 2 tons of softening waters, stir 15 minutes afterreaction liquid and flow into ultrafiltration in the ultrafiltration apparatus by the road, ultrafiltration apparatus adopts molecular weight cut-off greater than 5000 filter membrane ultra-filtration and separation; The filtrate that sees through ultra-filtration membrane enters in the nanofiltration jar by pipeline, gets back to through the solution of filter membrane and continues in the ultrafiltration jar to enter loop ultrafiltration in the ultrafiltration apparatus once more behind the enzymolysis;
(6), nanofiltration concentrates: the ultrafiltrate weight that flows in the nanofiltration jar reaches 1.8 ton hours, and ultrafiltrate flows in the nanofiltration equipment by the road, and nanofiltration equipment adopts molecular weight cut-off less than 500 filter membrane nanofiltration; The filtrate that sees through nanofiltration membrane by in the pipeline input ultrafiltration jar as the diluent of ultrafiltration; Irritate total amount of liquid when ultrafiltration and reach 2.5 ton hours, nanofiltration filtrate is directly drained; The liquid that sees through nanofiltration membrane is not got back to the nanofiltration that circulates in the nanofiltration jar by pipeline; The ultra-filtration and separation process reaches terminal point when ultrafiltration pot liquid volume is 300L, and this moment, ultrafiltration apparatus did not almost have flow, stopped ultrafiltration; The nanofiltration separation process reaches terminal point when nanofiltration pot liquid volume is 150L, and the flow of nanofiltration this moment equipment reduces half, stops nanofiltration;
(7), spraying drying: with the liquid spray drying in the nanofiltration jar, 150 ℃ of inlet temperatures, 60 ℃ of temperature outs.
(8), packing: the ultraviolet lamp sterilization packs.
Product is detected sense environmental conditions: 25 ℃ of temperature, humidity 60%, assay such as table two:
Table two
Embodiment 3:
It is as follows with the ox-hide to be that raw material is produced the technology of Collagen Hydrolysate:
(1), preparation work: with container and flushing of pipeline clean after, with softening water container and pipeline sky are walked one time.
(2), will to rectificate * wide≤1 * 1cm through the fresh food level ox-hide chopping after the depilation degreasing without storage;
(3), enzymolysis: adding 1.5 tons of water and weight in wet base in reactor is the ox-hide that 120kg shreds, and is steam heated to 65 ℃ under stirring, and adds 1.2Kg2709 proteolytic enzyme, and this moment, pH value was 8.5, and insulated and stirred reaction 3 hours has not had block cladding in the reactor at this moment.
(4), remove the solid particles thing: the reaction solution of (3) step reaction was left standstill 1 hour, and solid particles thing and oil layer are removed in the complete sedimentation of solid particles thing this moment;
(5), enzyme digestion reaction-separation coupling: the reaction solution that will remove behind solid particles thing and the oil layer is got in the ultrafiltration jar that is placed with 2 tons of softening waters, stir 20 minutes afterreaction liquid and flow into ultrafiltration in the ultrafiltration apparatus by the road, ultrafiltration apparatus adopts molecular weight cut-off greater than 5000 filter membrane ultra-filtration and separation; The filtrate that sees through ultra-filtration membrane enters in the nanofiltration jar by pipeline, gets back to through the solution of filter membrane and continues in the ultrafiltration jar to enter loop ultrafiltration in the ultrafiltration apparatus once more behind the enzymolysis;
(6), nanofiltration concentrates: the ultrafiltrate weight that flows in the nanofiltration jar reaches 2.2 ton hours, and ultrafiltrate flows in the nanofiltration equipment by the road, and nanofiltration equipment adopts molecular weight cut-off less than 500 filter membrane nanofiltration; The filtrate that sees through nanofiltration membrane by in the pipeline input ultrafiltration jar as the diluent of ultrafiltration; Irritate total amount of liquid when ultrafiltration and reach 2.5 ton hours, nanofiltration filtrate is directly drained; The liquid that sees through nanofiltration membrane is not got back to the nanofiltration that circulates in the nanofiltration jar by pipeline; The ultra-filtration and separation process reaches terminal point when ultrafiltration pot liquid volume is 500L, and this moment, ultrafiltration apparatus did not almost have flow, stopped ultrafiltration; The nanofiltration separation process reaches terminal point when nanofiltration pot liquid volume is 300L, and the flow of nanofiltration this moment equipment reduces half, stops nanofiltration;
(7), spraying drying: with the liquid spray drying in the nanofiltration jar, 180 ℃ of inlet temperatures, 90 ℃ of temperature outs.
(8), packing: the ultraviolet lamp sterilization packs.
Product is detected sense environmental conditions: 25 ℃ of temperature, humidity 60%, assay such as table three:
Table three
Described Sumizyme MP is refined through submerged fermentation by Bacillus licheniformis and forms.
Ultrafiltration apparatus model: 1.5T/H, manufacturer: river, Qingzhou, Shandong one Water Management Equipment Ltd..
Nanofiltration unit type: 1.5T/H, manufacturer: river, Qingzhou, Shandong one Water Management Equipment Ltd..
Claims (2)
1. the method for a preparing hydrolyzed collagen protein by fresh animal skin is characterized in that: mainly comprise following processing step:
(1), animal skin pre-treatment: will be through the fresh food level animal skin chopping after the depilation degreasing, length * wide≤1 * 1cm without storage;
(2), enzymolysis: adding 1.5 tons of water and weight in wet base in reactor is the animal skin of 100～120kg chopping, is steam heated to 40～65 ℃ under stirring, and adds 0.3～1.2Kg Sumizyme MP, insulated and stirred reaction 3～5 hours;
(3), remove the solid particles thing: the reaction solution of (2) step reaction was left standstill 0.5～1 hour, remove solid particles thing and oil layer;
(4), enzyme digestion reaction-separation coupling: the reaction solution that will remove behind solid particles thing and the oil layer is got in the ultrafiltration jar that is placed with 2 tons of softening waters, stirs employing molecular weight cut-off after 15～20 minutes greater than 5000 filter membrane ultra-filtration and separation; The filtrate that sees through ultra-filtration membrane enters in the nanofiltration jar by pipeline, and the solution that sees through filter membrane is got back to and continued loop ultrafiltration behind the enzymolysis in the ultrafiltration jar;
(5), nanofiltration concentrates: the ultrafiltrate weight that flows in the nanofiltration jar reaches 1.8～2.2 ton hours and adopts molecular weight cut-off less than 500 filter membrane nanofiltration; The filtrate that sees through nanofiltration membrane by in the pipeline input ultrafiltration jar as the diluent of ultrafiltration; Irritate total amount of liquid when ultrafiltration and reach 2.5 ton hours, nanofiltration filtrate is directly drained; The liquid that sees through nanofiltration membrane is not got back to the nanofiltration that circulates in the nanofiltration jar by pipeline; The ultra-filtration and separation process reaches terminal point when ultrafiltration pot liquid volume is 300～500L, stops ultrafiltration; The nanofiltration separation process reaches terminal point when nanofiltration pot liquid volume is 150～300 liters, stops nanofiltration;
(6), spraying drying: with the liquid spray drying in the nanofiltration jar.
2. the method for preparing hydrolyzed collagen protein by fresh animal skin as claimed in claim 1 is characterized in that: the processing condition of (6) one step spray-drying: 150～180 ℃ of inlet temperatures, 60～90 ℃ of temperature outs.
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| CN102125251B (en) * | 2010-12-09 | 2012-08-29 | 南昌大学 | Preparation method of oligopeptide flavor enhancer by controllable enzymolysis proteins |
| CN105648011B (en) * | 2016-03-04 | 2019-05-17 | 沾化恒鑫工业科技有限公司 | A kind of method that combined-enzyme method hydrolysis prepares cow leather collagen |
| CN107915773A (en) * | 2016-10-11 | 2018-04-17 | 浙江崇山生物制品有限公司 | A kind of method of collagen purifying |
| CN106701878A (en) * | 2017-02-20 | 2017-05-24 | 青海师范大学 | Method for extracting yak skin collagen by adopting enzyme process |
| CN108912224A (en) * | 2018-03-28 | 2018-11-30 | 通化百泉保健食品有限公司 | A kind of industrialized producing technology of Pigskin Protein oligopeptide |
| CN109321624A (en) * | 2018-11-15 | 2019-02-12 | 安徽嘉润生物科技有限责任公司 | Enzymolysis process for preparing active collagen peptide from fresh pigskin |
| CN114516912B (en) * | 2022-04-07 | 2022-11-25 | 斐缦(长春)医药生物科技有限责任公司 | Hydrolyzed collagen and preparation method and application thereof |
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