CN102242176A - Method for processing collagen peptide by using fish leftovers - Google Patents
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Abstract
The invention relates to a method for processing collagen peptides by using fish leftovers, belonging to the technical fields of aquatic product processing and comprehensive utilization of aquatic product leftovers. In the method, the fish leftovers such as fishskins, scales and fish viscera are used as raw materials for carrying out high-valued development utilization. The method specially comprises the following steps: firstly respectively treating and mixing the raw materials so as to obtain a fish leftover mixture; and then promoting step-by-step enzymolysis with ultrasonic wave, killing enzyme, centrifugalizing, decoloring, filtrating, carrying out reinforcing membrane separation with ultrasonic wave and nano filtrating and freeze drying so as to obtain collagen peptides with different molecular weights. According to the invention, the enzymolysis and membrane separation processes are promoted through ultrasonic wave, enzyme adding amount is less, enzymolysis time is short, production efficiency is high, and the obtained products with different molecular weights has no odor, is light in color, and can be used in industries such as medicaments, health products, food and the like.
Description
Technical field
The present invention relates to the processing of aquatic products technology, the tankage that particularly utilize fish to process prepare the method for collagen peptide.The invention belongs to processing of aquatic products and tankage comprehensive utilization technique field thereof.
Background technology
China's fish resource distributes wide, and kind is many, and output is big, but the deep process technology level is lower, how to be processed as the master with workshop-based craft, and processing variety is the freezing and bright fishery products of ice based on low value still, and primary processed items is many, and deep processed product is few; Technology content and added value of products is all very low, and high value-added product is few, and the tankage level of comprehensive utilization is not high, even it is abandoned.In fact, fish scrap both can be turned waste into wealth through processing, comprehensive utilization, can avoid contaminate environment again, also was the effective way that enterprise's synergy, fishman increase income.People are when processing or food fish, the shared proportion of tankage is quite big, is example with the paddlefish, decaptitates, peeling, magnetic tape trailer weight be 47.3% of fish body gross weight, 33.5% of fillet percentage of liveweight is lower than striped perch (40.0%), squid (45.7%), rainbow trout (57.5%).The major cause that yields poorly is that it accounts for the spoon kiss of total length 40.0%, and internal organ account for 9.0%, and fish-skin accounts for 1.5%.For another example, be processed into sushi sashimi with pagrosomus fish, ratio defective product is 25.0%-35.0% only usually, and tankage account for major part.At present domestic mainly is to be processed into feed or directly to abandon to the fish scrap utilization, and utility value is not very high, has brought pollution to environment simultaneously yet.And developed country can make full use of its tankage, creates good economic benefit and comprehensive social benefit.
Owing to contain amounts of protein in the fish-skin, what wherein content was maximum is type i collagen albumen, the highest 80.0% of its total protein that surpasses, collagen content is also abundanter in fish scale, the fish viscera in addition, its molecule has unique triple-helix structure, if it is not effectively handled, not only contaminate environment has also been wasted a large number of nutrients.
Collagen protein is the rich in protein of people's in-vivo content, accounts for 1/3rd of whole body gross protein.The collagen protein source is abundant, and some contain gelationus food, all contain collagen protein as Ungula Bovis seu Bubali muscle, pig's feet, fish-skin etc.But because causes such as mad cow disease, foot and mouth disease are very limited for the feedstock production collagen peptide with Lu Sheng, raw material turns to based on hydrocoles, and composition structure and the human body of fish are the most approaching, is the collagen protein source that tissue institute identification the most absorbs.
The collagen molecules amount is generally 50000～100000Dalton, and human body can not effectively absorb, and has only its enzymolysis is become collagen peptide (molecular weight＜3000Dalton), just can be by human body active and accessible absorption, need not digestion, make full use of, bring into play its function for bodily tissue.Collagen peptide can promote the formation of bone, strengthens the osso-albumin structure under the low calcium level, thereby has improved bone strength, has promptly reached the effect of preventing osteoporosis disease; Collagen peptide also has other many special physiological functions in addition; as protect stomach mucous membrane and antiulcer action, anti-allergic effects etc.; what need proposition especially is; the effect of collagen peptide aspect beauty treatment; timely replenishing collagen peptide; for improving the skin problem, delay senility, extraordinary effect is arranged.
The present invention utilizes fish offal material processed collagen protein peptide, and ultrasonic technology is applied to the ultra-filtration and separation process of the enzymolysis and the product thereof of neutral protease, flavor protease, adopts different membrane separation techniques to produce serial collagen peptide product.The invention has the advantages that: enzymolysis time is short, the production efficiency height, and enzyme concentration is few, and the ultra-filtration membrane flux is big, and the series product free from extraneous odour that obtains, and lighter color can be widely used in industries such as medicine, healthcare products, food.Enforcement of the present invention not only can reduce or avoid discarded environmental pollution that is caused of fish offal material and the waste of a large number of nutrients, and can turn waste into wealth, the exploitation high value added product, drive the development of processing of aquatic products industry and related industries, have remarkable economic efficiency, social benefit and ecological benefits.
Summary of the invention
The present invention relates to the processing of aquatic products technology, particularly utilize the method for fish offal material processed collagen protein peptide.The present invention is to be raw material with fish-skin, fish scale, fish viscera, handles the back respectively and mixes and obtaining the fish offal material mixture, adopts ultrasonic wave to promote the substep enzymolysis, the heating enzyme that goes out, and activated carbon decolorizing obtains primary products.Adopt membrane separation technique to carry out separation and purification then, select for use intensified by ultrasonic wave membrane sepn, nanofiltration, lyophilize to make the collagen peptide product of different molecular weight successively.
Utilize the method for fish offal material processed collagen protein peptide, its concrete operations step is as follows:
1. the preparation of fish offal material mixture is at first handled fish-skin, fish scale, fish viscera respectively, to take out foreign protein, is beneficial to the stripping of collagen protein.Fish-skin through thaw, clean, shred, quality for its 0.1mol/LNaOH of 20 times soak 2h, clean standby; Fish scale through thaw, cleaning, quality for its 0.4mol/LHCL of 20 times soak 2h, quality for its 0.1mol/LNaOH of 20 times soak 2h, clean standby; Fish viscera is standby through thawing, clean, rubbing; It is standby that fish offal material mixing after will handling respectively then obtains fish offal material mixture mixing.
2. ultrasonic wave promotes that neutral protease enzymolysis takes by weighing an amount of fish offal material mixture, adds deionized water, and making solid-to-liquid ratio is 1: 2.Ultrasonic frequency is 20kHz～40kHz, and power is 100W～400W, and regulating initial pH value is 7.0～7.5, and enzyme concentration is 0.01%～0.15%, and hydrolysis temperature is 45～55 ℃, and enzymolysis time is 30min～100min.
3. ultrasonic wave promotes the food flavor enzyme enzymolysis behind neutral protease enzymolysis, adds an amount of food flavor enzyme again and carries out further enzymolysis.Regulating initial pH value is 6.0～6.5, and enzyme concentration is 0.01%～0.15%, and hydrolysis temperature is 45～55 ℃, and enzymolysis time is 30min～100min.The ultrasonic wave parameter constant.
4. after the enzyme substep enzymolysis that goes out finishes, enzymolysis solution is heated to 85～90 ℃, keeps 10min～20min, heat the enzyme that goes out.
5. centrifugation is gone out and is carried out centrifugation behind the enzyme, removes lower floor's material, collects supernatant liquid.Whizzer adopts helical conveyor centrifuge, and rotating speed is rotating speed 3500～4000r/min, centrifugation time 10min～15min.
6. activated carbon decolorizing supernatant liquor that centrifugation is obtained adds the processing of decolouring of an amount of gac.The activated carbon particle size that is adopted is 1mm～2mm, and addition is 0.1%～5% of a solvent volume, and bleaching temperature is 55～85 ℃, and bleaching time is 30min～50min.
7. the supernatant liquor that will filter after will decolouring filters with 200 orders～400 order filter materials, removes gac.Equipment adopts flame filter press or vacuum filter.
8. the intensified by ultrasonic wave membrane sepn adopts ultra-filtration membrane to carry out separation and purification above-mentioned collagen peptide liquid, uses intensified by ultrasonic wave in the membrane sepn process.Its ultrasonic frequency is 20kHz～100kHz, power is 200W～800W, selecting molecular weight cut-off successively for use is that the ultra-filtration membrane of 10000Dalton, 3000Dalton, 1000Dalton carries out ultrafiltration, obtains the collagen protein peptide prod of 3000～10000Dalton, 1000～3000Dalton, the following 3 kinds of molecular weight range of 1000Dalton.
9. nanofiltration is further carried out membrane sepn again with the collagen protein peptide prod below the 1000Dalton, adopts the nanofiltration membrane separation technology.Adopting molecular weight cut-off successively is that the nanofiltration membrane of 800Dalton, 600Dalton, 400Dalton is carried out nanofiltration, obtains the collagen protein peptide prod of 800～1000Dalton, 600～800Dalton, the following 4 kinds of small molecules mass ranges of 400～600Dalton, 400Dalton.
10. the collagen protein peptide prod of lyophilize differing molecular mass range that membrane separation technique is obtained carries out lyophilize, obtains series product.
Description of drawings
Accompanying drawing is a process flow sheet of the present invention.
Embodiment
Example one
1. the preparation of fish offal material mixture is at first handled fish-skin, fish scale, fish viscera respectively, to take out foreign protein, is beneficial to the stripping of collagen protein.Fish-skin through thaw, clean, shred, quality for its 0.1mol/LNaOH of 20 times soak 2h, clean standby; Fish scale through thaw, cleaning, quality for its 0.4mol/LHCL of 20 times soak 2h, quality for its 0.1mol/LNaOH of 20 times soak 2h, clean standby; Fish viscera is standby through thawing, clean, rubbing; It is standby that fish offal material mixing after will handling respectively then obtains fish offal material mixture mixing.
2. ultrasonic wave promotes neutral protease enzymolysis to take by weighing the fish offal material mixture after 20g handles, and adds the 40mL deionized water.Ultrasonic frequency is for selecting 40kHz, and power is 200W, and regulating initial pH value is 7.0, and enzyme concentration is 0.05%, and hydrolysis temperature is 50 ℃, and enzymolysis time is 60min.
3. ultrasonic wave promotes the food flavor enzyme enzymolysis to carry out further enzymolysis through adding an amount of food flavor enzyme in the zymolyte behind the neutral protease enzymolysis.Regulating initial pH value is 6.5, and enzyme concentration is 0.05%, and hydrolysis temperature is 50 ℃, and enzymolysis time is 60min.The ultrasonic wave parameter remains unchanged.
4. after the enzyme substep enzymolysis that goes out finishes, carry out the water-bath enzyme that goes out.Bath temperature is selected 90 ℃ for use, and the enzyme time of going out is 15min.
5. centrifugation is gone out and is carried out centrifugation behind the enzyme, removes lower floor's material, collects supernatant liquid.Whizzer adopts helical conveyor centrifuge, and rotating speed is rotating speed 3500r/min, centrifugation time 15min, and behind centrifugal the finishing, it is standby to collect supernatant liquid.
6. activated carbon decolorizing supernatant liquor that centrifugation is obtained adds the processing of decolouring of an amount of gac.The activated carbon particle size that is adopted is 1mm, and addition is 1.0% of a solvent volume, and bleaching temperature is 75 ℃, and bleaching time is 30min.
7. the supernatant liquor that will filter after will decolouring filters with 400 order filter materials, removes gac.Equipment adopts flame filter press.
8. the intensified by ultrasonic wave membrane sepn adopts ultra-filtration membrane to carry out separation and purification above-mentioned collagen peptide liquid, uses intensified by ultrasonic wave in the membrane sepn process.Its ultrasonic frequency is 20kHz, power is 400W, selecting molecular weight cut-off successively for use is that the ultra-filtration membrane of 10000Dalton, 3000Dalton, 1000Dalton carries out ultrafiltration, obtains the collagen protein peptide prod of 3000～10000Dalton, 1000～3000Dalton, the following 3 kinds of molecular weight range of 1000Dalton.
9. nanofiltration is further carried out membrane sepn again with the collagen protein peptide prod below the 1000Dalton, adopts the nanofiltration membrane separation technology.Adopting molecular weight cut-off is the 800Dalton nanofiltration membrane separation, obtains the collagen protein peptide prod of the following 2 kinds of small molecules mass ranges of 800～1000Dalton, 800Dalton.
10. the collagen protein peptide prod of lyophilize differing molecular mass range that membrane separation technique is obtained carries out lyophilize, obtains product.
Example two
1. the preparation of fish offal material mixture is at first handled fish-skin, fish scale, fish viscera respectively, to take out foreign protein, is beneficial to the stripping of collagen protein.Fish-skin through thaw, clean, shred, quality for its 0.1mol/LNaOH of 20 times soak 2h, clean standby; Fish scale through thaw, cleaning, quality for its 0.4mol/LHCL of 20 times soak 2h, quality for its 0.1mol/LNaOH of 20 times soak 2h, clean standby; Fish viscera is standby through thawing, clean, rubbing; It is standby that fish offal material mixing after will handling respectively then obtains fish offal material mixture mixing.
2. ultrasonic wave promotes neutral protease enzymolysis to take by weighing the fish offal material mixture after 20g handles, and adds the 40ml deionized water.Ultrasonic frequency is for selecting 40kHz, and power is 400W, and regulating initial pH value is 7.0, and enzyme concentration is 0.1%, and hydrolysis temperature is 55 ℃, and enzymolysis time is 100min.
3. ultrasonic wave promotes an amount of food flavor enzyme of the adding of food flavor enzyme enzymolysis behind neutral protease enzymolysis to carry out further enzymolysis.Regulating initial pH value is 6.5, and enzyme concentration is 0.1%, and hydrolysis temperature is 55 ℃, and enzymolysis time is 100min.The ultrasonic wave parameter constant.
4. after the enzyme substep enzymolysis that goes out finishes, carry out the water-bath enzyme that goes out.Bath temperature is selected 85 ℃ for use, and the enzyme time of going out is 20min.
5. centrifugation is gone out and is carried out centrifugation behind the enzyme, removes lower floor's material, collects supernatant liquid.Whizzer adopts helical conveyor centrifuge, and rotating speed is rotating speed 4000r/min, centrifugation time 15min.
6. activated carbon decolorizing supernatant liquor that centrifugation is obtained adds the processing of decolouring of an amount of gac.The activated carbon particle size that is adopted is 2mm, and addition is 1.5% of a solvent volume, and bleaching temperature is 55 ℃, and bleaching time is 50min.
7. the supernatant liquor that will filter after will decolouring filters with 200 order filter materials, removes gac.Equipment adopts flame filter press.
8. the intensified by ultrasonic wave membrane sepn adopts ultra-filtration membrane to carry out separation and purification above-mentioned collagen peptide liquid, uses intensified by ultrasonic wave in the membrane sepn process.Its ultrasonic frequency is 800W for 20kHz power, selecting molecular weight cut-off successively for use is that the ultra-filtration membrane of 10000Dalton, 3000Dalton, 1000Dalton carries out ultrafiltration, obtains 3000～10000Dalton, 1000～3000Dalton, the following 3 kinds of collagen protein peptide prods than the macromole mass range of 1000Dalton.
9. nanofiltration is further carried out membrane sepn again with the collagen protein peptide prod below the 1000Dalton, adopts the nanofiltration membrane separation technology.Adopting molecular weight cut-off successively is that the nanofiltration membrane of 800Dalton, 600Dalton, 400Dalton is carried out nanofiltration, obtains the collagen protein peptide prod of 800～1000Dalton, 600～800Dalton, the following 4 kinds of small molecules mass ranges of 400～600Dalton, 400Dalton.
10. the collagen protein peptide prod of lyophilize differing molecular mass range that membrane separation technique is obtained carries out lyophilize, obtains product.
Claims (8)
1. utilize the method for fish offal material processed collagen protein peptide, handle fish-skin, fish scale, fish viscera at first respectively, then its mixing is obtained the fish offal material mixture, make product according to following technological process then: ultrasonic wave promotes neutral protease enzymolysis, ultrasonic wave to promote food flavor enzyme enzymolysis, the enzyme that goes out, centrifugation, activated carbon decolorizing, filtration, intensified by ultrasonic wave membrane sepn, nanofiltration, lyophilize.
2. the method for utilizing fish offal material processed collagen protein peptide as claimed in claim 1 is characterized in that above-mentioned fish offal material mixture is is raw material with fish-skin, fish scale, fish viscera, according to its characteristic, is mixed and made into after handling respectively; Fish-skin by thaw, clean, shred, alkaline purification, cleaning be standby; Fish scale by thaw, cleaning, acid treatment, alkaline purification, cleaning be standby; Fish viscera is standby by thawing, clean, rubbing.
3. the method for utilizing fish offal material processed collagen protein peptide as claimed in claim 1, it is characterized in that: described ultrasonic wave promotes neutral protease enzymolysis, its ultrasonic frequency is 20kHz～40kHz, power is 100W～400W, enzyme concentration is 0.01%～0.15% of a material gross weight, pH is 7.0～7.5 during enzymolysis, and hydrolysis temperature is 45～55 ℃, and enzymolysis time is 30min～100min.
4. the method for utilizing fish offal material processed collagen protein peptide as claimed in claim 1, it is characterized in that: described ultrasonic wave promotes the food flavor enzyme enzymolysis, its ultrasonic frequency is 20kHz～40kHz, power is 100W～400W, enzyme concentration is 0.01%～0.15% of a material gross weight, pH is 6.0～6.5 during enzymolysis, and temperature is 45～55 ℃ during enzymolysis, and enzymolysis time is 30min～100min.
5. the method for utilizing fish offal material processed collagen protein peptide as claimed in claim 1 is characterized in that: the described enzyme that goes out adopts and heats the enzyme that goes out, and enzyme-removal temperature is 85～90 ℃, and the enzyme time of going out is 10min～20min.
6. the method for utilizing fish offal material processed collagen protein peptide as claimed in claim 1, it is characterized in that: described decolouring is to adopt activated carbon decolorizing, the activated carbon particle size of selecting for use is 1mm～2mm, addition is 0.1%～5% of a solvent volume, bleaching temperature is 55～85 ℃, and bleaching time is 30min～50min.
7. the method for utilizing fish offal material processed collagen protein peptide as claimed in claim 1, it is characterized in that: described intensified by ultrasonic wave membrane sepn, its ultrasonic frequency is 20kHz～100kHz, power is 200W～800W, the molecular weight cut-off of film is respectively 1000Dalton, 1000～3000Dalton, 3000～10000Dalton, obtains the collagen protein peptide prod of 3000～10000Dalton, 1000～3000Dalton, the following 3 kinds of molecular weight range of 1000Dalton.
8. the method for utilizing fish offal material processed collagen protein peptide as claimed in claim 1, it is characterized in that: described nanofiltration, the molecular weight cut-off of its film is respectively 800Dalton, 600Dalton, 400Dalton, can obtain the collagen protein peptide prod of 800～1000Dalton, 600～800Dalton, the following 4 kinds of small molecules mass ranges of 400～600Dalton, 400Dalton.
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| CN102492761A (en) * | 2011-12-02 | 2012-06-13 | 安徽燕之坊食品有限公司 | Method for preparing active polypeptide from fish pomace |
| CN102613383A (en) * | 2012-04-24 | 2012-08-01 | 天津春宇食品配料有限公司 | Fish scale protein enzymolysis liquid and preparation method thereof |
| CN102987376A (en) * | 2012-07-24 | 2013-03-27 | 刘含光 | Method for preparing collagen peptide oral liquid |
| CN103315127A (en) * | 2013-06-24 | 2013-09-25 | 诸城绿维食品有限公司 | Method for preparing casing by extracting offal collagen corpus fibrosum of aquatic product |
| CN103773828A (en) * | 2012-10-23 | 2014-05-07 | 李丹榕 | Method for extraction of collagen from fish scale |
| CN103993061A (en) * | 2014-05-20 | 2014-08-20 | 海南美合泰生物科技有限公司 | Production method of fish collagen |
| CN104232713A (en) * | 2013-06-24 | 2014-12-24 | 诸城绿维食品有限公司 | Sewage treatment process for extracting collagen corpus fibrosum from aquatic product leftovers by virtue of enzymolysis method |
| CN104762283A (en) * | 2015-04-23 | 2015-07-08 | 海南大学 | Separation method of visceral protease in golden pomfret and protease as well as application |
| CN104946711A (en) * | 2014-03-27 | 2015-09-30 | 苏州吉利鼎海洋生物科技有限公司 | Production process of collagen |
| CN105054132A (en) * | 2015-08-13 | 2015-11-18 | 江苏省农业科学院 | Fish scale jelly production process |
| CN106563686A (en) * | 2016-10-21 | 2017-04-19 | 河南农业大学 | A method of subjecting livestock and poultry died of disease to ultrasonic enzymatic hydrolysis |
| CN107338278A (en) * | 2017-08-10 | 2017-11-10 | 江苏大学 | The method that ultrasonic in combination simulation digestion prepares collagen gel antioxidation polypeptide liquid |
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Application publication date: 20111116 |