CN102936611B - Collagen extracted from black butterflyfish skins with scales and application of collagen - Google Patents
Collagen extracted from black butterflyfish skins with scales and application of collagen Download PDFInfo
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- CN102936611B CN102936611B CN201210449583.7A CN201210449583A CN102936611B CN 102936611 B CN102936611 B CN 102936611B CN 201210449583 A CN201210449583 A CN 201210449583A CN 102936611 B CN102936611 B CN 102936611B
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Abstract
The invention relates to the technical field of collagen extraction from living bodies and particularly relates to collagen extracted from black butterflyfish skins with scales. The black butterflyfish skins with the scales are washed and then cut to be in a minced shape, the minced skins are immersed in sodium hydroxide, then sequentially filtered, washed to be neutral, filtered and extracted by using compound enzyme, the compound enzyme is composited by pepsin, papain and Alcalase compound protease according to an activity ratio of 1:1:2, the total activity is 0.04-0.08IU/g, the extraction time is 3-5 hours, the temperatures are between 40 DEG C and 60 DEG C, the power of hydrogen (PH) is 4-8, and the feed liquid ratio is 1: (8-15). The collagen is used in an adhesive in production of boneless fish. The compound enzyme is used for extracting the collagen from the black butterflyfish skins with the scales, the extraction rate is guaranteed, and simultaneously, the viscosity of the collagen is high; the collagen is used in the adhesive in production of the boneless fish and is ecological, environment-friendly and cost-saving; and the extracted collagen is used in the food adhesive, is safe and good in adhesion performances and free of peculiar smell and tastes good.
Description
Technical field
The present invention relates to collagen extraction techniques field in organism, particularly a kind of collagen extracted from the black sole skin of band squama, also relates to the application of described collagen.
Background technology
Collagen is a kind of important functional protein, and it and hyperplasia, differentiation, motion, immunity, joint lubrication, calcification, wound healing, organ support, body protective etc. is closely related, have caused now the extensive concern of people.Due to the biological function that it is special, its extract has been widely used in the various fields such as medicine, food, daily-use chemical industry, biosynthesis, as manufactured capsule for medicine, operation material, edible gelatin, photographic gelatin, cosmetics etc.
Collagen, gelatin, collagen (polypeptide) are three nouns easily obscured.Collagen refers to the natural a kind of structural protein be present in organism, containing the triple-helix structure region that one or several is made up of α-chain, molecular weight is about 300KD, it is extracted rear reservation triple-helix structure, in physiological conditions can spontaneous formation threadiness space higher structure, be insoluble to cold water and hot water, can not be utilized by protease, its goods are mainly used in medical biotechnology material.Gelatin is the collagen of sex change, and namely it has lost collagen original specific triple helix space structure, and range of molecular weight distributions broadens, 15KD-250KD, is insoluble to cold water but is dissolved in hot water, not having biologically active, have gelation, its goods are mainly used in food, daily-use chemical industry industry.Collagen (polypeptide) is the catabolite of collagen, and the triple-helix structure of collagen thoroughly unclamps and is degraded into polydisperse peptide section, and it is mixtures of polypeptides, and range of molecular weight distributions is very wide, several thousand to several ten thousand, and cold water solubles.Inventionbroadly gelatin also belongs to collagen, and just its molecular weight is larger.
The current raw material for the production of collagen goods is all skin and the bone of the terrestrial animal such as pig, ox substantially, and collagen extracts research and mainly concentrates on the edible adhesion agent of preparation, gel.The outburst of the zoonosis such as rabid ox disease in recent years and popular, make the security of the collagen goods of livestock products animal origin be subject to extensive query, many developed countries have prohibitted the use the collagen goods extracted from ox-hide and ox bone.
According to statistics, China's aquatic products annual production in recent years more than all more than 4,500 ten thousand tons, and the discarded object total amount of annual fish just reaches more than 200 ten thousand tons.As everyone knows, fish-skin, fish scale and fish-bone are the main discarded objects that aquatic products processing produces, and these discarded objects account for the 40-55% of raw material fish quality.If do not carry out effective disposal and utilization for these discarded objects, not only can cause the pollution of environment, also can waste a large amount of precious resources.It is reported, fish-skin, fish-bone are directly sold fish meal processing enterprise by current aquatic products processing enterprise, cheap.In fact contain a large amount of collagen in fish-skin, fish scale and fish-bone, in fish body, the collagen distribution of about 80% is in fish-skin, fish scale and fish-bone, as in fish-skin, collagen content is about 20%, and the collagen about containing about 50% in fish scale.If by the collagen extraction in these discarded objects out, there is considerable economic benefit.Therefore extract from raw materials of marine products and obtain safety, health, harmless collagen goods have market prospects widely.
Black sole skin removing moisture is protein substantially entirely, and fat, carbohydrate and content of ashes are very low.The collagen that protein accounts for fish-skin dry weight accounts for 98.91% of total protein content, and collagen accounts for 83.75% of protein, so fish-skin is the very good material of collagen extraction.Due to fat content trace in black sole skin, so need not special ungrease treatment be carried out in collagen leaching process.
Protein and ash content are the main components of black sole squama, and sum of the two exceedes 80% of fish scale gross weight.In fish scale, protein is primarily of collagen and scleroprotein composition, and wherein collagen accounts for 92.86% of total protein content, and visible fish scale is also the good source of collagen.Containing abundant inanimate matter in fish scale, mainly exist in the form of as hydroxyapatite, calcareous containing what enrich.Because the collagen in fish scale and hydroxyapatite are combined closely, form fine and close structure, scleroprotein also shields on surface simultaneously, and the existence of both may affect the extraction of collagen.
Also the report extracting collagen from fish skin and scale is had in prior art, the such as patent No. is the Chinese invention patent of 200610036860.6, disclose and add n-hexane in Java tilapia skin, remove foreign protein by NaOH solution after degreasing, then extract the method for collagen with acetum.Application number be 200410071942.5 Chinese invention patent application disclose remove fat and impurity after, alkali protease and acidity and neutral proteinase synergetic hydrolysis is used to obtain the method for collagen, but its for scope be ocean fish skin and freshwater fishskin, different fish-skins, composition is different, and those skilled in the art are difficult to that all fish-skins of prediction make in this way can successfully and the extraction collagen of high extraction.
Summary of the invention
In order to solve above from fish-skin, fish scale, extract collagen method unicity and recovery rate low, do not have the problem extracted collagen and record from black sole skin and fish scale, the invention provides a kind of collagen extracted from the black sole skin of band squama.
Present invention also offers the application of the described collagen extracted from the black sole skin of band squama.
The present invention is achieved by the following measures:
The collagen extracted from the black sole skin of band squama, is obtained by following steps:
After being with the black sole skin cleaning of squama, cut to rotten shape, by soaking with sodium hydroxide, filter, be washed till neutrality, filter, with multiplex-enzyme extraction, complex enzyme is pepsin, papain and Alcalase compound protease are composited according to activity ratio 1:1:2, total activity is 0.04-0.08 IU/g, and extraction time is 3-5 hour, and temperature is 40-60 DEG C, pH is 4-8, and solid-liquid ratio is 1:8-15.
Alcalase is the compound protease that Novozymes Company of Denmark produces, and be widely used in the extraction of collagen in recent years, have stronger hydrolysis ability to collagen, can destroy triple helix structure, thus collagen space structure is disintegrated, collagen recovery rate is very high.
Described collagen, extraction time is 4 hours, and temperature is 50 DEG C, and pH is 6, and solid-liquid ratio is 1:12.
Described collagen, complex enzyme total activity is 0.06IU/g.
Described collagen, the black sole skin of band squama cut to rotten shape uses the 0.1M soaking with sodium hydroxide 12h of 10 times of volumes.
Described collagen is used for without the adhesive in bone sashimi (raw fish) product.
Because the mass fraction of fish scale and fish-skin is approximately 18% and 82%, so recovery rate depends primarily on fish-skin.
Beneficial effect of the present invention: the collagen that the present invention extracts from band squama black sole skin is while guarantee recovery rate, and the collagen viscosity of extraction is high, is used in without the adhesive in bone sashimi (raw fish) product, not only ecological, environmental protective but also cost-saving; Use multiplex-enzyme extraction, while ensureing recovery rate, also obtain the high collagen of viscosity as far as possible.The collagen extracted is used for food adhesive, and bond properties is good, free from extraneous odour, and mouthfeel is good, safety.
Detailed description of the invention
For a better understanding of the present invention, further illustrate below in conjunction with specific embodiment.
embodiment 1:
The collagen extracted from the black sole skin of band squama, is obtained by following steps:
After being with the black sole skin cleaning of squama, cutting to rotten shape, soak with sodium hydroxide solution, filter, be washed till neutrality, filter, with multiplex-enzyme extraction, complex enzyme is pepsin, papain and Alcalase compound protease are composited according to activity ratio 1:1:2, total activity is 0.04IU/g, and extraction time is 5 hours, and temperature is 40 DEG C, pH is 4, and solid-liquid ratio is 1:15.
The black sole skin of band squama cut to rotten shape uses the 0.1M soaking with sodium hydroxide 12h of 10 times of volumes, and what use other concentration is also to realize.
Measuring recovery rate is 88.8%.
embodiment 2:
The collagen extracted from the black sole skin of band squama, is obtained by following steps:
After being with the black sole skin cleaning of squama, cutting to rotten shape, soak with sodium hydroxide solution, filter, be washed till neutrality, filter, with multiplex-enzyme extraction, complex enzyme is pepsin, papain and Alcalase compound protease are composited according to activity ratio 1:1:2, total activity is 0.08IU/g, and extraction time is 3 hours, and temperature is 60 DEG C, pH is 8, and solid-liquid ratio is 1:8.
Measuring recovery rate is 90.7%.
embodiment 3:
The collagen extracted from the black sole skin of band squama, is obtained by following steps:
After being with the black sole skin cleaning of squama, cutting to rotten shape, soak with sodium hydroxide solution, filter, be washed till neutrality, filter, with multiplex-enzyme extraction, complex enzyme is pepsin, papain and Alcalase compound protease are composited according to activity ratio 1:1:2, total activity is 0.06IU/g, and extraction time is 4 hours, and temperature is 50 DEG C, pH is 6, and solid-liquid ratio is 1:12.
Measuring recovery rate is 92.0%.
comparative example 1:
Compared with embodiment 3, only use pepsin to extract, all the other process conditions are completely the same with embodiment 3.Recovery rate is 35.6%.
comparative example 2:
Compared with embodiment 3, only use papain to extract, all the other process conditions are completely the same with embodiment 3.Recovery rate is 42.6%.
comparative example 3:
Compared with embodiment 3, only use Alcalase compound protease to extract, all the other process conditions are completely the same with embodiment 3.Recovery rate is 65.6%.
one, characteristic viscosity determining
Because collagen of the present invention is for food adhesive, so extraction process not only will consider recovery rate, also its functional characteristic and viscosity should be considered.
Ubbelohde viscosimetry is adopted to measure.Temperature is 25 ± 0.05 DEG C, gets the collagen powder 0.5g after the freeze-drying that the various embodiments described above and comparative example obtain, water-soluble, is settled to 100ml.Measure 1,2/3,1/2 concentration time delivery time, take aqueous solvent as contrast.
Computing formula is: specific viscosity η
sp=t/t
0-1
Reduced viscosity η
spthe specific viscosity that/C is extrapolated to when concentration is zero is inherent viscosity,
I.e. [η]=Lim
c → 0η
sp/ C.
In formula, t is the sample delivery time, t
0for the solvent delivery time, C is sample concentration.
Each embodiment inherent viscosity data are as shown in the table.
| Sequence number | Collagen concentration (g/ml) | Intercept D | Inherent viscosity [η] (dl/g) |
| Embodiment 1 | 0.005175 | 0.9156 | 2.1983 |
| Embodiment 2 | 0.005098 | 0.9502 | 2.1606 |
| Embodiment 3 | 0.005033 | 0.9843 | 2.2039 |
| Comparative example 1 | 0.005126 | 0.8769 | 1.9629 |
| Comparative example 2 | 0.004962 | 0.1201 | 0.2301 |
| Comparative example 3 | 0.005219 | 0.0112 | 0.0222 |
As can be seen from the above experimental data, the collagen yield of embodiment 3 is high, inherent viscosity is high, secondly be embodiment 2 and embodiment 1, the recovery rate of comparative example 1,2,3 and inherent viscosity are not satisfactory, so adopt the complex enzyme of pepsin, papain and Alcalase compound protease composition to carry out collagen extraction to band squama fish-skin, effect is satisfactory.
two, bond properties test
2.1 laboratory sample
Sample: the domestic tongue sole after processing without bone, fish temperature is lower than 10 DEG C.
Adhesive: the collagen extracted in the various embodiments described above, commercial organic binder (Japanese import).
experimental technique
Adhesive is evenly put on fish body section, takes the method for cold water bag pressure that fish body is bonded.
Cold water bag pressure 1.5 kg cold water/kg fish, bonding time 40min, binder dosage is 0.5 g/dm
2.
experimental result
Use embodiment 1, after adhesive that collagen that embodiment 2, comparative example 1 obtain is obtained and commodity in use adhesive, two panels difficult drop-off, split in after fried or boiling rear section, local monolithic is curling.
After the adhesive that the collagen using embodiment 3 to obtain is obtained, after bonding rear and fried or boiling, two panels all bonds closely.
After the adhesive that the collagen using comparative example 2 and comparative example 3 to obtain is obtained, after bonding, two panels comes off soon, after fried or into two pieces especially after boiling.
In addition after commercial organic binder bonding, product can taste the taste of adhesive, and the adhesive that the collagen extracted obtains does not have this shortcoming.
For the use situation of fish processing industry adhesive, propose the thinking utilizing the black sole skin of aquatic products processing discarded object band squama to produce adhesive, both solved the problem of the comprehensive utilization of discarded object, and met again the needs of the adhesive of safe source.Consider recovery rate and viscosity two evaluation indexes, the recovery rate obtained is up to 92%, and inherent viscosity is 2.2.The bond properties of product is slightly better than commercial organic binder, so the present invention is with a wide range of applications.
Claims (3)
1. the collagen extracted from the black sole skin of band squama, for the application without the adhesive in bone sashimi (raw fish) product, is characterized in that described collagen is obtained by following steps:
After being with the black sole skin cleaning of squama, cut to rotten shape, with the 0.1M soaking with sodium hydroxide 12h of 10 times of volumes, filter, be washed till neutrality, filter, with multiplex-enzyme extraction, complex enzyme is pepsin, papain and Alcalase compound protease are composited according to activity ratio 1:1:2, total activity is 0.04IU/g, and extraction time is 5 hours, and temperature is 40 DEG C, pH is 4, and solid-liquid ratio is 1:15.
2. the collagen extracted from the black sole skin of band squama, for the application without the adhesive in bone sashimi (raw fish) product, is characterized in that described collagen is obtained by following steps:
After being with the black sole skin cleaning of squama, cut to rotten shape, with the 0.1M soaking with sodium hydroxide 12h of 10 times of volumes, filter, be washed till neutrality, filter, with multiplex-enzyme extraction, complex enzyme is pepsin, papain and Alcalase compound protease are composited according to activity ratio 1:1:2, total activity is 0.08IU/g, and extraction time is 3 hours, and temperature is 60 DEG C, pH is 8, and solid-liquid ratio is 1:8.
3. the collagen extracted from the black sole skin of band squama, for the application without the adhesive in bone sashimi (raw fish) product, is characterized in that described collagen is obtained by following steps:
After being with the black sole skin cleaning of squama, cut to rotten shape, with the 0.1M soaking with sodium hydroxide 12h of 10 times of volumes, filter, be washed till neutrality, filter, with multiplex-enzyme extraction, complex enzyme is pepsin, papain and Alcalase compound protease are composited according to activity ratio 1:1:2, total activity is 0.06IU/g, and extraction time is 4 hours, and temperature is 50 DEG C, pH is 6, and solid-liquid ratio is 1:12.
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| CN103131746B (en) * | 2013-03-12 | 2015-03-25 | 程云开 | Extraction method of collagen peptide contained in scaly fish skin |
| CN104388512A (en) * | 2014-11-28 | 2015-03-04 | 桂林市和胤祥新型材料有限公司 | Method for preparing hydrolyzed collagen |
| CN105969832A (en) * | 2016-07-26 | 2016-09-28 | 渤海大学 | Preparation method of plaice skin collagen powder |
| CN109265538B (en) * | 2018-09-30 | 2021-11-26 | 大连海洋大学 | Active dipeptide from skin of flatfish |
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| CN1560270A (en) * | 2004-03-12 | 2005-01-05 | 中国海洋大学 | Process for preparing active peptide using fish skin collagen step directional enzynolysed by composit enzyme |
| CN101538602A (en) * | 2009-04-13 | 2009-09-23 | 湖北瑞邦生物科技有限公司 | Extraction method of fish skin collagen |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1560270A (en) * | 2004-03-12 | 2005-01-05 | 中国海洋大学 | Process for preparing active peptide using fish skin collagen step directional enzynolysed by composit enzyme |
| CN101538602A (en) * | 2009-04-13 | 2009-09-23 | 湖北瑞邦生物科技有限公司 | Extraction method of fish skin collagen |
Non-Patent Citations (2)
| Title |
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| 海洋生物胶原蛋白的制备及比较;孟昭宇等;《中国食品学报》;20031231;2003增刊275-278 * |
| 酶法制备鲽鱼鱼皮胶原蛋白肽及其清除超氧阴离子自由基的研究;王群等;《中国农学通报》;20111231;第27卷(第14期);87-93 * |
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