CN103130887B - The method of continuous production fish noggin, grease and collagen peptide - Google Patents
The method of continuous production fish noggin, grease and collagen peptide Download PDFInfo
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- CN103130887B CN103130887B CN201210101796.0A CN201210101796A CN103130887B CN 103130887 B CN103130887 B CN 103130887B CN 201210101796 A CN201210101796 A CN 201210101796A CN 103130887 B CN103130887 B CN 103130887B
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- 241000251468 Actinopterygii Species 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 59
- 108090000765 processed proteins & peptides Proteins 0.000 title claims abstract description 32
- 102000008186 Collagen Human genes 0.000 title claims abstract description 31
- 108010035532 Collagen Proteins 0.000 title claims abstract description 31
- 229920001436 collagen Polymers 0.000 title claims abstract description 31
- 239000004519 grease Substances 0.000 title claims abstract description 25
- 102000045246 noggin Human genes 0.000 title claims abstract description 20
- 108700007229 noggin Proteins 0.000 title claims abstract description 20
- 238000010924 continuous production Methods 0.000 title claims abstract description 11
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 12
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000000284 extract Substances 0.000 claims abstract description 9
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- 238000001556 precipitation Methods 0.000 claims description 38
- 239000002244 precipitate Substances 0.000 claims description 22
- 238000002386 leaching Methods 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 15
- 102000004190 Enzymes Human genes 0.000 claims description 12
- 108090000790 Enzymes Proteins 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 230000007935 neutral effect Effects 0.000 claims description 12
- 239000013049 sediment Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 14
- 230000008901 benefit Effects 0.000 abstract description 4
- -1 albumen Substances 0.000 abstract description 2
- 230000004071 biological effect Effects 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 235000018102 proteins Nutrition 0.000 description 10
- 239000000047 product Substances 0.000 description 7
- 235000019198 oils Nutrition 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 235000001014 amino acid Nutrition 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 235000021323 fish oil Nutrition 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
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- Peptides Or Proteins (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention discloses a kind of method of continuous production fish noggin, grease and collagen peptide, comprises the steps: to get the homogenate of fish head; Isoelectric point method extracts protein; Organic solvent method carries grease; Sumizyme MP enzymolysis process carries collagen peptide.The present invention realizes the production successively of albumen, grease and collagen peptide continuously, and have improving production efficiency, reduce the advantage of production cost, the industrialization being applicable to fishery field is produced, and promotes that economic benefit promotes, increases added value.And operating process of the present invention is simple, do not need complicated equipment; From fish processing waste fish head, reclaim the compositions such as albumen, grease and collagen peptide first simultaneously, realize the comprehensive utilization of fish head.Carry out at 0-4 DEG C, remain functional performance and the biological activity of reclaimed composition to greatest extent, be conducive to the further exploitation of these compositions.
Description
Technical field
The present invention relates to the complete processing based on fish head, relate to the method for a set of production fish noggin, grease and collagen peptide in particular.
Background technology
Since the 1950's, world fisheries ultimate production increases with the speed of 6%-7% always, although fishery production is already more than 100,000,000 tons, has the catches of nearly 1/3 to fail directly to be utilized by the mankind.China's fishery products total amount, more than 5,200 ten thousand tons, becomes world fisheries and produces the first big country for continuous 20 years.Fish head is the main tankage in the fish course of processing, occupies about the 15-30% of fish gross weight.Fish head rich in proteins, fat, calcium, phosphorus, iron, VITAMIN, the aminoacid pattern of protein needs close to human body, is rich in the unsaturated fatty acidss such as DHA, EPA and phosphatide in lipid acid, has certain value of exploiting and utilizing.
At present following approach is mainly contained to the exploitation of fish head: 1. directly freshly to freeze or freezing fish head, do the work in-process such as adult fish heads chafing dish, supply market.This method, mainly for part fish head, is applied limited; 2. fish head is dry, pulverizing, is ground into fishbone powder, is processed into animal-feed.Although this method is simple, the added value of product of producing is lower; 3. from fish head, reclaim protein (peptide) and fish oil, develop related products.This method Recent study is more, but related-art process is not yet ripe, does not really realize extensive commercial application.For utilizing the series of problems such as level is not high, and processed goods is with low content of technology, added value is low to fish head at present, be badly in need of finding solution.
Summary of the invention
The present invention aims to provide a kind of method preparing fish noggin, grease and collagen peptide, aim to provide and a kind ofly operate continuously can realize the method that albumen, grease and collagen peptide produce successively, thus reach the object of production cost of enhancing productivity, reduce, the industrialization based on the first-born product product of fish is made to become possibility, promote that fishery promotes economic benefit, increase added value.
In order to achieve the above object, the invention provides a kind of method preparing fish noggin, under 0-4 DEG C of condition, complete following steps:
Step1, get the homogenate of fish head, obtain homogenate;
Step2, isoelectric point method extract protein: mixed by the water of described homogenate with 1-6 times of volume, adjust pH is 10-13, stirring and leaching 5-30 minute; Be more than or equal to centrifugal 10-30 minute under 5000 × g, obtain the first upper phase and the first precipitation;
Step3-1, adjust the pH value of described first upper phase to be 3-6, be more than or equal to centrifugal 10-30 minute under 10000 × g, obtain the second upper phase and the second precipitation; Described second precipitation adjusts pH to neutral, obtains fish noggin after drying.
Present invention also offers a kind of method preparing fish hair oil fat, under 0-4 DEG C of condition, complete following steps:
Step1, get the homogenate of fish head, obtain homogenate;
Step2, isoelectric point method extract protein: mixed by the water of described homogenate with 1-6 times of volume, adjust pH is 10-13, stirring and leaching 5-30 minute; Be more than or equal to centrifugal 10-30 minute under 5000 × g, obtain the first upper phase and the first precipitation;
Step3-2, organic solvent method carry grease: described first precipitation mixed with envelope-bulk to weight ratio 1-5 normal hexane doubly, stirring and leaching 1-3 hour, is being more than or equal to centrifugal 10-30 minute under 5000 × g, centrifugal that the 3rd upper phase and the 3rd precipitates; Fish hair oil fat is obtained after described 3rd upper phase removing normal hexane.
Present invention also offers a kind of method preparing fish head collagen peptide, under 0-4 DEG C of condition, (except Sumizyme MP enzymolysis step) completes following steps:
Step1, get the homogenate of fish head, obtain homogenate;
Step2, isoelectric point method extract protein: mixed by the water of described homogenate with 1-6 times of volume, adjust pH is 10-13, stirring and leaching 5-30 minute; Be more than or equal to centrifugal 10-30 minute under 5000 × g, obtain the first upper phase and the first precipitation;
Step3-2, organic solvent method carry grease: described first precipitation mixed with envelope-bulk to weight ratio 1-5 normal hexane doubly, stirring and leaching 1-3 hour, is being more than or equal to centrifugal 10-30 minute under 5000 × g, centrifugal that the 3rd upper phase and the 3rd precipitates;
Step4, Sumizyme MP enzymolysis process carry collagen peptide: the 3rd precipitation mixed with volume 1-10 times of 0.1-0.3 mol/L sodium hydroxide solution, stirring and leaching 12-48 hour, be more than or equal to centrifugal 10-30 minute under 10000 × g, obtain the 4th upper phase and the 4th precipitation; 4th precipitation is mixed with 3-6 times of volume water, adjust pH 7-11, add Sumizyme MP, enzyme dosage is the 0.1-2% of the 4th Sediment weight, enzymolysis 1-4 hour at 40-70 DEG C, 100 DEG C of enzymes more than 10 minutes that go out, be more than or equal to centrifugal 10-30 minute under 10000 × g, collect the 5th upper phase, adjust pH to neutral, after drying, namely obtain fish head collagen peptide.
Under optimal way, in above-mentioned steps, adjust pH selects 1-6 mol/L sodium hydroxide to adjust or hydrochloric acid.
The present invention is based on above-mentioned production process, integrate production technique, a kind of method of continuous production fish noggin, grease and collagen peptide is provided, to enhance productivity, reduce production cost, specifically comprise the steps (except Sumizyme MP enzymolysis step, all the other operations all complete under 0-4 DEG C of condition):
Step1, get the homogenate of fish head, obtain homogenate;
Step2, isoelectric point method extract protein: mixed by the water of described homogenate with 1-6 times of volume, adjust pH is 10-13, stirring and leaching 5-30 minute; Centrifugal 10-30 minute, obtains the first upper phase and the first precipitation;
Step3-1, adjust the pH value of described first upper phase to be 3-6, centrifugal 10-30 minute, obtain the second upper phase and the second precipitation; Described second precipitation adjusts pH to neutral, obtains fish noggin after drying.
Step3-2, organic solvent method carry grease: described first precipitation mixed with envelope-bulk to weight ratio 1-5 normal hexane doubly, stirring and leaching 1-3 hour, centrifugal 10-30 minute, centrifugal that the 3rd upper phase and the 3rd precipitates; Fish hair oil fat is obtained after described 3rd upper phase removing normal hexane.
Step4, Sumizyme MP enzymolysis process carry collagen peptide: the 3rd precipitation mixed with volume 1-10 times of 0.1-0.3 mol/L sodium hydroxide solution, stirring and leaching 12-48 hour, centrifugal 10-30 minute, obtain the 4th upper phase and the 4th precipitation; 4th precipitation is mixed with 3-6 times of volume water, adjust pH 7-11, add Sumizyme MP, enzyme dosage is the 0.1-2% of the 4th Sediment weight, enzymolysis 1-4 hour at 40-70 DEG C, 100 DEG C of enzymes more than 10 minutes that go out, centrifugal 10-30 minute, collect the 5th upper phase, adjust pH to neutral, after drying, namely obtain fish head collagen peptide.
Under optimal way, adjust pH selects 1-6 mol/L sodium hydroxide to adjust or hydrochloric acid.
In addition, in above-mentioned technological process, Step2 is being more than or equal to centrifugal under 5000 × g must described first upper phase and first precipitation; In step Step3-1, be more than or equal to centrifugal under 10000 × g must described second upper phase and second precipitation; Step3-2, is being more than or equal to centrifugal under 5000 × g must described 3rd upper phase and the 3rd precipitation; In Step4, be more than or equal to centrifugal under 10000 × g must described 4th upper phase and the 4th precipitation and described 5th upper phase.Time centrifugal, the certain larger efficiency of the size of centrifugal force is higher, but corresponding cost is also higher, selects above-mentioned centrifugal force lower limit can realize production object preferably in the present invention, thus reaches the object reducing production cost.And the centrifugal upper limit, unrestrictedly, realize according to prior art feasible pattern.
The method of continuous production fish noggin of the present invention, grease and collagen peptide, compared with prior art tool of the present invention has the following advantages:
1, operating process is simple, does not need complicated equipment, is applicable to suitability for industrialized production.
2, from fish processing waste fish head, reclaim the compositions such as albumen, grease and collagen peptide first simultaneously, realize the comprehensive utilization of fish head.
3, whole operating process is all carried out (except Sumizyme MP enzymolysis step) at 0-4 DEG C, remains functional performance and the biological activity of reclaimed composition to greatest extent, is conducive to the further exploitation of these compositions.
In addition, in method provided by the invention, under particularly strictly realizing the condition of each procedure technology parameter, return can be strengthened at product production and product purity, qualitatively acquisition.
Embodiment
Embodiment 1: the method for continuous production fish noggin, grease and collagen peptide, whole operating process is carried out at 2 DEG C (except Sumizyme MP enzymolysis step), comprises the steps:
1, raw material obtains and process: the fish head of fresh (or freezen protective, flowing water thaws), removes the cheek, homogenate after cleaning.
2, isoelectric point method extracts protein: being mixed by the homogenate of fish head and 1 times of volume (volume/volume) 2 DEG C of water, is 10 with 1 mol/L sodium hydroxide adjust pH, stirring and leaching 5 minutes, under 5000 × g centrifugal 10 minutes, obtains upper phase A and precipitate A.Adjust the pH value of upper phase A to be 3 with 1 mol/L hydrochloric acid, under 10000 × g centrifugal 10 minutes, obtain upper phase B and precipitate B, precipitate B adjusted pH to neutral, namely obtains fish noggin after drying.
3, organic solvent method carries grease: precipitate A mixed with 1 times of volume (volume/mass) normal hexane, stirring and leaching 1 hour, under 5000 × g centrifugal 10 minutes, centrifugal upper phase C and precipitate C, and upper phase C to remove after normal hexane to obtain fish hair oil fat.
4, Sumizyme MP enzymolysis process carries collagen peptide: precipitate C mixed with 1 times of volume 0.2 mol/L sodium hydroxide solution, stirring and leaching 24 hours, under 10000 × g centrifugal 10 minutes, obtains upper phase D and precipitation D.D will be precipitated mix with 3 times of volume water, with 6 mol/L hydrochloric acid adjust pHs 7, add Sumizyme MP, enzyme dosage is 0.1% of precipitation D weight, enzymolysis 1 hour at 40 DEG C, 100 DEG C of enzymes 10 minutes of going out, under 10000 × g centrifugal 10 minutes, collect upper phase, adjust pH, to neutral, namely obtains fish head collagen peptide after drying.
Embodiment 2: the method for continuous production fish noggin, grease and collagen peptide, whole operating process is carried out at 4 DEG C (except Sumizyme MP enzymolysis step), comprises the steps:
1, raw material obtains and process: the fish head of fresh (or freezen protective, flowing water thaws), removes the cheek, homogenate after cleaning.
2, isoelectric point method extracts protein:.Being mixed by the homogenate of fish head and 6 times of volumes (volume/volume) 4 DEG C of water, is 13 with 6 mol/L sodium hydroxide adjust pHs, stirring and leaching 30 minutes, under 10000 × g centrifugal 30 minutes, obtains upper phase A and precipitate A.Adjust the pH value of upper phase A to be 6 with 6 mol/L hydrochloric acid, under 15000 × g centrifugal 10 minutes, obtain upper phase B and precipitate B, precipitate B adjusted pH to neutral, namely obtains fish noggin after drying.
3, organic solvent method carries grease: precipitate A mixed with 5 times of volume (volume/mass) normal hexanes, stirring and leaching 3 hours, under 15000 × g centrifugal 20 minutes, centrifugal upper phase C and precipitate C, and upper phase C to remove after normal hexane to obtain fish hair oil fat.
4, Sumizyme MP enzymolysis process carries collagen peptide: precipitate C mixed with 10 times of volume 0.1 mol/L sodium hydroxide solutions, stirring and leaching 48 hours, under 20000 × g centrifugal 20 minutes, obtains upper phase D and precipitation D.D will be precipitated mix with 6 times of volume water, with 6 mol/L sodium hydroxide adjust pHs 11, add Sumizyme MP, enzyme dosage is 2% of precipitation D weight, enzymolysis 4 hours at 70 DEG C, 100 DEG C of enzymes 30 minutes of going out, under 12000 × g centrifugal 15 minutes, collect upper phase, adjust pH, to neutral, namely obtains fish head collagen peptide after drying.
Embodiment 3: the method for continuous production fish noggin, grease and collagen peptide, whole operating process is carried out at 3 DEG C (except Sumizyme MP enzymolysis step), comprises the steps:
1, raw material obtains and process: the fish head of fresh (or freezen protective, flowing water thaws), removes the cheek, homogenate after cleaning.
2, isoelectric point method extracts protein:.Being mixed by the homogenate of fish head and 4 times of volumes (volume/volume) 3 DEG C of water, is 12 with 5 mol/L sodium hydroxide adjust pHs, stirring and leaching 10 minutes, under 10000 × g centrifugal 15 minutes, obtains upper phase A and precipitate A.Adjust the pH value of upper phase A to be 4 with 4 mol/L hydrochloric acid, under 15000 × g centrifugal 15 minutes, obtain upper phase B and precipitate B, precipitate B adjusted pH to neutral, namely obtains fish noggin after drying.
3, organic solvent method carries grease: precipitate A mixed with 3 times of volume (volume/mass) normal hexanes, stirring and leaching 2 hours, under >=5000 × g centrifugal 15 minutes, centrifugal upper phase C and precipitate C, upper phase C to remove after normal hexane to obtain fish hair oil fat.
4, Sumizyme MP enzymolysis process carries collagen peptide: precipitate C mixed with 5 times of volume 0.3 mol/L sodium hydroxide solutions, stirring and leaching 12 hours, under 15000 × g centrifugal 15 minutes, obtains upper phase D and precipitation D.D will be precipitated mix with 4 times of volume water, with 6 mol/L hydrochloric acid adjust pHs 9, add Sumizyme MP, enzyme dosage is 0.5% of precipitation D weight, enzymolysis 3 hours at 50 DEG C, 100 DEG C of enzymes 20 minutes of going out, under 10000 × g centrifugal 30 minutes, collect upper phase, adjust pH, to neutral, namely obtains fish head collagen peptide after drying.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (3)
1. a method for continuous production fish noggin, grease and collagen peptide, is characterized in that, comprises the steps:
S1, at 0-4 DEG C, get the homogenate of fish head, obtain homogenate;
S2, at 0-4 DEG C, isoelectric point method extract protein: mixed by the water of described homogenate with 1-6 times of volume, adjust pH is 10-13, stirring and leaching 5-30 minute; Centrifugal 10-30 minute, obtains the first upper phase and the first precipitation;
S3-1, at 0-4 DEG C, adjust the pH value of described first upper phase to be 3-6, centrifugal 10-30 minute, obtain the second upper phase and the second precipitation; Described second precipitation adjusts pH to neutral, obtains fish noggin after drying;
S3-2, at 0-4 DEG C, organic solvent method carries grease: described first precipitation mix with envelope-bulk to weight ratio 1-5 normal hexane doubly, stirring and leaching 1-3 hour, centrifugal 10-30 minute, centrifugally must the 3rd upper phase and the 3rd precipitate; Fish hair oil fat is obtained after described 3rd upper phase removing normal hexane;
S4, Sumizyme MP enzymolysis process carry collagen peptide: the 3rd precipitation mixed with volume 1-10 times of 0.1-0.3 mol/L sodium hydroxide solution, stirring and leaching 12-48 hour, centrifugal 10-30 minute, obtain the 4th upper phase and the 4th precipitation; 4th precipitation is mixed with 3-6 times of volume water, adjust pH 7-11, add Sumizyme MP, enzyme dosage is the 0.1-2% of the 4th Sediment weight, enzymolysis 1-4 hour at 40-70 DEG C, 100 DEG C of enzymes more than 10 minutes that go out, centrifugal 10-30 minute, collect the 5th upper phase, adjust pH to neutral, after drying, namely obtain fish head collagen peptide.
2. the method for continuous production fish noggin, grease and collagen peptide according to claim 1, it is characterized in that, adjust pH selects 1-6 mol/L sodium hydroxide or hydrochloric acid.
3. the method for continuous production fish noggin, grease and collagen peptide according to claim 1 or 2, is characterized in that,
In step S2, be more than or equal to centrifugal under 5000 × g must described first upper phase and first precipitation;
In step S3-1, be more than or equal to centrifugal under 10000 × g must described second upper phase and second precipitation;
In step S3-2, be more than or equal to centrifugal under 5000 × g must described 3rd upper phase and the 3rd precipitation;
In step S4, be more than or equal to centrifugal under 10000 × g must described 4th upper phase and the 4th precipitation and described 5th upper phase.
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| CN201210101796.0A CN103130887B (en) | 2012-03-31 | 2012-03-31 | The method of continuous production fish noggin, grease and collagen peptide |
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| CN103555804B (en) * | 2013-11-13 | 2015-09-16 | 陈忆凤 | A kind of preparation method of animals and plants mixed protein peptide |
| CN105601731B (en) * | 2014-09-03 | 2018-07-13 | 浙江崇山生物制品有限公司 | Purify the method for ox heel string collagen and its preparation of sponge |
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Non-Patent Citations (4)
| Title |
|---|
| Comparative studies on the yield and quality of solvent-extracted oil from salmon skin;Aryee and simpson;《Journal of food engineering》;20091231;第92卷;353-358 * |
| Protein isolation form gutted herring(clupea harengus) using pH-shift processes;Marmon S K等;《J.agric.food chem.》;20100909;第58卷;第10481页 * |
| Separation and quality of fish oil from precooked and non-precooked tuna heads;Chantachum 等;《food chemistry》;20001231;第69卷;289-294 * |
| 鳀鱼可溶性蛋白质及鱼油的开发;朱碧英 等;《东海海洋》;20010630;第19卷(第2期);60-62 * |
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