CN102757491B - Method for recycling water-soluble proteins in minced fish rinsing water - Google Patents
Method for recycling water-soluble proteins in minced fish rinsing water Download PDFInfo
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- CN102757491B CN102757491B CN2012102387522A CN201210238752A CN102757491B CN 102757491 B CN102757491 B CN 102757491B CN 2012102387522 A CN2012102387522 A CN 2012102387522A CN 201210238752 A CN201210238752 A CN 201210238752A CN 102757491 B CN102757491 B CN 102757491B
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Abstract
The invention relates to a method for recycling water-soluble proteins in minced fish rinsing water, which is characterized by comprising the following steps: salt-process low-temperature degreasing: adding a certain amount of table salt (NaCl) into minced fish rinsing water, stirring to sufficiently dissolve the table salt, and standing until grease precipitates and floats up to the surface, wherein the temperature of the rinsing water is controlled at 10 DEG C below in the whole process; isoelectric point protein precipitation: adding acid to the obtained liquid to regulate the pH value to 4.0-5.0, and standing to sufficiently stratify; preliminary protein recycling: discharging the supernatant part of the obtained liquid out by using a pump, and collecting the understratum protein precipitation layer; and protein recycling by centrifugation. The recycled protein can be directly packaged into finished product for freezing storage, or spray-dried into protein powder. The method provided by the invention is simple and easy to implement and is efficient; and the method can greatly reduce environmental pollution caused by improper discharge of protein-rich rinsing water, enhance the economic benefit of the minced fish production enterprise, and implement efficient utilization of resources, thereby having important meaning for environment-friendly sustainable development in minced fish processing industry.
Description
Technical field
The present invention relates to a kind of albumen recovery method, relate in particular to a kind of method that reclaims water-soluble protein in the rotten rinse water of fish.
Background technology
The fish gruel can be carried out rinsing to the flesh of fish in the middle of pre-treatment in the processing process, to remove its water miscible proteolytic enzyme and protoheme, finally reach the purpose that improves the rotten quality of fish.For a long time, owing to not having effective means to reclaim albumen, in rinse water, also be mixed with a large amount of greases simultaneously, and with dense fishy smell, manufacturing enterprise directly directly discharges the rotten rinse water of fish as trade effluent mostly, so not only to sewage disposal, bring huge pressure, and cause a large amount of wastes of protein resource.Up to now, the method that reclaims about the rotten rinse water of fish of having reported both at home and abroad has pH regulator method, ultrafiltration process, ion exchange method and flocculence etc.Ultrafiltration process good separating effect wherein, but production cost is too high, and ultra-filtration membrane easily results in blockage because grease solidifies; The ion exchange method complicated operation, treatment capacity is little, and the rate of recovery of albumen is not high; Though flocculence has good albumen recovering effect, the flocculation agent that mixes in the protein product of gained is difficult to remove, and directly affects its range of application; The relative manufacturing enterprise of pH regulator rule, simple, but the protein recovery of finding report is low at present, and separating effect is bad.Therefore, develop a kind of effective, simple albumen recovery method, the economic benefit for improving the rotten manufacturing enterprise of fish, realize effective utilization of resource, realizes that particularly the rotten processing enterprise of fish is significant to environmentally friendly Sustainable development.
Summary of the invention
The technical problem to be solved in the present invention is: the method that water-soluble protein in the rotten rinse water of a kind of easy, high efficiente callback fish is provided.
For achieving the above object, the invention provides following concrete technical scheme:
Reclaim the method for water-soluble protein in the rotten rinse water of fish, comprise the steps:
The salt method is low-temperature defatted: in the rotten rinse water of fish, add a certain amount of NaCl salt, controls whole process rinse water temperature at 10 ° below C, the stirring certain hour, fully dissolve salt, standing certain hour, make grease separate out and on float on surface; Wherein said salt adds the 0.1-5% that weight is the rotten rinse water volume weight of fish, is preferably 2-4%, and more preferably 3%.Described stirring certain hour and standing certain hour with the reality of salt fully dissolve with grease effectively separate out effect come fixed, such as stirring 30 minutes, standing one hour; In iso-electric point sedimentation albumen, time of repose was as the criterion with the abundant layering of feed liquid, such as standing three hours.
Iso-electric point sedimentation albumen: to above-mentioned steps gained feed liquid acid adding (such as being 5 mol/L HCl), to pH value of solution, be 4.0-5.0, standing certain hour, make its abundant layering;
Albumen tentatively reclaims: with pump, gained feed liquid supernatant is partly discharged, collect lower floor's protein deposition layer; The feed liquid supernatant of wherein discharging, protein concentration should be lower than 5 g/L, so that follow-up sewage disposal.
Reclaiming by centrifuge albumen: utilize the certain rotating speed of horizontal continuous centrifuge, certain flow rate, separating obtained protein liquid.In reclaiming by centrifuge albumen, flow velocity, according to joining centrifugal device performance consider that the final protein rate of recovery adjusts, is preferably flow velocity 500-1000 mL/min, 8,000 revolutions per seconds of rotating speeds.Feed velocity is suitably adjusted joining the centrifugal device performance according to factory, but flow velocity and the final protein rate of recovery be inversely proportional to, and need consider whole energy consumption and productive rate and be optimized adjusting.
Described protein liquid adds alkali and slowly regulates pH to neutral, with antifreezing agent, stirs, by forming machine packaging final prod, cold storage.Described antifreezing agent is composite by suitable proportion by sucrose, trehalose, sorbyl alcohol, is preferably the part by weight of 2:1:1, with the 5-10 % of protein content, adds.
Described albumen feed liquid can also, by rotary spraying drying tower, be spray dried to protein powder.The charging flow velocity is suitably adjusted joining the spray drying unit performance according to factory, and considers whole energy consumption and productive rate is optimized adjusting.The albumen feed liquid also can be added water absorbability and the viscosity of appropriate inorganic salt or carbohydrate reduction albumen.
The present invention also protects according to the resulting albumen of aforesaid method.
The present invention strengthens the ionic strength of albumen in rinse water by the method for adding salt, albumen is improved significantly at iso-electric point place effect of settling, finally reaches the effect of high efficiente callback water-soluble protein.3% salt concn of use preferred for this invention is not only applicable to the application of gefillte fish, and its salinity and seawater approach, and the discharge of wastewater of more coastal enterprise facilitates; Simultaneously, this method realizes effective removal of fat and bad flavor, and the protein product of gained is without obvious fishy smell, and lipid content is low, and the salt that it only contains separates simple, applied range.
Technological design principle of the present invention is: at low temperature, in highly water-soluble protein concentration (more than 30 g/L) situation, method by salt adding, strengthen the ionic strength of feed liquid, the grease and the albumen sepn that make to be combined with hydrophobic bond with albumen are separated out, and under low temperature condition, condense in the feed liquid top layer, thereby reach the purpose of removing grease.
By regulating the method for pH, make protein under isoelectric pH, due to the electrostatic repulsion flocking settling, due to the mode by adding salt, increase in addition the ionic strength of feed liquid, the electrostatic repulsion of its water-soluble protein also is reinforced, so effect of settling obviously improves.
Simultaneously, by feed liquid, separate, thereby the bad flavor in rinse water also effectively separates and reaches the purpose of albumen except the raw meat deodorizing with albumen.
Beneficial effect of the present invention is:
The present invention strengthens the ionic strength of albumen in rinse water by the method for adding salt, albumen is improved significantly at iso-electric point place effect of settling, finally reaches the effect of high efficiente callback water-soluble protein.The salt concn of use 3 % preferred for this invention is not only applicable to the production of gefillte fish, and its salinity and seawater approach, and the discharge of wastewater of more coastal enterprise facilitates; Simultaneously, this method realizes effective removal of fat and bad flavor, and the protein product of gained is without obvious fishy smell, and lipid content is low, and the salt that it only contains separates simple, applied range.
The present invention has mainly adopted the salt adding method to strengthen the ionic strength of rinse water, and stand at low temperature is removed grease, then passes through isoelectric point method sedimentation albumen, thereby realizes the efficient sharp separation of albumen in rinse water.The present invention adopts the method for adding salt to improve traditional isoelectric point method first, realizes the high efficiente callback of water-soluble protein.
The accompanying drawing explanation
Fig. 1 is the rotten rinse water of blue circle Scad fish rate of recovery figure under condition of different pH without interpolation salt the time, and wherein, the rinse water protein concentration is 30 g/L, and temperature is 10 ° of C, utilizes centrifuging to reclaim albumen;
Fig. 2 is the rotten rinse water of blue circle Scad fish rate of recovery figure under condition of different pH when the NaCl addition is 3 %, and wherein, the rinse water protein concentration is 30 g/L, and temperature is 10 ° of C, utilizes centrifuging to reclaim albumen;
Fig. 3 is the rotten rinse water of blue circle Scad fish rate of recovery figure under condition of different pH when the NaCl addition is 6 %, and wherein, the rinse water protein concentration is 30 g/L, and temperature is 10 ° of C, utilizes centrifuging to reclaim albumen;
Fig. 4 is the rotten rinse water of blue circle Scad fish rate of recovery figure under different protein concentrations when the NaCl addition is 3 %, and wherein, rinse water pH is 4.0, and temperature is 10 ° of C, utilizes centrifuging to reclaim albumen;
Fig. 5 is the impact of NaCl addition on protein recovery in the rotten rinse water of indigo plant circle Scad fish, and wherein, rinse water pH is 4.0, and protein concentration is 30 g/L, and temperature is 10 ° of C, utilizes centrifuging to reclaim albumen.
Embodiment
Below in conjunction with embodiment, embodiment of the present invention are described in detail, but it will be understood to those of skill in the art that the following example is only be used to the present invention is described, and should not be considered as limiting scope of the present invention.Unreceipted concrete technology or condition person in embodiment, according to the described technology of the document in this area or condition or carry out according to product description.The unreceipted person of production firm of agents useful for same or instrument, being can be by the conventional products of commercial acquisition.
The preparation of the rotten rinse water of embodiment 1: Lan Yuan Ajigasawa fish
1, from the market of farm produce, buying the indigo plant circle Scad that meat is good, color and luster is vivid is raw material, with clean frozen water, rinses, and removes dirt and the bacterium of surface attachment, then dissects, decaptitates, goes internal organ, water cleans for the second time again, generally washs 2 ~ 3 times;
2, the flesh of fish on the fish body is separated, with water low rate mixing 10 min of 3 ~ 10 ° of C, standing, so, after rinsing 2 ~ 3 times, with whizzer (Beckman, avanti-25) centrifuge dehydration, the supernatant liquor part of collecting above centrifugal gained, be the rotten rinse water of fish.
Embodiment 2: reclaim the water-soluble protein in the rotten rinse water of blue circle Scad fish
1, the salt method is low-temperature defatted: take in the rotten rinse water of indigo plant circle Scad fish of 10L that 300 g salt slowly add embodiment 1 gained (rinse water protein concentration 90 g/L), control whole process rinse water temperature at 10 ° below C, stirred 30 minutes, fully dissolve salt, standing one hour, make grease separate out and on float on surface, remove the grease of feed liquid surface flotation;
2, iso-electric point sedimentation albumen: to gained feed liquid acid adding (5 mol/L HCl) to pH value of solution to 4.0, standing three hours;
3, albumen tentatively reclaims: the gained feed liquid supernatant of layering is partly removed, collected lower floor's protein deposition layer;
4, reclaiming by centrifuge albumen: utilize gained protein liquid in high-speed and continuous whizzer (GW145L, good firm (Shanghai) mechanical means company limited) separation, 8,000 revolutions per seconds of rotating speeds, flow velocity 500 mL/min;
5, by Folin-phenol method test kit (Bio Rad Laboratories), measure protein content, calculate protein recovery: gained albumen weight in wet base 4722 g, water content 83 %, protein recovery 89.2 %;
6, gained albumen adds alkali (10 mol/L NaOH) and slowly regulates pH to neutral, with antifreezing agent 377 g(sucrose wherein: trehalose: sorbyl alcohol=2:1:1, weight ratio), stir, by forming machine packaging final prod, cold storage.
Embodiment 3: reclaim the water-soluble protein in the rotten rinse water of blue circle Scad fish
1, the salt method is low-temperature defatted: take in the rotten rinse water of indigo plant circle Scad fish that 90 g salt slowly add 3 L (rinse water protein concentration 90 g/L), control whole process rinse water temperature at 10 ° below C, stirred 30 minutes, fully dissolve salt, standing one hour, make grease separate out and on float on surface, remove the grease of feed liquid surface flotation;
2, iso-electric point sedimentation albumen: to gained feed liquid acid adding to pH value of solution to 4.0, standing three hours;
3, albumen tentatively reclaims: the gained feed liquid supernatant of layering is partly removed, collected lower floor's protein deposition layer;
4, spray-drying process reclaims albumen: gained albumen feed liquid is by rotary spraying drying machine (SP-1500, the suitable instrument science and technology in Shanghai), 115 ° of C of inlet temperature, and input speed 30 mL/min, be spray dried to protein powder;
5, by Folin-phenol method test kit (Bole company), measure protein content, calculate protein recovery;
6, gained albumen dry weight 260 g, water content 4 %, protein recovery 92.4 %.
Embodiment 4: the rotten rinse water of fish are the rate of recovery under condition of different pH without interpolation salt the time
1, get rotten rinse water (rinse water protein concentration 90 g/L) 3.5 L of fish, add consubstantiality accumulated ice water, stir evenly, obtaining the 7L protein concentration is 45 g/L rinse water, stirs 30 minutes, the gained feed liquid is divided equally into to 35 parts, every part of 200 mL;
2, iso-electric point sedimentation albumen: by above-mentioned 35 parts of feed liquids, divide 7 groups, 5 every group parallel, difference acid adding (5 mol/L HCl) regulator solution pH to 3.5,4,4.5,5,5,5,6,6.5, then be settled to 300 mL, standing three hours, the final protein concentration of its feed liquid was 30 g/L;
3, reclaiming by centrifuge albumen: utilize the separating obtained protein liquid of high-speed and continuous whizzer (BECKMAN), 8,000 revolutions per seconds of rotating speeds, centrifugal 10 minutes;
4, by Folin-phenol method kit measurement protein content, calculate protein recovery, result is as shown in Figure 1.
As can be seen from Figure 1: in the situation that do not add salt, the water-soluble protein rate of recovery in rinse water is the highest when pH 5.5, but its rate of recovery also only has 24.1 %, and the rate of recovery is low.
Embodiment 5: the rotten rinse water of fish rate of recovery under condition of different pH when the NaCl addition is 3 %
1, get rotten rinse water (rinse water protein concentration 90 g/L) 3.5 L of fish, add consubstantiality accumulated ice water, stir evenly, obtaining the 7L protein concentration is 45 g/L rinse water, stirs 30 minutes, the gained feed liquid is divided equally into to 35 parts, every part of 200 mL;
2, iso-electric point sedimentation albumen: by above-mentioned 35 parts of feed liquids, divide 7 groups, 5 every group parallel, and salt adding 9 g, be adjusted to respectively pH 3.0,3.5 after fully dissolving respectively, 4,4.5,5,5,5,6.0, then be settled to 300 mL, standing 3 hours, the final protein concentration of its feed liquid was 30 g/L;
3, reclaiming by centrifuge albumen: utilize gained protein liquid in the separation of high-speed and continuous whizzer, 8,000 revolutions per seconds of rotating speeds, centrifugal 10 minutes;
4, by Folin-phenol method kit measurement protein content, calculate protein recovery, result is as shown in Figure 2.
As can be seen from Figure 2: when the salt addition is 3 %, its albumen adds salt (Fig. 1) in the isoelectric precipitation characteristic of different pH with nothing and has significant difference, its best iso-electric point also is significantly improved by the rate of recovery that pH 5.5 moves to pH 4.0 and water-soluble protein, 24.1 % while adding salt by nothing bring up to 86.5 %, and effect is remarkable.
Embodiment 6: the rotten rinse water of fish rate of recovery under condition of different pH when the NaCl addition is 6 %
1, get rotten rinse water (rinse water protein concentration 90 g/L) 3.5 L of fish, add consubstantiality accumulated ice water, stir evenly, obtaining 7 L protein concentrations is 45 g/L rinse water, stirs 30 min, the gained feed liquid is divided equally into to 35 parts, every part of 200 mL;
2, iso-electric point sedimentation albumen: by above-mentioned 35 parts of feed liquids, divide 7 groups, 5 every group parallel, and salt adding 18 g, fully dissolve rear regulator solution pH to 3.0 respectively, 3.5 respectively, 4,4.5,5,5,5,6.0, then be settled to 300 mL, standing three hours, the final protein concentration of its feed liquid was 30 g/L;
3, reclaiming by centrifuge albumen: utilize gained protein liquid in the separation of high-speed and continuous whizzer, 8,000 revolutions per seconds of rotating speeds, centrifugal 10 min;
4, by Folin-phenol method kit measurement protein content, calculate protein recovery, result is as shown in Figure 3.
As can be seen from Figure 3: at the salt addition, be 6 %, it is similar when the grade electric settling character of water-soluble protein under different pH is 3% to addition, overall protein recovery improves to some extent, and wherein at the pH4.0 place, 86.5 %s of the rate of recovery during by 3 % salt are increased to 92.2 %.
Embodiment 7: the rotten rinse water of fish rate of recovery under different protein concentrations when the NaCl addition is 3 %
1, get the rotten rinse water (rinse water protein concentration 90 g/L) of fish; add appropriate frozen water; be made into the feed liquid of 8 groups of different protein concentrations: 10 g/L, 20 g/L, 30 g/L, 40 g/L, 50 g/L, 60 g/L, 70 g/L, 80 g/L; from each group feed liquid, getting respectively 900 mL; minutes 6 parts parallel; every part of parallel 150mL, salt adding 4.5 g, stirred 30 minutes respectively;
2, iso-electric point sedimentation albumen: add acid for adjusting pH to 4.0 in above-mentioned feed liquid, be settled to again 300 mL, standing three hours, its final protein concentration of respectively organizing feed liquid was respectively: 5 g/L, 10 g/L, 15 g/L, 20 g/L, 25 g/L, 30 g/L, 35 g/L, 40 g/L;
3, reclaiming by centrifuge albumen: utilize gained protein liquid in the separation of high-speed and continuous whizzer, 8,000 revolutions per seconds of rotating speeds, centrifugal 10 minutes;
4, by Folin-phenol method kit measurement protein content, calculate protein recovery, result is as shown in Figure 4.
As can be seen from Figure 4: when the salt addition is 3 %, the protein recovery of water-soluble protein when pH 4.0 increases and improves with protein concentration, at 5-30 mg/mL(g/L) in scope, the rate of recovery and the protein concentration of albumen are linear, when protein concentration at 30 mg/mL when above, more than protein recovery can reach 85 %, and amplification reduces gradually.In the production process of minced fillet of reality, the protein content in the rotten rinse water of the fish that produces is generally more than 50 g/L, so method is applicable to the rotten manufacturing enterprise of all fishes of Present Domestic.
The impact of embodiment 8:NaCl addition on protein recovery in the rotten rinse water of indigo plant circle Scad fish
1, get rotten rinse water (rinse water protein concentration 90 g/L) 4.5 L of fish, add consubstantiality accumulated ice water, stir evenly, obtaining 9 L protein concentrations is 45 g/L rinse water, stirs 30min, the gained feed liquid is divided equally into to 45 parts, every part of 200 mL;
2, iso-electric point sedimentation albumen: divide 9 groups by above-mentioned 45 parts of feed liquids, every group 5 parallel, in each group, add successively salt 0 g, 1 g, 2 g, 4 g, 6 g, 9 g, 12 g, 16 g, 20 g, add alkali and adjust pH value of solution to 4.0, be settled to again 300 mL, standing three hours, its ultimate density of respectively organizing albumen in feed liquid was 30 g/L;
3, reclaiming by centrifuge albumen: utilize gained protein liquid in the separation of high-speed and continuous whizzer, 8,000 revolutions per seconds of rotating speeds, centrifugal 10 min;
4, by Folin-phenol method kit measurement protein content, calculate protein recovery, result is as shown in Figure 5.
As can be seen from Figure 5: (30 g/L under certain protein concentration, i.e. 30 mg/mL), the rate of recovery of the water-soluble protein in the rotten rinse water of fish significantly improves with the interpolation of salt, at salt addition 3 % when above, its protein recovery amplification diminishes gradually, when the salt addition is that 8 % are when above, more than protein recovery can reach 95 %.But the Financial cost factor while considering practical application, the recommendation amount of salt are most preferably 3 % left and right in the 2-4% left and right.
Claims (13)
1. a method that reclaims water-soluble protein in the rotten rinse water of fish, is characterized in that, comprises the steps:
The salt method is low-temperature defatted: in the rotten rinse water of fish, add a certain amount of NaCl salt, controls whole process rinse water temperature at 10 ° below C, the stirring certain hour, fully dissolve salt, standing certain hour, make grease separate out and on float on surface;
Iso-electric point sedimentation albumen: it is 4.0-5.0 that above-mentioned steps gained feed liquid acid adding is adjusted to pH, and standing certain hour, make its abundant layering;
Albumen tentatively reclaims: with pump, gained feed liquid supernatant is partly discharged, collect lower floor's protein deposition layer;
Reclaiming by centrifuge albumen: utilize the certain rotating speed of horizontal continuous centrifuge, certain flow rate, protein isolate liquid.
2. method claimed in claim 1, is characterized in that, described salt addition is the 0.1-5% of the rotten rinse water weight of fish.
3. method claimed in claim 1, is characterized in that, described salt adds the 2-4% that weight is the rotten rinse water weight of fish.
4. method claimed in claim 1, is characterized in that, it is 3% of the rotten rinse water weight of fish that described salt adds weight.
5. method claimed in claim 1, is characterized in that, during described salt method is low-temperature defatted, stirs certain hour and standing certain hour and fully dissolve with grease and effectively separate out and determine with the reality of salt; In iso-electric point sedimentation albumen, time of repose is as the criterion with the abundant layering of feed liquid.
6. method claimed in claim 5, is characterized in that, during described salt method is low-temperature defatted, stirred standing one hour 30 minutes; In iso-electric point sedimentation albumen, standing three hours.
7. method claimed in claim 1, is characterized in that, in the preliminary recovery of albumen, and the feed liquid supernatant of discharging, protein concentration is lower than 5 g/L; In reclaiming by centrifuge albumen, flow velocity is according to joining centrifugal device performance consider that the final protein rate of recovery adjusts.
8. method claimed in claim 1, is characterized in that, in the preliminary recovery of albumen, and the feed liquid supernatant of discharging, protein concentration is lower than 5 g/L; In reclaiming by centrifuge albumen, flow velocity 500-1000 mL/min, 8,000 revolutions per seconds of rotating speeds.
9. method claimed in claim 1, is characterized in that, described protein liquid adds alkali and slowly regulates pH to neutral, with antifreezing agent, stirs, by forming machine packaging final prod, cold storage.
10. method claimed in claim 9, is characterized in that, described antifreezing agent is composite by suitable proportion by sucrose, trehalose, sorbyl alcohol.
11. method claimed in claim 9, is characterized in that, described antifreezing agent is pressed the part by weight of 2:1:1 by sucrose, trehalose, sorbyl alcohol, with the 5-10 % interpolation of protein content.
12. method claimed in claim 1, is characterized in that, the resulting albumen of described reclaiming by centrifuge albumen, by rotary spraying drying tower, is spray dried to protein powder.
13. method claimed in claim 1, is characterized in that, the rotten rinse water of fish comprise the rinse water from sea water fish and the rotten course of processing generation of freshwater fish.
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| CN108840902A (en) * | 2018-07-14 | 2018-11-20 | 泉州师范学院 | Canned sardines processes the recovery method of fish protein and its application in fish soup waste liquid |
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| CN106800584B (en) * | 2016-12-16 | 2019-10-25 | 浙江大学宁波理工学院 | The method of protein is recycled from Dai Yu Yu Porridge rinsing liquid |
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| CN112715743B (en) * | 2019-10-14 | 2022-06-10 | 湖北工业大学 | Method for recovering protein and fish oil in minced fillet rinsing water and reducing COD (chemical oxygen demand) |
| CN112778396A (en) * | 2020-12-31 | 2021-05-11 | 福建省水产研究所（福建水产病害防治中心） | Method for recovering water-soluble protein in minced fillet |
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