CN106800584A - Method of protein is reclaimed from Dai Yu Yu Porridge rinsing liquids - Google Patents
Method of protein is reclaimed from Dai Yu Yu Porridge rinsing liquids Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07K—PEPTIDES
- C07K1/00—General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
- C07K1/14—Extraction; Separation; Purification
- C07K1/30—Extraction; Separation; Purification by precipitation
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Abstract
The present invention discloses one kind and reclaims method of protein from Dai Yu Yu Porridge rinsing liquids, it is characterised in that：To the composite flocculation agent that shitosan and PAMC are constituted is added in Dai Yu Yu Porridge rinsing liquids, well mixed, centrifuging and taking supernatant simultaneously collects precipitation；Added in clear liquid then up as the PAMA of flocculant, well mixed, centrifuging and taking supernatant simultaneously collects precipitation；Precipitation twice merges, is dried to obtain protein.The present invention has the advantages that technique is easy, processing cost is low, cycle is short, and for the COD (COD) for reducing Dai Yu Yu Porridge rinsing liquids, environmental protection is significant.
Description
Technical field
The present invention relates to biological technical field, specifically refer to a kind of using shitosan-PAMC, anion
The flocculants such as polyacrylamide reclaim method of protein from Dai Yu Yu Porridge rinsing liquids.
Technical background
Hairtail also known as hairtail, dental strip fish, are net-rope Perciformes Trichiuridae animals, are a kind of China coast yield warps higher
Ji fish.Band fish protein is a kind of complete protein, nutritious containing eight kinds of amino acid needed by human.Hairtail is oppressed
It is white, it is to process the very good material for preparing Yu Porridge.Minced fillet is by adopting meat, rinsing, refined filtration, dehydration stirring and freezing to add by fish
The product that work is obtained, is to prepare Yu Porridge products such as：The raw material of fish ball, fish sausage, paupiette etc..Surimi product does not have fishy smell, rich bullet
Property, it is unique flavor, nutritious and cheap, it is deep to be liked by masses.In Yu Porridge process, rinsing is one key
Operation, is directly connected to the gel strength and whiteness of Yu Porridge, is played an important role to improving surimi product quality and keeping property.
Rinsing is usually the water for adding 3~5 times or so flesh of fish weight, and low rate mixing stands after being fully dissolved out water-solubility protein etc., makes
The flesh of fish fully sinks, and reclaims upper strata fish oil, and incline rinsing liquid, then adds water according to the above ratio, repeats rinsing 1~3 time；Thus may be used
See, rinsing process water consumption is very big, cause the water soluble protein for accounting for fish protein 30%~40% to enter rinsing liquid, form big
Amount eutrophy processing waste water, there are some researches show the COD (COD) of , Yu Porridge rinsing liquids is up to 8000-10000mg/L, such as
Really untreated just discharge will produce severe contamination to environment.Therefore, protein is reclaimed Cong Yu Porridge rinsing liquids, for reducing
COD, environmental protection is significant.
The common methods for reclaiming protein from surimi washings at present mainly have：Heating, isoelectric point precipitation, flocculation
Method etc..Heating power consumption is high, does not meet the requirement of energy-saving and emission-reduction, and increased the cost of enterprise.Isoelectric point precipitation is to pass through
The pH of rinsing liquid is reconciled to being allowed to precipitate near the isoelectric point of water soluble protein.Due to the grade electricity of protein in Yu Porridge rinsing liquids
The general rinsing liquid behind pH4.2~5.5, isoelectric point method protein precipitation of point is in highly acid, if directly discharge will cause water body
Acidifying pollution environment.Flocculence is to adding a certain amount of flocculant in surimi washings, protein is occurred de- steady and is condensed
Settled down into bulky grain, reach the purpose for reclaiming protein；Flocculence has operating process simple, the advantages of with low cost,
It is a kind of excellent Protein Recovery method.
Due to containing multiple proteins in surimi washings, and traditional flocculence often only collects single isoelectric point
Protein, causes wherein also containing the substantial amounts of protein not being recovered, and this part surimi washings is discharged into environment, can make
Into COD it is high, to environment produce severe contamination.But current still also non-someone is for different in Dai Yu Yu Porridge rinsing liquids
The protein of isoelectric point carries out the report of flocculence recovery.
The content of the invention
Above-mentioned deficiency of the present invention for prior art, there is provided a kind of using different flocculants, for different isoelectric points
Protein reclaimed, to reclaim protein to greatest extent, reduce the COD of Yu Porridge rinsing liquids, environmental protection from hairtail fish
Method of protein is reclaimed in Porridge rinsing liquids.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：One kind is returned from Dai Yu Yu Porridge rinsing liquids
Method of protein is received, wherein to the compound wadding that shitosan and PAMC composition are added in Dai Yu Yu Porridge rinsing liquids
Solidifying agent, well mixed, centrifuging and taking supernatant simultaneously collects precipitation；Added in clear liquid then up as the anion of flocculant poly- third
Acrylamide, well mixed, centrifuging and taking supernatant simultaneously collects precipitation；Precipitation twice merges, is dried to obtain protein.
The above-mentioned Dai Yu Yu Porridge rinsing liquids of the present invention, its specific preparation method is：By the hairtail flesh of fish (decaptitate, tail and interior
It is dirty) rub, it is first slow during the flesh of fish then is added into 4 DEG C as rinsing liquid, 0.3% (mass percent concentration) NaCl solution
Speed stirring 5~15 minutes, then fish is obtained with multilayer gauze (multilayer gauze can be 3-6 layers) filtering after standing 10~30 minutes
Porridge rinsing liquids, above-mentioned rinse cycle is repeated 1~3 time, and the filtrate for merging repeatedly rinsing filtering obtains fish Porridge rinsing liquids.
The concentration of the present invention above-mentioned shitosan and PAMC in Dai Yu Yu Porridge rinsing liquids is respectively
1.0g/L~3.0g/L, 0.02g/L~0.08g/L.
Above-mentioned shitosan is first to be added to hairtail into the form of the chitosan solution that mass concentration is 1% with peracetic acid formulation
In Yu Porridge rinsing liquids.
Above-mentioned PAMC is first to be configured to the cation polypropylene acyl that mass concentration is 0.025% with water
The form of amine aqueous solution is added in Dai Yu Yu Porridge rinsing liquids.
The present invention it is above-mentioned be added to concentration of the PAMA of supernatant in supernatant for 0.025g/L~
0.075g/L。
The above-mentioned PAMA of the present invention be first with water be configured to concentration of polymer solution be 0.025% it is cloudy from
The form of sub- polyacrylamide solution is added in supernatant.
The above-mentioned centrifugation of the present invention, be specifically：Centrifugation 10~15 minutes at 3500~4000rpm, 1~5 DEG C, then
Take supernatant and collect precipitation.
The above-mentioned drying of the present invention, dry 12 under the conditions of precipitation specifically is placed in into 50~60 DEG C, 0.08~0.1MPa~
24 hours, then it is size-reduced obtain final product reclaim after protein.
Method of protein is reclaimed in the above-mentioned Yu Yu Porridge rinsing liquids from Dai of the present invention, specific steps include：
(1) the hairtail flesh of fish is rubbed (decaptitate, tail and internal organ, meat is adopted by hand) and weighs weight；With 4 DEG C, 0.3%NaCl solution
Used as rinsing liquid, the weight ratio that the flesh of fish and NaCl solution are controlled during rinsing is 1:3~5, the flesh of fish is added to above-mentioned NaCl molten
In liquid, first low rate mixing 5~15 minutes, then with multilayer gauze (multilayer gauze can be 3-6 layers) mistake after standing 10~30 minutes
Filter, repeats rinsing 1~3 time, obtains Yu Porridge rinsing liquids；
(2) prepared to step (1) add in Yu Porridge rinsing liquids 1.0g/L~3.0g/L shitosans and 0.02g/L~
0.08g/L PAMCs, stir, and then stand and obtain mixture in 30~120 minutes；
(3) mixture obtained by step (2) is centrifuged, 3500~4000rpm, 1~5 DEG C, 10~15 minutes takes
Clear liquid simultaneously collects precipitation；
(4) to 0.025g/L~0.075g/L PAMAs are added in the supernatant obtained by step (3), stir
Uniformly, then stand and obtain mixture in 30~120 minutes；
(5) mixture obtained by step (4) is centrifuged, 3500~4000rpm, 1~5 DEG C, 10~15 minutes takes
Clear liquid simultaneously collects precipitation；
(6) precipitation that collection step (3) and step (5) are obtained, 50~60 DEG C, 0.08~0.1MPa dries 12~24 small
Shi Hou, the size-reduced protein obtained final product after reclaiming.
The present invention detects the protein concentration of Yu Porridge rinsing liquids and supernatant using conventional biuret method, and according to following
Formula calculates protein recovery.Protein recovery of the invention is 85~95%.
R (%)：Protein recovery；
C0：Surimi washings protein concentration；V0：Surimi washings volume
C：The supernatant protein concentration for finally giving；V：The supernatant volume for finally giving
The present invention has following remarkable advantage and beneficial effect：
(1) present invention carries out flocculence recovery, applicant for the protein of different isoelectric points in Dai Yu Yu Porridge rinsing liquids
Early-stage Study finds that the isoelectric point of the protein in Dai Yu Yu Porridge rinsing liquids is pH4~6 and pH9~10, is combined using first adding
It is the protein of pH4~6 that flocculant (shitosan-PAMC) reclaims isoelectric point, then adds anion pp
It is the protein of pH9~10 that acid amides reclaims isoelectric point；With only for isoelectric points of proteins in acid pH or the absorption method of alkaline pH
Compare, the present invention realizes the recovery to greatest extent of Dai Yu Yu Porridge rinsing liquid protein.
(2) present invention first uses composite flocculation agent (shitosan-PAMC) to isoelectric point in pH4~6
Protein carries out coagulation and recovery, compared with using only a kind of flocculant (shitosan or PAMC), improves egg
The rate of recovery of white matter.
(3) present invention is utilized Xiang addition shitosan-PAMC, anion pp acyl in Yu Porridge rinsing liquids
The method of the flocculants such as amine reclaims protein, has the advantages that technique is easy, processing cost is low, cycle is short, for reducing hairtail
The COD (COD) of Yu Porridge rinsing liquids, environmental protection is significant.
Specific embodiment
4 preferred embodiments are given below, but the present invention is not only limited to following examples.
Embodiment 1：
Hairtail is decaptitated, tail and internal organ, meat is adopted by hand, rub, flesh of fish 1kg is weighed, with 4 DEG C, 0.3%NaCl solution conducts
Rinsing liquid, the ratio that the flesh of fish and rinsing liquid are controlled during rinsing is 1:3, will 1kg the flesh of fish be added in 3kg rinsing liquids, first at a slow speed
Stirring 7 minutes, then repeat to rinse 1 time with four layers of filtered through gauze after standing 12 minutes, obtain Yu Porridge rinsing liquids；Rinsed Xiang Yu Porridge
1.0g/L shitosans (with peracetic acid formulation into solution, concentration is 1%) and 0.02g/L PAMCs is added (to use in liquid
Water is configured to solution, and concentration is 0.025%), to stir, and is centrifuged after standing 45 minutes：3800rpm, 3 DEG C, 10 minutes,
Take supernatant and collect precipitation；(solution, concentration are configured to 0.025g/L PAMAs are added in supernatant with water
0.025%), to stir, it is centrifuged after standing 30 minutes：3800th, 3 DEG C, 10 minutes, take supernatant and collect precipitation；
Precipitations obtained by 2 centrifugations of merging, 50 DEG C, 0.095MPa, after drying 20 hours, the size-reduced protein obtained final product after reclaiming.
The protein concentration of Yu Porridge rinsing liquids and supernatant is detected using biuret method, is computed showing that protein recovery is
86.2%.
Embodiment 2：
Hairtail is decaptitated, tail and internal organ, meat is adopted by hand, rub, flesh of fish 2kg is weighed, with 4 DEG C, 0.3%NaCl solution conducts
Rinsing liquid, the ratio that the flesh of fish and rinsing liquid are controlled during rinsing is 1:4, will 2kg the flesh of fish be added in 8kg rinsing liquids, first at a slow speed
Stirring 8 minutes, then repeat to rinse 2 times with four layers of filtered through gauze after standing 15 minutes, obtain Yu Porridge rinsing liquids；Rinsed Xiang Yu Porridge
2.0g/L shitosans (with peracetic acid formulation into solution, concentration is 1%) and 0.06g/L PAMCs is added (to use in liquid
Water is configured to solution, and concentration is 0.025%), to stir, and is centrifuged after standing 60 minutes：4000rpm, 4 DEG C, 15 minutes,
Take supernatant and collect precipitation；(solution, concentration are configured to 0.05g/L PAMAs are added in supernatant with water
0.025%), to stir, it is centrifuged after standing 90 minutes：4000th, 3 DEG C, 12 minutes, take supernatant and collect precipitation；
Precipitations obtained by 2 centrifugations of merging, 55 DEG C, 0.01MPa, after drying 18 hours, the size-reduced protein obtained final product after reclaiming.Adopt
The protein concentration of Yu Porridge rinsing liquids and supernatant is detected with biuret method, is computed showing that protein recovery is 90.6%.
Embodiment 3：
Hairtail is decaptitated, tail and internal organ, meat is adopted by hand, rub, flesh of fish 3kg is weighed, with 4 DEG C, 0.3%NaCl solution conducts
Rinsing liquid, the ratio that the flesh of fish and rinsing liquid are controlled during rinsing is 1:3, will 3kg the flesh of fish be added in 9kg rinsing liquids, first at a slow speed
Stirring 10 minutes, then repeat to rinse 2 times with four layers of filtered through gauze after standing 20 minutes, obtain Yu Porridge rinsing liquids；Rinsed Xiang Yu Porridge
2.5g/L shitosans (with peracetic acid formulation into solution, concentration is 1%) and 0.075g/L PAMCs are added in liquid
(solution is configured to water, concentration is 0.025%), to stir, is centrifuged after standing 90 minutes：4000rpm, 4 DEG C, 15 points
Clock, takes supernatant and collects precipitation；To added in supernatant 0.06g/L PAMAs (be configured to solution with water, it is dense
Spend 0.025%), to stir, be centrifuged after standing 120 minutes：4000th, 3 DEG C, 15 minutes, take supernatant and collect heavy
Form sediment；Precipitations obtained by 2 centrifugations of merging, 60 DEG C, 0.09MPa, after drying 22 hours, the size-reduced albumen obtained final product after reclaiming
Matter.The protein concentration of Yu Porridge rinsing liquids and supernatant is detected using biuret method, is computed showing that protein recovery is
92.0%.
Embodiment 4：
Hairtail is decaptitated, tail and internal organ, meat is adopted by hand, rub, flesh of fish 4kg is weighed, with 4 DEG C, 0.3%NaCl solution conducts
Rinsing liquid, the ratio that the flesh of fish and rinsing liquid are controlled during rinsing is 1:3, will 4kg the flesh of fish be added in 12kg rinsing liquids, first at a slow speed
Stirring 10 minutes, then repeat to rinse 3 times with four layers of filtered through gauze after standing 20 minutes, obtain Yu Porridge rinsing liquids；Rinsed Xiang Yu Porridge
3.0g/L shitosans (with peracetic acid formulation into solution, concentration is 1%) and 0.08g/L PAMCs is added (to use in liquid
Water is configured to solution, and concentration is 0.025%), to stir, and is centrifuged after standing 90 minutes：4000rpm, 4 DEG C, 15 minutes,
Take supernatant and collect precipitation；(solution, concentration are configured to 0.075g/L PAMAs are added in supernatant with water
0.025%), to stir, it is centrifuged after standing 120 minutes：4000rpm, 3 DEG C, 15 minutes, take supernatant and collect heavy
Form sediment；Precipitations obtained by 2 centrifugations of merging, 60 DEG C, 0.09MPa, after drying 22 hours, the size-reduced albumen obtained final product after reclaiming
Matter.The protein concentration of Yu Porridge rinsing liquids and supernatant is detected using biuret method, is computed showing that protein recovery is
95.0%.
The above embodiment of the present invention and data fully confirm that protein recovery of the invention is high, can up to for 85~
95%, the COD (COD) of Dai Yu Yu Porridge rinsing liquids is reduced, environmental protection is significant.
Claims (10)
1. one kind reclaims method of protein from Dai Yu Yu Porridge rinsing liquids, it is characterised in that：To adding in Dai Yu Yu Porridge rinsing liquids
The composite flocculation agent that shell adding glycan and PAMC are constituted, well mixed, centrifuging and taking supernatant simultaneously collects precipitation；So
Added as the PAMA of flocculant in backward supernatant, well mixed, centrifuging and taking supernatant simultaneously collects precipitation；
Precipitation twice merges, is dried to obtain protein.
2. method of protein is reclaimed in the Yu Yu Porridge rinsing liquids from Dai according to claim 1, it is characterised in that：Described
Dai Yu Yu Porridge rinsing liquids, its specific preparation method is：Hairtail is oppressed and is rubbed, then the flesh of fish is added to as rinsing liquid
4 DEG C, in 0.3%NaCl solution, first low rate mixing 5~15 minutes, then use multilayer filtered through gauze after standing 10~30 minutes is obtained
Fish Porridge rinsing liquids, above-mentioned rinse cycle is repeated 1~3 time, and the filtrate for merging repeatedly rinsing filtering obtains fish Porridge rinsing liquids.
3. method of protein is reclaimed in the Yu Yu Porridge rinsing liquids from Dai according to claim 1, it is characterised in that：Described
The concentration of shitosan and PAMC in Dai Yu Yu Porridge rinsing liquids is respectively 1.0g/L~3.0g/L, 0.02g/L
~0.08g/L.
4. method of protein is reclaimed in the Yu Yu Porridge rinsing liquids from Dai according to claim 3, it is characterised in that：Described
Shitosan is first to be added in Dai Yu Yu Porridge rinsing liquids into the form of the chitosan solution that mass concentration is 1% with peracetic acid formulation
's.
5. method of protein is reclaimed in the Yu Yu Porridge rinsing liquids from Dai according to claim 3, it is characterised in that：Described
PAMC is that the form for being first configured to the PAMC solution that mass concentration is 0.025% with water adds
Enter in Dai Yu Yu Porridge rinsing liquids.
6. method of protein is reclaimed in the Yu Yu Porridge rinsing liquids from Dai according to claim 1, it is characterised in that：It is described to add
It is 0.025g/L~0.075g/L to enter concentration of the PAMA to supernatant in supernatant.
7. method of protein is reclaimed in the Yu Yu Porridge rinsing liquids from Dai according to claim 6, it is characterised in that：Described
PAMA is the shape that the PAMA solution that concentration of polymer solution is 0.025% is first configured to water
Formula is added in supernatant.
8. method of protein is reclaimed in the Yu Yu Porridge rinsing liquids from Dai according to claim 1, it is characterised in that：Described
Centrifugation, be specifically：It is centrifuged 10~15 minutes at 3500~4000rpm, 1~5 DEG C, then takes supernatant and collect precipitation.
9. method of protein is reclaimed in the Yu Yu Porridge rinsing liquids from Dai according to claim 1, it is characterised in that：Described
Dry, dried 12~24 hours under the conditions of precipitation specifically is placed in into 50~60 DEG C, 0.08~0.1MPa, it is then size-reduced to obtain final product
Protein after recovery.
10. method of protein is reclaimed from Dai Yu Yu Porridge rinsing liquids according to claim 1-9 any claims, its
It is characterised by：Specific step includes：
(1) the hairtail flesh of fish is rubbed and weighs weight；With 4 DEG C, 0.3%NaCl solution controlled as rinsing liquid, during rinsing the flesh of fish and
The weight ratio of NaCl solution is 1:3~5, the flesh of fish is added in above-mentioned NaCl solution, first low rate mixing 5~15 minutes, then
Multilayer filtered through gauze is used after standing 10~30 minutes, rinsing 1~3 time is repeated, fish Porridge rinsing liquids are obtained；
(2) 1.0g/L~3.0g/L shitosans and 0.02g/L~0.08g/L are added in preparing Yu Porridge rinsing liquids to step (1)
PAMC, stirs, and then stands and obtains mixture in 30~120 minutes；
(3) mixture obtained by step (2) is centrifuged, 3500~4000rpm, 1~5 DEG C, 10~15 minutes takes supernatant
And collect precipitation；
(4) to 0.025g/L~0.075g/L PAMAs are added in the supernatant obtained by step (3), stirring is equal
It is even, then stand and obtain mixture in 30~120 minutes；
(5) mixture obtained by step (4) is centrifuged, 3500~4000rpm, 1~5 DEG C, 10~15 minutes takes supernatant
And collect precipitation；
(6) precipitation that collection step (3) and step (5) are obtained, 50~60 DEG C, 0.08~0.1MPa, after drying 12~24 hours,
The size-reduced protein obtained final product after reclaiming.
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| CN112679593A (en) * | 2020-12-28 | 2021-04-20 | 华中农业大学 | Method for recovering sarcoplasmic proteins in minced fillet rinsing liquid by combining acid treatment with chitosan flocculation and application |
| 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 |
| WO2024124632A1 (en) * | 2022-12-13 | 2024-06-20 | 江苏大学 | Method for recovering proteins from minced-fish washing waste liquid on the basis of low-temperature plasma technique |
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| WO2024124632A1 (en) * | 2022-12-13 | 2024-06-20 | 江苏大学 | Method for recovering proteins from minced-fish washing waste liquid on the basis of low-temperature plasma technique |
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| CN106800584B (en) | 2019-10-25 |
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