CN105803023A - Method for preparing aquatic livestock small molecule peptide without fishy smell or bitter taste - Google Patents

Method for preparing aquatic livestock small molecule peptide without fishy smell or bitter taste Download PDF

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Publication number
CN105803023A
CN105803023A CN201610311734.0A CN201610311734A CN105803023A CN 105803023 A CN105803023 A CN 105803023A CN 201610311734 A CN201610311734 A CN 201610311734A CN 105803023 A CN105803023 A CN 105803023A
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China
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raw meat
hardship
patient
aquatic animal
abnormal smells
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Inventor
潘剑宇
陈得科
孙恢礼
蔡冰娜
万鹏
陈华
孙大儒
孙小钰
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South China Sea Institute of Oceanology of CAS
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South China Sea Institute of Oceanology of CAS
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Priority to CN201610311734.0A priority Critical patent/CN105803023A/en
Publication of CN105803023A publication Critical patent/CN105803023A/en
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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P21/00Preparation of peptides or proteins
    • C12P21/06Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K1/00General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14Extraction; Separation; Purification
    • C07K1/30Extraction; Separation; Purification by precipitation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K1/00General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14Extraction; Separation; Purification
    • C07K1/34Extraction; Separation; Purification by filtration, ultrafiltration or reverse osmosis
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07KPEPTIDES
    • C07K1/00General methods for the preparation of peptides, i.e. processes for the organic chemical preparation of peptides or proteins of any length
    • C07K1/14Extraction; Separation; Purification
    • C07K1/36Extraction; Separation; Purification by a combination of two or more processes of different types

Abstract

The invention belongs to the technical field of biologics, and in particular relates to a method for preparing aquatic livestock small molecule peptide without fishy smell or bitter taste. The method comprises the following steps: S1, performing enzyme deactivation on aquatic livestock enzymatic hydrolysate, and concentrating so as to obtain a treated liquid; S2, cooling the treated liquid, centrifuging so as to remove grease and impurities, and retaining the supernate; S3, performing alcohol precipitation on the supernate, leaving to stand, centrifuging so as to remove polysaccharide and macromolecule protein, and retaining the supernate; S4, performing ultra-filtration on the supernate, adding an antioxidant bacteriostatic agent into the retained liquid, and uniformly stirring; S5, recycling ethanol from the retained liquid, and drying, thereby obtaining the aquatic livestock small molecule peptide without fishy smell or bitter taste. The method is simple to operate and efficient in treatment, fishy smell and fishy bitter taste of aquatic livestock can be effectively removed, the fishy smell caused by oxidation of product grease can be effectively inhibited, trimethylamine caused by microorganisms or enzyme can be inhibited, and the expiration date of a product can be prolonged.

Description

A kind of preparation method of the abnormal smells from the patient aquatic animal small-molecular peptides of hardship without raw meat
Technical field
The invention belongs to biological technical field, the preparation method being specifically related to a kind of abnormal smells from the patient aquatic animal small-molecular peptides of hardship without raw meat.
Background technology
Aquatic animal is rich in high quality protein, utilize protease hydrolyzed method can prepare multiple biologically active protein, peptide, the protein peptide of aquatic animal is prone to absorb, Nutrition highlights, and is widely used in fields such as professional Medical Degree, special medicine purposes formula food, health food, bread and cheese and high-end skin care item.But, aquatic animal itself and protein hydrolysate are often with fish-stench and raw meat bitterness, have a strong impact on the Consumers' Acceptance of final products, product high osmosis salt content is higher, there is the risk of gastrointestinal upset, and the uncontrollable of hydrolytic process can produce a large amount of free amino acid and bitterness oligopeptide, reduces small-molecular peptides yield, these unfavorable factors all limit production and the extensive use of aquatic animal small-molecular peptides.
At present, the raw meat hardship abnormal smells from the patient method of going of aquatic animal protein zymolyte mainly has absorption method, investment, masking method, extraction etc..As Chinese patent 201510099398.3 discloses the decoloration deodorization method of a kind of ocean activity collagen peptidase hydrolyzed liquor, wherein use Powdered Activated Carbon to carry out decoloration deodorization, reach eliminating sargassum smell purpose by controlling temperature and adsorption time;Chinese patent 201310641052.2 discloses a kind of method utilizing low value peeled shrimp to produce Macrobrachium nipponensis dried meat, utilizes absorption and embedding to cover the raw meat bitterness of peeled shrimp by adding beta-schardinger dextrin-and shrimp shell chitosan;Chinese patent 200710113483.6 discloses a kind of holothurian essence and preparation method thereof, and it uses the pungent flavor seasoning extracting solution such as Cortex cinnamomi japonici (Ramulus Cinnamomi), Fructus Citri tangerinae skin, anise to shelter fishy smell;Chinese patent 201310437558.1 discloses a kind of de-bitter, the fishy smell method of aquatic products protein zymolyte and screening agent thereof, uses the flavoring agents such as ethylmaltol, ethyl acetate, cooking wine and Sal to shelter fishy smell;Chinese patent 201410534650.4 and 201110432428.X disclose the use of the supercritical carbon dioxide method for extracting method to remove peptides fishy smell.Having obvious limitation with deodorization method up: activated carbon adsorption non-selectivity, peptide matters loss is serious;Investment need to add relatively large adjuvant, and the imperfection of embedding makes fishy smell yet suffer from, and the bigger quality of embedded particles is uneven, and after structural deterioration, fishy smell reappears;Current masking method is both needed to add penetrating odor or the pungent taste flavoring substance of dense perfume (or spice) to cover fishy smell, reduces purity and the abnormal smells from the patient originally of peptide;Supercritical extraction method, equipment requirements high price is expensive, and complex process and treating capacity are low, is not suitable for large-scale promotion and uses.
Additionally, also have above technical tie-up ultrafiltration purification to go the method for raw meat to reach raw meat purpose.A kind of de-bitter, the fishy smell method of aquatic products protein zymolyte and screening agent thereof is disclosed such as Chinese invention 201310437558.1, make use of ultrafiltration and shelter the method for associating aquatic product protein zymolyte is processed, polysulfone hollow fibre hyperfiltration treatment is used for removing high molecular weight protein and enrichment micromolecule active polypeptide, adds ethylmaltol, ethyl lactate, cooking wine and Sal etc. and is used for sheltering hardship, fishy smell.Chinese invention 200810026735.6 discloses a kind of method of efficient dispelling fishy smell of pinctada martensii enzymolyzing liquid, use prosparol that fishy smell volatile ingredient is embedded, ultrafilter membrane again through 5000Da~20000Da is removed, and filtered solution prepares product for it.Hyperfiltration treatment in above patented method, all it is used for removing the bigger material of large protein equimolecular quantity, small-molecular peptides strongly limit efficiency and the production capacity of actual production by the speed of ultrafilter membrane, simultaneously the material such as high osmosis inorganic salt and bitterness oligopeptide also together with pass through ultrafilter membrane, can not removing stench material completely, the purity of protein peptide is also affected by extreme influence.
Furthermore, current aquatic animal zymolyte go deodorization method to be substantially to remove raw meat in preparation process, but product regenerates fishy odor follow-up depositing in process due to microorganism, enzyme effect or Oxidation of Fat and Oils, and the conversion of precursor substance as nitrogenous in sulfur-bearing and the autoxidation decomposition of free fatty can produce fishy smell.Tea polyphenols and curcumin are all extract the Natural antioxidant obtained from plant, through retrieval, still find no the application in suppressing aquatic animal small-molecular peptides product microorganism and enzyme effect, oxidation of the compositions of tea polyphenols and curcumin.
Therefore, it is necessary to the preparation method researching and developing a kind of aquatic animal small-molecular peptides, it is simple to operate, processes efficiently, and effectively removes fish-stench and the raw meat bitterness of aquatic animal, and long-acting suppression fishy odor produces, and extends shelf life of products.
Summary of the invention
In order to overcome the deficiencies in the prior art, the preparation method that it is an object of the invention to provide a kind of abnormal smells from the patient aquatic animal small-molecular peptides of hardship without raw meat, it is simple to operate, process efficiently, effectively remove fish-stench and the raw meat bitterness of aquatic animal simultaneously, fishy odor can be produced by long-acting suppression product Oxidation of Fat and Oils, and suppress microorganism or enzyme effect to produce trimethylamine, extend shelf life of products.
To achieve these goals, technical scheme is as follows:
The preparation method of a kind of abnormal smells from the patient aquatic animal small-molecular peptides of hardship without raw meat, comprises the following steps:
S1. the aquatic animal enzymolysis solution prepared by enzymatic isolation method, after enzyme denaturing, is concentrated into total solid matter 20~40%, obtains treatment fluid;
S2. described treatment fluid is cooled to 10~4 DEG C, the floating oils and fats in centrifugal segregation upper strata and bottom impurity, retain supernatant;
S3. adding ethanol to the volume fraction of ethanol toward described supernatant is 50~80%, staticly settles polysaccharide and high molecular weight protein, centrifugal segregation precipitate polysaccharides and high molecular weight protein, retains upper liquid;
S4. select the ultrafilter membrane of molecular cut off 1000~5000Da, described upper liquid is carried out ultrafiltration, in the trapped fluid obtained, add the antioxidation antibacterial of total solid matter weight 0.001~0.1% and stir;
S5. described trapped fluid reclaims ethanol under vacuum and low temperature, and drying prepares without raw meat hardship abnormal smells from the patient aquatic animal small-molecular peptides dry powder.
Further, centrifugation rate when being centrifuged in described step S2 is 1600~2000r/min.
Further, the ethanol in described step S3 is dehydrated alcohol.
Further, described antioxidation antibacterial is the compositions of tea polyphenols and curcumin.
Further, the weight ratio of described tea polyphenols and curcumin is 1: (2~3).
In technical solution of the present invention, the aquatic animal enzymolysis solution prepared by enzymatic isolation method centrifugal segregation oils and fats and impurity after cooling, then precipitate with ethanol Polysaccharide removing and high molecular weight protein are carried out, then high osmosis salt, free amino acid and bitterness oligopeptide are removed in ultrafiltration, it is eventually adding antioxidation antibacterial, concentration, dry prepared finished product.First cooling down and be centrifuged, be to make oils and fats solidify, float on upper strata after centrifugal, middle level is clear liquid, and lower floor is impurity, improves separating effect, also avoids oils and fats that next step operation is produced impact simultaneously.The operation of precipitate with ethanol is partly in order to Polysaccharide removing and high molecular weight protein so that separate more abundant, and when also making follow-up ultrafiltration, small-molecular peptides filtyration velocity is accelerated, and improves production efficiency, and improves the purity of small-molecular peptides;Make use of the volatile character of ethanol on the other hand, reclaim under vacuum and low temperature and the process of ethanol is taken away volatile fish-stench material and moisture, thus realizing the preparation without fish-stench and raw meat bitterness aquatic animal small-molecular peptides.
Tea polyphenols has antioxidation, can strengthen the activity of antioxidase, it is suppressed that oxidase, free radical is purged, and tea polyphenols also has certain antibacterial, bactericidal action simultaneously.For product in the follow-up problem deposited and regenerate fishy odor due to microorganism, enzyme effect or Oxidation of Fat and Oils in process, inventor tentatively adds tea polyphenols in product, found that the shelf-life of aquatic animal small-molecular peptides product is obviously prolonged (extending 3 months compared with before being not added with), but after depositing after a while, in product, the content of the property material trimethylamine of bad smell raises, and have impact on the local flavor of product.Curcumin has antioxidation equally, antibacterial effect, but its poor stability, degradable, and with color, when curcumin is applied individually to any aquatic animal small-molecular peptides product by inventor, find that it does not have obvious effect to extending shelf life of products, to suppress trimethylamine generation also without obvious effect, but curcumin and tea polyphenols be composite rear use by a certain percentage, can not only effectively extend shelf life of products (extending 5 months compared with before being not added with), fishy odor can be produced by long-acting suppression product Oxidation of Fat and Oils simultaneously, and suppress microorganism or enzyme effect to produce trimethylamine.Especially tea polyphenols and curcumin are with weight ratio for 1: action effect when (2~3) are composite is best.
Therefore, compared with prior art, present invention have an advantage that
(1) preparation method of the present invention is without adsorption treatment, it is prevented that protein peptide is lost;Do fishy smell without flavoring ingredients such as spice, salt, spice to shelter, nonirritant, less salt, Hyposmolality;By cooling down centrifugal, precipitate with ethanol, ultrafiltration, concentration, dry can be prepared by without raw meat hardship abnormal smells from the patient aquatic animal small-molecular peptides dry powder, technique is simple, stable, and condition is controlled, and treating capacity is big, speed fast, produces efficient, can industrialization large-scale production.
(2) preparation method of the present invention can effectively remove fish-stench and the raw meat bitterness of aquatic animal, and by adding the antioxidation antibacterial being made up of tea polyphenols and curcumin, long-acting suppression product Oxidation of Fat and Oils produces fishy odor, and suppress the microorganisms such as antibacterial or enzyme effect to produce trimethylamine, significantly extend shelf life of products.
Accompanying drawing explanation
Fig. 1 is the situation of change figure of trimethylamine in the embodiment of the present invention 1 product;
Fig. 2 is the situation of change figure of trimethylamine in the embodiment of the present invention 2 product;
Fig. 3 is the situation of change figure of trimethylamine in the embodiment of the present invention 3 product;
Fig. 4 is the situation of change figure of trimethylamine in the embodiment of the present invention 4 product;
Fig. 5 is the situation of change figure of trimethylamine in the embodiment of the present invention 5 product;
Fig. 6 is the situation of change figure of trimethylamine in the embodiment of the present invention 6 product;
Fig. 7 is the situation of change figure of trimethylamine in the embodiment of the present invention 7 product;
Fig. 8 is the situation of change figure of trimethylamine in the embodiment of the present invention 8 product;
Fig. 9 is the situation of change figure of trimethylamine in the embodiment of the present invention 9 product;
Figure 10 is the situation of change figure of trimethylamine in comparative example 1 product of the present invention;
Figure 11 is the situation of change figure of trimethylamine in comparative example 2 product of the present invention;
Figure 12 is the situation of change figure of trimethylamine in comparative example 3 product of the present invention;
Figure 13 is the situation of change figure of trimethylamine in comparative example 4 product of the present invention;
Figure 14 is the situation of change figure of trimethylamine in comparative example 5 product of the present invention;
Figure 15 is the situation of change figure of trimethylamine in comparative example 6 product of the present invention.
Detailed description of the invention
Describing the present invention in detail below in conjunction with specific embodiment, illustrative examples and explanation in this present invention are used for explaining the present invention, but not as a limitation of the invention.
In the present invention, described enzymatic isolation method is method commonly used in the art, for instance use papain that aquatic animal is carried out enzymolysis, solid-to-liquid ratio is 1: (3~4), and enzyme concentration is 0.6~0.8%, and hydrolysis temperature is 55~60 DEG C, hydrolysis time is 2~3h, and pH value is 6.0~7.0.
Embodiment 1, the present invention are without the preparation method of raw meat hardship abnormal smells from the patient Concha Ostreae small-molecular peptides
S1. the Carnis ostreae enzymolysis solution prepared by enzymatic isolation method, after 100 DEG C of enzyme denaturing, is concentrated into total solid matter 30%, obtains treatment fluid;
S2. described treatment fluid is cooled to 6 DEG C, the floating oils and fats in centrifugal segregation upper strata and bottom impurity, retain supernatant;Centrifugation rate time centrifugal is 2000r/min;
S3. adding dehydrated alcohol to the volume fraction of ethanol toward described supernatant is 60%, staticly settles polysaccharide and high molecular weight protein, centrifugal segregation precipitate polysaccharides and high molecular weight protein, retains upper liquid;
S4. select the ultrafilter membrane of molecular cut off 5000Da, described upper liquid is carried out ultrafiltration, in the trapped fluid obtained, add the antioxidation antibacterial of total solid matter weight 0.08% and stir;Described antioxidation antibacterial is tea polyphenols and curcumin with the composite compositions of weight ratio 1: 2;
S5. described trapped fluid reclaims ethanol, the spray-dried prepared abnormal smells from the patient Concha Ostreae small-molecular peptides dry powder of hardship without raw meat under vacuum and low temperature.
Embodiment 2, the present invention are without the preparation method of raw meat hardship abnormal smells from the patient Octopus small-molecular peptides
S1. the Octopus meat enzymolysis solution prepared by enzymatic isolation method, after 100 DEG C of enzyme denaturing, is concentrated into total solid matter 40%, obtains treatment fluid;
S2. described treatment fluid is cooled to 4 DEG C, the floating oils and fats in centrifugal segregation upper strata and bottom impurity, retain supernatant;Centrifugation rate time centrifugal is 2000r/min;
S3. adding dehydrated alcohol to the volume fraction of ethanol toward described supernatant is 50%, staticly settles polysaccharide and high molecular weight protein, centrifugal segregation precipitate polysaccharides and high molecular weight protein, retains upper liquid;
S4. select the ultrafilter membrane of molecular cut off 1000Da, described upper liquid is carried out ultrafiltration, in the trapped fluid obtained, add the antioxidation antibacterial of total solid matter weight 0.001% and stir;Described antioxidation antibacterial is tea polyphenols and curcumin with the composite compositions of weight ratio 1: 3;
S5. described trapped fluid reclaims ethanol, the spray-dried prepared abnormal smells from the patient Octopus small-molecular peptides dry powder of hardship without raw meat under vacuum and low temperature.
Embodiment 3, the present invention are without the preparation method of raw meat hardship abnormal smells from the patient Stichopus japonicus small-molecular peptides
S1. the Stichopus japonicus meat enzymolysis solution prepared by enzymatic isolation method, after 100 DEG C of enzyme denaturing, is concentrated into total solid matter 30%, obtains treatment fluid;
S2. described treatment fluid is cooled to 6 DEG C, the floating oils and fats in centrifugal segregation upper strata and bottom impurity, retain supernatant;Centrifugation rate time centrifugal is 1800r/min;
S3. adding dehydrated alcohol to the volume fraction of ethanol toward described supernatant is 60%, staticly settles polysaccharide and high molecular weight protein, centrifugal segregation precipitate polysaccharides and high molecular weight protein, retains upper liquid;
S4. select the ultrafilter membrane of molecular cut off 3000Da, described upper liquid is carried out ultrafiltration, in the trapped fluid obtained, add the antioxidation antibacterial of total solid matter weight 0.01% and stir;Described antioxidation antibacterial is tea polyphenols and curcumin with the composite compositions of weight ratio 1: 2;
S5. described trapped fluid reclaims ethanol, the spray-dried prepared abnormal smells from the patient Stichopus japonicus small-molecular peptides dry powder of hardship without raw meat under vacuum and low temperature.
Embodiment 4, the present invention are without the preparation method of raw meat hardship abnormal smells from the patient Macrobrachium nipponensis small-molecular peptides
S1. the Macrobrachium nipponensis enzymolysis solution prepared by enzymatic isolation method, after 100 DEG C of enzyme denaturing, is concentrated into total solid matter 25%, obtains treatment fluid;
S2. described treatment fluid is cooled to 8 DEG C, the floating oils and fats in centrifugal segregation upper strata and bottom impurity, retain supernatant;Centrifugation rate time centrifugal is 2000r/min;
S3. adding dehydrated alcohol to the volume fraction of ethanol toward described supernatant is 70%, staticly settles polysaccharide and high molecular weight protein, centrifugal segregation precipitate polysaccharides and high molecular weight protein, retains upper liquid;
S4. select the ultrafilter membrane of molecular cut off 2000Da, described upper liquid is carried out ultrafiltration, in the trapped fluid obtained, add the antioxidation antibacterial of total solid matter weight 0.05% and stir;Described antioxidation antibacterial is tea polyphenols and curcumin with the composite compositions of weight ratio 1: 3;
S5. described trapped fluid reclaims ethanol, the spray-dried prepared abnormal smells from the patient Macrobrachium nipponensis small-molecular peptides dry powder of hardship without raw meat under vacuum and low temperature.
Embodiment 5, the present invention are without the preparation method of raw meat hardship abnormal smells from the patient Carnis Haliotidis small-molecular peptides
S1. the Carnis Haliotidis meat enzymolysis solution prepared by enzymatic isolation method, after 100 DEG C of enzyme denaturing, is concentrated into total solid matter 40%, obtains treatment fluid;
S2. described treatment fluid is cooled to 4 DEG C, the floating oils and fats in centrifugal segregation upper strata and bottom impurity, retain supernatant;Centrifugation rate time centrifugal is 1600r/min;
S3. adding dehydrated alcohol to the volume fraction of ethanol toward described supernatant is 50%, staticly settles polysaccharide and high molecular weight protein, centrifugal segregation precipitate polysaccharides and high molecular weight protein, retains upper liquid;
S4. select the ultrafilter membrane of molecular cut off 4000Da, described upper liquid is carried out ultrafiltration, in the trapped fluid obtained, add the antioxidation antibacterial of total solid matter weight 0.006% and stir;Described antioxidation antibacterial is tea polyphenols and curcumin with the composite compositions of weight ratio 1: 2;
S5. described trapped fluid reclaims ethanol, the spray-dried prepared abnormal smells from the patient Carnis Haliotidis small-molecular peptides dry powder of hardship without raw meat under vacuum and low temperature.
Embodiment 6, the present invention are without the preparation method of raw meat hardship abnormal smells from the patient mussel small-molecular peptides
S1. the mussel meat enzymolysis solution prepared by enzymatic isolation method, after 100 DEG C of enzyme denaturing, is concentrated into total solid matter 20%, obtains treatment fluid;
S2. described treatment fluid is cooled to 10 DEG C, the floating oils and fats in centrifugal segregation upper strata and bottom impurity, retain supernatant;Centrifugation rate time centrifugal is 1600r/min;
S3. adding dehydrated alcohol to the volume fraction of ethanol toward described supernatant is 80%, staticly settles polysaccharide and high molecular weight protein, centrifugal segregation precipitate polysaccharides and high molecular weight protein, retains upper liquid;
S4. select the ultrafilter membrane of molecular cut off 5000Da, described upper liquid is carried out ultrafiltration, in the trapped fluid obtained, add the antioxidation antibacterial of total solid matter weight 0.1% and stir;Described antioxidation antibacterial is tea polyphenols and curcumin with the composite compositions of weight ratio 1: 2;
S5. described trapped fluid reclaims ethanol, the spray-dried prepared abnormal smells from the patient mussel small-molecular peptides dry powder of hardship without raw meat under vacuum and low temperature.
Embodiment 7, the present invention are without the preparation method of raw meat hardship abnormal smells from the patient tuna small-molecular peptides
S1. the tuna enzymolysis solution prepared by enzymatic isolation method, after 100 DEG C of enzyme denaturing, is concentrated into total solid matter 20%, obtains treatment fluid;
S2. described treatment fluid is cooled to 10 DEG C, the floating oils and fats in centrifugal segregation upper strata and bottom impurity, retain supernatant;Centrifugation rate time centrifugal is 2000r/min;
S3. adding dehydrated alcohol to the volume fraction of ethanol toward described supernatant is 50%, staticly settles polysaccharide and high molecular weight protein, centrifugal segregation precipitate polysaccharides and high molecular weight protein, retains upper liquid;
S4. select the ultrafilter membrane of molecular cut off 1000Da, described upper liquid is carried out ultrafiltration, in the trapped fluid obtained, add the antioxidation antibacterial of total solid matter weight 0.1% and stir;Described antioxidation antibacterial is tea polyphenols and curcumin with the composite compositions of weight ratio 1: 3;
S5. described trapped fluid reclaims ethanol under vacuum and low temperature, and drying prepares without raw meat hardship abnormal smells from the patient tuna small-molecular peptides dry powder.
Embodiment 8, the present invention are without the preparation method of raw meat hardship abnormal smells from the patient morrhua small-molecular peptides
S1. the codfish enzymolysis solution prepared by enzymatic isolation method, after 100 DEG C of enzyme denaturing, is concentrated into total solid matter 30%, obtains treatment fluid;
S2. described treatment fluid is cooled to 5 DEG C, the floating oils and fats in centrifugal segregation upper strata and bottom impurity, retain supernatant;Centrifugation rate time centrifugal is 1800r/min;
S3. adding dehydrated alcohol to the volume fraction of ethanol toward described supernatant is 60%, staticly settles polysaccharide and high molecular weight protein, centrifugal segregation precipitate polysaccharides and high molecular weight protein, retains upper liquid;
S4. select the ultrafilter membrane of molecular cut off 5000Da, described upper liquid is carried out ultrafiltration, in the trapped fluid obtained, add the antioxidation antibacterial of total solid matter weight 0.03% and stir;Described antioxidation antibacterial is tea polyphenols and curcumin with the composite compositions of weight ratio 1: 2.5;
S5. described trapped fluid reclaims ethanol under vacuum and low temperature, and drying prepares without raw meat hardship abnormal smells from the patient morrhua small-molecular peptides dry powder.
Embodiment 9, the present invention are without the preparation method of raw meat hardship abnormal smells from the patient tilapia small-molecular peptides
S1. the Tilapia enzymolysis solution prepared by enzymatic isolation method, after 100 DEG C of enzyme denaturing, is concentrated into total solid matter 35%, obtains treatment fluid;
S2. described treatment fluid is cooled to 7 DEG C, the floating oils and fats in centrifugal segregation upper strata and bottom impurity, retain supernatant;Centrifugation rate time centrifugal is 1600r/min;
S3. adding dehydrated alcohol to the volume fraction of ethanol toward described supernatant is 70%, staticly settles polysaccharide and high molecular weight protein, centrifugal segregation precipitate polysaccharides and high molecular weight protein, retains upper liquid;
S4. select the ultrafilter membrane of molecular cut off 1000Da, described upper liquid is carried out ultrafiltration, in the trapped fluid obtained, add the antioxidation antibacterial of total solid matter weight 0.007% and stir;Described antioxidation antibacterial is tea polyphenols and curcumin with the composite compositions of weight ratio 1: 3;
S5. described trapped fluid reclaims ethanol, the spray-dried prepared abnormal smells from the patient tilapia small-molecular peptides dry powder of hardship without raw meat under vacuum and low temperature.
Comparative example 1
Compared with embodiment 1, this comparative example is distinctive in that: step S2 treatment fluid, without cooling, is centrifuged under direct room temperature, and observing centrifugal rear middle level is emulsion.Other parameters and operation are with embodiment 6.
Comparative example 2
Compared with embodiment 1, this comparative example is distinctive in that: it is 30% that step S3 adds dehydrated alcohol to the volume fraction of ethanol toward described supernatant.Other parameters and operation are with embodiment 6.
Comparative example 3
Compared with embodiment 1, this comparative example is distinctive in that: be used alone tea polyphenols as antioxidation antibacterial.Other parameters and operation are with embodiment 6.
Comparative example 4
Compared with embodiment 1, this comparative example is distinctive in that: be used alone curcumin as antioxidation antibacterial.Other parameters and operation are with embodiment 6.
Comparative example 5
Compared with embodiment 1, this comparative example is distinctive in that: the weight ratio 1: 1 of tea polyphenols and curcumin.Its other parameters and operation are with embodiment 6.
Comparative example 6
Compared with embodiment 1, this comparative example is distinctive in that: the weight ratio 1: 4 of tea polyphenols and curcumin.Its other parameters and operation are with embodiment 6.
Test example one
The finished product of above-described embodiment 1~9 and comparative example 1~6 is dissolved into 15% aqueous solution, adopts fish-stench and the raw meat bitterness value of each sample after sensory evaluation method evaluation and test eliminating sargassum smell.
According to modern food sensory evaluation method, respectively stink smell and fishy smell are judged.Judged by 10 subjective appreciation persons, adopt and first hear the mode tasted afterwards, give a mark to the fishy odor of laboratory sample respectively, score principle is full marks 5 points, using deionized water as without with reference to (score value is for 0 point), untreated enzymolysis stock solution is full marks reference (score value is 5 points), and score value is more big, then sample fishy odor is more heavy, and concrete standards of grading see attached list shown in 1.Result sees attached list shown in 2.
The fishy odor standards of grading of subordinate list 1 sample
The fishy odor appraisal result of subordinate list 2 each sample
Project Fish-stench score value Raw meat bitterness score value
Embodiment 1 1.0±0.3 0.5±0.3
Embodiment 2 0.8±0.2 0.7±0.4
Embodiment 3 0.7±0.3 0.8±0.4
Embodiment 4 1.9±0.6 1.5±0.6
Embodiment 5 1.7±0.4 0.7±0.2
Embodiment 6 0.8±0.3 0.5±0.2
Embodiment 7 1.3±0.5 0.8±0.3
Embodiment 8 1.6±0.4 0.7±0.3
Embodiment 9 1.5±1.0 0.7±0.2
Comparative example 1 3.0±0.9 2.4±0.7
Comparative example 2 4.3±1.0 3.0±0.8
Comparative example 3 1.3±0.3 0.9±0.4
Comparative example 4 2.0±0.6 1.2±0.5
Comparative example 5 1.5±0.4 1.0±0.2
Comparative example 6 1.9±0.4 1.3±0.3
From subordinate list 2:
(1) preparation method of the present invention can effectively remove fish-stench and the raw meat bitterness of the aquatic animals such as fish, shrimp, mussel, Stichopus japonicus, and fish-stench score value is all below 2, and fish-stench is gently or very gently, raw meat bitterness score value is below 1.5, and raw meat bitterness is very light.
(2) comparative example 1 treatment fluid is centrifuged at normal temperatures, comparative example 2 changes ethanol volume during precipitate with ethanol, the fish-stench of its prepared product is improved compared with embodiment 1 with raw meat bitterness score value, illustrates that in preparation method of the present invention, the change of certain parameter all can affect the removal effect of fish-stench and raw meat bitterness.
(3) comparative example 3~6 changes kind and the ratio of antioxidation antibacterial, the fish-stench of its product also all has raising in various degree with raw meat bitterness score value compared with embodiment 1, illustrates that antioxidation antibacterial of the present invention can remove fish-stench and raw meat bitterness to a certain extent.
Test example two
The finished product of above-described embodiment 1~9 and comparative example 1~6 is dissolved into 15% aqueous solution, measure trimethylamine content, and detect the situation of change of different shelf time trimethylamine, simultaneously to be not added with the product of antioxidation antibacterial as blank control sample (being specifically shown in Fig. 1~15).
From Fig. 1~9, aquatic animal small-molecular peptides product (blank control sample) content of the property material trimethylamine of bad smell in shelf time being not added with antioxidation antibacterial of the present invention is significantly raised, with the addition of the aquatic animal small-molecular peptides product (embodiment sample) of antioxidation antibacterial of the present invention then slightly to rise, compared to blank control sample, antioxidation antibacterial of the present invention microorganism such as antibacterial in effective and long-acting suppression product or enzyme effect can produce trimethylamine.
Comparative example 3 uses tea polyphenols as antioxidation antibacterial, to the certain effect that has suppressing trimethylamine, but not as good as embodiment 1 (being specifically shown in Figure 12);Comparative example 4 uses curcumin as antioxidation antibacterial, and the generation of trimethylamine is substantially free of inhibition (being specifically shown in Figure 13);Comparative example 5 and 6 changes the ratio of antioxidation antibacterial of the present invention, and compared to embodiment 1, the inhibition of trimethylamine is deteriorated (being specifically shown in Figure 14 and 15) by it.
Below being only the preferred embodiment of the present invention, it is noted that above-mentioned preferred implementation is not construed as limitation of the present invention, protection scope of the present invention should be as the criterion with claim limited range.For those skilled in the art, without departing from the spirit and scope of the present invention, it is also possible to make some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.

Claims (5)

1. the preparation method without raw meat hardship abnormal smells from the patient aquatic animal small-molecular peptides, it is characterised in that comprise the following steps:
S1. the aquatic animal enzymolysis solution prepared by enzymatic isolation method, after enzyme denaturing, is concentrated into total solid matter 20~40%, obtains treatment fluid;
S2. described treatment fluid is cooled to 10~4 DEG C, the floating oils and fats in centrifugal segregation upper strata and bottom impurity, retain supernatant;
S3. adding ethanol to the volume fraction of ethanol toward described supernatant is 50~80%, staticly settles polysaccharide and high molecular weight protein, centrifugal segregation precipitate polysaccharides and high molecular weight protein, retains upper liquid;
S4. select the ultrafilter membrane of molecular cut off 1000~5000Da, described upper liquid is carried out ultrafiltration, in the trapped fluid obtained, add the antioxidation antibacterial of total solid matter weight 0.001~0.1% and stir;
S5. described trapped fluid reclaims ethanol under vacuum and low temperature, and drying prepares without raw meat hardship abnormal smells from the patient aquatic animal small-molecular peptides dry powder.
2. as claimed in claim 1 without the preparation method of raw meat hardship abnormal smells from the patient aquatic animal small-molecular peptides, it is characterised in that centrifugation rate time centrifugal in described step S2 is 1600~2000r/min.
3. as claimed in claim 1 without the preparation method of raw meat hardship abnormal smells from the patient aquatic animal small-molecular peptides, it is characterised in that the ethanol in described step S3 is dehydrated alcohol.
4. as claimed in claim 1 without the preparation method of raw meat hardship abnormal smells from the patient aquatic animal small-molecular peptides, it is characterised in that described antioxidation antibacterial is the compositions of tea polyphenols and curcumin.
5. as claimed in claim 4 without the preparation method of raw meat hardship abnormal smells from the patient aquatic animal small-molecular peptides, it is characterised in that the weight ratio of described tea polyphenols and curcumin is 1: (2~3).
CN201610311734.0A 2016-05-10 2016-05-10 Method for preparing aquatic livestock small molecule peptide without fishy smell or bitter taste Pending CN105803023A (en)

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CN111109552A (en) * 2020-01-03 2020-05-08 中国海洋大学 Preparation method of oyster full nutrition powder capable of removing fishy smell and bitter taste

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CN103981246A (en) * 2014-05-30 2014-08-13 广东海洋大学 Method for extracting bitter peptides from fish protein enzymolysis solution

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111109552A (en) * 2020-01-03 2020-05-08 中国海洋大学 Preparation method of oyster full nutrition powder capable of removing fishy smell and bitter taste
CN111109552B (en) * 2020-01-03 2022-06-21 中国海洋大学 Preparation method of oyster full nutrition powder capable of removing fishy smell and bitter taste

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Application publication date: 20160727