CN109593599A - A kind of extracting method of clam quasi-grease and protein - Google Patents
A kind of extracting method of clam quasi-grease and protein Download PDFInfo
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- CN109593599A CN109593599A CN201811620561.6A CN201811620561A CN109593599A CN 109593599 A CN109593599 A CN 109593599A CN 201811620561 A CN201811620561 A CN 201811620561A CN 109593599 A CN109593599 A CN 109593599A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
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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
- C07K1/145—Extraction; Separation; Purification by extraction or solubilisation
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Medicinal Chemistry (AREA)
- Molecular Biology (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Genetics & Genomics (AREA)
- General Health & Medical Sciences (AREA)
- Biophysics (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Meat, Egg Or Seafood Products (AREA)
Abstract
The invention discloses the extracting methods of a kind of clam quasi-grease and protein, using Important Economic type shellfish clam as raw material, by taking meat, are homogenized, are freeze-dried and crush 40~80 mesh clam meal of acquisition.Utilize supercritical CO2Extract the grease in clam meal.The residual powder after extraction grease is used to clam albuminoid therewith to extract, clam proteinoid is obtained after freeze-drying.The present invention is based on supercritical CO for the first time2It extracts and combines physics extraction method effective acquisition clam nutrition component protein matter and grease.Clam quasi-grease obtained by this method clarifies bright, stay in grade, avoids the loss of oxidation deterioration and Heat sensitive active ingredient, and gained clam class high-quality protein is undenatured, character is stablized, and quality is good, it can be used for the exploitation of high value added product, to realize the higher value application of low value clam class.
Description
Technical field
The present invention relates to protein and grease processing technology field, more specifically to a kind of clam quasi-grease and albumen
The extracting method of matter.
Background technique
Clam class is ranked first of the big cultivated shellfish in China four, and national yield is more than 4,000,000 tons within 2017.Its nutritive value compared with
The type composition and ratio of height, rich in protein, amino acid are reasonable, easily digested;Calcic, magnesium, iron, zinc etc.
The nutrients such as a variety of mineral elements and micro-element needed by human can be used as the nutrient source and healthy food of the mankind, deep to be consumed
The favor of person.Clam class is rich in phosphatide type ω -3 long-chain polyunsaturated fatty acid simultaneously, for prevention " three high " and cardiovascular and cerebrovascular disease
Disease has good effect.
However, due to the high easily corrupt deterioration of the aquatic products such as clam class water content, it is difficult to the characteristics of transporting and storing, consumption master
Coastal area is concentrated on, hinterland market is not yet opened on a large scale.Clam class product especially high value added product in the market
Relatively deficient, clam class resource is not utilized effectively.Therefore clam class be good marine animal albumen and active grease it is good come
Source can be used for the exploitation of high value added product.
Traditional animal protein and grease extracting mode mostly uses organic solvent extraction, be easy to cause albuminous degeneration and
Dissolvent residual, for food production, there are some potential safety problemss, and reduce the quality and stability of product.
Summary of the invention
The present invention is directed to the main nutrient composition protein of effective acquisition clam class and greases, and keep its physicochemical property and life
Object activity is constant.
In order to reach above-mentioned target, the present invention provides a kind of based on supercritical CO2Extraction combines the green of inorganic physical method
Extracting method obtains above two nutrient, makes its higher value application.
A kind of extracting method of clam quasi-grease and protein, includes the following steps:
S1, using clam class as raw material, take clam meat homogenate, vacuum freeze drying, make products therefrom moisture content lower than 10%;
The product that S2, step S1 are obtained crosses 40~80 meshes, obtains clam meal after crushing;
S3, under the conditions of 20~30Mpa of Fluid pressure, 30~50 DEG C of extraction temperature, 1~3h of extraction time, supercritical CO2
Grease in extraction step S1 clam meal;Wherein, by supercritical CO2Clam meal after oil and grease extracting is known as residual powder;
S4, residual powder obtained by S3 is mixed by the w/v of 1kg/ (20~30) L with distilled water, and adjusts pH with NaOH
After 10~13,2~6 DEG C of value sufficiently impregnates 2~3h, it is centrifuged to obtain supernatant A and precipitate A;
S5, precipitate A is mixed by the w/v of 1kg/ (3~4) L with distilled water, and with NaOH adjusting pH value 11~
13,2~6 DEG C, 100~300rpm/min at the uniform velocity stir 0.5~2h, be centrifuged to obtain supernatant B and precipitate B;
S6, supernatant A and supernatant B are mixed into obtain supernatant C, HCl is added to adjust pH value to 3.5~5.0,2-6 DEG C of standing
After 25~40min, supernatant D is taken, supernatant D is centrifuged to obtain precipitate C by gained;
S7, by precipitate C through vacuum freeze drying, obtain clam proteinoid.
Under preferred embodiment, the actual conditions of homogenate described in step S1 are as follows: 6000~8000rpm/min of revolving speed, when homogenate
Between 3~5min;The clam class is clam, clam or Ruditapes philippinarum;The vacuum freeze drying specifically: -50 DEG C, 2~
4h, -40 DEG C, 3~5h, -30 DEG C, 3~6h, -20 DEG C, 5~10h, -10 DEG C, 5~15h, 0 DEG C, 10~15h, 5 DEG C, 10~15h,
10 DEG C, 10~15h.
It under preferred embodiment, is centrifuged described in step S4 are as follows: 4 DEG C, 5000~8000 × g, 10~20min of centrifugation.
It under preferred embodiment, is centrifuged described in step S5 are as follows: 4 DEG C, 5000~8000 × g, 10~20min of centrifugation.
It under preferred embodiment, is centrifuged described in step S6 are as follows: 4 DEG C, 5000~8000 × g, 10~20min of centrifugation.
Vacuum freeze drying described in step S7 specifically: -50 DEG C, 2~4h, -40 DEG C, 3~5h, -30 DEG C, 3~6h, -20
DEG C, 5~10h, -10 DEG C, 5~15h, 0 DEG C, 10~15h, 5 DEG C, 10~15h, 10 DEG C, 10~15h.
Under preferred embodiment, the extracting method of the clam quasi-grease and protein includes the following steps:
S1, it takes clam meat, be homogenized 5min under the conditions of 7000rpm/min, and utilizing vacuum freeze drying, obtaining moisture content
Freeze-drying sample lower than 10%;The vacuum freeze drying are as follows: -50 DEG C, 2h, -40 DEG C, 3h, -30 DEG C, 5h, -20 DEG C, 5h, -10
DEG C, 5h, 0 DEG C, 10h, 5 DEG C, 15h, 10 DEG C, 15h.
S2,80 meshes will be crossed after step S1 obtained freeze-drying sample comminution, obtain clam freeze-dried powder;
S3,300g clam freeze-dried powder is taken, utilizes supercritical CO2Abstraction instrument extracting pressure 30Mpa, 50 DEG C of extraction temperature,
Extraction time 1.5h extracts grease;Wherein, by supercritical CO2Clam meal after oil and grease extracting is known as residual powder;
S4, residual powder obtained by step S3 is taken out from extraction kettle, is mixed by the w/v of 1kg/25L with distilled water,
And 11,2 DEG C of immersion 3h of pH value are adjusted with NaOH, supernatant A and precipitate A are obtained in 6000 × g, 4 DEG C of centrifugation 20min;
S5, precipitate A obtained by step S4 is mixed by the w/v of 1kg/3L with distilled water, and adjusts pH value with NaOH
12,6 DEG C, 200rpm stirring 2h, are centrifuged to obtain supernatant B and precipitate B;
S6, supernatant B obtained by supernatant A obtained by step S4 and step S5 is mixed into obtain supernatant C, HCl is added to adjust pH value
Supernatant D is obtained after to 4.0,6 DEG C of standing 30min, and supernatant D is obtained into precipitate C after 6000 × g, 6 DEG C of centrifugation 20min;
S7, precipitate C obtained by step S6 is passed through into vacuum freeze drying, obtains clam albumen;The vacuum freeze drying are as follows:-
50 DEG C, 2h, -40 DEG C, 3h, -30 DEG C, 5h, -20 DEG C, 5h, -10 DEG C, 5h, 0 DEG C, 10h, 5 DEG C, 15h, 10 DEG C, 15h.
The beneficial effects of the present invention are:
1, it is based on supercritical CO2In the clam quasi-grease that abstraction technique obtains polyunsaturated fatty acid ratio be up to 40.2~
47.4%, and the technique on protein physicochemical property without influence;
2, the residual powder of clam class after lipid extraction extracts protein, and purity is up to 82.6~87.8%, and character is stablized,
Without denaturation;
3, the clam quasi-grease in conjunction with obtained by above-mentioned technique and protein can be respectively used to food development, and low value clam class may be implemented
Higher value application.
Specific embodiment
Below by specific implementation example, the present invention will be further described.
Embodiment 1:
S1, using Ruditapes philippinarum as raw material, being peeled off, it is dry that 3min, vacuum refrigeration are homogenized under the conditions of taking meat, 8000rpm/min
It is dry, obtain the freeze-drying sample that moisture content is 6.92%;The design parameter of vacuum freeze drying be -50 DEG C, 4h, -40 DEG C, 5h, -30
DEG C, 6h, -20 DEG C, 10h, -10 DEG C, 10h, 0 DEG C, 10h, 5 DEG C, 10h, 10 DEG C, 15h;
S2, by step S1 obtained freeze-drying sample comminution, cross 60 meshes, obtain Ruditapes philippinarum freeze-dried powder;
S3,300g Ruditapes philippinarum freeze-dried powder is taken, utilizes supercritical CO2Abstraction instrument is in extracting pressure 20MPa, extraction temperature
40 DEG C, extraction time 2h, extract to obtain grease 10.85g, yield 3.62%;
S4, residual powder obtained by step S3 is taken out from extraction kettle, is mixed by the w/v of 1kg/20L with distilled water,
And be adjusted to after 11,4 DEG C of pH value sufficiently impregnates 2h with NaOH, 5000 × g centrifugation 15min obtains supernatant A and precipitate A;
S5, precipitate A obtained by step S4 is mixed by the w/v of 1kg/3L with distilled water, and adjusts pH value with NaOH
12,4 DEG C, 100rpm stir 1h, 5000 × g centrifugation 20min obtain supernatant B and precipitate B;
S6, supernatant B obtained by supernatant A obtained by step S4 and step S5 is mixed into obtain supernatant C, HCl is added to adjust pH value
Supernatant D is taken after to 3.5,4 DEG C of standing 25min, obtains precipitate C after 5000 × g of supernatant D is centrifuged 15min;
S7, gained precipitate C in step S6 is passed through into vacuum freeze drying, grinding obtains philippine clam albumen, undenatured
And measuring its purity through kjeldahl determination is 82.6%;The design parameter of vacuum freeze drying be -50 DEG C, 4h, -40 DEG C, 5h, -30
DEG C, 6h, -20 DEG C, 10h, -10 DEG C, 10h, 0 DEG C, 10h, 5 DEG C, 10h, 10 DEG C, 15h.
Embodiment 2:
S1, using clam as raw material, peel off and meat, gained clam meat taken to be homogenized 4min under the conditions of 6000rpm/min, and using true
Vacuum freecing-dry freeze-drying, obtained freeze-drying sample moisture content are 6.43%;The design parameter of the vacuum freeze drying is -50
DEG C, 2h, -40 DEG C, 3h, -30 DEG C, 3h, -20 DEG C, 10h, -10 DEG C, 15h, 0 DEG C, 15h, 5 DEG C, 10h, 10 DEG C, 10h;
S2, by after step S1 obtained freeze-drying sample comminution, cross 70 meshes, obtain clam freeze-dried powder;
S3,300g clam freeze-dried powder is taken, utilizes supercritical CO2Abstraction instrument is in extracting pressure 25MPa, and 30 DEG C of extraction temperature,
Grease 12.98g, yield 4.33% is obtained by extraction under the conditions of being 3h in extraction time;
S4, the resulting residual powder of step S3 is taken out from extraction kettle, it is mixed by the w/v and distilled water of 1kg/30L
It closes, and with after 13,6 DEG C of sufficiently submergence 2.5h of NaOH adjusting pH value, obtains supernatant A and precipitating in 8000 × g, 6 DEG C of centrifugation 10min
A;
S5, precipitate A obtained by step S4 is mixed by the w/v of 1kg/4L with distilled water, and adjusts pH value with NaOH
12,4 DEG C, 300rpm stir 1.5h, 8000g centrifugation 10min obtain supernatant B and precipitate B;
S6, supernatant A and B are mixed into obtain supernatant C, obtains supernatant after adding HCl to adjust pH value to 5.0,4 DEG C of standing 40min
Liquid D obtains precipitate C after supernatant D to be centrifuged to 10min at 8000 × g, 4 DEG C;
S7, gained precipitate C in step S6 is crushed after vacuum freeze drying and obtains clam albumen powder, quality is good
Good, without denaturation, and measuring purity through kjeldahl determination is 86.8%;The design parameter of the vacuum freeze drying be -50 DEG C,
2h, -40 DEG C, 3h, -30 DEG C, 3h, -20 DEG C, 10h, -10 DEG C, 15h, 0 DEG C, 15h, 5 DEG C, 10h, 10 DEG C, 10h.
Embodiment 3:
S1, using clam as raw material, take clam meat, gained clam meat to be homogenized 5min under the conditions of 7000rpm/min by peeling off, and
The freeze-drying sample that moisture content is 7.23% is obtained by vacuum freeze drying;The design parameter of the vacuum freeze drying is -50
DEG C, 2h, -40 DEG C, 3h, -30 DEG C, 5h, -20 DEG C, 5h, -10 DEG C, 5h, 0 DEG C, 10h, 5 DEG C, 15h, 10 DEG C, 15h;
S2, by after above-mentioned freeze-drying sample comminution, cross 80 meshes, obtain clam freeze-dried powder;
S3,300g clam freeze-dried powder is taken, utilizes supercritical CO2Abstraction instrument is in extracting pressure 30MPa, and 50 DEG C of extraction temperature,
Grease 15.48g is obtained by extraction under the conditions of being 1.5h in extraction time, and calculating yield is 5.16%;
S4, residual powder obtained by step S3 is taken out from extraction kettle, is mixed by the mass volume ratio of 1kg/25L with distilled water,
And with after 11,2 DEG C of sufficiently submergence 3h of NaOH adjusting pH value, 20min is centrifuged at 6000 × g, 4 DEG C and obtains supernatant A and precipitate A;
S5, precipitate A is mixed by the w/v of 1kg/3L with distilled water, and with 12,6 DEG C of pH value of NaOH adjusting,
Supernatant B and precipitate B are obtained after 200rpm stirring and leaching 2h;
S6, supernatant A and B are mixed into obtain supernatant C, obtains supernatant after adding HCl to adjust pH value to 4.0,6 DEG C of standing 30min
Liquid D obtains precipitate C after supernatant D to be centrifuged to 20min at 6000 × g, 6 DEG C;
S7, gained precipitate C in step S6 to be passed through into vacuum freeze drying, obtains clam albumen, physical characteristic is stablized, without
Denaturation, and measuring its purity through kjeldahl determination is 87.8%, the design parameter of the vacuum freeze drying are -50 DEG C, 2h, -40
DEG C, 3h, -30 DEG C, 5h, -20 DEG C, 5h, -10 DEG C, 5h, 0 DEG C, 10h, 5 DEG C, 15h, 10 DEG C, 15h.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art within the technical scope of the present disclosure, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (9)
1. a kind of extracting method of clam quasi-grease and protein, which comprises the steps of:
S1, it takes the meat of clam class by homogenate, vacuum freeze drying, makes products therefrom moisture content lower than 10%;
S2, the product for obtaining step S1 crush, and cross 40~80 meshes, obtain clam meal;
S3, supercritical CO2Grease in clam meal obtained by extraction step S2, design parameter are as follows: 20~30Mpa of Fluid pressure, extraction temperature
30~50 DEG C, 1~3h of extraction time are spent, obtains grease and residual powder respectively;
S4, the residual powder in step S3 is mixed according to the w/v of 1kg/ (20~30) L with distilled water, adjusting pH value 10~
13,2~6 DEG C of 2~3h of immersion, are centrifuged to obtain supernatant A and precipitate A;
S5, precipitate A obtained by step S4 is mixed by the w/v of 1kg/ (3~4) L with distilled water, adjusts pH value 11~13,
2~6 DEG C, 100~300rpm/min, 0.5~2h of stirring, are centrifuged to obtain supernatant B and precipitate B;
S6, supernatant B obtained by supernatant A obtained by step S4 and step S5 is mixed, obtains supernatant C, adjusts supernatant C pH value
To 3.5~5.0,2~6 DEG C of 25~40min of standing, supernatant D is obtained;Gained supernatant D is centrifuged to obtain precipitate C;
S7, by precipitate C vacuum freeze drying obtained by step S6, obtain clam proteinoid.
2. the extracting method of clam quasi-grease and protein according to claim 1, which is characterized in that clam class described in the S1 is
Clam, clam or Ruditapes philippinarum.
3. the extracting method of clam quasi-grease and protein according to claim 1, which is characterized in that be homogenized tool described in step S1
Body are as follows: 6000~8000rpm/min of revolving speed, 3~5min of Homogenization time.
4. the extracting method of clam quasi-grease and protein according to claim 1, which is characterized in that vacuum described in step S1 is cold
It is lyophilized dry specifically: -50 DEG C, 2~4h, -40 DEG C, 3~5h, -30 DEG C, 3~6h, -20 DEG C, 5~10h, -10 DEG C, 5~15h, 0
DEG C, 10~15h, 5 DEG C, 10~15h, 10 DEG C, 10~15h.
5. the extracting method of clam quasi-grease and protein according to claim 1, which is characterized in that be centrifuged tool described in step S4
Body are as follows: 4 DEG C, 5000~8000 × g, 10~20min of centrifugation.
6. the extracting method of clam quasi-grease and protein according to claim 1, which is characterized in that be centrifuged tool described in step S5
Body are as follows: 4 DEG C, 5000~8000 × g, 10~20min of centrifugation.
7. the extracting method of clam quasi-grease and protein according to claim 1, which is characterized in that be centrifuged tool described in step S6
Body are as follows: 4 DEG C, 5000~8000 × g, 10~20min of centrifugation.
8. the extracting method of clam quasi-grease and protein according to claim 1, which is characterized in that vacuum described in step S7 is cold
It is lyophilized dry specifically: -50 DEG C, 2~4h, -40 DEG C, 3~5h, -30 DEG C, 3~6h, -20 DEG C, 5~10h, -10 DEG C, 5~15h, 0
DEG C, 10~15h, 5 DEG C, 10~15h, 10 DEG C, 10~15h.
9. the extracting method of clam quasi-grease and protein according to claim 1, which comprises the steps of:
S1, it takes clam meat, be homogenized 5min under the conditions of 7000rpm/min, obtaining moisture content using vacuum freeze drying and be lower than
10% sample;The vacuum freeze drying are as follows: 50 DEG C, 2h, -40 DEG C, 3h, -30 DEG C, 5h, -20 DEG C, 5h, -10 DEG C, 5h, 0
DEG C, 10h, 5 DEG C, 15h, 10 DEG C, 15h;
S2,80 meshes will be crossed after step S1 obtained freeze-drying sample comminution, obtain clam freeze-dried powder;
S3, clam freeze-dried powder obtained by 300g step S2 is taken, utilizes supercritical CO2Abstraction instrument is in extracting pressure 30Mpa, extraction temperature
50 DEG C, extraction time be 1.5h under the conditions of extract grease;
S4, residual powder is taken out from extraction kettle, is mixed by the w/v of 1kg/25L with distilled water, and adjust pH with NaOH
11,2 DEG C of immersion 3h of value obtain supernatant A and precipitate A in 6000 × g, 4 DEG C of centrifugation 20min;
S5, precipitate A obtained by step S4 is mixed by the w/v of 1kg/3L with distilled water, and adjusts pH value 12,6 with NaOH
DEG C, 200rpm stir 2h, after centrifugation supernatant B and precipitate B;
S6, supernatant B obtained by supernatant A obtained by step S4 and step S5 is mixed into obtain supernatant C, add HCl adjust pH value to
Supernatant D is obtained after 4.0,6 DEG C of standing 30min, and supernatant D is obtained into precipitate C after 6000 × g, 6 DEG C of centrifugation 20min;
S7, by precipitate C vacuum freeze drying obtained by step S6, obtain clam albumen;The vacuum freeze drying are as follows: 50 DEG C, 2h ,-
40 DEG C, 3h, -30 DEG C, 5h, -20 DEG C, 5h, -10 DEG C, 5h, 0 DEG C, 10h, 5 DEG C, 15h, 10 DEG C, 15h.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101965897A (en) * | 2010-10-19 | 2011-02-09 | 浙江大学 | Processing method for mussel isolated protein |
CN106261972A (en) * | 2016-08-22 | 2017-01-04 | 得利斯集团有限公司 | A kind of extracting method of Carnis Mactrae peptide |
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- 2018-12-28 CN CN201811620561.6A patent/CN109593599A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101965897A (en) * | 2010-10-19 | 2011-02-09 | 浙江大学 | Processing method for mussel isolated protein |
CN106261972A (en) * | 2016-08-22 | 2017-01-04 | 得利斯集团有限公司 | A kind of extracting method of Carnis Mactrae peptide |
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Application publication date: 20190409 |