CN113265010A - Salmon proteoglycan extraction process - Google Patents
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- CN113265010A CN113265010A CN202110402952.6A CN202110402952A CN113265010A CN 113265010 A CN113265010 A CN 113265010A CN 202110402952 A CN202110402952 A CN 202110402952A CN 113265010 A CN113265010 A CN 113265010A
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- 235000012211 aluminium silicate Nutrition 0.000 claims description 6
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 6
- 108090000526 Papain Proteins 0.000 claims description 5
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- 102000004142 Trypsin Human genes 0.000 claims description 5
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- SQDAZGGFXASXDW-UHFFFAOYSA-N 5-bromo-2-(trifluoromethoxy)pyridine Chemical compound FC(F)(F)OC1=CC=C(Br)C=N1 SQDAZGGFXASXDW-UHFFFAOYSA-N 0.000 description 3
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- GVJHHUAWPYXKBD-UHFFFAOYSA-N d-alpha-tocopherol Natural products OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
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- 229940111202 pepsin Drugs 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
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- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Sustainable Development (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Meat, Egg Or Seafood Products (AREA)
Abstract
The invention relates to a salmon proteoglycan extraction process, which comprises the following raw materials: the extraction method of salmon head cartilage comprises the following steps: (1) pretreatment of raw materials: cleaning salmon head, boiling in clear water for 3-4h, cooling the boiled fish head cartilage, washing off residues on the surface by using clear water, drying the washed fish head cartilage in a blast drier to constant weight, crushing the dried fish head cartilage by using a crusher, and further crushing the crushed fish head cartilage by using a superfine crusher to obtain fish head cartilage superfine powder; (2) alkali extraction: weighing a certain mass of fish head cartilage superfine powder, adding a 5% NaOH solution, and extracting for 12h in a shaking table; (3) ultrasonic: the solution after alkali extraction is extracted with the assistance of ultrasonic waves. The method adopts the modes of alkali extraction, enzymolysis and alcohol precipitation to extract the proteoglycan in the salmon, reduces the use of reagents, and has higher extraction rate and purity, environmental protection, economy and high product safety.
Description
Technical Field
The invention relates to the technical field of salmon processing, in particular to a salmon proteoglycan extraction process.
Background
Salmon, also known as salmon, migratory fishes, one of world famous economic fish species. Fresh salmon has bright fish scales, complete fish skin, fine and smooth meat and orange red color, and is suitable for being sliced and eaten raw. Salmon is rich in vitamin A, B, D, E and various mineral elements (such as zinc, selenium and phosphorus), and also contains a large amount of polyunsaturated fatty acids which cannot be synthesized by human body, especially omega-3 fatty acids, which are the main components of brain gold and deep sea fish oil and are beneficial to human health. With the enhancement of the health care consciousness of people, the demand of the domestic market for salmon is increasing. The processing and production of the salmon can cause the generation of more leftovers, and improper treatment of a plurality of leftovers not only can cause the waste of resources, but also can cause damage to the environment. The chondroitin sulfate contained in salmon cartilage has various biological activities of increasing bone density, promoting nerve cell division and development, diminishing inflammation, resisting tumor, resisting virus, resisting oxidation, reducing blood fat, improving immunity and the like, can effectively prevent arteriosclerosis of a human body, and can prevent and treat the attack of coronary heart disease. Chondroitin sulfate has become a popular health product additive at present, and is also often used as a dietary supplement for relieving joint discomfort and improving joint pain. Most factories for producing chondroitin sulfate adopt a concentrated alkali method, a dilute alkali method, a neutral salt method and the like, a large amount of salt, alkali and the like can cause pollution to the environment, and the product purity is low.
Disclosure of Invention
The invention aims to provide a salmon proteoglycan extraction process, which extracts proteoglycan in salmon by adopting a mode of alkali extraction-enzymolysis-alcohol precipitation, reduces the use of alkali, salt and the like, increases a decoloring step, improves the purity of a product and solves the problems mentioned in the background technology.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a salmon proteoglycan extraction process comprises the following raw materials: the extraction method of salmon head cartilage comprises the following steps:
(1) pretreatment of raw materials: cleaning salmon head, boiling in clear water for 3-4h, cooling the boiled fish head cartilage, washing off residues on the surface by using clear water, drying the washed fish head cartilage in a blast drier to constant weight, crushing the dried fish head cartilage by using a crusher, and further crushing the crushed fish head cartilage by using a superfine crusher to obtain fish head cartilage superfine powder;
(2) alkali extraction: weighing a certain mass of fish head cartilage superfine powder, adding a 5% NaOH solution, and extracting for 12h in a shaking table;
(3) ultrasonic: extracting the solution after alkali extraction with ultrasonic wave;
(4) centrifugal filtration: centrifuging the solution after ultrasonic extraction in a centrifuge, reserving supernatant for later use, adding 5% NaOH solution into filter residue according to the solid-to-liquid ratio of 1:2, performing ultrasonic-assisted extraction for 1h, reserving supernatant after centrifugal filtration, and combining the filtrates;
(5) enzymolysis: adding acid or alkali solution into the filtrate to adjust the pH value to 8.0-9.0, adding enzyme A according to the solid-liquid ratio of 1:1000, carrying out enzymolysis on the mixed solution at 40-50 ℃ for 2-3h, raising the temperature to 85-90 ℃ after enzymolysis, inactivating for 20-30min, cooling the inactivated solution to room temperature, adjusting the solution, adding enzyme B according to the solid-liquid ratio of 1:1000, carrying out enzymolysis on the mixed solution at 55-65 ℃ for 4-5h, raising the temperature to 85-90 ℃ after enzymolysis, inactivating for 20-30min, and cooling the inactivated solution to room temperature;
(6) and (3) decoloring: performing pressure suction filtration on the solution after enzymolysis, filtering, retaining filtrate, adding an adsorbent into the filtrate for adsorption decolorization, quickly heating to 90 ℃, stirring for 30min, cooling, performing reduced pressure suction filtration, and retaining the filtrate for later use;
(7) alcohol precipitation: adjusting pH of the filtrate to 6.8-7.2, adding 95% ethanol according to a solid-to-liquid ratio of 1:4, precipitating for 9-10h, removing supernatant, washing the precipitate with 95% ethanol for 3-4 times, centrifuging at 6000r/min for 15-20min, and retaining the precipitate after centrifugation;
(8) and (3) drying: collecting precipitate, and oven drying at 60-80 deg.C in an electrothermal constant temperature blast drying oven to obtain salmon proteoglycan.
In the alkali extraction process in the step (2), the addition of NaOH solution is added according to the solid-to-liquid ratio of 1:30, the parameters of the shaking table are set to be 120r/min, and the temperature is 20-30 ℃.
Further, in the ultrasonic process in the step (3), the ultrasonic parameters are set to be 400W of power, the temperature is set to be 45 ℃, and the time is 3-4 h.
Further, the enzyme A is trypsin, and the enzyme B is papain.
Further, the solution in the enzymolysis process in the step (5) is placed in a shaking table, and the rotating speed of the shaking table is 120 r/min.
Further, the adsorbent is activated carbon and kaolin.
After the extraction process is adopted, the invention has the following advantages:
the method adopts the modes of alkali extraction, enzymolysis and alcohol precipitation to extract proteoglycan in the salmon, and compared with the existing extraction modes of a concentrated alkali method, a dilute alkali method, a neutral salt method and the like, the extraction yield is increased, only NaOH solution, ethanol and a small amount of acid and alkali are used for adjusting the pH value, other reagents are not added, the impurity removal step is not added in the extraction process, the method is environment-friendly and economic, and the product safety is high; during alkali extraction, an ultrasonic-assisted extraction link is added, and the filter residue is subjected to secondary extraction, so that the extraction yield of substances can be improved; the invention also adds the step of decolorization, wherein kaolin and active carbon are used for decolorization, no reagent and impurity are introduced, and the final purity of the product is improved; the pepsin is used in a condition that the pH value of the solution is required to be smaller, and a large amount of acid solution is required to be added for regulation during reaction.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example one
A salmon proteoglycan extraction process comprises the following raw materials: the extraction method of salmon head cartilage comprises the following steps:
(1) pretreatment of raw materials: cleaning salmon head, boiling in clear water for 3h, cooling the fish head cartilage, washing off residues on the surface by using clear water, drying the cleaned fish head cartilage in a blast drier to constant weight, crushing the dried fish head cartilage by using a crusher, and further crushing the crushed fish head cartilage by using a superfine crusher to obtain fish head cartilage superfine powder;
(2) alkali extraction: weighing 10kg of fish head cartilage superfine powder, adding 300L of 5% NaOH solution, setting the parameters of a shaker to be 120r/min, setting the temperature to be 20 ℃, and extracting for 12 h;
(3) ultrasonic: extracting the solution subjected to alkali extraction with the assistance of ultrasonic waves, wherein the ultrasonic parameters are set to be 400W in power, 45 ℃ in temperature and 3h in time;
(4) centrifugal filtration: centrifuging the solution after ultrasonic extraction in a centrifuge, reserving supernatant for later use, adding 5% NaOH solution into filter residue according to the solid-to-liquid ratio of 1:2, performing ultrasonic-assisted extraction for 1h, reserving supernatant after centrifugal filtration, and combining the filtrates;
(5) enzymolysis: adding an acid or alkali solution into the filtrate to adjust the pH value to 8.0, adding trypsin according to the solid-to-liquid ratio of 1:1000, carrying out enzymolysis on the mixed solution at 40 ℃ for 3h, raising the temperature to 85 ℃ for inactivation for 30min after enzymolysis, cooling the inactivated solution to room temperature, adjusting the solution, adding papain according to the solid-to-liquid ratio of 1:1000, carrying out enzymolysis on the mixed solution at 55 ℃ for 5h, raising the temperature to 85 ℃ for inactivation for 30min after enzymolysis, and cooling the inactivated solution to room temperature;
(6) and (3) decoloring: performing pressure suction filtration on the solution after enzymolysis, filtering, retaining filtrate, adding active carbon and kaolin into the filtrate for adsorption decolorization, rapidly heating to 90 ℃, stirring for 30min, cooling, performing reduced pressure suction filtration, and retaining the filtrate for later use;
(7) alcohol precipitation: adjusting the pH of the filtrate to 6.8, adding 95% ethanol according to the solid-liquid ratio of 1:4 for precipitation for 9h, removing the supernatant, washing the precipitate with 95% ethanol for 3 times, centrifuging at 6000r/min for 15min, and retaining the precipitate after centrifugation;
(8) and (3) drying: collecting precipitate, and oven drying at 60 deg.C in an electrothermal constant temperature blast drying oven to obtain salmon proteoglycan.
Example two
A salmon proteoglycan extraction process comprises the following raw materials: the extraction method of salmon head cartilage comprises the following steps:
(1) pretreatment of raw materials: cleaning salmon head, boiling in clear water for 4h, cooling the fish head cartilage, washing off residues on the surface by using clear water, drying the cleaned fish head cartilage in a blast drier to constant weight, crushing the dried fish head cartilage by using a crusher, and further crushing the crushed fish head cartilage by using a superfine crusher to obtain fish head cartilage superfine powder;
(2) alkali extraction: weighing 30kg of fish head cartilage superfine powder, adding 900L of 5% NaOH solution, setting the parameters of a shaker to be 120r/min, and extracting at 30 ℃ for 12 h;
(3) ultrasonic: extracting the solution subjected to alkali extraction by using ultrasonic waves in an auxiliary way, setting the ultrasonic parameters to be 400W, setting the temperature to be 45 ℃, and setting the time to be 4 h;
(4) centrifugal filtration: centrifuging the solution after ultrasonic extraction in a centrifuge, reserving supernatant for later use, adding 5% NaOH solution into filter residue according to the solid-to-liquid ratio of 1:2, performing ultrasonic-assisted extraction for 1h, reserving supernatant after centrifugal filtration, and combining the filtrates;
(5) enzymolysis: adding an acid or alkali solution into the filtrate to adjust the pH value to 9.0, adding trypsin according to the solid-to-liquid ratio of 1:1000, carrying out enzymolysis on the mixed solution at 50 ℃ for 2h, raising the temperature to 90 ℃ for inactivation for 20min after enzymolysis, cooling the inactivated solution to room temperature, adjusting the solution, adding papain according to the solid-to-liquid ratio of 1:1000, carrying out enzymolysis on the mixed solution at 65 ℃ for 4h, raising the temperature to 90 ℃ for inactivation for 20min after enzymolysis, and cooling the inactivated solution to room temperature;
(6) and (3) decoloring: performing pressure suction filtration on the solution after enzymolysis, filtering, retaining filtrate, adding kaolin and active carbon into the filtrate for adsorption decolorization, rapidly heating to 90 ℃, stirring for 30min, cooling, performing reduced pressure suction filtration, and retaining the filtrate for later use;
(7) alcohol precipitation: adjusting the pH of the filtrate to 7.2, adding 95% ethanol according to the solid-liquid ratio of 1:4 for precipitation for 10h, removing the supernatant, washing the precipitate with 95% ethanol for 4 times, centrifuging at 6000r/min for 20min, and retaining the precipitate after centrifugation;
(8) and (3) drying: collecting precipitate, and oven drying at 80 deg.C in an electrothermal constant temperature blast drying oven to obtain salmon proteoglycan.
EXAMPLE III
A salmon proteoglycan extraction process comprises the following raw materials: the extraction method of salmon head cartilage comprises the following steps:
(1) pretreatment of raw materials: cleaning salmon head, boiling in clear water for 4h, cooling the fish head cartilage, washing off residues on the surface by using clear water, drying the cleaned fish head cartilage in a blast drier to constant weight, crushing the dried fish head cartilage by using a crusher, and further crushing the crushed fish head cartilage by using a superfine crusher to obtain fish head cartilage superfine powder;
(2) alkali extraction: weighing 100kg of fish head cartilage superfine powder, adding 3000L of 5% NaOH solution, setting the parameters of a shaking table to be 120r/min, and extracting at 30 ℃ for 12 h;
(3) ultrasonic: extracting the solution subjected to alkali extraction by using ultrasonic waves in an auxiliary way, setting the ultrasonic parameters to be 400W, setting the temperature to be 45 ℃, and setting the time to be 4 h;
(4) centrifugal filtration: centrifuging the solution after ultrasonic extraction in a centrifuge, reserving supernatant for later use, adding 5% NaOH solution into filter residue according to the solid-to-liquid ratio of 1:2, performing ultrasonic-assisted extraction for 1h, reserving supernatant after centrifugal filtration, and combining the filtrates;
(5) enzymolysis: adding an acid or alkali solution into the filtrate to adjust the pH value to 8.5, adding trypsin according to the solid-to-liquid ratio of 1:1000, carrying out enzymolysis on the mixed solution at 45 ℃ for 3h, raising the temperature to 90 ℃ for inactivation for 30min after enzymolysis, cooling the inactivated solution to room temperature, adjusting the solution, adding papain according to the solid-to-liquid ratio of 1:1000, carrying out enzymolysis on the mixed solution at 60 ℃ for 4.5h, raising the temperature to 90 ℃ for inactivation for 30min after enzymolysis, and cooling the inactivated solution to room temperature;
(6) and (3) decoloring: performing pressure suction filtration on the solution after enzymolysis, filtering, retaining filtrate, adding kaolin and active carbon into the filtrate for adsorption decolorization, rapidly heating to 90 ℃, stirring for 30min, cooling, performing reduced pressure suction filtration, and retaining the filtrate for later use;
(7) alcohol precipitation: adjusting the pH of the filtrate to 7.0, adding 95% ethanol according to the solid-liquid ratio of 1:4 for precipitation for 10h, removing the supernatant, washing the precipitate with 95% ethanol for 4 times, centrifuging at 6000r/min for 20min, and retaining the precipitate after centrifugation;
(8) and (3) drying: collecting precipitate, and drying in an electric heating constant temperature blast drying oven at 70 deg.C to obtain salmon proteoglycan.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (6)
1. The salmon proteoglycan extraction process is characterized by comprising the following raw materials: the extraction method of salmon head cartilage comprises the following steps:
(1) pretreatment of raw materials: cleaning salmon head, boiling in clear water for 3-4h, cooling the boiled fish head cartilage, washing off residues on the surface by using clear water, drying the washed fish head cartilage in a blast drier to constant weight, crushing the dried fish head cartilage by using a crusher, and further crushing the crushed fish head cartilage by using a superfine crusher to obtain fish head cartilage superfine powder;
(2) alkali extraction: weighing a certain mass of fish head cartilage superfine powder, adding a 5% NaOH solution, and extracting for 12h in a shaking table;
(3) ultrasonic: extracting the solution after alkali extraction with ultrasonic wave;
(4) centrifugal filtration: centrifuging the solution after ultrasonic extraction in a centrifuge, reserving supernatant for later use, adding 5% NaOH solution into filter residue according to the solid-to-liquid ratio of 1:2, performing ultrasonic-assisted extraction for 1h, reserving supernatant after centrifugal filtration, and combining the filtrates;
(5) enzymolysis: adding acid or alkali solution into the filtrate to adjust the pH value to 8.0-9.0, adding enzyme A according to the solid-liquid ratio of 1:1000, carrying out enzymolysis on the mixed solution at 40-50 ℃ for 2-3h, raising the temperature to 85-90 ℃ after enzymolysis, inactivating for 20-30min, cooling the inactivated solution to room temperature, adjusting the solution, adding enzyme B according to the solid-liquid ratio of 1:1000, carrying out enzymolysis on the mixed solution at 55-65 ℃ for 4-5h, raising the temperature to 85-90 ℃ after enzymolysis, inactivating for 20-30min, and cooling the inactivated solution to room temperature;
(6) and (3) decoloring: performing pressure suction filtration on the solution after enzymolysis, filtering, retaining filtrate, adding an adsorbent into the filtrate for adsorption decolorization, quickly heating to 90 ℃, stirring for 30min, cooling, performing reduced pressure suction filtration, and retaining the filtrate for later use;
(7) alcohol precipitation: adjusting pH of the filtrate to 6.8-7.2, adding 95% ethanol according to a solid-to-liquid ratio of 1:4, precipitating for 9-10h, removing supernatant, washing the precipitate with 95% ethanol for 3-4 times, centrifuging at 6000r/min for 15-20min, and retaining the precipitate after centrifugation;
(8) and (3) drying: collecting precipitate, and oven drying at 60-80 deg.C in an electrothermal constant temperature blast drying oven to obtain salmon proteoglycan.
2. The extraction process of salmon proteoglycan of claim 1, wherein during the alkali extraction in step (2), NaOH solution is added according to the solid-to-liquid ratio of 1:30, the parameters of the shaker are set to 120r/min, and the temperature is 20-30 ℃.
3. The salmon proteoglycan extracting process of claim 1, wherein in said step (3), the ultrasonic parameters are set to 400W, the temperature is set to 45 ℃, and the time is 3-4 h.
4. The process for extracting salmon proteoglycan of claim 1, wherein said enzyme A is trypsin and said enzyme B is papain.
5. The process of claim 1, wherein the solution is placed in a shaking table during the enzymolysis in step (5), and the rotation speed of the shaking table is 120 r/min.
6. The salmon proteoglycan extracting process of claim 1, wherein said adsorbent is activated carbon and kaolin.
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| WO2004039994A1 (en) * | 2002-11-01 | 2004-05-13 | Nippon Barrier Free Co., Ltd. | Sodium chondroitin sulfate, chondroitin sulfate-containing material and processes for producing the same |
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