CN1827755A - Preparation method of scallop splanchna active components - Google Patents
Preparation method of scallop splanchna active components Download PDFInfo
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- CN1827755A CN1827755A CNA2006100730851A CN200610073085A CN1827755A CN 1827755 A CN1827755 A CN 1827755A CN A2006100730851 A CNA2006100730851 A CN A2006100730851A CN 200610073085 A CN200610073085 A CN 200610073085A CN 1827755 A CN1827755 A CN 1827755A
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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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Abstract
A method for extracting active components of scallop viscera consists of supercritically extracting the scallop viscera fat by disposing raw materials, charging and controlling the abstraction temperature, pressure and carbon dioxide flux, after collecting the fat, extracting the polysaccharides of the scallop viscera by disintegrating, enzyme-hydrolyzing, alcohol-sinking, drying and purifying the degreased scallop viscera. The supercritical carbon dioxide extractive technique is a new chemical isolation technique developed quickly in recent years and can be widely used in food, spice, drug, chemistry and other domains. The said scallop viscera contains not only abundant unsaturated fatty acid but also abundant polysaccharide matters. The invention supercritically extracts the scallop viscera fat and extracts the polysaccharides of the degreased scallop viscera, which changes the waste to usefulness and makes the scallop viscera fully used.
Description
Technical field the present invention relates to a kind of method, particularly the comprehensive utilization method of sea-food processing waste.
Background technology scallop delicious flavour, nutritious is rich in the amino acid of calcium, phosphorus, zinc, selenium and other trace elements and needed by human.Processing and utilization report to scallop muscle is a lot of at present, but a large amount of waste scallop splanchnas of its processing are often ignored by the people.Studies show that not only containing abundant unsaturated fatty acids in the scallop splanchna also contains abundant polysaccharide material, but be not much accounted of always and study.
The extraction process of comb shell polysaccharide is disclosed in the Chinese patent application 200510047410 (CN1749281A), wherein raw material is whole corporality tissues (comprising scallop post, the cheek, sexual gland, internal organ, shirt rim etc.) that Patinopecten yessoensis shells, and also can be scallop post, " tankage " (cheek, sexual gland, internal organ, shirt rim etc. all or part of) or scallop post and part " tankage ".Though this technology can be extracted the polysaccharide in the scallop splanchna,, there are shortcomings such as the polysaccharide yield is low, purity is bad in the result of extraction, and in addition, the fat in the internal organ also wastes.
Studies show that and contain abundant lipid acid in the scallop splanchna fat, wherein polyunsaturated fatty acid EPA content is higher, and as the regulatory factor of organism, EPA has the effect that reduces platelet aggregation, and cerebral thrombosis and arteriosclerosis are also had prevention effect.
Research and report about the scallop culture technical elements are a lot, but the research of relevant its nutritive value aspect and report are very few.Particularly about utilize supercritical technology to extract scallop splanchna fat and make full use of degreasing after the scallop splanchna method of extracting polysaccharide again do not appear in the newspapers as yet.
In order to overcome the deficiencies in the prior art, the inventor is surprised to find that, before extracting the scallop splanchna polysaccharide, use supercritical extraction method, the fat of extraction scallop splanchna, the productive rate and the purity of polysaccharide have not only been improved, and the fat that is extracted itself is exactly extraordinary nutritious prod, can also be used to further extracting polyunsaturated fatty acid.
Summary of the invention the present invention is to be raw material with the scallop splanchna, and the raw material after adopting modern biotechnology and food new and high technology extraction scallop splanchna fat and making full use of degreasing extracts the method for polysaccharide.
Specifically, the present invention relates to a kind of preparation method of scallop splanchna active components, it is characterized in that comprising steps such as raw material drying, pulverizing, supercritical extraction fat, enzymolysis, alcohol precipitation, drying, purifying, wherein said activeconstituents is the polysaccharide and the fat of scallop splanchna.
One, the supercritical extraction of scallop splanchna fat
1, raw material and processing: get fresh scallop splanchna and keep temperature of charge below 40 ℃ in freeze drier, vacuum-freeze-dry 3000min reaches below 4% material moisture.Be crushed to 20 orders with pulverizer afterwards.
2, the extracting process of Scallop Fat
Extraction process flow: charging--control extraction temperature--control extracting pressure---control CO
2Flow--extraction--control separation temperature and pressure---separate
Specific implementation method: open supercritical extraction equipment, setting extraction temperature is its intensifications of 30～70 ℃ of waits, and adds the material that accounts for extraction kettle volume 1/3 simultaneously in extraction kettle.Treat that extraction temperature reaches after the set(ting)value, the control extracting pressure is 20～40Mpa, CO
2Flow is 10～40L/h, and supercritical extraction scallop splanchna fat behind extraction 45～120min, is that 30～40 ℃ and separating pressure are to isolate fat under the condition of 6～10Mpa in separation temperature, and collects.
Two, the scallop splanchna behind the extraction fat extracts the method for polysaccharide
Scallop splanchna behind the extraction fat extracts the method for polysaccharide can carry out according to the extraction process that discloses comb shell polysaccharide among the CN1749281A.
Also can carry out as follows:
Scallop splanchna behind the extraction fat is taken out from extraction kettle, the pH value that adds 10～60 times of volumes is 6～8 buffered soln, and to add massfraction be that 0.1%～1% enzyme activity is the papoid of 90～1,000,000 units/gram, and enzymolysis is 1～8 hour in 50～80 ℃ of waters.Be warming up to 90 ℃ of enzymes that go out afterwards rapidly.High speed centrifugation 10min under the condition of 4000n/min, the throw out that obtains are insoluble hydrolyzate.To the centrifugal mother liquid obtained massfraction that slowly adds 2～6 times of volumes is 95% ethanol, and constantly stir this moment, and in 10 ℃ of following temperature overnight.Centrifugal afterwards, the gained supernatant liquor can carry out underpressure distillation, and not only recyclable ethanol can also obtain the scallop splanchna hydrolysate, collects the centrifugal throw out, and in 40～70 ℃ of dryings or vacuum-drying, the product that obtains is the scallop splanchna polysaccharide crude.Polysaccharide is dissolved in the water of 10～50 times of quality, the centrifugal insolubles of removing adds solid K in supernatant liquor
2CO
3, making its concentration in solution is 0.5～4mol/L, refrigeration below 10 ℃ is spent the night.Collecting precipitation below 10 ℃.Water with 5～25 times of quality dissolves it again, transfers pH to 9～11 with alkaline solution, keeps 45～55 ℃ to drip H
2O
2The sugared at the most hydrolyzed solution that decolours is the light yellow terminal point that is.The centrifugal insolubles of removing in cooling back, clear liquid is cooled to below 4 ℃, transfers pH to 1.5～2.5 with acid, and the centrifugal precipitation of removing adds solid K in the clear liquid
2CO
3, make its concentration in solution reach 0.5～4mol/L, refrigeration is spent the night, and collecting precipitation below 10 ℃ is used washing with alcohol, the acetone dehydration, drying promptly gets the pure product of scallop splanchna polysaccharide.
The present invention has following advantage:
1. the present invention extracts scallop splanchna fat and extracts polysaccharide with the scallop splanchna after the degreasing with postcritical method, turns waste into wealth, and scallop splanchna is fully utilized.
2. the present invention adopts the method for supercritical extraction to extract scallop splanchna fat, has improved 9% yield than Soxhlet extraction method.
3. the present invention adopts postcritical method extraction fat, has got rid of the possibility of meeting the oxygen oxidation and seeing photoresponse, makes fat can keep its natural flavor.
Embodiment
Example 1 is got fresh scallop splanchna and is kept temperature of charge below 40 ℃ in freeze drier, and vacuum-freeze-dry 3000min reaches below 4% material moisture.Be crushed to 20 orders with pulverizer afterwards.Open supercritical extraction equipment, setting extraction temperature is 40 ℃ of its intensifications of wait, and adds the 30g material simultaneously in extraction kettle.Treat that extraction temperature reaches after the set(ting)value, the control extracting pressure is 25Mpa, CO
2Flow is 20L/h, and supercritical extraction scallop splanchna fat after the extraction 60min, is that 30 ℃ and separating pressure are to isolate fat under the condition of 7Mpa and collect in separation temperature.Scallop splanchna after the degreasing is taken out, and the pH value that adds 20 times of volumes is 7 buffered soln that add massfraction again and be 0.1% papoid, enzymolysis is 1 hour in 60 ℃ of water-baths from extraction kettle.Be warming up to 90 ℃ of enzymes that go out afterwards rapidly.High speed centrifugation 10min under the condition of 4000n/min, the throw out that obtains are insoluble hydrolyzate.To the centrifugal mother liquid obtained massfraction that slowly adds 3 times of volumes is 95% ethanol, and constantly stir this moment, and in 10 ℃ of following temperature overnight.Centrifugal afterwards, the gained supernatant liquor can carry out underpressure distillation, not only recyclable ethanol, can also obtain the scallop splanchna hydrolysate, collect the centrifugal throw out, and dewater with 90% washing with alcohol, acetone successively, in 50 ℃ of dryings, the product that obtains is the scallop splanchna polysaccharide crude.Crude polysaccharides is dissolved in the water of 10 times of quality, the centrifugal insolubles of removing adds solid K in supernatant liquor
2CO
3, making its concentration in solution is 0.5mol/L, refrigeration below 10 ℃ is spent the night.Collecting precipitation below 10 ℃.Water with 5 times of quality dissolves it again, transfers pH to 9 with alkaline solution, keeps 45 ℃ to drip H
2O
2The sugared at the most hydrolyzed solution that decolours is the light yellow terminal point that is.The centrifugal insolubles of removing in cooling back, clear liquid is cooled to below 4 ℃, transfers pH to 1.5 with acid, and the centrifugal precipitation of removing adds solid K in the clear liquid
2CO
3, make its concentration in solution reach 0.5mol/L, refrigeration is spent the night, and collecting precipitation below 10 ℃ is used washing with alcohol, acetone dehydration, drying.Promptly get the pure product of scallop splanchna polysaccharide.
Example 2 is got fresh scallop splanchna and is kept temperature of charge below 40 ℃ in freeze drier, and vacuum-freeze-dry 3000min reaches below 4% material moisture.Be crushed to 20 orders with pulverizer afterwards.Open supercritical extraction equipment, setting extraction temperature is 50 ℃ of its intensifications of wait, and adds the 35g material simultaneously in extraction kettle.Treat that extraction temperature reaches after the set(ting)value, the control extracting pressure is 30Mpa, CO
2Flow is 25L/h, and supercritical extraction scallop splanchna fat after the extraction 60min, is that 35 ℃ and separating pressure are to isolate fat under the condition of 8Mpa and collect in separation temperature.Scallop splanchna after the degreasing is taken out, and the pH value that adds 30 times of volumes is 8 buffered soln that add massfraction again and be 0.5% papoid, enzymolysis is 2 hours in 60 ℃ of water-baths from extraction kettle.Be warming up to 90 ℃ of enzymes that go out afterwards rapidly.High speed centrifugation 10min under the condition of 4000n/min, the throw out that obtains are insoluble hydrolyzate.To the centrifugal mother liquid obtained massfraction that slowly adds 3 times of volumes is 95% ethanol, and constantly stir this moment, and in 10 ℃ of following temperature overnight.Centrifugal afterwards, the gained supernatant liquor can carry out underpressure distillation, not only recyclable ethanol, can also obtain the scallop splanchna hydrolysate, collect the centrifugal throw out, and dewater with 90% washing with alcohol, acetone successively, in 50 ℃ of dryings, the product that obtains is the scallop splanchna polysaccharide crude.Crude polysaccharides is dissolved in the water of 20 times of quality, the centrifugal insolubles of removing adds solid K in supernatant liquor
2CO
3, making its concentration in solution is 0.5mol/L, refrigeration below 10 ℃ is spent the night.Collecting precipitation below 10 ℃.Water with 10 times of quality dissolves it again, transfers pH to 9 with alkaline solution, keeps 45 ℃ to drip H
2O
2The sugared at the most hydrolyzed solution that decolours is the light yellow terminal point that is.The centrifugal insolubles of removing in cooling back, clear liquid is cooled to below 4 ℃, transfers pH to 1.5 with acid, and the centrifugal precipitation of removing adds solid K in the clear liquid
2CO
3, make its concentration in solution reach 0.5mol/L, refrigeration is spent the night, and collecting precipitation below 10 ℃ is used washing with alcohol, acetone dehydration, drying.Promptly get the pure product of scallop splanchna polysaccharide.
Example 3 is got fresh scallop splanchna and is kept temperature of charge below 40 ℃ in freeze drier, and vacuum-freeze-dry 3000min reaches below 4% material moisture.Be crushed to 20 orders with pulverizer afterwards.Open supercritical extraction equipment, set extraction temperature and be 55 ℃ and wait for its intensification, and in extraction kettle, add the 30g material simultaneously.Treat that extraction temperature reaches after the set(ting)value, the control extracting pressure is that 35Mpa, CO2 flow are 30L/h, and supercritical extraction scallop splanchna fat after the extraction 60min, is that 35 ℃ and separating pressure are to isolate fat under the condition of 9Mpa and collect in separation temperature.Scallop splanchna after the degreasing is taken out, and the pH value that adds 30 times of volumes is 8 buffered soln that add massfraction again and be O.3% papoid, enzymolysis is 2 hours in 60 ℃ of waters from extraction kettle.Be warming up to 90 ℃ of enzymes that go out afterwards rapidly.High speed centrifugation 10min under the condition of 4000n/min, the throw out that obtains are insoluble hydrolyzate.To the centrifugal mother liquid obtained massfraction that slowly adds 4 times of volumes is 95% ethanol, and constantly stir this moment, and in 10 ℃ of following temperature overnight.Centrifugal afterwards, the gained supernatant liquor can carry out underpressure distillation, not only recyclable ethanol, can also obtain the scallop splanchna hydrolysate, collect the centrifugal throw out, and dewater with 90% washing with alcohol, acetone successively, in 50 ℃ of dryings, the product that obtains is the scallop splanchna polysaccharide crude.Crude polysaccharides is dissolved in the water of 40 times of quality, the centrifugal insolubles of removing adds solid K 2CO3 in supernatant liquor, and making its concentration in solution is 0.5mol/L, and refrigeration below 10 ℃ is spent the night.Collecting precipitation below 10 ℃.Water with 20 times of quality dissolves it again, transfers pH to 9 with alkaline solution, keeps 45 ℃ of sugared at the most hydrolyzed solutions of dropping H2O2 decolouring to be the light yellow terminal point that is.The centrifugal insolubles of removing in cooling back, clear liquid is cooled to below 4 ℃, transfers pH to 1.5 with acid, the centrifugal precipitation of removing, add solid K 2CO3 in the clear liquid, make its concentration in solution reach 0.5mol/L, refrigeration is spent the night, collecting precipitation below 10 ℃, use washing with alcohol, acetone dehydration, drying.Promptly get the pure product of scallop splanchna polysaccharide.
Claims (9)
1, a kind of preparation method of scallop splanchna active components is characterized in that comprising raw material drying, pulverizing, supercritical extraction fat, enzymolysis, alcohol precipitation, drying, purification step, and wherein said activeconstituents is scallop splanchna fat or polysaccharide.
2, the preparation method of scallop splanchna active components as claimed in claim 1, it is characterized in that described raw material drying step comprises that scallop splanchna is put into freeze drier keeps temperature of charge below 40 ℃, vacuum-freeze-dry 3000min reaches below 4% material moisture.
3, the preparation method of scallop splanchna active components as claimed in claim 1 or 2 is characterized in that described pulverising step comprises raw material is crushed to below 20 orders with pulverizer.
4, the preparation method of scallop splanchna active components as claimed in claim 3 is characterized in that the fatty step of described extraction comprises that the control extraction temperature is that 30～70 ℃, extracting pressure are 20～40Mpa, CO
2Flow is to use supercritical CO under the condition of 10～40L/h
2Extraction equipment extraction Patinopecten yessoensis interior fat 45～120min is that 30～40 ℃ and separating pressure are to isolate fat under the condition of 6～10Mpa in separation temperature afterwards, and collects.
5, as the preparation method of each described scallop splanchna active components of claim 1 to 4, it is characterized in that described enzymolysis step comprises the scallop splanchna behind supercritical extraction fat, the pH value that adds 10～60 times of volumes is 6～8 buffered soln, adding massfraction again and be 0.1%～1% enzyme activity is the papoid of 90～1,000,000 units/gram, in 50～80 ℃ of water-baths, heated 1～8 hour, behind the enzyme that goes out again with the centrifugal removal of impurities of enzymolysis solution.
6,, it is characterized in that described alcohol precipitation step comprises that the massfraction that the enzymolysis solution after the removal of impurities is added 2～6 times of volumes is 95% ethanol alcohol precipitation as the preparation method of each described scallop splanchna active components of claim 1 to 5.
7,, it is characterized in that described drying step comprises that the Crude polysaccharides that alcohol is settled out is in 40～70 ℃ of dryings or vacuum-drying as each described Patinopecten yessoensis internal organ polysaccharide extracting process of claim 1-6.
8,, it is characterized in that described purifying process comprises Crude polysaccharides is dissolved in the water of 10～50 times of quality that the centrifugal insolubles of removing adds solid K in supernatant liquor as the preparation method of each described scallop splanchna active components of claim 1-7
2CO
3, making its concentration in solution is 0.5～4mol/L, refrigeration below 10 ℃ is spent the night, and collecting precipitation below 10 ℃, the water with 5～25 times of quality dissolves it again, transfers pH to 9～11 with alkaline solution, keeps 45～55 ℃ to drip H
2O
2The sugared at the most hydrolyzed solution that decolours is the light yellow terminal point that is, the centrifugal insolubles of removing in cooling back, and clear liquid is cooled to below 4 ℃, transfers pH to 1.5～2.5 with acid, and the centrifugal precipitation of removing adds solid K in the clear liquid
2CO
3, make its concentration in solution reach 0.5～4mol/L, refrigeration is spent the night, and collecting precipitation below 10 ℃ is used washing with alcohol, acetone dehydration, drying.
9, the product that makes of claim 4 or 8 described methods.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100730851A CN100497569C (en) | 2006-04-13 | 2006-04-13 | Preparation method of scallop splanchna active components |
| JP2007545823A JP4406032B2 (en) | 2005-10-11 | 2006-10-10 | Scallop polysaccharide extraction method |
| PCT/CN2006/002649 WO2007041950A1 (en) | 2005-10-11 | 2006-10-10 | Extraction method of patinopecten yessoensis polysaccharide |
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| CNB2006100730851A CN100497569C (en) | 2006-04-13 | 2006-04-13 | Preparation method of scallop splanchna active components |
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| CN100497569C CN100497569C (en) | 2009-06-10 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503721B (en) * | 2008-11-27 | 2012-01-11 | 浙江珍世堂生物科技有限公司 | Method for extracting swan-mussel polysaccharide |
| CN102477101A (en) * | 2010-11-22 | 2012-05-30 | 河北农业大学 | Method for extracting bay scallop polysaccharide |
| CN102603911A (en) * | 2012-03-12 | 2012-07-25 | 浙江大学 | Corbicula fluminea glycosaminoglycan and preparation method and usage thereof |
| CN102627700A (en) * | 2012-04-25 | 2012-08-08 | 河北农业大学 | Method for extracting polysaccharides from skirt edges and internal organs of scallops by hydrolysis method |
| CN103172760A (en) * | 2013-03-26 | 2013-06-26 | 大连工业大学 | Method for preparing sulfated glycogen based on oysters or scallops |
| CN103749940A (en) * | 2014-01-10 | 2014-04-30 | 上海海洋大学 | Comprehensive utilization method of saury internal organs |
| CN103936876A (en) * | 2014-04-18 | 2014-07-23 | 广西还珠海洋生物科技有限公司 | Method of extracting crude polysaccharide from palea steindachneri shell |
| CN104970192A (en) * | 2014-04-14 | 2015-10-14 | 中国科学院海洋研究所 | Functional protein feed additive and preparation method thereof |
| CN105131143A (en) * | 2015-09-29 | 2015-12-09 | 江苏锦宇环境工程有限公司 | Preparing method of scallop viscera oligosaccharide |
| CN106188329A (en) * | 2016-08-05 | 2016-12-07 | 大连工业大学 | The extracting method of a kind of scallop polysaccharide and goods |
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2006
- 2006-04-13 CN CNB2006100730851A patent/CN100497569C/en active Active
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503721B (en) * | 2008-11-27 | 2012-01-11 | 浙江珍世堂生物科技有限公司 | Method for extracting swan-mussel polysaccharide |
| CN102477101A (en) * | 2010-11-22 | 2012-05-30 | 河北农业大学 | Method for extracting bay scallop polysaccharide |
| CN102603911A (en) * | 2012-03-12 | 2012-07-25 | 浙江大学 | Corbicula fluminea glycosaminoglycan and preparation method and usage thereof |
| CN102603911B (en) * | 2012-03-12 | 2014-11-26 | 浙江大学 | Corbicula fluminea glycosaminoglycan and preparation method and usage thereof |
| CN102627700A (en) * | 2012-04-25 | 2012-08-08 | 河北农业大学 | Method for extracting polysaccharides from skirt edges and internal organs of scallops by hydrolysis method |
| CN103172760A (en) * | 2013-03-26 | 2013-06-26 | 大连工业大学 | Method for preparing sulfated glycogen based on oysters or scallops |
| CN103749940B (en) * | 2014-01-10 | 2016-08-17 | 上海海洋大学 | A kind of saury internal organs method of comprehensive utilization |
| CN103749940A (en) * | 2014-01-10 | 2014-04-30 | 上海海洋大学 | Comprehensive utilization method of saury internal organs |
| CN104970192A (en) * | 2014-04-14 | 2015-10-14 | 中国科学院海洋研究所 | Functional protein feed additive and preparation method thereof |
| CN103936876A (en) * | 2014-04-18 | 2014-07-23 | 广西还珠海洋生物科技有限公司 | Method of extracting crude polysaccharide from palea steindachneri shell |
| CN103936876B (en) * | 2014-04-18 | 2016-02-10 | 广西还珠海洋生物科技有限公司 | A kind of method extracting Crude polysaccharides from steindachner soft-shelled turtle carapace |
| CN105131143A (en) * | 2015-09-29 | 2015-12-09 | 江苏锦宇环境工程有限公司 | Preparing method of scallop viscera oligosaccharide |
| CN106188329A (en) * | 2016-08-05 | 2016-12-07 | 大连工业大学 | The extracting method of a kind of scallop polysaccharide and goods |
| CN106188329B (en) * | 2016-08-05 | 2019-04-09 | 大连工业大学 | A kind of extracting method and product of scallop polysaccharide |
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