CN103087814A - Astaxanthin-rich shrimp sauce and enzyme-assisted supercritical extraction method thereof - Google Patents
Astaxanthin-rich shrimp sauce and enzyme-assisted supercritical extraction method thereof Download PDFInfo
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- CN103087814A CN103087814A CN2013100504437A CN201310050443A CN103087814A CN 103087814 A CN103087814 A CN 103087814A CN 2013100504437 A CN2013100504437 A CN 2013100504437A CN 201310050443 A CN201310050443 A CN 201310050443A CN 103087814 A CN103087814 A CN 103087814A
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- 241000238557 Decapoda Species 0.000 title claims abstract description 49
- JEBFVOLFMLUKLF-IFPLVEIFSA-N Astaxanthin Natural products CC(=C/C=C/C(=C/C=C/C1=C(C)C(=O)C(O)CC1(C)C)/C)C=CC=C(/C)C=CC=C(/C)C=CC2=C(C)C(=O)C(O)CC2(C)C JEBFVOLFMLUKLF-IFPLVEIFSA-N 0.000 title claims abstract description 27
- 239000001168 astaxanthin Substances 0.000 title claims abstract description 27
- 235000013793 astaxanthin Nutrition 0.000 title claims abstract description 27
- MQZIGYBFDRPAKN-ZWAPEEGVSA-N astaxanthin Chemical compound C([C@H](O)C(=O)C=1C)C(C)(C)C=1/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=CC1=C(C)C(=O)[C@@H](O)CC1(C)C MQZIGYBFDRPAKN-ZWAPEEGVSA-N 0.000 title claims abstract description 27
- 229940022405 astaxanthin Drugs 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 27
- 235000015067 sauces Nutrition 0.000 title claims abstract description 17
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 11
- 102000004190 Enzymes Human genes 0.000 title claims abstract description 6
- 108090000790 Enzymes Proteins 0.000 title claims abstract description 6
- 238000000605 extraction Methods 0.000 claims abstract description 26
- 239000002699 waste material Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 3
- MBLBDJOUHNCFQT-LXGUWJNJSA-N aldehydo-N-acetyl-D-glucosamine Chemical compound CC(=O)N[C@@H](C=O)[C@@H](O)[C@H](O)[C@H](O)CO MBLBDJOUHNCFQT-LXGUWJNJSA-N 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 7
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- 239000001569 carbon dioxide Substances 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 2
- 238000012792 lyophilization process Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 235000013305 food Nutrition 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 238000005211 surface analysis Methods 0.000 abstract description 2
- 108090000526 Papain Proteins 0.000 abstract 1
- 239000004365 Protease Substances 0.000 abstract 1
- 229940088598 enzyme Drugs 0.000 abstract 1
- 235000013376 functional food Nutrition 0.000 abstract 1
- 238000013433 optimization analysis Methods 0.000 abstract 1
- 229940055729 papain Drugs 0.000 abstract 1
- 235000019834 papain Nutrition 0.000 abstract 1
- 239000000047 product Substances 0.000 description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 238000012545 processing Methods 0.000 description 7
- 241000239366 Euphausiacea Species 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- HDLNSTQYXPTXMC-UHFFFAOYSA-N Astaxanthin-diacetat Natural products O=C1C(OC(=O)C)CC(C)(C)C(C=CC(C)=CC=CC(C)=CC=CC=C(C)C=CC=C(C)C=CC=2C(CC(C(=O)C=2C)OC(C)=O)(C)C)=C1C HDLNSTQYXPTXMC-UHFFFAOYSA-N 0.000 description 3
- 239000013543 active substance Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229920002101 Chitin Polymers 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001976 enzyme digestion Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 2
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 2
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 102000035195 Peptidases Human genes 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000003811 acetone extraction Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000008827 biological function Effects 0.000 description 1
- 230000037237 body shape Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- -1 keto-acid carotenoid Chemical class 0.000 description 1
- ZGEGCLOFRBLKSE-UHFFFAOYSA-N methylene hexane Natural products CCCCCC=C ZGEGCLOFRBLKSE-UHFFFAOYSA-N 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 235000014102 seafood Nutrition 0.000 description 1
- 238000010898 silica gel chromatography Methods 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Landscapes
- Meat, Egg Or Seafood Products (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to a shrimp sauce rich in astaxanthin and an enzyme-assisted supercritical extraction method thereof. Setting extraction temperature, extraction pressure and input amount of papain as three factors to be optimized, and performing optimization analysis by using a response surface analysis method to obtain the optimal conditions for extracting the astaxanthin-rich shrimp sauce. The obtained product can be directly eaten as functional food or added into other foods as an additional material, so that the health-care effect is enhanced, and the comprehensive environment-friendly utilization of wastes is realized.
Description
Technical field
The present invention relates to a kind of shrimp processing waste that utilizes---shrimp head, shrimp shell and shrimp tail assist supercritical carbon dioxide extraction to be rich in the method for the shrimp sauce of astaxanthin by proteolytic enzyme, belong to the Food science high-technology field.
Background technology
Astaxanthin is a kind of keto-acid carotenoid that extensively is present in organic sphere, belongs to the terpenes unsaturated compound.Known astaxanthin in the protection of anti-oxidant, painted, light, promote breeding, strengthen immunity, central nervous system healthy aspects such as protection, preventing cardiovascular disease and ultraviolet radiation preventing have excellent biological function; therefore in recent years, the extraction and separation method of natural astaxanthin becomes study hotspot.Natural astaxanthin has huge application potential and development prospect as a kind of natural medicine in industries such as medicine, cultivation, food and chemical industry.
The present invention adopts the shrimp processing waste as main raw material, extracts the shrimp sauce be rich in astaxanthin, raw material is turned waste into wealth reach the purpose of utilize resources synthetically.The common method of extracting astaxanthin and grease from the shrimp processing waste has enzymolysis process, organic solvent extraction method, super critical extraction.Wherein enzymolysis process utilizes the enzyme digestion reaction of different sorts enzyme to obtain product, but this method can only decompose material merely, follow-uply also needs to have further extraction process that target compound is extracted.Organic solvent extraction method solvent commonly used has ethanol, acetone, methylene dichloride and normal hexane etc., publication number is CN102503877A, application number is 201110387069.0 patent " a kind of extracting method of astaxanthin ", at first the method adopts low-concentration ethanol solution to extract, the mixed solvent that forms with methylene dichloride and hexane again extracts, and obtains astaxanthin.Product is single, and has dissolvent residual.Publication number is CN102603589A, and application number is 201210038732.0 invention " a kind of method from freezing krill Extraction and enrichment astaxanthin ester ", utilizes ethanol to extract, and then utilizes the concentrated grease that can contain astaxanthin of normal hexane.But the method raw material is the whole shrimp of krill, and cost is high, and normal hexane is residual, the infringement quality product.Publication number is CN102731359A, application number is 201210249101.3 patent " a kind of method of extracting astaxanthin and ester thereof from krill ", take freezing krill as raw material, use extraction using alcohol, add the chitin acetic acid solution after concentrated, add again ethanol elution, filter to get red paste.This patent products obtained therefrom is paste body shape but not clarified oil attitude, therefore product purity is not high, impurity is more.Publication number is CN102731361A, application number is 201210249118.9 the patent method of fast enriching astaxanthin and ester thereof " a kind of from krill ", this invention utilizes dried krill to be raw material, the extraction that adds normal hexane or cyclohexane or sherwood oil or 6# gasoline, add again white VE powder whip attachment, be eluted to the VE powder red paste that bleaches to get with acetone, can get the astaxanthin ester elutriant through silica gel column chromatography, steam separately and desolventize to get astaxanthin ester.The astaxanthin part that does not move down during the capital wash-out is through acetone extraction.This invented technology flow process is complicated, needs the multistep extraction, absorption, and lock out operation, and this method products obtained therefrom contains organic solvent residual, is difficult to reach the food safety rank.
Supercritical fluid extraction is as a kind of novel extractive technique, and rate of mass transfer is fast, and no solvent residue and product separation are easy, is widely used in the extraction and purification of active substance.Carbonic acid gas is shown one's talent in numerous supercutical fluids because of its stagnation point gentleness, safety, environmental protection, nontoxic and economic dispatch advantage, is applied to many kinds of substance especially in foodstuffs industry in the extraction process of active substance.At present the supercritical extraction technology is combined this pattern with enzyme digestion reaction, more application in the research that chemical reaction efficiency promotes, the bright extraction separation that is applied to less active substance.The present invention wants to provide a kind of novel combination extracting mode, efficient and easy acquisition product.GIcNAc-GlcN glycosidic link that there are some researches show the alternative degraded of papoid chitin, so the present invention adopts papoid to participate in the extraction of astaxanthin as auxiliary enzymes.
Summary of the invention
The present invention has mainly solved the existing shortcoming that the traditional extraction process extraction efficiency is lower, flow process is loaded down with trivial details, and the mode of the novel combination extraction that utilizes the auxiliary supercritical co of papoid is provided, thereby obtains to be rich in the shrimp sauce product of astaxanthin.
Technical problem to be solved by this invention is to realize by following technical scheme:
The present invention utilizes the shrimp processing waste---the shrimp head, and shrimp shell and shrimp tail utilize the auxiliary supercritical carbon dioxide extraction of papoid to be rich in the method for the shrimp sauce of astaxanthin, are characterized in:
1) with the shrimp head, the processing wastes such as shrimp shell and shrimp tail carry out vacuum lyophilization, curve of vacuum is set as 15 ~ 20Mpa, temperature curve setting is to keep 300min after 0-30min is warming up to 50 ℃, then be down to 40 ℃ in 30min, and keep 40 ℃ until curve and setting curve keeping parallelism after one hour or constant weight, are considered as vacuum lyophilization finishes;
2) will carry out shrimp head after vacuum lyophilization, shrimp shell and shrimp tail are put into pulverizer and are pulverized, and are crushed to after the 40-60 order standby;
3) take quantitative shrimp head, shrimp shell and shrimp tail powder (being designated hereinafter simply as shrimp med) add papoid, and ratio is 2 ~ 8%, stirs;
4) shrimp med after completing steps 3 is packed in supercritical extraction reactor, the control extracting pressure is 150 ~ 350Bar, and extraction temperature is 30 ~ 50 ℃, and carbon dioxide flow is 1 ~ 3L/min and extraction time 10 ~ 120min, carries out overcritical dynamic extraction;
6) collect product by separating opening, the separating opening Temperature Setting is 80 ℃.
Product that the present invention obtains is a kind of shrimp sauce that is rich in astaxanthin, and product is clarification oily matter, is bright-coloured orange red, has the distinctive seafood fragrance of shrimp sauce.After the response surface analysis method was optimized, in shrimp med, the oil extraction rate can reach more than 10%, utilized GC-MS and HLPC to analyze, and in shrimp sauce, the unsaturated fatty acids total amount can reach 30% ~ 63%, and content astaxanthin can reach 50 μ g/g ~ 527 μ g/g.
The present invention has obvious advantage:
1) rich choice of products.Can obtain to be rich in the shrimp sauce of astaxanthin by this technique.Both preserve the shrimp sauce that contains unsaturated fatty acids, be rich in again astaxanthin, strengthened the health-care effect of product;
2) Product Green environmental protection purity is high.Product no solvent residue and product purity by the supercritical carbon dioxide extraction gained are high;
3) technique is simply easy to implement.The present invention only need to get final product through raw material processing and supercritical extraction.
Embodiment:
By following embodiment, technical scheme of the present invention is described in further detail, following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment:
1) the Chinese prawn processing waste is carried out pre-treatment through vacuum lyophilization.Curve of vacuum is set as 15 ~ 20Mpa, temperature curve setting is to keep 300min after 0-30min is warming up to 50 ℃, then be down to 40 ℃ in 30min, and keep 40 ℃ until curve and setting curve keeping parallelism after one hour or constant weight, vacuum lyophilization finishes;
2) will carry out shrimp head after vacuum lyophilization, shrimp shell and shrimp tail are put into medicinal herb grinder and are pulverized, and are crushed to the 40-60 order standby;
3) take 15g shrimp head, shrimp shell and shrimp tail powder (being designated hereinafter simply as shrimp med) add papoid, and ratio is 6%, stirs, and in the supercritical extraction reactor of packing into, carries out supercritical carbon dioxide extraction;
4) controlling extracting pressure is 300Bar, and extraction temperature is 40 ℃, and carbon dioxide flow 2L/min, extraction time are 60min, carry out overcritical dynamic extraction, and the separating opening Temperature Setting is 80 ℃.
Through above step, in shrimp med, the percentage extraction of shrimp sauce is 11.2%, and wherein content astaxanthin is 518 μ g/g.
Claims (2)
1. shrimp sauce and an enzyme thereof that is rich in astaxanthin assisted supercritical extraction method, it is characterized in that comprising following preparation process:
(1) with the shrimp head, after shrimp shell and shrimp tail the like waste carry out vacuum lyophilization, pulverize, obtain the shrimp head, shrimp shell and shrimp tail powder (being designated hereinafter simply as shrimp med);
(2) take a certain amount of shrimp med, add papoid, stir in the supercritical extraction reactor of packing into, carry out supercritical carbon dioxide extraction;
(3) collect by separating opening the shrimp sauce that product obtains being rich in astaxanthin.
2. method according to claim 1 is characterized in that the following aspects:
(1) in the vacuum lyophilization process, curve of vacuum is set as 15 ~ 20Mpa, temperature curve setting is to keep 300min after 0-30min is warming up to 50 ℃, then be down to 40 ℃ in 30min, and keep 40 ℃ until curve and setting curve keeping parallelism after one hour or constant weight, are considered as vacuum lyophilization finishes;
(2) will carry out shrimp head after vacuum lyophilization, shrimp shell and shrimp tail are put into pulverizer to be crushed to the 40-60 order standby;
(3) the papoid add-on is controlled to be 0 ~ 10% of material total amount;
(4) extraction conditions during the supercritical carbon dioxide extraction shrimp sauce is: extracting pressure 150 ~ 400Bar, 30 ~ 60 ℃ of extraction temperature, carbon dioxide flow 1 ~ 3L/min, extraction time 10 ~ 120min, 80 ℃ of separating opening temperature.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106833864A (en) * | 2016-12-28 | 2017-06-13 | 中国计量大学 | A kind of method that utilization shrimp processing byproduct prepares shrimp sauce |
| CN109735392A (en) * | 2019-01-28 | 2019-05-10 | 江南大学 | A kind of preparation method of high astaxanthin, high phospholipid shrimp sauce |
| CN110357799A (en) * | 2019-07-29 | 2019-10-22 | 云南钰腾生物科技有限公司 | A kind of extraction element and extraction process of astaxanthin |
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| CN102071101A (en) * | 2011-01-21 | 2011-05-25 | 山东科芮尔生物制品有限公司 | Method for extracting phospholipid-enriched krill oil from Antarctic krill |
| CN102358865A (en) * | 2011-09-14 | 2012-02-22 | 山东科芮尔生物制品有限公司 | Method of extracting Euphausia superba oil by using supercritical carbon dioxide |
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2013
- 2013-02-13 CN CN2013100504437A patent/CN103087814A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071101A (en) * | 2011-01-21 | 2011-05-25 | 山东科芮尔生物制品有限公司 | Method for extracting phospholipid-enriched krill oil from Antarctic krill |
| CN102358865A (en) * | 2011-09-14 | 2012-02-22 | 山东科芮尔生物制品有限公司 | Method of extracting Euphausia superba oil by using supercritical carbon dioxide |
Non-Patent Citations (2)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106833864A (en) * | 2016-12-28 | 2017-06-13 | 中国计量大学 | A kind of method that utilization shrimp processing byproduct prepares shrimp sauce |
| CN109735392A (en) * | 2019-01-28 | 2019-05-10 | 江南大学 | A kind of preparation method of high astaxanthin, high phospholipid shrimp sauce |
| CN110357799A (en) * | 2019-07-29 | 2019-10-22 | 云南钰腾生物科技有限公司 | A kind of extraction element and extraction process of astaxanthin |
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