CN102334686B - Rapid low temperature extraction method for total astaxanthin from frozen Euphausia superba Dana - Google Patents
Rapid low temperature extraction method for total astaxanthin from frozen Euphausia superba Dana Download PDFInfo
- Publication number
- CN102334686B CN102334686B CN 201110201341 CN201110201341A CN102334686B CN 102334686 B CN102334686 B CN 102334686B CN 201110201341 CN201110201341 CN 201110201341 CN 201110201341 A CN201110201341 A CN 201110201341A CN 102334686 B CN102334686 B CN 102334686B
- Authority
- CN
- China
- Prior art keywords
- krill
- astaxanthin
- total astaxanthin
- total
- freezing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
- Meat, Egg Or Seafood Products (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
Abstract
The invention relates to a rapid low temperature extraction method for total astaxanthin from frozen Euphausia superba Dana. The method comprises the following steps: (1) directly adding a frozen raw material of Euphausia superba Dana into a mixed solvent of ethyl acetate and ethylene glycol monomethyl ether, crushing the frozen raw material, homogenizing obtained mixture, and carrying out centrifugation, wherein, the upper layer of an obtained solution is clear liquid of a mixed solution of ester and ether, and the lower layer of the obtained solution is a mixture of water and minced shrimp; (2) taking the clear liquid of the mixed solution of ester and ether for pressure reduced recovery of the solvent, and carrying out drying so as to obtain crimson thick grease, that is, the extract of total astaxanthin of Euphausia superba Dana; (3) dissolving the extract of total astaxanthin of Euphausia superba Dana in anhydrous alcohol to produce a solution with a concentration of 300 to 500 mg/mL, and carrying out separation and collection. The method provided in the invention has the advantages of a simple process, low temperature and a short operation time, which enables the danger of oxidation deterioration in the process of extraction to be effectively reduced; the content of total astaxanthin in the obtained product is more than or equal to 0.5%.
Description
Technical field
The invention belongs to the preparation field of krill astaxanthin, particularly relate to the quick low-temperature extraction method of the total astaxanthin of a kind of freezing krill.
Background technology
Krill also claims South Pole large krill, latin name Euphausia superba Dana, and shell-fish is the halomereid of surrounding waters, South Pole reserves maximum, stock biomass is up to 6.5～10.0 hundred million tons.Protein, lipid isoreactivity composition enrich in the krill, especially are rich in omega-3 polyunsaturated fatty acids, astaxanthin constituents etc. in the lipid component, have very high nutritive value and anti-oxidation efficacy.Wherein, the astaxanthin constituents mainly is astaxanthin (Astaxanthin, be again ASX, namely 3,3 '-dihydroxy-4,4 '-diketone-bata-carotene,＞80%), also comprise part astaxanthin mono fatty acid ester, astaxanthin double acid ester etc., have higher ability aspect anti-oxidant and the elimination free radical.Therefore, the mixture of various astaxanthin constituents more than the preparation from resourceful krill, namely total astaxanthin has comparatively wide application prospect.
The conventional chemical solvent extraction process of marine animal lipid component generally comprises following process: the pulverizing of thawing, cut into slices of freezing individuality, or the individual pulverizing of freeze-drying, then or/and getting, water extraction prepares total extract with organic solvent, and used organic solvent can adopt alcohols, such as ethanol, methyl alcohol; With total extract behind the water-soluble or methanol aqueous solution, with higher alkane (benzinum, n-hexane, cyclohexane), or the halogenated hydrocarbon solvents such as ester class, chloroform or carrene such as ethyl acetate extraction, get the solvent extraction phase, be drying to obtain the lipid component position after reclaiming solvent, wherein used alkane (or ester class, halogenated hydrocarbon) solvent preferably adopts cyclohexane or ethyl acetate.Lipid component also can directly extract or carbon dioxide (CO by above-mentioned alkane, ester class or halogenated hydrocarbon solvent
2) the supercritical extract acquisition.
Astaxanthin constituents oxidation deterioration very easily under higher temperature for obtaining the total astaxanthin of high-quality krill, must adopt targetedly low temperature extraction and preparation technique in the krill.Low-temperature extraction method for total astaxanthin in krill source there is no bibliographical information at present.
Summary of the invention
Technical problem to be solved by this invention provides the quick low-temperature extraction method of the total astaxanthin of a kind of freezing krill, this technique is simple, temperature is low, the operating time is short, can effectively reduce the danger of oxidation deterioration in the preparation process, and total content astaxanthin is more than or equal to 0.5% in the products obtained therefrom.
The quick low-temperature extraction method of the total astaxanthin of a kind of freezing krill of the present invention comprises:
(1) the freezing raw material of krill directly being added volume ratio is 1: 1-5: in 1 ethyl acetate and the mixed solvent of glycol monoethyl ether, then pulverize homogenate, centrifugal, the upper strata is ester ether mixed solution clear liquid, and lower floor is the rotten mixture of water and shrimp;
(2) get above-mentioned ester ether mixed solution clear liquid, dry behind the decompression and solvent recovery, obtain peony thickness grease, i.e. the total Astaxanthin extraction thing of krill;
(3) the total Astaxanthin extraction thing of above-mentioned krill is dissolved in the solution that forms 300-500mg/mL in the absolute ethyl alcohol, separates, collect peony thickness grease and be the total astaxanthin of krill.
The freezing raw material of krill in the described step (1) is for-18 ℃ or more be low to moderate-30 ℃ freezing raw material.
The freezing raw material of per kilogram krill in the described step (1) adds the above-mentioned mixed solvent of 1L-3L.
Ethyl acetate in the described step (1) and the volume ratio of glycol monoethyl ether are 1: 1-5: 1, and preferred 2: 1.
The time of the pulverizing homogenate in the described step (1) is preferably 6min.
Centrifugal condition in the described step (1) is preferably 4 ℃ of low-temperature centrifugation 6min, and rotating speed 6500 turns/min.
The rotten mixture of water in the described step (1) and shrimp adds the above-mentioned mixed solvent of 1L-3L according to the per kilogram raw material, repeats 1 homogenate, centrifugal process, collects the ester ether mixed solution clear liquid on upper strata; Then mix with ester ether mixed solution clear liquid in the step (1) and carry out remaining step.
Sephadex LH-20 gel filtration chromatography post is chosen in separation in the described step (3), according to the ratio loading of the sample solution of every 30-50mL bed volume 1mL, through the absolute ethyl alcohol wash-out, collect red look section, water-bath≤40 ℃ reduced pressure concentration reclaims absolute ethyl alcohol, and get final product.
The total content astaxanthin that extracts among the present invention is more than or equal to 0.50%.
Beneficial effect
Outstanding feature of the present invention is to provide new quick low temperature preparation method for the total astaxanthin of krill, its preparation technology is simple, have advantages of that the temperature of extraction is low, the operating time is short, can effectively reduce the danger of oxidation deterioration in the preparation process, total content astaxanthin is more than or equal to 0.5% in the products obtained therefrom.The raw material sources of krill are abundant, inexpensive, and total astaxanthin of preparation has the sharp prospect of good exploitation, can be used for preparing functional food etc.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Krill-18 a ℃ freezing individuality is got 2.0kg at every turn, chooses 2: 1 ester ether mixed solvent of ethyl acetate and glycol monoethyl ether volume ratio, directly adds 4L and forms the low-temperature mixed thing, pulverizes homogenate 6min again; 4 ℃ of low-temperature centrifugation 6min, rotating speed 6500 turns/min; Topple over after centrifugal and collect upper strata ester ether mixed solution; Lower layer of water and meat gruel mixture add 4L ester ether mixed solvent again and repeat 1 homogenate, centrifugal process; Merge 2 times upper strata ester ether mixed solution, reduced pressure concentration reclaims solvent, and drying obtains peony thickness grease, i.e. the total Astaxanthin extraction thing of krill.Repeatedly extract, product is between the 50.8-63.2 gram, and its recovery rate is 2.54-3.16%.
Astaxanthin constituents content in the total Astaxanthin extraction thing of krill, the total astaxanthin adopts the ultraviolet-visible spectrophotometer method to analyze, during mensuration, with the astaxanthin standard sample at its CHCl
3In the solution according to " Chinese pharmacopoeia (version in 2005) appendix VA UV-VIS spectrophotometry is measured working curve, prepare again certain density testing sample solution, measure its absorbance, utilize the content astaxanthin in the total Astaxanthin extraction thing of working curve calculating krill, the total astaxanthin.Analyze through the ultraviolet-visible spectrophotometer method, the content of total astaxanthin calculates with the standard items astaxanthin in the total Astaxanthin extraction thing of krill, is 0.334-0.388%.
Embodiment 2
Krill-18 a ℃ freezing individuality is got 2.0kg, choose 2: 1 ester ether mixed solvent of ethyl acetate and glycol monoethyl ether volume ratio, add this ester ether mixed solvent of 2.4L, press embodiment 1 flow process and extract the total Astaxanthin extraction thing of krill, get product 51.6g, its recovery rate is 2.58%.Analyze through the ultraviolet-visible spectrophotometer method, the content of total astaxanthin calculates with the standard items astaxanthin in the total Astaxanthin extraction thing of krill that this law is extracted, and is 0.346%.
Embodiment 3
Krill-18 a ℃ freezing individuality is got 2.0kg, choose 1: 1 ester ether mixed solvent of ethyl acetate and glycol monoethyl ether volume ratio, add this ester ether mixed solvent of 4.0L, press embodiment 1 flow process and extract the total Astaxanthin extraction thing of krill, product 58.7g, its recovery rate are 2.94%.Analyze through the ultraviolet-visible spectrophotometer method, the content of total astaxanthin calculates with the standard items astaxanthin in the total Astaxanthin extraction thing of krill that this law is extracted, and is 0.386%.
Embodiment 4
Extract the total Astaxanthin extraction thing of krill that obtains by embodiment 1 and get 3.0g at every turn, be dissolved in absolute ethyl alcohol and form the 10mL concentrated solution, choose the Sephadex LH-20 gel filtration chromatography post of bed volume 300mL, loading is through the absolute ethyl alcohol wash-out, collect red look section, water-bath≤40 ℃ reduced pressure concentration reclaims absolute ethyl alcohol, and lucifuge is dry, gets peony thickness grease, be the total astaxanthin product of krill, repeatedly the product that obtains of repeated experiments is between 2.00-2.45g.Analyze through the ultraviolet-visible spectrophotometer method, total content astaxanthin is 0.508-0.557% in the standby product that obtains of this legal system.
Claims (5)
1. the extracting method of the total astaxanthin of freezing krill comprises:
(1) directly join the freezing raw material of krill in the mixed solvent, mixed solvent was comprised of according to volume ratio ethyl acetate and glycol monoethyl ether in 1: 1～5: 1, then pulverized homogenate, and is centrifugal, the upper strata is ester ether mixed solution clear liquid, and lower floor is the rotten mixture of water and shrimp;
(2) get above-mentioned ester ether mixed solution clear liquid, dry behind the decompression and solvent recovery, obtain peony thickness grease, i.e. the total Astaxanthin extraction thing of krill;
(3) the total Astaxanthin extraction thing of above-mentioned krill is dissolved in the solution that forms 300-500mg/mL in the absolute ethyl alcohol, separates, collect peony thickness grease and be the total astaxanthin of krill; Wherein, separate and to choose Sephadex LH-20 gel filtration chromatography post, according to the ratio loading of the sample solution of every 30-50mL bed volume 1mL, through the absolute ethyl alcohol wash-out, collect red look section, water-bath≤40 ℃ reduced pressure concentration reclaims absolute ethyl alcohol, and get final product.
2. the extracting method of the total astaxanthin of a kind of freezing krill according to claim 1, it is characterized in that: the freezing raw material of per kilogram krill in the described step (1) adds the above-mentioned mixed solvent of 1L-3L.
3. the extracting method of the total astaxanthin of a kind of freezing krill according to claim 1, it is characterized in that: the ethyl acetate in the described step (1) and the volume ratio of glycol monoethyl ether are 2: 1.
4. the extracting method of the total astaxanthin of a kind of freezing krill according to claim 1, it is characterized in that: the time of the pulverizing homogenate in the described step (1) is 6min.
5. the extracting method of the total astaxanthin of a kind of freezing krill according to claim 1, it is characterized in that: the rotten mixture of the water in the described step (1) and shrimp adds the above-mentioned mixed solvent of 1L-3L according to the per kilogram raw material, repeat 1 homogenate, centrifugal process, collect the ester ether mixed solution clear liquid on upper strata; Then mix with ester ether mixed solution clear liquid in the step (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110201341 CN102334686B (en) | 2011-07-19 | 2011-07-19 | Rapid low temperature extraction method for total astaxanthin from frozen Euphausia superba Dana |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110201341 CN102334686B (en) | 2011-07-19 | 2011-07-19 | Rapid low temperature extraction method for total astaxanthin from frozen Euphausia superba Dana |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102334686A CN102334686A (en) | 2012-02-01 |
| CN102334686B true CN102334686B (en) | 2013-01-09 |
Family
ID=45510825
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110201341 Expired - Fee Related CN102334686B (en) | 2011-07-19 | 2011-07-19 | Rapid low temperature extraction method for total astaxanthin from frozen Euphausia superba Dana |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102334686B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104109657A (en) * | 2014-07-07 | 2014-10-22 | 浙江万里学院 | Euphausia superba transglutaminase and application thereof |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746205B (en) * | 2012-07-18 | 2014-07-23 | 山东师范大学 | Method for extracting astaxanthin monoester from antarctic krill |
| CN102731358B (en) * | 2012-07-18 | 2014-05-14 | 山东师范大学 | Method for extracting astaxanthin diester from antarctic krill |
| CN102731361B (en) * | 2012-07-18 | 2014-06-18 | 山东师范大学 | Method for rapidly enriching astaxanthin and ester thereof from Euphausia superba |
| CN102731360B (en) * | 2012-07-18 | 2015-03-25 | 山东师范大学 | Method for extracting astaxanthin from antarctic krill |
| CN102807518B (en) * | 2012-07-18 | 2014-08-27 | 山东师范大学 | Method for extracting astaxanthin and astaxanthin ester from Euphausia superba by using A beta-8 macroporous resin |
| CN102746204B (en) * | 2012-07-18 | 2014-08-06 | 山东师范大学 | Method for using VE powder to quickly adsorb astaxanthin of antarctic krill and esters of astaxanthin and for VE separation |
| CN102731359B (en) * | 2012-07-18 | 2014-06-18 | 山东师范大学 | Extraction method of astaxanthin and ester thereof from antarctic krill |
| CN105085232A (en) * | 2015-07-23 | 2015-11-25 | 山东师范大学 | Method for extracting calcium stearate from euphausia superba and purifying calcium stearate |
| CN116948741A (en) * | 2023-07-10 | 2023-10-27 | 江苏海洋大学 | Method for extracting euphausia superba oil from frozen euphausia superba |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381337A (en) * | 2007-09-03 | 2009-03-11 | 陈锦猜 | Astaxanthin extraction method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2358862B (en) * | 1999-12-21 | 2004-07-21 | Fermentron Ltd | Processes for Extracting Carotenoids from Biomass Carotenoid Sources |
-
2011
- 2011-07-19 CN CN 201110201341 patent/CN102334686B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101381337A (en) * | 2007-09-03 | 2009-03-11 | 陈锦猜 | Astaxanthin extraction method |
Non-Patent Citations (1)
| Title |
|---|
| 许培雅等.虾壳虾青素提取工艺的研究.《粮食与饲料工业》.2003,(第02期),第27-28页. * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104109657A (en) * | 2014-07-07 | 2014-10-22 | 浙江万里学院 | Euphausia superba transglutaminase and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102334686A (en) | 2012-02-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102334686B (en) | Rapid low temperature extraction method for total astaxanthin from frozen Euphausia superba Dana | |
| CN102041166B (en) | Method for extracting krill oil with high phosphatide content from Antarctic krills | |
| Anaëlle et al. | Green improved processes to extract bioactive phenolic compounds from brown macroalgae using Sargassum muticum as model | |
| Chao et al. | Ultrasound-enhanced subcritical water extraction of polysaccharides from Lycium barbarum L. | |
| US8624046B2 (en) | Krill oil and method for manufacturing the same | |
| US8871217B2 (en) | Method for producing fucoxanthin | |
| CN102911138B (en) | The extracting and purifying method of fucoxanthin in a kind of brown alga | |
| Lim et al. | Ionic liquids as green solvent and their applications in bioactive compounds extraction from plants | |
| CN101999521A (en) | Oil tea peel extract containing oil tea peel polyphenol as well as preparation method and application of oil tea peel extract | |
| CN103524596A (en) | Antioxidative peptide of shark protein as well as preparation method and use thereof | |
| CN105175380A (en) | Method for preparing Yunnan pine bark procyanidine | |
| CN102405988A (en) | Method for extracting krill oil with high phospholipid content from krill | |
| CN105732452A (en) | Method for extracting phaffia rhodozyma intracellular astaxanthin | |
| Liu et al. | A novel approach for the simultaneous extraction of dihydroquercetin and arabinogalactan from Larix gmelinii by homogenate-ultrasound-synergistic technique using the ionic liquid | |
| CN112043731A (en) | Preparation method of whole ganoderma lucidum spore oil nanoemulsion rich in ganoderic acid | |
| JP7042764B2 (en) | Tomato extract and its manufacturing method, as well as foods and drinks and cosmetics containing tomato extract | |
| Gavahian et al. | Power ultrasound for valorization of Citrus limon (cv. Eureka) waste: Effects of maturity stage and drying method on bioactive compounds, antioxidant, and anti-diabetic activity | |
| Santos et al. | Conventional and emerging techniques for extraction of bioactive compounds from fruit waste | |
| CN102511569B (en) | Production method for extracting allicin oil from garlic | |
| CN102031116A (en) | New method for preparing rosemary natural antioxidant | |
| Goksen | Elucidation and quantification health-promoting phenolic compounds, antioxidant properties and sugar levels of ultrasound assisted extraction, aroma compositions and amino acids profiles of macroalgae, Laurencia papillosa | |
| CN103509047A (en) | Extraction process of phosphatidylcholine with antarctic krill as source and preparation method of phosphatidylserine | |
| JP2017019756A (en) | Tomato extract and its producing method, and food and drink and cosmetic including tomato extract | |
| CN108559622B (en) | Method for extracting krill oil for ship | |
| CN101933947B (en) | Method for extracting fatty compounds from bee pollen |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent for invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 200090 Shanghai military road, Yangpu District, No. 300 Applicant after: East China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences Address before: 200090 No. 100, military road, Shanghai, Yangpu District Applicant before: East China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20130109 Termination date: 20160719 |