CN116042309A - Extraction method of astaxanthin-rich krill oil - Google Patents

Extraction method of astaxanthin-rich krill oil Download PDF

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Publication number
CN116042309A
CN116042309A CN202310054308.3A CN202310054308A CN116042309A CN 116042309 A CN116042309 A CN 116042309A CN 202310054308 A CN202310054308 A CN 202310054308A CN 116042309 A CN116042309 A CN 116042309A
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astaxanthin
extraction
rich
krill oil
krill
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周涛
高来绪
方勇
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Shandong Kangjing Marine Bioengineering Co ltd
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Shandong Kangjing Marine Bioengineering Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/02—Pretreatment
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/10—Production of fats or fatty oils from raw materials by extracting
    • C11B1/102—Production of fats or fatty oils from raw materials by extracting in counter-current; utilisation of an equipment wherein the material is conveyed by a screw
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/10—Production of fats or fatty oils from raw materials by extracting
    • C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B1/00—Production of fats or fatty oils from raw materials
    • C11B1/10—Production of fats or fatty oils from raw materials by extracting
    • C11B1/106—Production of fats or fatty oils from raw materials by extracting using ultra-sounds
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B3/00—Refining fats or fatty oils
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Microbiology (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Abstract

The invention discloses an extraction method of astaxanthin-rich krill oil, belonging to the technical field of food and chemical industry, comprising the following steps: thawing the antarctic krill stored in a low-temperature freezing way, drying until the water content is less than or equal to 10%, and crushing to obtain antarctic krill powder for later use; adding a eutectic solvent into shrimp powder, and then carrying out countercurrent ultrasonic extraction for 1-5h at 4-10 ℃ to obtain a crude extract; placing the crude extract in a supercritical extraction kettle, and performing supercritical carbon dioxide extraction to obtain crude shrimp oil; and removing the solvent from the crude shrimp oil by rotary evaporation to obtain the astaxanthin-rich krill oil. The invention skillfully combines the organic solvent extraction and the supercritical extraction, adjusts and optimizes the technological parameters, ensures the content of the effective components such as astaxanthin and the like in the krill oil to the greatest extent, and improves the quality of the krill oil.

Description

Extraction method of astaxanthin-rich krill oil
Technical Field
The invention relates to the technical field of food and chemical industry, in particular to an extraction method of astaxanthin-rich krill oil.
Background
Astaxanthin is a carotenoid family member, but due to structural difference, the oxidation resistance of astaxanthin is greatly different, and experiments show that the oxidation resistance of astaxanthin is 10 times of that of beta-carotene, 4 times of that of lutein and many times of that of vitamin E, and the astaxanthin is an oxidation resistant substance with good free radical resistance and aging resistance. Astaxanthin is extremely beneficial for the health of the brain and nervous system, as it can cross the blood brain barrier and is directly available to the brain and central nervous system.
Astaxanthin has effects of enhancing immunity and resisting cancer, can regulate gene activity, inhibit malignant tumor metastasis, effectively prevent and slow down cancer, and has effects of preventing oral cancer and bladder cancer, and inhibiting liver cancer. Studies have shown that the effect of astaxanthin in inhibiting tumorigenesis is in the inhibition of tumor proliferation.
The antarctic krill belongs to crustaceans, about 85 krill species in the global ocean, and about 7 to 8 krill species distributed in the antarctic ring sea area of 50 degrees south latitude are named antarctic krill. The body length is 5.5-6.0cm, the service life is 5-7 years, the weight is about 2g, the trunk is transparent, and the reproductive capacity is strong. In the antarctic sea area, antarctic krill has a biomass of about 3.42-5.36 tons and is the largest biological resource in single species worldwide. Euphausia superba is rich in nutrients including proteins, lipids, and antioxidant substances such as astaxanthin, flavonoids, and vitamins A, E.
The euphausia superba oil extracted from euphausia superba powder contains rich natural high-esterified astaxanthin, and meanwhile, phosphorus element in euphausia superba is enriched. Phospholipids are the material basis of life, and cell membranes are composed of about 30% phospholipids. The phospholipid is composed of lecithin, inositol phospholipid, cephalin, etc. These phospholipids have corresponding functions on various parts and organs of the human body. In general terms, the basic functions of phospholipids are: the euphausia superba oil has the effects of enhancing brain, improving immunity and regeneration, detoxifying, cleaning blood, building skin, delaying aging, preventing and treating cardiovascular diseases, relieving inflammation pain, relieving premenstrual syndrome and the like due to the fact that the euphausia superba oil contains phospholipid type unsaturated fatty acid.
Disclosure of Invention
In view of the above, the invention provides an extraction method of krill oil rich in astaxanthin, which optimizes the preparation process of the krill oil, skillfully combines organic solvent extraction and supercritical extraction, adjusts and optimizes process parameters, maximally ensures the content of effective components such as astaxanthin in the krill oil, and improves the quality of the krill oil.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
an extraction method of astaxanthin-rich krill oil comprises the following steps:
(1) Thawing the antarctic krill stored in a low-temperature freezing way, drying until the water content is less than or equal to 10%, and crushing to obtain antarctic krill powder for later use;
(2) Adding a eutectic solvent into shrimp powder, and then carrying out countercurrent ultrasonic extraction for 1-5h at 4-10 ℃ to obtain a crude extract;
(3) Placing the crude extract in a supercritical extraction kettle, and performing supercritical carbon dioxide extraction to obtain crude shrimp oil;
(4) And removing the solvent from the crude shrimp oil by rotary evaporation to obtain the astaxanthin-rich krill oil.
Preferably, the low temperature is less than-50 ℃.
The beneficial effects brought by the optimization are as follows: the freezing preservation at low temperature can greatly reduce the oxidation speed of the antarctic krill astaxanthin, thereby improving the astaxanthin content in the antarctic krill grease obtained by extraction.
Preferably, the drying temperature is 60-70 ℃.
Preferably, the solid-to-liquid ratio of the shrimp meal to the co-melting solvent is 1:30-50g/mL.
Preferably, the eutectic solvent is DL-menthol and thymol.
The beneficial effects brought by the optimization are as follows: compared with other extraction solvents, the extraction solvent is environment-friendly, the yield of the euphausia superba grease is obviously improved, and the astaxanthin and the ester content of the extracted euphausia superba grease are greatly improved.
Preferably, the molar ratio of DL-menthol to thymol is (1:2): (2:1).
The beneficial effects brought by the optimization are as follows: the eutectic solvent with the volume ratio dissolves astaxanthin and astaxanthin ester from the antarctic krill sample with higher water content, does not generate emulsification phenomenon, and has fewer dissolved impurities.
Preferably, the supercritical extraction is carried out for 50-150min at 35-45deg.C under 35-45MPa and CO 2 The flow rate is 0.5-1.5L/min.
The beneficial effects brought by the optimization are as follows: the process parameters of supercritical extraction affect the purity of astaxanthin, and the purity of astaxanthin in krill oil obtained by the extraction of the parameters is highest.
Preferably, the temperature of the rotary evaporation is 30-40 ℃.
Compared with the prior art, the invention has the following beneficial effects
(1) The shrimp oil rich in astaxanthin can be obtained by the method. Not only the shrimp oil containing unsaturated fatty acid is preserved, but also the shrimp oil is rich in astaxanthin, so that the health care effect of the product is enhanced;
(2) The solvent extraction and the supercritical carbon dioxide extraction are combined, the process is simple, and the purity of the obtained product is high;
(3) The solvent is selected from DL-menthol and thymol, and is nontoxic, has little damage to astaxanthin structure and is environment-friendly.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
An extraction method of astaxanthin-rich krill oil comprises the following steps:
(1) Thawing Euphausia superba preserved at-50deg.C, drying at 70deg.C until water content is less than or equal to 10%, and pulverizing to obtain Euphausia superba powder;
(2) Adding DL-menthol and thymol into shrimp powder, and performing countercurrent ultrasonic extraction at 10deg.C for 1 hr to obtain crude extract;
wherein, the solid-to-liquid ratio of the shrimp powder to the co-melting solvent is 1:40g/mL, and the mol ratio of DL-menthol and thymol is 2:1;
(3) Placing the crude extract in a supercritical extraction kettle, and performing supercritical carbon dioxide extraction to obtain crude shrimp oil;
wherein the extraction time in supercritical extraction is 150min, the extraction temperature is 45deg.C, the extraction pressure is 45MPa, and CO is used for extracting 2 The flow rate was 1.5L/min.
(4) And (3) removing the solvent from the crude shrimp oil by rotary evaporation at 40 ℃ to obtain the astaxanthin-rich krill oil.
Example 2
An extraction method of astaxanthin-rich krill oil comprises the following steps:
(1) Thawing Euphausia superba preserved at-80deg.C, drying at 60deg.C until water content is less than or equal to 10%, and pulverizing to obtain Euphausia superba powder;
(2) Adding DL-menthol and thymol into shrimp powder, and performing countercurrent ultrasonic extraction at 4deg.C for 5 hr to obtain crude extract;
wherein, the solid-liquid ratio of the shrimp meal to the co-melting solvent is 1:35g/mL; the molar ratio of DL-menthol to thymol is 1:1.5;
(3) Placing the crude extract in a supercritical extraction kettle, and performing supercritical carbon dioxide extraction to obtain crude shrimp oil;
wherein the extraction time in supercritical extraction is 50min, the extraction temperature is 35deg.C, the extraction pressure is 35MPa, and CO is used 2 The flow rate is 0.5/min;
(4) And (3) removing the solvent from the crude shrimp oil by rotary evaporation at 30 ℃ to obtain the astaxanthin-rich krill oil.
Example 3
An extraction method of astaxanthin-rich krill oil comprises the following steps:
(1) Thawing Euphausia superba preserved at-60deg.C, drying at 65deg.C until water content is less than or equal to 10%, and pulverizing to obtain Euphausia superba powder;
(2) Adding DL-menthol and thymol into shrimp powder, and performing countercurrent ultrasonic extraction at 7deg.C for 3 hr to obtain crude extract;
wherein, the solid-liquid ratio of the shrimp meal to the co-melting solvent is 1:42g/mL; the molar ratio of DL-menthol to thymol is 1:1;
(3) Placing the crude extract in a supercritical extraction kettle, and performing supercritical carbon dioxide extraction to obtain crude shrimp oil;
wherein the extraction time in supercritical extraction is 100min, the extraction temperature is 40 ℃, the extraction pressure is 40MPa, and CO is used for extracting 2 The flow rate is 1L/min
(4) And (3) removing the solvent from the crude shrimp oil by rotary evaporation at 35 ℃ to obtain the astaxanthin-rich krill oil.
Comparative example 1
The extraction process was the same as in example 3, except that the antarctic krill in step (1) was a commercially available dry antarctic krill.
Comparative example 2
The extraction method is the same as in example 3, except that the euphausia superba is crushed and then the shrimp meal is directly put into a supercritical extraction kettle for extraction.
Comparative example 3
The extraction process was the same as in example 3, except that in step (2) the solvent was ethanol.
Comparative example 4
The extraction method is the same as in example 3, except that the parameters in the supercritical extraction in step (3) are: the extraction time is 200min, the extraction temperature is 50 ℃, the extraction pressure is 50MPa, and CO 2 The flow rate was 2L/min.
Astaxanthin content in krill oil of examples 1-3 and comparative examples 1-4 was measured and the results are shown in Table 1:
TABLE 1
Figure BDA0004059820640000061
As can be seen from the data in Table 1, the astaxanthin content is affected by a plurality of parameters in the extraction process, and the invention skillfully combines the organic solvent extraction with the supercritical extraction, adjusts and optimizes the process parameters, maximally ensures the content of effective components such as astaxanthin in the krill oil, and improves the quality of the krill oil.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other. For the device disclosed in the embodiment, since it corresponds to the method disclosed in the embodiment, the description is relatively simple, and the relevant points refer to the description of the method section.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (8)

1. The extraction method of the krill oil rich in astaxanthin is characterized by comprising the following steps of:
(1) Thawing the antarctic krill stored in a low-temperature freezing way, drying until the water content is less than or equal to 10%, and crushing to obtain antarctic krill powder for later use;
(2) Adding a eutectic solvent into shrimp powder, and then carrying out countercurrent ultrasonic extraction for 1-5h at 4-10 ℃ to obtain a crude extract;
(3) Placing the crude extract in a supercritical extraction kettle, and performing supercritical carbon dioxide extraction to obtain crude shrimp oil;
(4) And removing the solvent from the crude shrimp oil by rotary evaporation to obtain the astaxanthin-rich krill oil.
2. The method of claim 1, wherein the cryopreservation is performed at a temperature less than-50 ℃.
3. The method for extracting astaxanthin-rich krill oil according to claim 1, wherein said drying temperature is 60-70 ℃.
4. The method for extracting astaxanthin-rich krill oil according to claim 1, wherein the solid-to-liquid ratio of the shrimp powder to the co-melted solvent is 1:30-50g/mL.
5. The method for extracting astaxanthin-rich krill oil according to claim 1, wherein said eutectic solvent is DL-menthol and thymol.
6. The method for extracting astaxanthin-rich krill oil according to claim 5, wherein said DL-menthol and thymol are in a molar ratio of (1:2): (2:1).
7. The method for extracting astaxanthin-rich krill oil according to claim 1, wherein the supercritical extraction is performed for 50-150min at 35-45deg.C under 35-45MPa and CO 2 The flow rate is 0.5-1.5L/min.
8. The method for extracting astaxanthin-rich krill oil according to claim 1, wherein the temperature of the rotary evaporation is 30-40 ℃.
CN202310054308.3A 2023-02-03 2023-02-03 Extraction method of astaxanthin-rich krill oil Pending CN116042309A (en)

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