CN105542936B - A kind of extracting method of antarctic krill oil - Google Patents
A kind of extracting method of antarctic krill oil Download PDFInfo
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- CN105542936B CN105542936B CN201510943810.5A CN201510943810A CN105542936B CN 105542936 B CN105542936 B CN 105542936B CN 201510943810 A CN201510943810 A CN 201510943810A CN 105542936 B CN105542936 B CN 105542936B
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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
- C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
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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
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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
- C11B1/10—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
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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
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
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- Life Sciences & Earth Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Wood Science & Technology (AREA)
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Abstract
The invention discloses a kind of extracting methods of antarctic krill oil, and using krill processing byproduct as raw material, after enzymatic hydrolysis, filtering, centrifugal treating, freeze-drying obtains the lipoprotein powder rich in shrimp sauce；Using ethyl alcohol as Extraction solvent, the lipoprotein powder of freeze-drying is extracted using three stage countercurrents, removes filter residue, and evaporative removal solvent obtains the thick shrimp sauce of krill rich in phosphatide and astaxanthin.The invention avoids the discarded pollutions generated to environment of by-product, while can produce the shrimp sauce product of high added value, improve the rate of return on investment of krill industry.
Description
Technical field
The invention belongs to food processing technology field, it is related to extracting shrimp sauce in a kind of processing byproduct from krill
Method.
Background technique
Krill (Euphausia superba) also known as large krill or Antarctic krill, are that quantity is maximum on the earth
One of single living resources.The krill biology total amount of the Antarctic Ocean is at hundred million tons of 4-15.5 according to statistics.And the South Pole 2010-2011
The amount of fishing of krill only has 210,000 tons, well below South Pole ocean living resources conservation association formulate can amount of fishing (8,600,000
Ton), far below the 0.1% of biological total amount.In recent years, with the gradually failure of worldwide traditional fishery resource, in antarctic waters
Concern of the huge krill resource by some deep-sea fishing developed countries, China have also been included in krill resource
One of the main exploitation kind of Development for Distant Water Fishery from now on.
Krill is full of nutrition, it was reported that protein content 17.4%, fatty 1.1%, ash content in krill shrimp
About 2.3%.Krill fat in polyunsaturated fatty acid (PUFA) rich in, the EPA of especially n-3 series with
DHA.These PUFA with healthy functions mostly with the presence of phosphatide mating type, are easier to be absorbed and utilized for human body.Research finds shrimp
The bioavailability of oil is better than shrimp, fish oil.In addition, (Astaxanthin) containing astaxanthin abundant in krill shrimp shell, this
It is a Carotenoids, not only there is strong anti-oxidation ability, but also possess the incomparable peace of artificial synthesized class polyphenoils
Quan Xing has more correlative study report both at home and abroad.
In recent years, become hot spot about the research of antarctic krill oil both at home and abroad.Industrial shrimp sauce extracts mainly with full shrimp
For raw material, extracted with organic solvent.Waste that is increasing, generating in process is utilized with krill resource
More and more, this can not only adversely affect natural environment, and a kind of waste to resource.Research finds krill
The height of the more full shrimp of fat content in processing byproduct, reaches 3.3% or so, and EPA rich in and DHA.And current state
Mainly using full shrimp as raw material, the research for krill processing byproduct is relatively fewer for the inside and outside extraction about krill oil.
Summary of the invention
The purpose of this section is to summarize some aspects of the embodiment of the present invention and briefly introduce some preferable implementations
Example.It may do a little simplified or be omitted to avoid our department is made in this section and the description of the application and the title of the invention
Point, the purpose of abstract of description and denomination of invention it is fuzzy, and this simplification or omit and cannot be used for limiting the scope of the invention.
In view of extracted in the above-mentioned and/or existing processing byproduct from krill shrimp sauce there are the problem of, propose this
Invention.
Therefore, present invention purpose therein be to provide it is a kind of using the preparation of krill processing byproduct rich in phosphatide and shrimp
The method of green element krill oil.
In order to solve the above technical problems, the invention provides the following technical scheme: a kind of extracting method of antarctic krill oil,
Using krill processing byproduct as raw material, after enzymatic hydrolysis, filtering, centrifugal treating, freeze-drying obtains the rouge egg rich in shrimp sauce
White powder；Using ethyl alcohol as Extraction solvent, the lipoprotein powder being lyophilized using the extraction of three stage countercurrents, removal filter residue, evaporative removal solvent,
Obtain the thick shrimp sauce of krill rich in phosphatide and astaxanthin；Wherein, the enzymatic hydrolysis: 100 DEG C of boiling processing byproducts 5~
10min is later 1: 4 addition water according to processing byproduct and water quality ratio, keeps 10min after adjusting the temperature to 30~60 DEG C,
PH 8.0~8.5 is adjusted, the alkali protease of 2000~5000U/g albumen is added, is protected from light, is stirred to react 1.5~3.5h；It is described
Centrifugation: pH is first adjusted to shrimp albumen isoelectric point 4.5, after standing 30min, filtrate is centrifuged through 3000r/min~5000r/min
15min separates supernatant with sediment, collects paste sediment；Three stage countercurrent extracts: 50 DEG C of Extracting temperature, rouge egg
The mass volume ratio 1: 9 of white powder and ethyl alcohol, single-stage extraction time 0.5h.
A kind of preferred embodiment of extracting method as antarctic krill oil of the present invention, in which: the krill
Processing byproduct be krill through flesh separator four times squeeze adopt meat after obtain shrimp shell, shrimp head by-product.
A kind of preferred embodiment of extracting method as antarctic krill oil of the present invention, in which: the filtering: 60~
80 mesh silks by after enzymatic hydrolysis residue and enzymolysis liquid separate.
A kind of preferred embodiment of extracting method as antarctic krill oil of the present invention, in which: the freeze-drying:
Centrifugal sediment is freeze-dried, the lipoprotein powder rich in shrimp sauce is obtained, fat content is 50%~60%.
A kind of preferred embodiment of extracting method as antarctic krill oil of the present invention, in which: the evaporation:
0.1MPa >=vacuum degree >=0.08MPa is evaporated in vacuo at 45~50 DEG C, and solvent evaporated obtains thick shrimp sauce.
A kind of preferred embodiment of extracting method as antarctic krill oil of the present invention, in which: the adjusting enzymatic hydrolysis
System pH 8.0~8.5 uses mass percent to be adjusted for 20%~50% KOH solution.
A kind of preferred embodiment of extracting method as antarctic krill oil of the present invention, in which: the adjusting pH to
Shrimp albumen isoelectric point 4.5, uses mass percent to be adjusted for 10%~50% hydrochloric acid.
A kind of preferred embodiment of extracting method as antarctic krill oil of the present invention, in which: the freeze-drying,
It is frozen into solid-state under the conditions of -10 DEG C~-50 DEG C, then rises moisture therein directly without liquid
China is at gaseous state.
The present invention combines enzymatic hydrolysis and organic leach extraction method, and the shrimp sauce in krill processing byproduct is enriched with and is mentioned
It takes, 25g krill processes lipoprotein of the by-product through the available about 2.5~3g of the processing such as enzymatic hydrolysis, therefore reduces then
Solvent needed for energy consumption and extraction process needed for raw material drying.The invention avoids the discarded dirts generated to environment of by-product
Dye, while the shrimp sauce product of high added value can be produced, improve the rate of return on investment of krill industry.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill of field, without any creative labor, it can also be obtained according to these attached drawings other
Attached drawing.Wherein:
Fig. 1 three stage countercurrent of the present invention extracts flow diagram, wherein A illustrates lipoprotein powder；B illustrates alcohol solvent；
→ signal material trend；Extracting solution is collected in signal；
The extracting method process flow diagram of antarctic krill oil in Fig. 2 one embodiment of the invention；
The influence schematic diagram of drying mode prawn oleic acid valence selected by Fig. 3 present invention.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, right with reference to the accompanying drawings of the specification
A specific embodiment of the invention is described in detail.
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention, but the present invention can be with
Implemented using other than the one described here other way, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar popularization, therefore the present invention is not limited by the specific embodiments disclosed below.
Secondly, " one embodiment " or " embodiment " referred to herein, which refers to, may be included at least one realization side of the invention
A particular feature, structure, or characteristic in formula." in one embodiment " that different places occur in the present specification not refers both to
The same embodiment, nor the individual or selective embodiment mutually exclusive with other embodiments.
Embodiment 1
(1) meat is adopted by krill four times, obtained processing byproduct is as raw material.
(2) by raw material at 100 DEG C boiling 10min, be added distilled water (mass ratio=1: 4), adjust temperature be 50 DEG C, protect
After holding 10min, pH8.5 is adjusted, alkali protease 3000U/g albumen is added, after digesting 2h, boils 10min enzyme deactivation later, it is cooling
Afterwards, with after the filtering of 80 mesh thin,tough silk yarns, filtrate is collected.
(3) after the filtrate for obtaining above-mentioned steps is adjusted to pH4.5,30min is stood, it is heavy that 8000r/min is centrifuged to obtain paste
It forms sediment, carries out freeze-drying process.
(4) using ethyl alcohol as Extraction solvent, the shrimp sauce in freeze-drying lipoprotein is extracted using the method that multi-stage countercurrent continuously extracts,
Extracting series is 3 grades, and the solid-liquid ratio (w/v) of every grade of extraction is 1: 9, solid-liquid ratio 1: 9 (m: V), extraction time 30min.Extract knot
Shu Hou, centrifugation removal filter residue, filter vacuum obtain thick shrimp sauce after evaporating recycling design, and the final recovery rate of grease is about 75%, shrimp
Content of phospholipid 23% in oil, 1250 μ g/g shrimp sauce of content astaxanthin.The final recovery rate of grease refers to the shrimp sauce that ethyl alcohol extracts
Account for the percentage of shrimp sauce total amount in processing byproduct.
Embodiment 2
(1) meat is adopted by krill four times, obtained processing byproduct is as raw material.
(2) by raw material at 100 DEG C boiling 10min, be added distilled water (mass ratio=1: 4), adjust temperature be 30 DEG C, protect
After holding 10min clock, pH8.5 is adjusted, alkali protease 2000U/g albumen is added, after digesting 1h, boils 10min enzyme deactivation later, it is cold
But after, after the filtering of 80 mesh thin,tough silk yarns, filtrate is collected.
(3) after the filtrate for obtaining above-mentioned steps is adjusted to pH4.5,30min is stood, it is heavy that 8000r/min is centrifuged to obtain paste
It forms sediment, carries out freeze-drying process.
(4) using ethyl alcohol as Extraction solvent, the shrimp sauce in freeze-drying lipoprotein is extracted using the method that multi-stage countercurrent continuously extracts,
Extracting series is 3 grades, and the solid-liquid ratio (w/v) of every grade of extraction is 1: 9, solid-liquid ratio 1: 9 (m: V), extraction time 30min.Extract knot
Shu Hou, centrifugation removal filter residue, filter vacuum obtain thick shrimp sauce after evaporating recycling design, and the final recovery rate of grease is about 60%, shrimp
Content of phospholipid 20% in oil, 1050 μ g/g shrimp sauce of content astaxanthin.The final recovery rate of grease refers to the shrimp sauce that ethyl alcohol extracts
Account for the percentage of shrimp sauce total amount in processing byproduct.
Embodiment 3
(1) meat is adopted by krill four times, obtained processing byproduct is as raw material.
(2) by raw material at 100 DEG C boiling 10min, be added distilled water (mass ratio=1: 4), adjust temperature be 60 DEG C, protect
After holding 10min clock, pH8.5 is adjusted, alkali protease 5000U/g albumen is added, after digesting 3h, boils 10min enzyme deactivation later, it is cold
But after, after the filtering of 80 mesh thin,tough silk yarns, filtrate is collected.
(3) after the filtrate for obtaining above-mentioned steps is adjusted to pH4.5,30min is stood, it is heavy that 8000r/min is centrifuged to obtain paste
It forms sediment, carries out freeze-drying process.
(4) using ethyl alcohol as Extraction solvent, the shrimp sauce in freeze-drying lipoprotein is extracted using the method that multi-stage countercurrent continuously extracts,
Extracting series is 3 grades, and the solid-liquid ratio (w/v) of every grade of extraction is 1: 9, solid-liquid ratio 1: 9 (m: V), extraction time 30min.Extract knot
Shu Hou, centrifugation removal filter residue, filter vacuum obtain thick shrimp sauce after evaporating recycling design, and the final recovery rate of grease is about 70%, shrimp
Content of phospholipid 20% in oil, 1020 μ g/g shrimp sauce of content astaxanthin.The final recovery rate of grease refers to the shrimp sauce that ethyl alcohol extracts
Account for the percentage of shrimp sauce total amount in processing byproduct.
The method that 5~10min thermophilic digestion is used in embodiment, main there are two purposes: 1. lipase inactivates, and prevents enzyme
Fat splitting in solution preocess；2. albuminous degeneration is conducive to the hydrolysis of albumen enzyme effect.
If the volume that distilled water is added is very few, enzymatic hydrolysis system is not easy to stir, and influences the hydrolysis result of protease.It is steamed if being added
The volume of distilled water is more, will increase the workload of the operations such as filtering, centrifugation, therefore selects that the distilled water that mass ratio is 1: 4 is added,
On the basis of can guarantee hydrolysis result, reduce the workload of subsequent operation.Hydrolysis temperature, enzymolysis time and zymolyte ratio
It is the key factor for influencing lipoprotein, shrimp sauce yield.If enzymatic hydrolysis is insufficient, lipoprotein can not be sufficiently separated with shrimp shell；If
Enzymatic hydrolysis excessively, will lead to part albumen and fat separation, and a small amount of fat is miscible with water, it is difficult to separate and collect.Most preferred enzymatic hydrolysis
Condition is: 2h is reacted at 55 DEG C, alkali protease additive amount is 3000U/g albumen or so.Lipoprotein is enriched in raw material at this time
Nearly the 85% of shrimp sauce.The dosage of subsequent energy consumption for drying and solvent can be greatlyd save by digesting process of enriching.
The present invention reaches 50% using freeze-drying, lipoprotein butt fat content.Freeze-drying can be significant
Reduce the influence that the drying modes such as conventional hot blast drying aoxidize shrimp sauce.
Using ethyl alcohol as Extraction solvent, it is more conducive to the extraction and enrichment of this polar substances of phosphatide.The grade of use
Number is three-level, and single-stage extraction condition is temperature 50 C, solid-liquid ratio 1: 9 (m: V), extraction time 30min.After centrifugation removal filter residue,
Filtrate is evaporated in vacuo under 45~50 DEG C, vacuum degree >=0.08MPa, solvent evaporated, obtains thick shrimp sauce.It is extracted by multi-stage countercurrent
The final recovery rate of shrimp sauce can be made to reach 75%, content of phospholipid 23% in shrimp sauce, 1250 μ g/g shrimp sauce of content astaxanthin.
It should be noted that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to preferable
Embodiment describes the invention in detail, those skilled in the art should understand that, it can be to technology of the invention
Scheme is modified or replaced equivalently, and without departing from the spirit and scope of the technical solution of the present invention, should all be covered in this hair
In bright scope of the claims.
Claims (5)
1. a kind of extracting method of antarctic krill oil, it is characterised in that: using krill processing byproduct as raw material, digested,
After filtering, centrifugal treating, freeze-drying obtains the lipoprotein powder rich in shrimp sauce；It is inverse using three-level using ethyl alcohol as Extraction solvent
Stream extracts the lipoprotein powder of freeze-drying, removes filter residue, and evaporative removal solvent obtains the thick shrimp of krill rich in phosphatide and astaxanthin
Oil；Wherein,
The krill processing byproduct be krill through flesh separator four times squeeze adopt meat after obtain shrimp shell, shrimp head by-product
Object；
The enzymatic hydrolysis: 100 DEG C of boiling 5~10min of processing byproduct add later according to processing byproduct with water quality ratio for 1:4
Enter water, 10min is kept after adjusting the temperature to 30~60 DEG C, adjust enzymatic hydrolysis system pH 8.0~8.5,2000~5000U/g is added
The alkali protease of albumen, is protected from light, and is stirred to react 1.5~3.5h；
The centrifugation: pH is adjusted to shrimp albumen isoelectric point 4.5, after standing 30min, filtrate is through 3000r/min~5000r/min
It is centrifuged 15min, supernatant is separated with sediment, collects paste sediment；
The freeze-drying: centrifugal sediment is freeze-dried, and solid-state is frozen under the conditions of -10 DEG C~-50 DEG C, then true
So that moisture therein is directly sublimed into gaseous state without liquid under 1.3~5Pa of sky, obtain the lipoprotein powder rich in shrimp sauce, fat contains
Amount is 50%~60%；
Three stage countercurrent extracts: 50 DEG C of Extracting temperature, the mass volume ratio 1:9 of lipoprotein powder and ethyl alcohol, the single-stage extraction time
0.5h。
2. the extracting method of antarctic krill oil as described in claim 1, it is characterised in that: the filtering: 60~80 mesh silks
By after enzymatic hydrolysis residue and enzymolysis liquid separate.
3. the extracting method of antarctic krill oil as described in claim 1, it is characterised in that: the evaporation: 0.1MPa >=vacuum
Degree >=0.08MPa is evaporated in vacuo at 45~50 DEG C, and solvent evaporated obtains thick shrimp sauce.
4. the extracting method of antarctic krill oil as described in claim 1, it is characterised in that: the adjusting enzymatic hydrolysis system pH 8.0
~8.5, use mass percent to be adjusted for 20%~50% KOH solution.
5. the extracting method of antarctic krill oil as described in claim 1, it is characterised in that: described adjusting pH to shrimp albumen etc.
Electricity point 4.5, uses mass percent to be adjusted for 10%~50% hydrochloric acid.
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| CN106588976B (en) * | 2016-12-13 | 2018-06-29 | 山东省科学院生物研究所 | The method that high-purity omega-3 polyunsaturated fatty acids phosphatide is extracted from shrimp head |
| CN106588977B (en) * | 2016-12-13 | 2018-06-29 | 山东省科学院生物研究所 | A kind of method that high-purity marine phospholipids are extracted from krill |
| CN107197927A (en) * | 2017-05-02 | 2017-09-26 | 浙江工业大学 | The boat-carrying continuous process of the continuous dry-making method of dried of boat-carrying of krill and its peeled shrimp that shells |
| CN107216350A (en) * | 2017-07-05 | 2017-09-29 | 武汉轻工大学 | Method of phosphatide and products thereof is extracted in a kind of processing byproduct from cray |
| CN107518281A (en) * | 2017-09-15 | 2017-12-29 | 武汉轻工大学 | A kind of vermicelli of flavor containing cray and trophic function composition and preparation method thereof |
| CN107904009B (en) * | 2017-12-21 | 2021-01-08 | 山东师范大学 | Method for re-extracting grease from euphausia superba residues |
| CN108559622B (en) * | 2018-03-19 | 2021-03-26 | 中国水产科学研究院东海水产研究所 | Method for extracting krill oil for ship |
| JP7156627B2 (en) * | 2018-03-30 | 2022-10-19 | 岩手県 | Method for producing krill component-containing composition |
| CN109601691A (en) * | 2019-01-23 | 2019-04-12 | 日照职业技术学院 | Lipid enrichment method synchronous with protein in a kind of arctic sweet tea shrimp processing byproduct |
| CN109735392B (en) * | 2019-01-28 | 2021-04-27 | 江南大学 | Preparation method of high-astaxanthin and high-phospholipid shrimp sauce |
| CN110862871A (en) * | 2019-11-13 | 2020-03-06 | 武汉轻工大学 | Method for efficiently enriching n-3PUFA lipid from aquatic product processing by-products |
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| CN103283930B (en) * | 2013-05-24 | 2014-11-26 | 江南大学 | Method for comprehensively utilizing euphausia superba shells |
| CN104357206A (en) * | 2014-11-18 | 2015-02-18 | 董寰 | Method for preparing phospholipid-rich Antarctic krill oil by water enzyme process |
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