CN107418721A - Low arsenic krill fluid composition and preparation method thereof - Google Patents
Low arsenic krill fluid composition and preparation method thereof Download PDFInfo
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- CN107418721A CN107418721A CN201710296022.0A CN201710296022A CN107418721A CN 107418721 A CN107418721 A CN 107418721A CN 201710296022 A CN201710296022 A CN 201710296022A CN 107418721 A CN107418721 A CN 107418721A
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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
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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
- A23D9/04—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
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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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
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
-
- 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
- C11B3/12—Refining fats or fatty oils by distillation
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- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
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Abstract
Low arsenic krill fluid composition and preparation method thereof, the composition is prepared by following methods：(1) after washing raw material with ethanol water, extracted with ethyl acetate and ethanol according to the mixed solvent of arbitrary proportion；(2) extract solution is with adsorbent arsenic removal；(3) molecular distillation desolvation.This preparation technology is simple to operate, consume energy low, products obtained therefrom total arsenic content is low, and content of phospholipid is high and is rich in the multiple beneficial composition such as astaxanthin and the race's aliphatic acid of ω 3 (EPA and DHA), is a kind of mode for effectively obtaining low total arsenic content antarctic krill oil.
Description
Technical field
The present invention relates to a kind of method that krill oil is extracted from krill, it is directed to preparation-obtained by this method
The krill oil product of low total arsenic content.
Background technology
Krill is distributed mainly on the free of contamination South Pole marine site of low temperature, is a kind of crustacean plankton, using algae as
Food, its reserves is huge, about 1,000,000,000 tons.Krill rich in multiple beneficial composition include ω -3 races aliphatic acid (EPA and
DHA), phosphatide, astaxanthin, linoleic acid, leukotrienes, palmitic acid etc., it is a kind of preferable natural health care, but due to South Pole phosphorus
Heavy metal arsenic (total arsenic) in shrimp containing 2-3ppm, it is higher that it extracts total arsenic (organo-arsenic and inorganic arsenic) content in gained krill oil
(general 7-10ppm), its inorganic arsenic are generally 0.05-0.10ppm, organo-arsenic 7-10ppm.Because the heavy metal arsenic of excess can be done
Disturb the eubolism of cell, influence breathing and oxidizing process, make cell occur lesion, therefore krill oil in food apply by
Limitation.
At present, on the market krill oil product its total arsenic content is higher, generally 7-10ppm, is also removed without krill oil
Report in terms of total arsenic.After the completion of the A of Chinese patent CN 102041166 are using the extraction extraction of nonpolar or weakly polar organic solvent
Krill oil add polar organic solvent and be enriched with, nitrogen or carbon dioxide remove polar solvent, its shortcoming to be nonpolar or
Low pole extraction efficiency is low.The A of Chinese patent CN 102405988 are using shearing extraction 1-4 times, and ethanol is solvent, nitrogen or two
Carbonoxide removes organic solvent, but ethanol is solvent, extraction time length, needs to soak before shearing, reduces extraction efficiency.China
The A of patent CN 101652462 report a kind of krill oil extracting mode of carbon dioxide supercritical extraction, although low temperature extraction is more
Help to retain benefit materials, but its extraction efficiency is not high, and high energy consumption, equipment cost are big.Chinese patent CN
The method that 1324394 A report acetone low temperature extraction krill oil, filter residue are extracted using ethanol for the second time, lipid grading extraction,
Slag recovering enzyme and protein, this technique is complex, and time-consuming and acetone can be to product quality for the dissolvent residual of solvent
And later stage application has an impact.The A2 of patent WO 2014/013335 report to be entered using ethanol to the krill oil for completing extraction
Row low temperature removes saturated fatty acid, the method for improving unrighted acid ratio, and beneficiating ingredient content is high in its product：EPA is high
In 22%, DHA higher than 10%, vegetable oil acid 3%-9%, astaxanthin 20-4000ppm, but there is not total arsenic content related data.
Other Li Dinglong etc., the method removed using composite to drink reclaimed water micro amount of arsenic was reported in 2007；Liu builds, in
The arsenic adsorbed using modified kaolin in water is reported within 2009, but arsenic is typically inorganic with arsenate and arsenite etc. in water
Form is present, and its content is not high and relatively easily removes, and the arsenic overwhelming majority in antarctic krill oil is deposited in the form of organo-arsenic
High in, its content, molecular weight is relatively large, and removing difficulty is high, and there has been no the xi phases for closing total arsenic removing in antarctic krill oil at present
Close report.
The content of the invention
The present invention is intended to provide a kind of krill oil product and its production method.This method can should comprehensively take into account production
Harmful components removal and the reservation of beneficiating ingredient in product.
Therefore, present invention firstly provides a kind of preparation method of low arsenic krill fluid composition, with the South Pole after crushing
Krill meal is raw material, is comprised the following steps：
(1) after washing raw material with ethanol water, extracted with ethyl acetate and ethanol according to the mixed solvent of arbitrary proportion；
(2) extract solution is with adsorbent arsenic removal；
(3) molecular distillation desolvation.
Further, the present invention also provides the low arsenic krill fluid composition obtained by the above method.
The preparation method complex optimum of the low arsenic krill fluid composition of the invention described above Feedstock treating and extraction remove
Miscellaneous technical process, the total arsenic content in antarctic krill oil is reduced by the way of advance washing and absorption are combined, simultaneously
The content of Hubeiwan such as ω -3 races aliphatic acid (EPA and DHA), phosphatide, astaxanthin etc. in krill oil is not destroyed.Extract solution is adopted
Desolvation is carried out with the mode of molecular distillation, effectively removes dissolvent residual.So as to obtain the low arsenic antarctic krill oil of high quality
Composition product.
Embodiment
The present invention is intended to provide the high quality Antarctic krill oil product of low arsenic.The excellent specific property of the product is entirely due to this hair
Bright advanced efficient preparation method is obtained.
The preparation method of low arsenic krill fluid composition of the present invention, using the euphausia superba powder after crushing as original
Material, including the step such as raw material washing, extraction, absorption arsenic removal and solvent removal.
Firstly, it is necessary to the euphausia superba powder as raw material is washed using ethanol water washing.Wherein, second used
Alcohol solution is the ethanol-water solution that ethanol weight/mass percentage composition is 10~50%；Wherein particularly preferred concentration of alcohol 30% is left
Right ethanol water.In the embodiment of washing, the mass ratio of raw material and ethanol water is 1:4~6.It is preferred that 1:5.
The washing typically continues 10~40min under the conditions of 25~30 DEG C.
Completing the raw material krill meal of washing will be entered by ethyl acetate and ethanol according to the mixed solvent of arbitrary proportion in next step
Row extraction.In specific embodiment, the mass ratio of the extraction step raw material and mixed solvent is 1:8~12.It is preferred that 1:10.
And the mixed solvent used in extraction step is ethyl acetate and ethanol according to volume ratio 3:7~8:2 mixing
Solvent.Ethyl acetate and ethanol are according to volume ratio 3~8:2 mixture, more preferred mixed proportion include but unlimited
In 6:4、7:3 and 8:2；Wherein, most preferably 7:3.
More specifically in embodiment, extraction is divided into be carried out twice, extracts about 1h every time.
After completing extraction, extract solution is needed with adsorbent arsenic removal.In embodiment, wherein described adsorbent is living
Property charcoal, diatomite, attapulgite or chitosan, and its material in source.The mass ratio of adsorbent and extract solution is 1:90~
110.It is preferred that use 1:100.
In the embodiment of absorption arsenic removal, adsorb under 50 ± 2 DEG C of temperature conditionss, operate at twice, every time about 1h.
After absorption arsenic removal, gained liquid is with molecular distillation desolvation.Specific operating parameter includes operating pressure 10Pa,
Temperature 60 C, inlet amount 2.0L/h.
In the preparation method of low arsenic krill fluid composition described by the invention described above, the group of the technical parameter of optimization
Close, the different preferable technical schemes on preparation method can be obtained.With suitable for different production environments and product demand
Under the conditions of production.The either a program of the preparation method of the low arsenic krill fluid composition, can prepare and meet this hair
The product of bright requirement.The purpose of another aspect of the present invention is then the low arsenic antarctic krill oil combination for protecting the above method to prepare
Thing.
As one of distinctive feature, there is low arsenic krill fluid composition of the invention extremely low controllable total arsenic to contain
Amount, is 0.5-2ppm.
In addition, effectively remained in raw material krill meal by the low arsenic krill fluid composition prepared by the above method
Other various Hubeiwans：According to weight/mass percentage composition, content of phospholipid 35-45%, content astaxanthin is up to more than 200ppm；
EPA content is more than 12%；DHA content is more than 8.5%.
Present disclosure is further described in a manner of specific embodiment below.
Embodiment 1
Low-arsenic phosphorus shrimp sauce composition product A is prepared by the following method
1) extract：For euphausia superba powder through being extracted 2 times at 50 DEG C of ethanol (top pure grade), each solid-to-liquid ratio is 1:5(kg：Kg),
Filtered after extraction, merge extract solution；
2) solvent volatilizees：Extract solution desolvation by the way of molecular distillation, operating pressure 10Pa, temperature 60 C, enters
Doses 2.0L/h, product A is made
Products obtained therefrom A is after tested：Content of phospholipid 49% (national standard GB/T5537-2008), total arsenic content 8.1ppm (national standards
GB5009.11-2014), EPA content 14.7g/100g (national standard GB/T28404), DHA content 9.4g/100g (national standard GB/
T28404), content astaxanthin 187ppm (HPLC), (the krill oil quality of krill oil yield 19%：Raw material euphausia superba powder quality).
Embodiment 2
Low-arsenic phosphorus shrimp sauce composition product B is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 10% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：For euphausia superba powder through being extracted 2 times at 50 DEG C of ethanol (top pure grade), each solid-to-liquid ratio is 1:5(kg：L), carry
Filtered after taking, merge extract solution；
4) solvent volatilizees：Extract solution desolvation by the way of molecular distillation, operating pressure 10Pa, temperature 60 C, enters
Doses 2.0L/h；
Products obtained therefrom B is after tested：Content of phospholipid 48% (national standard GB/T5537-2008), total arsenic content 6.3ppm (national standards
GB5009.11-2014), EPA content 14.2g/100g (national standard GB/T28404), DHA content 9.2g/100g (national standard GB/
T28404), content astaxanthin 171ppm (HPLC), (the krill oil quality of krill oil yield 18%：Raw material euphausia superba powder quality).
Embodiment 3
Low-arsenic phosphorus shrimp sauce composition product C is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 20% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：For euphausia superba powder through being extracted 2 times at 50 DEG C of ethanol (top pure grade), each solid-to-liquid ratio is 1:5(kg：Kg),
Filtered after extraction, merge extract solution；
4) solvent volatilizees：Extract solution desolvation by the way of molecular distillation, operating pressure 10Pa, temperature 60 C, enters
Doses 2.0L/h.
Products obtained therefrom C is after tested：Content of phospholipid 47% (national standard GB/T5537-2008), total arsenic content 4.0ppm (national standards
GB5009.11-2014), EPA content 13.7g/100g (national standard GB/T28404), DHA content 9.0g/100g (national standard GB/
T28404), content astaxanthin 163ppm (HPLC), (the krill oil quality of krill oil yield 18%：Raw material euphausia superba powder quality).
Embodiment 4
Low-arsenic phosphorus shrimp sauce composition product D is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 30% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg) filter gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：For euphausia superba powder through being extracted 2 times at 50 DEG C of ethanol (top pure grade), each solid-to-liquid ratio is 1:5(kg：Kg),
Filtered after extraction, merge extract solution；
4) solvent volatilizees：Extract solution desolvation by the way of molecular distillation, operating pressure 10Pa, temperature 60 C, enters
Doses 2.0L/h.
Products obtained therefrom D is after tested：Content of phospholipid 46% (national standard GB/T5537-2008), total arsenic content 3.8ppm (national standards
GB5009.11-2014), EPA content 13.1g/100g (national standard GB/T28404), DHA content 8.7g/100g (national standard GB/
T28404), content astaxanthin 153ppm (HPLC), (the krill oil quality of krill oil yield 17%：Raw material euphausia superba powder quality).
Embodiment 5
Low-arsenic phosphorus shrimp sauce composition product E is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 40% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：For euphausia superba powder through being extracted 2 times at 50 DEG C of ethanol (top pure grade), each solid-to-liquid ratio is 1:5(kg：Kg),
Filtered after extraction, merge extract solution；
4) solvent volatilizees：Extract solution desolvation by the way of molecular distillation, operating pressure 10Pa, temperature 60 C, enters
Doses 2.0L/h.
Products obtained therefrom E is after tested：Content of phospholipid 46% (national standard GB/T5537-2008), total arsenic content 3.4ppm (national standards
GB5009.11-2014), EPA content 12.8g/100g (national standard GB/T28404), DHA content 7.9g/100g (national standard GB/
T28404), content astaxanthin 147ppm (HPLC), (the krill oil quality of krill oil yield 16%：Raw material euphausia superba powder quality).
Embodiment 6
Low-arsenic phosphorus shrimp sauce composition product F is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 50% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：For euphausia superba powder through being extracted 2 times at 50 DEG C of ethanol (top pure grade), each solid-to-liquid ratio is 1:5(kg：Kg),
Filtered after extraction, merge extract solution；
4) solvent volatilizees：Extract solution desolvation by the way of molecular distillation, operating pressure 10Pa, temperature 60 C, enters
Doses 2.0L/h.
Products obtained therefrom F is after tested：Content of phospholipid 45% (national standard GB/T5537-2008), total arsenic content 3.3ppm (national standards
GB5009.11-2014), EPA content 11.9g/100g (national standard GB/T28404), DHA content 7.2g/100g (national standard GB/
T28404), content astaxanthin 122ppm (HPLC), (the krill oil quality of krill oil yield 16%：Raw material euphausia superba powder quality).
Embodiment 7
Low-arsenic phosphorus shrimp sauce composition product G is prepared by the following method
1) extract：For euphausia superba powder through being extracted 2 times at 50 DEG C of ethanol (top pure grade), each solid-to-liquid ratio is 1:5(kg：Kg),
Filtered after extraction, merge extract solution；
2) adsorb：Extract solution is adsorbed using activated carbon, 50 DEG C of adsorption temp, solid-to-liquid ratio 1:100(kg：Kg),
Adsorption time 1h, secondary filter after once adsorbing, 0.45 μm, vacuum -0.1MPa of filter sizes, filtrate use the same terms weight
Relapse it is attached once；
3) solvent volatilizees：Filtrate desolvation by the way of molecular distillation, operating pressure 10Pa, temperature 60 C, charging
Measure 2.0L/h.
Products obtained therefrom G is after tested：Content of phospholipid 47% (national standard GB/T5537-2008), total arsenic content 5.6ppm (national standards
GB5009.11-2014), EPA content 14.4g/100g (national standard GB/T28404), DHA content 9.2g/100g (national standard GB/
T28404), content astaxanthin 159ppm (HPLC), (the krill oil quality of krill oil yield 18%：Raw material euphausia superba powder quality).
Embodiment 8
Low-arsenic phosphorus shrimp sauce composition product H is prepared by the following method
1) extract：Euphausia superba powder ethyl acetate is 7 according to volume ratio with ethanol:3 mixed solvent extraction (acetic acid second
Ester and ethanol are top pure grade), extract 2 times at 50 DEG C, solid-to-liquid ratio 1:10(kg：Kg), filtered after extraction, merge extract solution；
2) solvent volatilizees：Filtrate desolvation by the way of molecular distillation, operating pressure 10Pa, temperature 60 C, charging
Measure 2.0L/h.
Products obtained therefrom H is after tested：Content of phospholipid 47% (national standard GB/T5537-2008), total arsenic content 6.4ppm (national standards
GB5009.11-2014), EPA content 15.1g/100g (national standard GB/T28404), DHA content 9.8g/100g (national standard GB/
T28404), content astaxanthin 329ppm (HPLC), (the krill oil quality of krill oil yield 18%：Raw material euphausia superba powder quality).
Embodiment 9
Low-arsenic phosphorus shrimp sauce composition product I is prepared by the following method
1) extract：Euphausia superba powder ethyl acetate is 7 according to volume ratio with ethanol:3 mixed solvent extraction (acetic acid second
Ester and ethanol are top pure grade), extract 2 times at 50 DEG C, solid-to-liquid ratio 1:10(kg：Kg), filtered after extraction, merge extract solution；
2) adsorb：Extract solution is adsorbed using activated carbon, 50 DEG C of adsorption temp, solid-to-liquid ratio 1:100(kg：Kg),
Adsorption time 1h, secondary filter after once adsorbing, 0.45 μm, vacuum -0.1MPa of filter sizes, filtrate use the same terms weight
Relapse it is attached once；
3) solvent volatilizees：Filtrate desolvation by the way of molecular distillation, operating pressure 10Pa, temperature 60 C, charging
Measure 2.0L/h.
Products obtained therefrom I is after tested：Content of phospholipid 46% (national standard GB/T5537-2008), total arsenic content 5.3ppm (national standards
GB5009.11-2014), EPA content 14.1g/100g (national standard GB/T28404), DHA content 9.0g/100g (national standard GB/
T28404), content astaxanthin 281ppm (HPLC), (the krill oil quality of krill oil yield 17%：Raw material euphausia superba powder quality).
Embodiment 10
Low-arsenic phosphorus shrimp sauce composition product J is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 30% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：Euphausia superba powder is 7 according to volume ratio through ethyl acetate and ethanol:3 mixed solvent (ethyl acetate with
Ethanol is top pure grade) to extract 2 times at 50 DEG C, each solid-to-liquid ratio is 1:5(kg：Kg), filtered after extraction, merge extract solution；
4) solvent volatilizees：Extract solution desolvation by the way of molecular distillation, operating pressure 10Pa, temperature 60 C, enters
Doses 2.0L/h.
Products obtained therefrom J is after tested：Content of phospholipid 46% (national standard GB/T5537-2008), total arsenic content 3.6ppm (national standards
GB5009.11-2014), EPA content 13.8g/100g (national standard GB/T28404), DHA content 8.6g/100g (national standard GB/
T28404), content astaxanthin 272ppm (HPLC), (the krill oil quality of krill oil yield 17%：Raw material euphausia superba powder quality).
Embodiment 11
Low-arsenic phosphorus shrimp sauce composition product K is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 30% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：For euphausia superba powder through being extracted 2 times at 50 DEG C of ethanol (top pure grade), each solid-to-liquid ratio is 1:5(kg：Kg),
Filtered after extraction, merge extract solution；
4) adsorb：Extract solution is adsorbed using activated carbon, 50 DEG C of adsorption temp, solid-to-liquid ratio 1:100(kg：Kg),
Adsorption time 1h, secondary filter after once adsorbing, 0.45 μm, vacuum -0.1MPa of filter sizes, filtrate use the same terms weight
Relapse it is attached once；
5) solvent volatilizees：Filtrate desolvation by the way of molecular distillation, operating pressure 10Pa, temperature 60 C, charging
Measure 2.0L/h.
Products obtained therefrom K is after tested：Content of phospholipid 45% (national standard GB/T5537-2008), total arsenic content 3.2ppm (national standards
GB5009.11-2014), EPA content 11.6g/100g (national standard GB/T28404), DHA content 7.7g/100g (national standard GB/
T28404), content astaxanthin 119ppm (HPLC), (the krill oil quality of krill oil yield 18%：Raw material euphausia superba powder quality).
Embodiment 12
Low-arsenic phosphorus shrimp sauce composition product L is prepared by the following method
Washing：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 30% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：For euphausia superba powder through being extracted 2 times at 50 DEG C of ethyl acetate (top pure grade), each solid-to-liquid ratio is 1:5(kg：
Kg), filtered after extraction, merge extract solution；
4) adsorb：Extract solution is adsorbed using activated carbon, 50 DEG C of adsorption temp, solid-to-liquid ratio 1:100(kg：Kg),
Adsorption time 1h, secondary filter after once adsorbing, 0.45 μm, vacuum -0.1MPa of filter sizes, filtrate use the same terms weight
Relapse it is attached once；
5) solvent volatilizees：Filtrate desolvation by the way of molecular distillation, operating pressure 10Pa, temperature 60 C, charging
Measure 2.0L/h.
Products obtained therefrom L is after tested：Content of phospholipid 35% (national standard GB/T5537-2008), total arsenic content 1.6ppm (national standards
GB5009.11-2014), EPA content 9.6g/100g (national standard GB/T28404), DHA content 6.8g/100g (national standard GB/
T28404), content astaxanthin 170ppm (HPLC), (the krill oil quality of krill oil yield 11%：Raw material euphausia superba powder quality).
Embodiment 13
Low-arsenic phosphorus shrimp sauce composition product M is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 30% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：Dried euphausia superba powder ethyl acetate is 8 according to volume ratio with ethanol:2 mixed solvent carries
Take (ethyl acetate and ethanol are top pure grade), extracted 2 times at 50 DEG C, solid-to-liquid ratio 1:10(kg：Kg), filter, close after extraction
And extract solution；
4) adsorb：Extract solution is adsorbed using activated carbon, 50 DEG C of adsorption temp, solid-to-liquid ratio 1:100(kg：Kg),
Adsorption time 1h, secondary filter after once adsorbing, 0.45 μm, vacuum -0.1MPa of filter sizes, filtrate use the same terms weight
Relapse it is attached once；
5) solvent volatilizees：Filtrate desolvation by the way of molecular distillation, operating pressure pressure 10Pa, temperature 60 C,
Inlet amount 2.0L/h.
Products obtained therefrom M tests through National Standard Method：Fat content 36%, total arsenic content 0.9ppm, EPA content 10.9g/100g (states
Mark GB/T28404), DHA content 7.4g/100g (national standard GB/T28404), content astaxanthin 231ppm (HPLC), krill oil are received
(the krill oil quality of rate 14%：Raw material euphausia superba powder quality).
Embodiment 14
Low-arsenic phosphorus shrimp sauce composition product N is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 30% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：Dried euphausia superba powder ethyl acetate is 7 according to volume ratio with ethanol:3 mixed solvent carries
Take (ethyl acetate and ethanol are top pure grade), extracted 2 times at 50 DEG C, solid-to-liquid ratio 1:10(kg：Kg), filter, close after extraction
And extract solution；
4) adsorb：Extract solution is adsorbed using activated carbon, 50 DEG C of adsorption temp, solid-to-liquid ratio 1:100(kg：Kg),
Adsorption time 1h, secondary filter after once adsorbing, 0.45 μm, vacuum -0.1MPa of filter sizes, filtrate use the same terms weight
Relapse it is attached once；
5) solvent volatilizees：Filtrate desolvation by the way of molecular distillation, operating pressure pressure 10Pa, temperature 60 C,
Inlet amount 2.0L/h.
Products obtained therefrom N tests through National Standard Method：Fat content 45%, total arsenic content 0.8ppm, EPA content 12.8g/100g (states
Mark GB/T28404), DHA content 8.8g/100g (national standard GB/T28404), content astaxanthin 209ppm (HPLC), krill oil are received
(the krill oil quality of rate 16%：Raw material euphausia superba powder quality).
Embodiment 15
Low-arsenic phosphorus shrimp sauce composition product O is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 30% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：Dried euphausia superba powder ethyl acetate is 6 according to volume ratio with ethanol:4 mixed solvent carries
Take (ethyl acetate and ethanol are top pure grade), extracted 2 times at 50 DEG C, solid-to-liquid ratio 1:10(kg：Kg), filter, close after extraction
And extract solution；
4) adsorb：Extract solution is adsorbed using activated carbon, 50 DEG C of adsorption temp, solid-to-liquid ratio 1:100(kg：Kg),
Adsorption time 1h, secondary filter after once adsorbing, 0.45 μm, vacuum -0.1MPa of filter sizes, filtrate use the same terms weight
Relapse it is attached once；
5) solvent volatilizees：Filtrate desolvation by the way of molecular distillation, operating pressure pressure 10Pa, temperature 60 C,
Inlet amount 2.0L/h.
Products obtained therefrom O tests through National Standard Method：Fat content 41%, total arsenic content 1.0ppm, EPA content 11.9g/100g (states
Mark GB/T28404), DHA content 7.6g/100g (national standard GB/T28404), content astaxanthin 187ppm (HPLC), krill oil are received
(the krill oil quality of rate 15%：Raw material euphausia superba powder quality).
Embodiment 16
Low-arsenic phosphorus shrimp sauce composition product P is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 30% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：Dried euphausia superba powder ethyl acetate is 5 according to volume ratio with ethanol:5 mixed solvent carries
Take (ethyl acetate and ethanol are top pure grade), extracted 2 times at 50 DEG C, solid-to-liquid ratio 1:10(kg：Kg), filter, close after extraction
And extract solution；
4) adsorb：Extract solution is adsorbed using activated carbon, 50 DEG C of adsorption temp, solid-to-liquid ratio 1:100(kg：Kg),
Adsorption time 1h, secondary filter after once adsorbing, 0.45 μm, vacuum -0.1MPa of filter sizes, filtrate use the same terms weight
Relapse it is attached once；
5) solvent volatilizees：Filtrate desolvation by the way of molecular distillation, operating pressure pressure 10Pa, temperature 60 C,
Inlet amount 2.0L/h.
Products obtained therefrom P tests through National Standard Method：Fat content 40%, total arsenic content 1.5ppm, EPA content 11.1g/100g (states
Mark GB/T28404), DHA content 7.3g/100g (national standard GB/T28404), content astaxanthin 169ppm (HPLC), krill oil are received
(the krill oil quality of rate 14%：Raw material euphausia superba powder quality).
Embodiment 17
Low-arsenic phosphorus shrimp sauce composition product Q is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 30% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：Dried euphausia superba powder ethyl acetate is 4 according to volume ratio with ethanol:6 mixed solvent carries
Take (ethyl acetate and ethanol are top pure grade), extracted 2 times at 50 DEG C, solid-to-liquid ratio 1:10(kg：Kg), filter, close after extraction
And extract solution；
4) adsorb：Extract solution is adsorbed using activated carbon, 50 DEG C of adsorption temp, solid-to-liquid ratio 1:100(kg：Kg),
Adsorption time 1h, secondary filter after once adsorbing, 0.45 μm, vacuum -0.1MPa of filter sizes, filtrate use the same terms weight
Relapse it is attached once；
5) solvent volatilizees：Filtrate desolvation by the way of molecular distillation, operating pressure pressure 10Pa, temperature 60 C,
Inlet amount 2.0L/h.
Products obtained therefrom Q tests through National Standard Method：Fat content 40%, total arsenic content 1.9ppm, EPA content 10.0g/100g (states
Mark GB/T28404), DHA content 6.5g/100g (national standard GB/T28404), content astaxanthin 158ppm (HPLC), krill oil are received
(the krill oil quality of rate 16%：Raw material euphausia superba powder quality).
Embodiment 18
Low-arsenic phosphorus shrimp sauce composition product R is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 30% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：Dried euphausia superba powder ethyl acetate is 3 according to volume ratio with ethanol:7 mixed solvent carries
Take (ethyl acetate and ethanol are top pure grade), extracted 2 times at 50 DEG C, solid-to-liquid ratio 1:10(kg：Kg), filter, close after extraction
And extract solution；
4) adsorb：Extract solution is adsorbed using activated carbon, 50 DEG C of adsorption temp, solid-to-liquid ratio 1:100(kg：Kg),
Adsorption time 1h, secondary filter after once adsorbing, 0.45 μm, vacuum -0.1MPa of filter sizes, filtrate use the same terms weight
Relapse it is attached once；
5) solvent volatilizees：Filtrate desolvation by the way of molecular distillation, operating pressure pressure 10Pa, temperature 60 C,
Inlet amount 2.0L/h.
Products obtained therefrom R tests through National Standard Method：Fat content 42%, total arsenic content 2.1ppm, EPA content 8.6g/100g (national standards
GB/T28404), DHA content 5.2g/100g (national standard GB/T28404), content astaxanthin 143ppm (HPLC), krill oil yield
17% (krill oil quality：Raw material euphausia superba powder quality).
Embodiment 19
Low-arsenic phosphorus shrimp sauce composition product S is prepared by the following method
1) wash：Euphausia superba powder is washed, solid-to-liquid ratio 1 through 30% (mass ratio) ethanol water in 30 DEG C of mechanical agitations:5
(kg：Kg), time 30min, filtering；
2) dry：Filtering gained euphausia superba powder is dried in vacuo, 50 DEG C of drying temperature, vacuum -0.1MPa；
3) extract：Dried euphausia superba powder ethyl acetate is 7 according to volume ratio with ethanol:3 mixed solvent carries
Take (ethyl acetate and ethanol are top pure grade), extracted 2 times at 50 DEG C, solid-to-liquid ratio 1:10(kg：Kg), filter, close after extraction
And extract solution；
4) adsorb：The pH value of extract solution is adjusted to 5.0 with citric acid, extract solution adsorbed using activated carbon, is adsorbed
Temperature 50 C, solid-to-liquid ratio 1:100(kg：Kg), adsorption time 1h, secondary filter after once adsorbing, 0.45 μm of filter sizes, very
Reciprocal of duty cycle -0.1MPa, filtrate repeat absorption once using the same terms；
5) solvent volatilizees：Filtrate desolvation by the way of molecular distillation, operating pressure 10Pa, temperature 60 C, charging
Measure 2.0L/h.
Products obtained therefrom S tests through National Standard Method：Fat content 45%, total arsenic content 0.5ppm, (the national standard GB/ of EPA content 12.4%
T28404), DHA content 8.6% (national standard GB/T28404), content astaxanthin 203ppm (HPLC), (phosphorus of krill oil yield 16%
Shrimp sauce quality：Raw material euphausia superba powder quality).
Claims (10)
1. the preparation method of low arsenic krill fluid composition, using the euphausia superba powder after crushing as raw material, comprises the following steps：
(1) after washing raw material with ethanol water, extracted with ethyl acetate and ethanol according to the mixed solvent of arbitrary proportion；
(2) extract solution is with adsorbent arsenic removal；
(3) molecular distillation desolvation.
2. according to the method for claim 1, it is characterised in that the matter of raw material and ethanol water in the step (1)
Amount is than being 1:4~6.
3. according to the method for claim 1, it is characterised in that the quality of raw material and mixed solvent in the step (1)
Than being 1:8~12.
4. according to the method for claim 1, it is characterised in that organic solvent in the step (1) for ethyl acetate and
Ethanol is according to volume ratio 3:7~8:2 mixed solvent.
5. according to the method for claim 1, it is characterised in that in described step (2), described adsorbent is activity
Charcoal, diatomite, attapulgite or chitosan.
6. according to the method for claim 1, it is characterised in that in described step (2), the quality of adsorbent and extract solution
Than for 1:90~110.
7. according to the method for claim 1, it is characterised in that absorption arsenic removal operates at twice in the step (2), every time
1h, 50 ± 2 DEG C of adsorption temp.
8. according to the method for claim 1, it is characterised in that the operating pressure of molecular distillation in described step (3)
10Pa, temperature 60 C, inlet amount 2.0L/h.
9. low arsenic krill fluid composition prepared by method according to claim 1.
10. low arsenic krill fluid composition according to claim 2, it is characterised in that total arsenic in described composition
Content 0.5-2ppm.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108659947A (en) * | 2018-06-12 | 2018-10-16 | 山东蓝奥生物技术有限公司 | A kind of method, antarctic krill oil and albumen powder preparing antarctic krill oil and albumen powder using krill |
| CN110016386A (en) * | 2019-04-22 | 2019-07-16 | 华中农业大学 | A kind of de- bitter processing method of idesia oil |
| CN110025640A (en) * | 2019-06-03 | 2019-07-19 | 汤臣倍健股份有限公司 | A kind of production method of Rhizoma Drynariae extract |
| CN110724596A (en) * | 2019-10-10 | 2020-01-24 | 浙江海洋大学 | Method for removing arsenic in euphausia superba oil |
| CN110878231A (en) * | 2019-06-25 | 2020-03-13 | 山东鲁华海洋生物科技有限公司 | Low-arsenic euphausia superba oil and preparation method thereof |
| CN112126517A (en) * | 2020-09-30 | 2020-12-25 | 无锡定象改性硅胶材料有限公司 | Low-arsenic high-phospholipid process for improving quality of initial shrimp sauce |
| CN114214116A (en) * | 2021-09-30 | 2022-03-22 | 无锡定象改性硅胶材料有限公司 | Antarctic krill extract dearsenization treatment method and application of adsorbent in dearsenization |
| CN114836260A (en) * | 2022-05-25 | 2022-08-02 | 深圳市齐盛伟生物科技有限公司 | Extraction method for effectively removing arsenic in euphausia superba oil |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101297708A (en) * | 2008-06-06 | 2008-11-05 | 石勇 | Method from preparing high-purity edible fish oil from coarse fish oil |
| CN102099451A (en) * | 2008-05-15 | 2011-06-15 | 普罗诺瓦生物医药挪威公司 | Krill oil process |
| CN103320217A (en) * | 2013-07-11 | 2013-09-25 | 日照海大博远海洋生物科技有限公司 | Method for extracting krill oil rich in phospholipid from euphausia superba |
| CN104327936A (en) * | 2014-10-27 | 2015-02-04 | 浙江工业大学 | Method for extracting antarctic krill oil by using autolytic enzyme system |
-
2017
- 2017-04-28 CN CN201710296022.0A patent/CN107418721A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102099451A (en) * | 2008-05-15 | 2011-06-15 | 普罗诺瓦生物医药挪威公司 | Krill oil process |
| CN101297708A (en) * | 2008-06-06 | 2008-11-05 | 石勇 | Method from preparing high-purity edible fish oil from coarse fish oil |
| CN103320217A (en) * | 2013-07-11 | 2013-09-25 | 日照海大博远海洋生物科技有限公司 | Method for extracting krill oil rich in phospholipid from euphausia superba |
| CN104327936A (en) * | 2014-10-27 | 2015-02-04 | 浙江工业大学 | Method for extracting antarctic krill oil by using autolytic enzyme system |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108659947A (en) * | 2018-06-12 | 2018-10-16 | 山东蓝奥生物技术有限公司 | A kind of method, antarctic krill oil and albumen powder preparing antarctic krill oil and albumen powder using krill |
| CN110016386A (en) * | 2019-04-22 | 2019-07-16 | 华中农业大学 | A kind of de- bitter processing method of idesia oil |
| CN110025640A (en) * | 2019-06-03 | 2019-07-19 | 汤臣倍健股份有限公司 | A kind of production method of Rhizoma Drynariae extract |
| CN110025640B (en) * | 2019-06-03 | 2020-11-24 | 汤臣倍健股份有限公司 | Method for producing drynaria extract |
| CN110878231A (en) * | 2019-06-25 | 2020-03-13 | 山东鲁华海洋生物科技有限公司 | Low-arsenic euphausia superba oil and preparation method thereof |
| CN110724596A (en) * | 2019-10-10 | 2020-01-24 | 浙江海洋大学 | Method for removing arsenic in euphausia superba oil |
| CN112126517A (en) * | 2020-09-30 | 2020-12-25 | 无锡定象改性硅胶材料有限公司 | Low-arsenic high-phospholipid process for improving quality of initial shrimp sauce |
| CN112126517B (en) * | 2020-09-30 | 2023-11-24 | 无锡定象改性硅胶材料有限公司 | Low-arsenic high-phospholipid process for improving initial shrimp oil quality |
| CN114214116A (en) * | 2021-09-30 | 2022-03-22 | 无锡定象改性硅胶材料有限公司 | Antarctic krill extract dearsenization treatment method and application of adsorbent in dearsenization |
| CN114214116B (en) * | 2021-09-30 | 2022-11-11 | 无锡定象改性硅胶材料有限公司 | Antarctic krill extract dearsenization treatment method and application of adsorbent in dearsenization |
| CN114836260A (en) * | 2022-05-25 | 2022-08-02 | 深圳市齐盛伟生物科技有限公司 | Extraction method for effectively removing arsenic in euphausia superba oil |
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Application publication date: 20171201 |