CN107663473A - Extracting method, capsule and the preparation method of krill oil - Google Patents
Extracting method, capsule and the preparation method of krill oil Download PDFInfo
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- CN107663473A CN107663473A CN201711118852.0A CN201711118852A CN107663473A CN 107663473 A CN107663473 A CN 107663473A CN 201711118852 A CN201711118852 A CN 201711118852A CN 107663473 A CN107663473 A CN 107663473A
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- 238000000034 method Methods 0.000 title claims abstract description 56
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- 238000002360 preparation method Methods 0.000 title description 2
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- 241000239366 Euphausiacea Species 0.000 claims abstract description 66
- 238000012545 processing Methods 0.000 claims abstract description 54
- 239000000203 mixture Substances 0.000 claims abstract description 42
- 238000010257 thawing Methods 0.000 claims abstract description 31
- 239000003960 organic solvent Substances 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000007701 flash-distillation Methods 0.000 claims abstract description 7
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- 230000000050 nutritive effect Effects 0.000 abstract description 3
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- 229940022405 astaxanthin Drugs 0.000 description 6
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- OAIJSZIZWZSQBC-GYZMGTAESA-N lycopene Chemical compound CC(C)=CCC\C(C)=C\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\C=C(/C)CCC=C(C)C OAIJSZIZWZSQBC-GYZMGTAESA-N 0.000 description 1
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Classifications
-
- 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
-
- 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
- C11B1/02—Pretreatment
- C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
-
- 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
- C11B1/06—Production of fats or fatty oils from raw materials by pressing
-
- 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
- C11B1/12—Production of fats or fatty oils from raw materials by melting out
- C11B1/16—Production of fats or fatty oils from raw materials by melting out with steam
-
- 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
-
- 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
- C11B3/006—Refining fats or fatty oils by extraction
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Microbiology (AREA)
- Biochemistry (AREA)
- Meat, Egg Or Seafood Products (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Edible Oils And Fats (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a kind of extracting method of krill oil, comprise the following steps：Liquid is collected after frost microwave thawing processing is repeated after krill body surface moisture is dried up；Krill is made after the quick-frozen powder of krill to ultrasonic disruption processing after being well mixed with liquid I and obtains mixture II；The centrifugal treating of mixture II is obtained into residue I and liquid III；The instantaneous differential pressure flash distillation process of residue I is obtained into liquid IV and residue II；Residue II is squeezed into processing and obtains primary krill oil and residue III；Digested after residue III, liquid and liquid III are mixed into acquisition mixture III and centrifugal treating obtains the secondary krill oil of organic solvent extraction acquisition after enzymolysis liquid；Krill oil is refined after secondary krill oil, liquid IV are mixed into centrifugation removal of impurities water removal with primary krill oil.The recovery rate of the krill oil of the inventive method is high, the active component that can be effectively retained in krill oil, and the nutritive value of the product finally obtained is high, and organic solvent-free remains.
Description
Technical field
The present invention relates to bioactive substance and functional food factory formula technical field, more particularly to a kind of krill
The extracting method of oil.
Background technology
Krill aboundresources, growing environment is without industrial pollution.Krill oil is from krill (Euphausia
Superba the lipid of extraction, main component include in)：Glyceride, phosphatide, astaxanthin, sterol etc..Contain simultaneously in krill oil
Natural antioxidant astaxanthin, content up to 100mg/kg~300mg/kg, its oxidation resistance be significantly larger than vitamin E,
The materials such as lycopene, it is referred to as the most strong natural materials of antioxidation activity.It is existing research be proved krill oil rich in it is a variety of not
Saturated fatty acid, wherein long-chain omega-3 polyunsaturated fatty acids EPA and DHA content are up to 15.86%.Different from fish oil and fish liver
Oily ω -3 triglycerides form, the omega-fatty acid of krill oil are attached on phosphatide, this long-chain polyunsaturated fatty acid phosphatide
Bioactivity compound molecule small intestine can be directly entered after by stomach fully absorbs, add bioavilability, and finally
Improve ω -3: ω -6 fatty acid proportion.And krill oil intrinsic natural powerful antioxidant astaxanthin be also attached to phosphorus
Fat, so as to generate more stable lasting antioxidant effect.Shown according to experiment, the compound sub life of krill oil bioactivity
Thing availability is 95%~98%, and the bioavilability of fish oil only 61%~64%, and what main cause was that krill oil contains is phosphorus
Fat aliphatic acid, and almost 100% triglycerides that fish oil contains.Research shows：Krill oil (2g/d) can increase obese people
EPA and DHA concentration in blood, positive effect are said higher than taking herring oil (2g/d) and taking olive oil (2g/d) amplification
Understand that krill oil has good absorbability in human body；And after measured, krill oil does not produce any toxic side effect.
The extracting method of domestic and international krill oil mainly has：Organic solvent method, enzymolysis assisted extraction method, supercritical fluid extraction
The methods of, compared with other method, organic solvent method has that technique is simple, extraction efficiency is high, low cost and other advantages, is still industry
Change the most frequently used method, but shrimp sauce is extracted using the method for organic solvent as raw material using full shrimp and problems be present：It is organic molten
Agent extraction can have problem of solvent residual unavoidably, have impact on the utilization of krill protein, and other nutritional ingredients are damaged,
It has impact on making full use of for krill resource.
The content of the invention
It is an object of the invention to solve at least the above, and provide the advantages of at least will be described later.
It is a still further object of the present invention to provide a kind of extracting method of krill oil, the recovery rate of the krill oil of this method
Height, the active component that can be effectively retained in krill oil, the nutritive value of the product finally obtained is high, and organic solvent-free remains.
In order to realize according to object of the present invention and further advantage, there is provided a kind of extracting method of krill oil, bag
Include following steps：
Step 1: carrying out body surface moisture drying in 3 hours to it after krill fishing, and collect the liquid I of blowout；
Step 2: the krill frost processing after body surface is dried up, is handled, regelation of laying equal stress on freezes using microwave thawing afterwards
Handled 2-3 times with microwave thawing；
Step 3: collect the liquid after evaporating and cool down in microwave thawing processing procedure；
Step 4: the quick-frozen rear pulverization process that carries out of the krill of step 3 is obtained into the quick-frozen powder of krill；
Step 5: by volume 2:1-2 ratio is added to be well mixed after liquid I into the quick-frozen powder of the krill and obtained
Mixture I is obtained, the mixture I is carried out into ultrasonic disruption processing obtains mixture II；
Step 6: mixture II is carried out into centrifugal treating obtains residue I and liquid III；
Step 7: the instantaneous differential pressure flash distillation process of residue I is obtained into liquid IV and residue II, wherein instantaneous differential pressure flashes
Temperature is no more than 95 DEG C；
Step 8: residue II is carried out into squeezing processing obtains primary krill oil and residue III；
Step 9: by residue III, liquid and liquid III according to volume ratio 1-2:1:1 ratio, which is sufficiently mixed, to be mixed
Thing III, after appropriate protease is added after mixture III is warming up into 35-45 DEG C thereto and stands 30-50min after being well mixed,
The centrifugal treating of mixture III is obtained into enzymolysis liquid；Wherein, the addition of protease is the 1% of the quality of mixture III；
Step 10: the enzymolysis liquid and organic solvent are sufficiently mixed the secondary krill oil of extraction；
Step 11: after the organic solvent in secondary krill oil is reclaimed, by secondary krill oil, liquid IV and primary krill
Krill oil is refined after oil mixing centrifugation removal of impurities water removal.
Preferably, it is further comprising the steps of in the step 1：
It is online that krill is uniformly laid on to the multilayer drying being distributed from up to down, multilayer drying net is arranged on relatively a,
In closed drying unit；
B, it is passed through dry nitrogen thereto from the bottom of the drying unit, nitrogen temperature is 50-60 DEG C；
C, nitrogen is discharged after multilayer drying net from the outlet of drying unit；
D, the nitrogen with vapor of discharge obtains liquid I after steam separates.
Preferably, the actual conditions of microwave thawing processing is in the step 2：The time of microwave thawing is 10-
20s, and keep krill body temperature to be no more than 90 DEG C during microwave thawing.
Preferably, in the step 2, it is -6~-2 DEG C to freeze temperature inside the krill of processing.
Preferably, liquid I, liquid and liquid III enter hermetically sealed can and saved backup, and nitrogen is filled with hermetically sealed can.
Preferably, the frequency of ultrasonic wave is 20-25KHz in the step 5, and ultrasonication total duration is 4-8min,
At interval of 2-4s ultrasonications once, a duration 10-15s, the acoustical power of ultrasonic wave is 3-5W/cm2。
Preferably, the step 7 is further comprising the steps of：
E, the annular seal space for the instantaneous differential pressure processing unit for being contained with the residue I is vacuumized；
F, vapours to its interior temperature is passed through into annular seal space and is no more than 95 DEG C, pressure 0.15-0.25Mpa, Zhi Houbao
Pressure processing 20-40s；
G, by the sealing cavity pressure in 3s pressure release to 5-6kpa；
H, at interval of 30-45s repeat steps a, step b and step c once, altogether repeatedly 2-3 times.
Preferably, it is 93 DEG C, pressure 0.25Mpa that vapours to its interior temperature is passed through in the f, into annular seal space,
Pressurize afterwards handles 35s.
Preferably, multiple step a, step b and step c are led in the f, into annular seal space once, is repeated 3 times altogether.
Preferably, residue II is entered to put into carry out in screw extruder to squeezing processing, squeezing processing in the step 8
Including one-level squeezing and two level squeezing：
Wherein, screw extruder is correspondingly arranged on two one-level press cylinders and two level press cylinder, wherein, two one-level squeezings
The bottom connection of the shell body I of cylinder is set, and the screw rod in two one-level press cylinders does not contact so that two one-level press cylinders are in
Angle less than 90 degree；
Two level squeezes cylinder, and the upper end of its shell is connected to the bottom junctions of the shell body II of two one-level press cylinders,
And the maximum gauge of shell body II is less than 1.5 times of the minimum diameter of shell body I.
The present invention comprises at least following beneficial effect：
In the extracting method of krill oil provided by the invention, krill carries out the extraction of krill oil through body surface drying again,
Improve the mass percent concentration of grease in primary expressing process；
Krill is freezed to-microwave thawing circular treatment 2-3 times, during frost, intracellular ice crystal forms cutting damage
Hinder cell membrane, cell membrane is destroyed after defrosting, can be achieved to carry out the cell of krill primary freeze thawing rupture of membranes processing, in addition,
The temperature of microwave thawing is kept to be no more than 95 DEG C, the nutritional ingredient preserved to greatest extent in krill is not destroyed；
, can be tentatively by krill again through low power supersound process after the quick-frozen crushing of krill of rupture of membranes processing
In nutritional ingredient discharged including a part of krill oil, through centrifugal treating obtain liquid III；
By the residue I carry out instantaneous differential pressure flash distillation process obtain liquid IV so that in krill most of moisture and
Krill oil moment goes out from krill meal obtains liquid IV, and krill oil must be isolated after centrifugal treating；
By residue II, further squeezing processing obtains primary krill oil and residue III, is able to enter the grease in krill
One step separates；
Mixture III is digested thoroughly to collect the grease in krill (krill oil), in the process, due to mixing
The grease of euphausia superba powder is separated substantially in thing III, it is only necessary to which minimal amount of organic solvent can be achieved to the South Pole
The thorough extraction of the grease of krill meal, it will not cause to waste, a large amount of uses for reducing organic solvent, the residual of organic solvent also may be used
To ignore.
To sum up, the recovery rate of the krill oil of the inventive method is high, the active component that can be effectively retained in krill oil, finally obtains
The nutritive value of the product obtained is high, and organic solvent-free remains.
Further advantage, target and the feature of the present invention embodies part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Embodiment
With reference to embodiment, the present invention is described in further detail, to make those skilled in the art with reference to specification
Word can be implemented according to this.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of individual other elements or its combination.
Embodiment 1
A kind of extracting method of krill oil, comprises the following steps：
Step 1: carrying out body surface moisture drying in 3 hours to it after krill fishing, and collect the liquid I of blowout；
Wherein, it is further comprising the steps of in the step 1：Krill is uniformly laid on to the multilayer drying being distributed from up to down a,
On the net, multilayer drying net is arranged in relatively closed drying unit；B, it is passed through thereto from the bottom of the drying unit dry
Dry nitrogen, nitrogen temperature are 50 DEG C；C, nitrogen is discharged after multilayer drying net from the outlet of drying unit；D, the band of discharge
The nitrogen for having vapor obtains liquid I after steam separates；
Step 2: the krill frost processing after body surface is dried up, is handled, regelation of laying equal stress on freezes using microwave thawing afterwards
Handled 2 times with microwave thawing；It is -6 DEG C to freeze temperature inside the krill of processing；The time of microwave thawing is 10-
20s, and it is 90 DEG C that krill body temperature is kept during microwave thawing；
Step 3: collect the liquid after evaporating and cool down in microwave thawing processing procedure；
Step 4: the quick-frozen rear pulverization process that carries out of the krill of step 3 is obtained into the quick-frozen powder of krill；
Step 5: by volume 2:1 ratio is well mixed acquisition after liquid I is added into the quick-frozen powder of the krill
Mixture I, the mixture I is subjected to ultrasonic disruption processing and obtains mixture II；Wherein, the frequency of ultrasonic wave is 20KHz,
Ultrasonication total duration is 4min, and at interval of 2s ultrasonications once, a duration 10s, the acoustical power of ultrasonic wave is 3W/
cm2；
Step 6: mixture II is carried out into centrifugal treating obtains residue I and liquid III；
Step 7: the instantaneous differential pressure flash distillation process of residue I is obtained into liquid IV and residue II, wherein instantaneous differential pressure flashes
Temperature is 95 DEG C；Wherein, it is further comprising the steps of：E, the annular seal space of the instantaneous differential pressure processing unit of the residue I will be contained with
Vacuumize；F, it is 95 DEG C, pressure 0.25Mpa that vapours to its interior temperature is passed through into annular seal space, the processing of pressurize afterwards 20s；
G, by the sealing cavity pressure in 3s pressure release to 5kpa；H, at interval of 30s repeat steps a, step b and step c once, one
It is repeated 2 times altogether；
Step 8: residue II is carried out into squeezing processing obtains primary krill oil and residue III；By residue in the step 8
II enters to put into carry out squeezing processing in screw extruder, and squeezing processing includes one-level squeezing and two level squeezing：Wherein, screw extrusion
Machine is correspondingly arranged on two one-level press cylinders and two level press cylinder, wherein, the bottom connection of the shell body I of two one-level press cylinders
Set, and the screw rod in two one-level press cylinders does not contact so that two one-level press cylinders are in the angle less than 90 degree；Two level pressure
Cylinder is squeezed, the upper end of its shell is connected to the bottom junctions of the shell body II of two one-level press cylinders, and shell body II is most
Major diameter is less than 1.5 times of the minimum diameter of shell body I；
Step 9: by residue III, liquid and liquid III according to volume ratio 1:1:1 ratio is sufficiently mixed acquisition mixture
III, mixture III is warming up to after 35 DEG C after adding appropriate protease thereto and standing 30min after being well mixed, by mixture
III centrifugal treating obtains enzymolysis liquid；Wherein, the addition of protease is the 1% of the quality of mixture III；
Step 10: the enzymolysis liquid and organic solvent are sufficiently mixed the secondary krill oil of extraction；Organic solvent selects quality
Fraction is 95% ethanol or acetone；
Step 11: after the organic solvent in secondary krill oil is reclaimed, by secondary krill oil, liquid IV and primary krill
Krill oil is refined after oil mixing centrifugation removal of impurities water removal.
Wherein, liquid I, liquid and liquid III enter hermetically sealed can and saved backup, and nitrogen is filled with hermetically sealed can.
Embodiment 2
A kind of extracting method of krill oil, comprises the following steps：
Step 1: carrying out body surface moisture drying in 2.5 hours to it after krill fishing, and collect the liquid of blowout
Ⅰ；Wherein, it is further comprising the steps of in the step 1：Krill is uniformly laid on to the multilayer being distributed from up to down to dry a,
Dry online, multilayer drying net is arranged in relatively closed drying unit；B, it is passed through thereto from the bottom of the drying unit
Dry nitrogen, nitrogen temperature are 55 DEG C；C, nitrogen is discharged after multilayer drying net from the outlet of drying unit；D, discharge
Nitrogen with vapor obtains liquid I after steam separates；
Step 2: the krill frost processing after body surface is dried up, is handled, regelation of laying equal stress on freezes using microwave thawing afterwards
Handled 3 times with microwave thawing；It is -4 DEG C to freeze temperature inside the krill of processing；The time of microwave thawing is 15s,
And it is 88 DEG C that krill body temperature is kept during microwave thawing；
Step 3: collect the liquid after evaporating and cool down in microwave thawing processing procedure；
Step 4: the quick-frozen rear pulverization process that carries out of the krill of step 3 is obtained into the quick-frozen powder of krill；
Step 5: by volume 1:1 ratio is well mixed acquisition after liquid I is added into the quick-frozen powder of the krill
Mixture I, the mixture I is subjected to ultrasonic disruption processing and obtains mixture II；Wherein, the frequency of ultrasonic wave is 25KHz,
Ultrasonication total duration is 6min, and at interval of 4s ultrasonications once, a duration 15s, the acoustical power of ultrasonic wave is 5W/
cm2；
Step 6: mixture II is carried out into centrifugal treating obtains residue I and liquid III；
Step 7: the instantaneous differential pressure flash distillation process of residue I is obtained into liquid IV and residue II, wherein instantaneous differential pressure flashes
Temperature is 90 DEG C；Wherein, it is further comprising the steps of：E, the annular seal space of the instantaneous differential pressure processing unit of the residue I will be contained with
Vacuumize；F, it is 90 DEG C, pressure 0.20Mpa that vapours to its interior temperature is passed through into annular seal space, the processing of pressurize afterwards 30s；
G, by the sealing cavity pressure in 3s pressure release to 6kpa；H, at interval of 35s repeat steps a, step b and step c once, one
It is repeated 3 times altogether；
Step 8: residue II is carried out into squeezing processing obtains primary krill oil and residue III；By residue in the step 8
II enters to put into carry out squeezing processing in screw extruder, and squeezing processing includes one-level squeezing and two level squeezing：Wherein, screw extrusion
Machine is correspondingly arranged on two one-level press cylinders and two level press cylinder, wherein, the bottom connection of the shell body I of two one-level press cylinders
Set, and the screw rod in two one-level press cylinders does not contact so that two one-level press cylinders are in the angle less than 90 degree；Two level pressure
Cylinder is squeezed, the upper end of its shell is connected to the bottom junctions of the shell body II of two one-level press cylinders, and shell body II is most
Major diameter is less than 1.5 times of the minimum diameter of shell body I；
Step 9: by residue III, liquid and liquid III according to volume ratio 2:1:1 ratio is sufficiently mixed acquisition mixture
III, mixture III is warming up to after 45 DEG C after adding appropriate protease thereto and standing 50min after being well mixed, by mixture
III centrifugal treating obtains enzymolysis liquid；Wherein, the addition of protease is the 2% of the quality of mixture III；
Step 10: the enzymolysis liquid and organic solvent are sufficiently mixed the secondary krill oil of extraction；Organic solvent selects quality
Fraction is 95% ethanol or acetone；
Step 11: after the organic solvent in secondary krill oil is reclaimed, by secondary krill oil, liquid IV and primary krill
Krill oil is refined after oil mixing centrifugation removal of impurities water removal.
Wherein, liquid I, liquid and liquid III enter hermetically sealed can and saved backup, and nitrogen is filled with hermetically sealed can.
Embodiment 3
A kind of extracting method of krill oil, comprises the following steps：
Step 1: carrying out body surface moisture drying in 2 hours to it after krill fishing, and collect the liquid I of blowout；
Wherein, it is further comprising the steps of in the step 1：Krill is uniformly laid on to the multilayer drying being distributed from up to down a,
On the net, multilayer drying net is arranged in relatively closed drying unit；B, it is passed through thereto from the bottom of the drying unit dry
Dry nitrogen, nitrogen temperature are 60 DEG C；C, nitrogen is discharged after multilayer drying net from the outlet of drying unit；D, the band of discharge
The nitrogen for having vapor obtains liquid I after steam separates；
Step 2: the krill frost processing after body surface is dried up, is handled, regelation of laying equal stress on freezes using microwave thawing afterwards
Handled 3 times with microwave thawing；It is -2 DEG C to freeze temperature inside the krill of processing；The time of microwave thawing is 20s,
And it is 85 DEG C that krill body temperature is kept during microwave thawing；
Step 3: collect the liquid after evaporating and cool down in microwave thawing processing procedure；
Step 4: the quick-frozen rear pulverization process that carries out of the krill of step 3 is obtained into the quick-frozen powder of krill；
Step 5: by volume 1:1 ratio is well mixed acquisition after liquid I is added into the quick-frozen powder of the krill
Mixture I, the mixture I is subjected to ultrasonic disruption processing and obtains mixture II；Wherein, the frequency of ultrasonic wave is 25KHz,
Ultrasonication total duration is 8min, and at interval of 4s ultrasonications once, a duration 15s, the acoustical power of ultrasonic wave is 5W/
cm2；
Step 6: mixture II is carried out into centrifugal treating obtains residue I and liquid III；
Step 7: the instantaneous differential pressure flash distillation process of residue I is obtained into liquid IV and residue II, wherein instantaneous differential pressure flashes
Temperature is no more than 95 DEG C；Wherein, it is further comprising the steps of：E, the close of the instantaneous differential pressure processing unit of the residue I will be contained with
Envelope chamber vacuumizes；F, it is 93 DEG C, pressure 0.25Mpa that vapours to its interior temperature is passed through into annular seal space, the processing of pressurize afterwards
35s；G, by the sealing cavity pressure in 3s pressure release to 6kpa；H, at interval of 30-45s repeat steps a, step b and step c
Once, it is repeated 3 times altogether；
Step 8: residue II is carried out into squeezing processing obtains primary krill oil and residue III；By residue in the step 8
II enters to put into carry out squeezing processing in screw extruder, and squeezing processing includes one-level squeezing and two level squeezing：Wherein, screw extrusion
Machine is correspondingly arranged on two one-level press cylinders and two level press cylinder, wherein, the bottom connection of the shell body I of two one-level press cylinders
Set, and the screw rod in two one-level press cylinders does not contact so that two one-level press cylinders are in the angle less than 90 degree；Two level pressure
Cylinder is squeezed, the upper end of its shell is connected to the bottom junctions of the shell body II of two one-level press cylinders, and shell body II is most
Major diameter is less than 1.5 times of the minimum diameter of shell body I；
Step 9: by residue III, liquid and liquid III according to volume ratio 1:1:1 ratio is sufficiently mixed acquisition mixture
III, mixture III is warming up to after 45 DEG C after adding appropriate protease thereto and standing 50min after being well mixed, by mixture
III centrifugal treating obtains enzymolysis liquid；Wherein, the addition of protease is the 3% of the quality of mixture III；
Step 10: the enzymolysis liquid and organic solvent are sufficiently mixed the secondary krill oil of extraction；Organic solvent selects quality
Fraction is 95% ethanol or acetone；
Step 11: after the organic solvent in secondary krill oil is reclaimed, by secondary krill oil, liquid IV and primary krill
Krill oil is refined after oil mixing centrifugation removal of impurities water removal.
Wherein, liquid I, liquid and liquid III enter hermetically sealed can and saved backup, and nitrogen is filled with hermetically sealed can.
Krill oil is prepared as experimental group 1, experimental group 2 and experimental group 3 using above-described embodiment 1-3 method, is corresponded to
Embodiment 1-3, it is respectively control group 1, control group 2 and control group 3 to set three groups of control groups, wherein, after being caught to krill
Processing opportunity it is identical, quick-frozen → crushing → homogenate → organic solvent extraction → vacuum rotating is directly carried out after body surface is dried and is steamed
The processing procedure of hair → refined krill oil.
Krill using following methods to experimental group 1, experimental group 2, experimental group 3, control group 1, control group 2 and control group 3
The physicochemical property of oil is measured：
1) yield calculates：Shrimp sauce yield/%=krill oil qualities (g)/drying krill meal quality (g) × 100%
2) krill oil samples are delivered to logical mark standard technique and service (Shanghai) Co., Ltd. by EPA, the measure of DHA content, are entrusted
It is held in the palm on behalf of detection.According to the survey of total fat, saturated fat (acid), unsaturated fat (acid) in GB/T22223-2008 food
It is fixed, using the EPA in hydrolysis extraction-gas chromatography measure shrimp sauce, DHA content.
3) assay of vitamin E and content astaxanthin：The measure of content of vitamin E refers to (AOCS Official
MethodCe 8-89,1998) method.Sample (0.05g) is dissolved in 10mL n-heptane solutions, and extract uses HPLC-FLD, 4.6 ×
150mm silicagel columns are analyzed；Mobile phase is heptane：Isopropanol (100:0.4), flow velocity 1mL/min；The detection of tocopherol is using glimmering
Light detects, excitation light wave a length of 290nm, wavelength of transmitted light 330nm；The methods of content astaxanthin measure refers to F.S.H.Lu,
(testing result see the table below 1).
The yield and physicochemical property of the krill oil of table 1
It was found from upper table 1, experimental group 1, experimental group 2 and experimental group 3 obtain than control group 1, control group 2 and control group 3
Higher krill oil yield, and phosphatide, VE, astaxanthin, EPA and DHA that content is higher, retain the activity of krill oil into
Point；And the organic solvent content used in experimental group 1, experimental group 2 and embodiment 1-3 corresponding to experimental group 3 is few, almost without having
Solvent remains.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, it is of the invention and unlimited
In specific details and shown here as the embodiment with description.
Claims (10)
1. a kind of extracting method of krill oil, it is characterised in that comprise the following steps：
Step 1: carrying out body surface moisture drying in 3 hours to it after krill fishing, and collect the liquid I of blowout；
Step 2: after body surface is dried up krill frost processing, handled afterwards using microwave thawing, regelation of laying equal stress on freeze and it is micro-
Ripple, which thaws, to be handled 2-3 times；
Step 3: collect the liquid after evaporating and cool down in microwave thawing processing procedure；
Step 4: the quick-frozen rear pulverization process that carries out of the krill of step 3 is obtained into the quick-frozen powder of krill；
Step 5: by volume 2:1-2 ratio is mixed after adding liquid I into the quick-frozen powder of the krill
Compound I, the mixture I is subjected to ultrasonic disruption processing and obtains mixture II；
Step 6: mixture II is carried out into centrifugal treating obtains residue I and liquid III；
Step 7: the instantaneous differential pressure flash distillation process of residue I is obtained into liquid IV and residue II, wherein instantaneous differential pressure flash temperature
No more than 95 DEG C；
Step 8: residue II is carried out into squeezing processing obtains primary krill oil and residue III；
Step 9: by residue III, liquid and liquid III according to volume ratio 1-2:1:1 ratio is sufficiently mixed acquisition mixture
III, will after adding appropriate protease after mixture III is warming up into 35-45 DEG C thereto and standing 30-50min after being well mixed
The centrifugal treating of mixture III obtains enzymolysis liquid；Wherein, the addition of protease is the 1% of the quality of mixture III；
Step 10: the enzymolysis liquid and organic solvent are sufficiently mixed the secondary krill oil of extraction；
Step 11: by after the organic solvent recovery in secondary krill oil, secondary krill oil, liquid IV and primary krill oil are mixed
Krill oil is refined after closing centrifugation removal of impurities water removal.
2. the extracting method of krill oil as claimed in claim 1, it is characterised in that also include following step in the step 1
Suddenly：
It is online that krill is uniformly laid on to the multilayer drying being distributed from up to down, multilayer drying net is arranged on relatively closed a,
Drying unit in；
B, it is passed through dry nitrogen thereto from the bottom of the drying unit, nitrogen temperature is 50-60 DEG C；
C, nitrogen is discharged after multilayer drying net from the outlet of drying unit；
D, the nitrogen with vapor of discharge obtains liquid I after steam separates.
3. the extracting method of krill oil as claimed in claim 1, it is characterised in that microwave thawing is handled in the step 2
Actual conditions is：The time of microwave thawing is 10-20s, and keeps krill body temperature not during microwave thawing
More than 90 DEG C.
4. the extracting method of krill oil as claimed in claim 1, it is characterised in that in the step 2, freeze the south of processing
Temperature is -6~-2 DEG C inside the krill of pole.
5. the extracting method of krill oil as claimed in claim 1, it is characterised in that liquid I, liquid and liquid III enter close
Sealed cans are saved backup, and nitrogen is filled with hermetically sealed can.
6. the extracting method of krill oil as claimed in claim 1, it is characterised in that the frequency of ultrasonic wave is in the step 5
20-25KHz, ultrasonication total duration are 4-8min, at interval of 2-4s ultrasonications once, a duration 10-15s, are surpassed
The acoustical power of sound wave is 3-5W/cm2。
7. the extracting method of krill oil as claimed in claim 1, it is characterised in that the step 7 is further comprising the steps of：
E, the annular seal space for the instantaneous differential pressure processing unit for being contained with the residue I is vacuumized；
F, vapours to its interior temperature is passed through into annular seal space and is no more than 95 DEG C, pressure 0.15-0.25Mpa, afterwards at pressurize
Manage 20-40s；
G, by the sealing cavity pressure in 3s pressure release to 5-6kpa；
H, at interval of 30-45s repeat steps a, step b and step c once, altogether repeatedly 2-3 times.
8. the extracting method of krill oil as claimed in claim 7, it is characterised in that vapours is passed through in f, into annular seal space extremely
Its interior temperature is 93 DEG C, pressure 0.25Mpa, the processing of pressurize afterwards 35s.
9. the extracting method of krill oil as claimed in claim 7, it is characterised in that lead to multiple step a, step in f, into annular seal space
Rapid b and step c once, is repeated 3 times altogether.
10. the extracting method of krill oil as claimed in claim 1, it is characterised in that enter to throw by residue II in the step 8
Enter and squeezing processing is carried out in screw extruder, squeezing processing includes one-level squeezing and two level squeezing：
Wherein, screw extruder is correspondingly arranged on two one-level press cylinders and two level press cylinder, wherein, two one-level press cylinders
The bottom connection of shell body I is set, and the screw rod in two one-level press cylinders does not contact so that two one-level press cylinders are in be less than
90 degree of angle；
Two level squeezes cylinder, and the upper end of its shell is connected to the bottom junctions of the shell body II of two one-level press cylinders, and outside
The maximum gauge of housing II is less than 1.5 times of the minimum diameter of shell body I.
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Cited By (1)
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| CN108559622A (en) * | 2018-03-19 | 2018-09-21 | 中国水产科学研究院东海水产研究所 | A kind of krill oil process can be used for boat-carrying |
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