CN105907456A - Fine processing method of fish oil - Google Patents

Fine processing method of fish oil Download PDF

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Publication number
CN105907456A
CN105907456A CN201610294092.8A CN201610294092A CN105907456A CN 105907456 A CN105907456 A CN 105907456A CN 201610294092 A CN201610294092 A CN 201610294092A CN 105907456 A CN105907456 A CN 105907456A
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fish oil
oil
enzymolysis
processing method
fish
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CN201610294092.8A
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CN105907456B (en
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谢超
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Guangzhou Changshengkang Biotechnology Co., Ltd.
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Zhejiang Ocean University ZJOU
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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
    • 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
    • C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
    • 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
    • C11B3/16—Refining fats or fatty oils by mechanical means

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  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Microbiology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Biochemistry (AREA)
  • Mechanical Engineering (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Immobilizing And Processing Of Enzymes And Microorganisms (AREA)

Abstract

The invention relates to the field of the processing of fish products and discloses a fine processing method of fish oil. The fine processing method of fish oil comprises the following steps: a, washing fish guts, removing giblets, pounding the fish guts to prepare a blank material; b, adding the blank material into an enzymolysis solution containing an immobilized magnetic composite enzyme for carrying out enzymolysis, and recycling the immobilized magnetic composite enzyme by using a magnet after carrying out enzymolysis; c, filtering the enzymolysis solution to remove residues, then standing and layering, and separating to obtain upper fish oil and lower oil-water mixed solution; d, transferring the oil-water mixed solution to a foam separating column, aerating the bottom of the foam separating column, generating a foam layer on the upper layer of the oil-water mixed solution, and separating the foam layer from the liquid in time; e, carrying out centrifugal separation on the oil-water mixed solution to obtain upper fish oil; f, mixing the upper fish oil obtained in step c with the upper fish oil obtained in step e to prepare the fish oil. The processing method of the fish oil is simple in the process and high in the extraction efficiency and the extraction rate; the processed fish oil is high in purity, free of fishy smell and pure in color.

Description

A kind of exquisite processing method of fish oil
Technical field
The present invention relates to fish product manufacture field, particularly relate to the exquisite processing method of a kind of fish oil.
Background technology
Fish oil is one of important composition composition of Fish, and fish oil, rich in multiple unsaturated fatty acids such as EPA and DHA, has The functions such as blood pressure lowering, allaying tiredness, prevention cerebral thrombosis, raising memory.Therefore fish oil is widely used in food, medical treatment, raises The fields such as material industry.
The preparation method of fish oil is predominantly at present: 1, is put into by raw material in boiling water and carries out decocting in water, then by fish floating for upper strata Oil is by being centrifuged or being gone out by organic solvent extraction.The fish oil purity extracted by said method is the highest, easily by water, protein, The impurity such as colloid substance are brought into, need to carry out further Refining, operate extremely complex.2, put in enzymolysis solution by raw material Row enzymolysis, takes upper strata fish oil after enzymolysis, then fish oil is decoloured, eliminating sargassum smell, remove impurity process.
As the Chinese patent of Application No. 201410468003.8 discloses a kind of fish flour processing byproduct fish oil decoloration deodorization Method, uses kieselguhr to decolour low value fish oil, can preferably remove fish flour processing byproduct fish oil color；Use yeast powder Carry out the eliminating sargassum smell of fish flour processing byproduct fish oil, be successfully realized the removing of fish oil fishy smell.
Fish processing fent fish oil is extracted as the Chinese patent of Application No. 200710031626.9 discloses a kind of enzymatic isolation method Technology, its method step is pre-treatment: Fish processing fent clean after, blend；Protease hydrolysis: use neutrality Protease enzyme double with papain hydrolyzes simultaneously；Oil-water separation: hydrolyzed solution filter and remove residue by centrifugation, filtrate machine by centrifugation is carried out Oil-water separation, obtains fish oil and hydrolyzed protein；Pyloric fat acid: fish oil obtains refined fish after degumming, deacidification, decolouring and deodorize Oil.
Above two method all have employed second method to prepare fish oil, prepares the purity relatively first method purity of fish oil more Height, but the extraction ratio for fish oil is not ideal enough, and need to carry out follow-up decolouring, eliminating sargassum smell, remove impurity process, technique is more Loaded down with trivial details, affect production efficiency.
Summary of the invention
In order to solve above-mentioned technical problem, the invention provides the exquisite processing method of a kind of fish oil.The present invention is for fish oil Processing method technique is simple, and extraction efficiency and extraction ratio are high, and the fish oil purity that processing obtains is high, and without fishy smell, color is pure.
The concrete technical scheme of the present invention is: the exquisite processing method of a kind of fish oil, sequentially includes the following steps:
A, Fish internal organs are carried out roguing, smash to pieces, prepare blank.
B, described blank is added to the enzymolysis solution containing immobilization magnetic coupling enzyme carries out enzymolysis, wherein blank, enzymolysis solution Mass ratio be 1:2.5-3.5, the enzyme content in enzymolysis solution is 0.05-0.2%, and hydrolysis temperature is 40-50 DEG C, enzymolysis time 2-6h, Enzymolysis solution pH controls at 6.5-7；With Magnet, described immobilization magnetic coupling enzyme is reclaimed after enzymolysis.
Blank utilizes immobilization magnetic coupling enzyme carry out enzymolysis, immobilization magnetic coupling enzyme is supported on carrier due to enzyme, Receiving the fixing protection of carrier, be difficult to protected from environmental and make enzymatic activity reduce, therefore enzymolysis efficiency is higher；On the other hand, Containing magnetic core particle in immobilization magnetic coupling enzyme, after enzymolysis completes, only magnetic field need to be utilized to be entered by immobilization magnetic coupling enzyme Row is assembled, and then separates and recovers, not only convenient separation, and immobilization magnetic coupling enzyme can reuse, and reduces into This.Traditional method needs after enzymolysis enzymolysis solution is carried out high temperature enzyme denaturing, and for fish oil, meeting in high-temperature process Causing fish oil degeneration cracking, cause effective ingredient to run off, nutritive value declines.The inventive method is without high temperature enzyme denaturing process, energy Enough at utmost reservation fish oil effective ingredient.
Additionally, the carrier in the immobilization magnetic coupling enzyme of the present invention, there is the three-dimensional net structure of complexity, have the highest Voidage, therefore adsorptivity is very strong, not only effective to enzyme immobilizatio, and while enzymolysis, it is possible to Fish internal organs In raw meat class material (amine substance) and pigment adsorb so that fish oil the most i.e. carries out decolouring in enzymolysis process, eliminating sargassum smell Processing, a step completes, it is not necessary to follow-up carry out relevant treatment again, and therefore the preparation efficiency of fish oil is higher.
C, to step b process after enzymolysis solution filter cleaner, then stratification, isolated upper strata fish oil and lower floor's profit Mixed liquor.
In this step, the fish oil purity on upper strata is the highest, can directly separate, and in the oil water mixture of lower floor, by Stirring in the existence and enzymolysis process of emulsion, vibration, define relatively stable oil-in-water emulsion systems, stand, Profit all cannot be separated by centrifugal treating effectively.
D, described oil-water mixture is transferred in foam separation post, is ventilated in the bottom of described foam separation post, profit Mixed liquor upper strata produces froth bed, is separated with liquid in time by froth bed；Wherein, Ventilation Rate is 2-4L/min, processes Time is 10-30min, and oil mixing with water liquid temp is 20-30 DEG C, and oil-water mixture pH controls at 6-7.
Oil-water mixture is carried out foam separation, in the foaming process of foam separation, due to emulsifier in oil-water mixture Having the strongest surface tension, and the surface of foam is gas-liquid separation interface, therefore emulsifier can be gathered in foam surface, right Foam is collected separating such that it is able to separated from oil-water mixture by emulsifier.When emulsion in oil-water mixture After the content of matter is substantially reduced, the oil-in-water system in oil-water mixture is disintegrated, and oil-water separation difficulty is substantially reduced.
E, by step d process after oil-water mixture be centrifuged separate, obtain upper strata fish oil.
F, upper strata fish oil mixing step c and step e obtained, i.e. prepare fish oil.
The fish oil processing method of the present invention, not only technique is simple, and from can the oil-water mixture of lower floor extract further Fish oil, the extraction ratio of fish oil is higher, and fish oil purity is the highest, and without fishy smell, color is transparent pure.
As preferably, before carrying out step b, described blank entered pretreatment: be 30-40 DEG C by blank in the temperature of excess Water in impregnate swelling 1-2h.
Carrying out blank impregnating swelling treatment before enzymolysis, it is possible to make cell membrane be in the state of swelling, cell membrane is easier to broken, Thus beneficially enzymolysis.
As preferably, in step b, while blank is carried out enzymolysis, enzymolysis solution is carried out supersonic oscillations process.? Enzymolysis process carries out supersonic oscillations process, it is possible to accelerate the breakage of cell membrane, improve enzymolysis efficiency.But also bring simultaneously Shortcoming: comprehend the emulsifying effectiveness strengthening enzymolysis solution at supersonic oscillations so that oil-water separation difficulty increases, but by this The foam separation technique of bright subsequent process can solve the problem that this problem.
As preferably, the preparation method of described immobilization magnetic coupling enzyme is: the acetic acid dissolving the chitosan in 8-12wt% is molten In liquid, prepared concentration is the chitosan solution of 2-3wt%；Composite aerogel granule and ferroso-ferric oxide is added in chitosan solution Particle, prepares mixing suspension；Wherein, the quality of composite aerogel granule is 0.5-1.5 times of chitosan, ferroso-ferric oxide grain 0.5-1 times that quality is chitosan of son；Dripping quality in mixing suspension is to mix the Arlacel-80 of suspension 3-5% and carry out Ultrasound wave dispersion and emulsion, then adds glutaraldehyde and volume that volume is mixing suspension 0.1-0.3% in first backward mixing suspension For mixing the sodium hydroxide solution of the 4wt% of suspension 0.5-1 times and stirring, then adsorb with Magnet, separate liquid After, solid matter is carried out, prepares Magnetic Microspheres-Carrier after lyophilization；Described Magnetic Microspheres-Carrier is dispersed in compound Enzyme content is in the solution of 0.1-0.3wt%, stirs 1-3h, form immobilization magnetic coupling enzyme at 25-35 DEG C, will be solid with Magnet Surely change magnetic coupling enzyme adsorbing separation, clean, be dried；Wherein, the quality of Magnetic Microspheres-Carrier is the 0.1-0.4 of compound enzyme quality Times.
Magnetic Microspheres-Carrier prepared by the inventive method, is carried out chitosan, composite aerogel granule and ferroso-ferric oxide particle Compound, with ferroso-ferric oxide particle for magnetic core, with chitosan for being coated carrier, it is that complex " is inlayed " at composite aerogel granule In chitosan, after the crosslinking of glutaraldehyde, compound fastness is higher, recently after the activation of sodium hydroxide, formation Magnetic Microspheres-Carrier has well being coated property to enzyme material, and self has the highest porosity, it is possible to in enzymolysis solution Raw meat class material, pigment, heavy metal ion carry out active adsorption, adsorption rate is high, and adsorption capacity is big such that it is able to a step realizes Enzymolysis, eliminating sargassum smell, desolventing technology, improve extraction efficiency.
As preferably, the preparation method of described composite aerogel granule is: by furfural, water soluble phenol resin, sepiolite powder Mix with water 4-6:1:0.4-0.6:100 in mass ratio, obtain mixed liquor after stirring, by concentration be under agitation The ammonia of 0.5mol/L is added drop-wise in mixed liquor until mixed liquor is neutrality；Then at 55-65 DEG C, react 10-20h, be combined Charcoal colloidal sol；Activated carbon composite colloidal sol is mixed with TiO 2 sol 1:0.5-1.5 in mass ratio, after stirring, obtains mixed sols, After mixed sols is at room temperature stood aging 1-2 days, first with dehydrated alcohol, mixed sols solvent is replaced 12-24h, then with just Hexane carries out solvent displacement 6-12h to mixed sols, prepares pluralgel after removing normal hexane；Finally use CO 2 supercritical Fluid i.e. prepares composite aerogel granule to pulverizing after pluralgel dried.
Composite aerogel granule prepared by the inventive method is charcoal/meerschaum/titanium dioxide composite aerogel, this composite aerogel Having the porosity of superelevation, pore-size differs, is distributed extensively, it is possible to adsorb different materials, and adsorption efficiency is high, energy Enough effectively enzymolysis solution is carried out eliminating sargassum smell, decolouring.And there is preferable hydrophilic, fish oil will not be adsorbed.
As preferably, described compound enzyme is the mixture of neutral protease, trypsin and papain.Compound protease Enzymolysis efficiency can be greatly improved.
As preferably, the mass ratio of described neutral protease, trypsin and papain is 1:1-2:1.
As preferably, in step b, in enzymolysis solution, add the sodium chloride that quality is enzymolysis solution 4-6wt%.The addition of sodium chloride The separating degree of profit can be increased so that profit is more easily separated.
As preferably, the internal diameter of described foam separation post is 40-50mm, the loading height of oil water mixture in foam separation post For 40-50cm.The specification of the foam separation post of the present invention is according to the Fish specific setting of internal organs enzymolysis solution, it is possible to increase foam Separation efficiency, farthest isolates emulsifier.
It is compared with the prior art, the invention has the beneficial effects as follows: the present invention is simple for the processing method technique of fish oil, extracts Efficiency and extraction ratio are high, and the fish oil purity that processing obtains is high, and without fishy smell, color is pure.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The preparation of early stage reagent:
The preparation of composite aerogel granule: furfural, water soluble phenol resin, sepiolite powder and water 5:1:0.5:100 in mass ratio is mixed, Obtain mixed liquor after stirring, under agitation the ammonia that concentration is 0.5mol/L is added drop-wise in mixed liquor until mixed liquor In neutrality；Then at 60 DEG C, react 15h, obtain activated carbon composite colloidal sol；By activated carbon composite colloidal sol with TiO 2 sol in mass ratio 1:1 mixes, and obtains mixed sols, after mixed sols at room temperature stands aging 1.5 days, first use dehydrated alcohol after stirring Mixed sols solvent is replaced 18h, then with normal hexane, mixed sols is carried out solvent displacement 9h, prepare compound after removing normal hexane Gel；Co 2 supercritical fluid is finally used i.e. to prepare composite aerogel granule to pulverizing after pluralgel dried.
The preparation of immobilization magnetic coupling enzyme: dissolve the chitosan in the acetic acid solution of 10wt%, prepared concentration is 2.5wt% Chitosan solution；In chitosan solution, add composite aerogel granule and ferroso-ferric oxide particle, prepare mixing suspension； Wherein, the quality of composite aerogel granule is 1 times of chitosan, and the quality of ferroso-ferric oxide particle is 0.75 times of chitosan； Dripping quality in mixing suspension is to mix the Arlacel-80 of suspension 4% and carry out ultrasound wave dispersion and emulsion, then the most backward mixed Close and suspension adds the glutaraldehyde that volume is mixing suspension 0.2% and the hydrogen-oxygen of the 4wt% that volume is mixing suspension 0.75 times Change sodium solution also to stir, then adsorb with Magnet, after separating liquid, solid matter is carried out, lyophilization Rear prepared Magnetic Microspheres-Carrier；Described Magnetic Microspheres-Carrier is dispersed in the solution that compound enzyme content is 0.2wt%, at 30 DEG C Stirring 2h, formed immobilization magnetic coupling enzyme, with Magnet by immobilization magnetic coupling enzyme adsorbing separation, clean, be dried；Wherein, The quality of Magnetic Microspheres-Carrier is 0.25 times of compound enzyme quality.
Wherein, described compound enzyme is the mixture of neutral protease, trypsin and papain, and neutral protease, The mass ratio of trypsin and papain is 1:1.5:1.
The exquisite processing method of a kind of fish oil, sequentially includes the following steps:
A, Fish internal organs are carried out roguing, smash to pieces, prepare blank, blank is impregnated molten in the water that temperature is 35 DEG C of excess Swollen 1.5h, the most standby.
B, described blank is added in the enzymolysis solution containing immobilization magnetic coupling enzyme, under the conditions of supersonic oscillations, carry out enzyme Solving, wherein blank, the mass ratio of enzymolysis solution are 1:3, and the enzyme content in enzymolysis solution is 0.125%, and hydrolysis temperature is 45 DEG C, enzyme Solution time 4h, enzymolysis solution pH control at 6.5-7；With Magnet, described immobilization magnetic coupling enzyme is reclaimed after enzymolysis.
C, to step b process after enzymolysis solution filter cleaner, then stratification, isolated upper strata fish oil and lower floor's profit Mixed liquor.
D, described oil-water mixture is transferred in foam separation post, is ventilated in the bottom of described foam separation post, profit Mixed liquor upper strata produces froth bed, is separated with liquid in time by froth bed；Wherein, Ventilation Rate is 3L/min, during process Between be 20min, oil mixing with water liquid temp is 25 DEG C, and oil-water mixture pH controls at 6-7.The internal diameter of described foam separation post is 45mm, in foam separation post, the loading height of oil water mixture is 45cm.
E, by step d process after oil-water mixture be centrifuged separate, obtain upper strata fish oil.
F, upper strata fish oil mixing step c and step e obtained, i.e. prepare fish oil.
Embodiment 2
The preparation of early stage reagent:
The preparation of composite aerogel granule: furfural, water soluble phenol resin, sepiolite powder and water 4:1:0.4:100 in mass ratio is mixed, Obtain mixed liquor after stirring, under agitation the ammonia that concentration is 0.5mol/L is added drop-wise in mixed liquor until mixed liquor In neutrality；Then at 55 DEG C, react 20h, obtain activated carbon composite colloidal sol；By activated carbon composite colloidal sol with TiO 2 sol in mass ratio 1:0.5 mixes, and obtains mixed sols, after mixed sols at room temperature stands aging 1 day, first use dehydrated alcohol after stirring Mixed sols solvent is replaced 12h, then with normal hexane, mixed sols is carried out solvent displacement 12h, prepare compound after removing normal hexane Gel；Co 2 supercritical fluid is finally used i.e. to prepare composite aerogel granule to pulverizing after pluralgel dried.
The preparation of immobilization magnetic coupling enzyme: dissolve the chitosan in the acetic acid solution of 8wt%, prepared concentration is 2wt%'s Chitosan solution；In chitosan solution, add composite aerogel granule and ferroso-ferric oxide particle, prepare mixing suspension；Its In, the quality of composite aerogel granule is 0.5 times of chitosan, and the quality of ferroso-ferric oxide particle is 0.5 times of chitosan；To Dripping quality in mixing suspension is to mix the Arlacel-80 of suspension 3% and carry out ultrasound wave dispersion and emulsion, then first backward mixing Suspension adds the glutaraldehyde that volume is mixing suspension 0.1% and the hydroxide of the 4wt% that volume is mixing suspension 0.5 times Sodium solution also stirs, and then adsorbs with Magnet, separates after liquid, is carried out solid matter, after lyophilization Prepare Magnetic Microspheres-Carrier；Described Magnetic Microspheres-Carrier is dispersed in the solution that compound enzyme content is 0.1wt%, stirs at 25 DEG C Mix 3h, form immobilization magnetic coupling enzyme, with Magnet by immobilization magnetic coupling enzyme adsorbing separation, clean, be dried；Wherein, The quality of Magnetic Microspheres-Carrier is 0.1 times of compound enzyme quality.
Wherein, described compound enzyme is the mixture of neutral protease, trypsin and papain, and neutral protease, The mass ratio of trypsin and papain is 1:1:1.
The exquisite processing method of a kind of fish oil, sequentially includes the following steps:
A, Fish internal organs are carried out roguing, smash to pieces, prepare blank, blank is impregnated molten in the water that temperature is 30 DEG C of excess Swollen 2h, the most standby.
B, adding in the enzymolysis solution containing immobilization magnetic coupling enzyme by described blank, adding quality in enzymolysis solution is enzymolysis The sodium chloride of liquid 4wt%.Carrying out enzymolysis under the conditions of supersonic oscillations, wherein blank, the mass ratio of enzymolysis solution are 1:2.5, enzyme The enzyme content solved in liquid is 0.05%, and hydrolysis temperature is 40 DEG C, enzymolysis time 6h, and enzymolysis solution pH controls at 6.5-7；After enzymolysis With Magnet, described immobilization magnetic coupling enzyme is reclaimed.
C, to step b process after enzymolysis solution filter cleaner, then stratification, isolated upper strata fish oil and lower floor's profit Mixed liquor.
D, described oil-water mixture is transferred in foam separation post, is ventilated in the bottom of described foam separation post, profit Mixed liquor upper strata produces froth bed, is separated with liquid in time by froth bed；Wherein, Ventilation Rate is 2L/min, during process Between be 30min, oil mixing with water liquid temp is 20 DEG C, and oil-water mixture pH controls at 6-7.The internal diameter of described foam separation post is 40mm, in foam separation post, the loading height of oil water mixture is 40cm.
E, by step d process after oil-water mixture be centrifuged separate, obtain upper strata fish oil.
F, upper strata fish oil mixing step c and step e obtained, i.e. prepare fish oil.
Embodiment 3
The preparation of early stage reagent:
The preparation of composite aerogel granule: furfural, water soluble phenol resin, sepiolite powder and water 6:1:0.6:100 in mass ratio is mixed, Obtain mixed liquor after stirring, under agitation the ammonia that concentration is 0.5mol/L is added drop-wise in mixed liquor until mixed liquor In neutrality；Then at 65 DEG C, react 10h, obtain activated carbon composite colloidal sol；By activated carbon composite colloidal sol with TiO 2 sol in mass ratio 1:1.5 mixes, and obtains mixed sols, after mixed sols at room temperature stands aging 2 days, first use dehydrated alcohol after stirring Mixed sols solvent is replaced 24h, then with normal hexane, mixed sols is carried out solvent displacement 6h, prepare compound after removing normal hexane Gel；Co 2 supercritical fluid is finally used i.e. to prepare composite aerogel granule to pulverizing after pluralgel dried.
The preparation of immobilization magnetic coupling enzyme: dissolve the chitosan in the acetic acid solution of 12wt%, prepared concentration is 3wt% Chitosan solution；In chitosan solution, add composite aerogel granule and ferroso-ferric oxide particle, prepare mixing suspension； Wherein, the quality of composite aerogel granule is 1.5 times of chitosan, and the quality of ferroso-ferric oxide particle is 1 times of chitosan； Dripping quality in mixing suspension is to mix the Arlacel-80 of suspension 5% and carry out ultrasound wave dispersion and emulsion, then the most backward mixed Close and suspension adds the glutaraldehyde that volume is mixing suspension 0.3% and the hydroxide of the 4wt% that volume is mixing suspension 1 times Sodium solution also stirs, and then adsorbs with Magnet, separates after liquid, is carried out solid matter, after lyophilization Prepare Magnetic Microspheres-Carrier；Described Magnetic Microspheres-Carrier is dispersed in the solution that compound enzyme content is 0.3wt%, stirs at 35 DEG C Mix 1h, form immobilization magnetic coupling enzyme, with Magnet by immobilization magnetic coupling enzyme adsorbing separation, clean, be dried；Wherein, The quality of Magnetic Microspheres-Carrier is 0.4 times of compound enzyme quality.
Wherein, described compound enzyme is the mixture of neutral protease, trypsin and papain, and neutral protease, The mass ratio of trypsin and papain is 1:2:1.
The exquisite processing method of a kind of fish oil, sequentially includes the following steps:
A, Fish internal organs are carried out roguing, smash to pieces, prepare blank, blank is impregnated molten in the water that temperature is 40 DEG C of excess Swollen 1h, the most standby.
B, adding in the enzymolysis solution containing immobilization magnetic coupling enzyme by described blank, adding quality in enzymolysis solution is enzymolysis The sodium chloride of liquid 6wt%.Carrying out enzymolysis under the conditions of supersonic oscillations, wherein blank, the mass ratio of enzymolysis solution are 1:3.5, enzyme The enzyme content solved in liquid is 0.2%, and hydrolysis temperature is 50 DEG C, enzymolysis time 2h, and enzymolysis solution pH controls at 6.5-7；After enzymolysis With Magnet, described immobilization magnetic coupling enzyme is reclaimed.
C, to step b process after enzymolysis solution filter cleaner, then stratification, isolated upper strata fish oil and lower floor's profit Mixed liquor.
D, described oil-water mixture is transferred in foam separation post, is ventilated in the bottom of described foam separation post, profit Mixed liquor upper strata produces froth bed, is separated with liquid in time by froth bed；Wherein, Ventilation Rate is 4L/min, during process Between be 10min, oil mixing with water liquid temp is 30 DEG C, and oil-water mixture pH controls at 6-7.The internal diameter of described foam separation post is 50mm, in foam separation post, the loading height of oil water mixture is 50cm.
E, by step d process after oil-water mixture be centrifuged separate, obtain upper strata fish oil.
F, upper strata fish oil mixing step c and step e obtained, i.e. prepare fish oil.
The extraction ratio of fish oil that embodiment 1-3 prepares, purity, fishy smell sense organ, color are as shown in the table:
Extraction ratio Purity Fishy smell sense organ Color
Embodiment 1 90.3% 94.4% 0 Clear pale yellow color
Embodiment 2 95.2% 96.6% 0 Clear pale yellow color
Embodiment 3 92.8% 95.9% 0 Clear pale yellow color
Wherein, fishy smell subjective appreciation is classified as: without fishy smell 0, slightly fishy smell 1, fishy smell more weak 2, has fishy smell 3, fishy smell general 4, Fishy smell lays particular stress on 5, and fishy smell heavier 6, fishy smell weighs 7 very much.
Raw materials used, equipment in the present invention, unless otherwise noted, is the conventional raw material of this area, equipment；In the present invention Method therefor, unless otherwise noted, is the conventional method of this area.
The above, be only presently preferred embodiments of the present invention, not impose any restrictions the present invention, every according to skill of the present invention Any simple modification, change and the equivalent transformation that above example is made by art essence, all still falls within technical solution of the present invention Protection domain.

Claims (9)

1. the exquisite processing method of a fish oil, it is characterised in that sequentially include the following steps:
A, Fish internal organs are carried out roguing, smash to pieces, prepare blank；
B, described blank is added to the enzymolysis solution containing immobilization magnetic coupling enzyme carries out enzymolysis, wherein blank, the mass ratio of enzymolysis solution are 1:2.5-3.5, and the enzyme content in enzymolysis solution is 0.05-0.2%, and hydrolysis temperature is 40-50 DEG C, enzymolysis time 2-6h, enzymolysis solution pH control at 6.5-7；With Magnet, described immobilization magnetic coupling enzyme is reclaimed after enzymolysis；
C, to step b process after enzymolysis solution filter cleaner, then stratification, isolated upper strata fish oil and lower floor's oil-water mixture；
D, being transferred in foam separation post by described oil-water mixture, ventilate the bottom of described foam separation post, oil-water mixture upper strata produces froth bed, is separated with liquid in time by froth bed；Wherein, Ventilation Rate is 2-4L/min, and the process time is 10-30min, and oil mixing with water liquid temp is 20-30 DEG C, and oil-water mixture pH controls at 6-7；
E, by step d process after oil-water mixture be centrifuged separate, obtain upper strata fish oil；
F, upper strata fish oil mixing step c and step e obtained, i.e. prepare fish oil.
The exquisite processing method of a kind of fish oil the most as claimed in claim 1, it is characterised in that before carrying out step b, described blank entered pretreatment: in the water that temperature is 30-40 DEG C of excess, blank is impregnated swelling 1-2h.
The exquisite processing method of a kind of fish oil the most as claimed in claim 1, it is characterised in that in step b, while blank is carried out enzymolysis, carries out supersonic oscillations process to enzymolysis solution.
The exquisite processing method of a kind of fish oil the most as claimed in claim 1, it is characterised in that the preparation method of described immobilization magnetic coupling enzyme is: dissolving the chitosan in the acetic acid solution of 8-12wt%, prepared concentration is the chitosan solution of 2-3wt%；In chitosan solution, add composite aerogel granule and ferroso-ferric oxide particle, prepare mixing suspension；Wherein, the quality of composite aerogel granule is 0.5-1.5 times of chitosan, and the quality of ferroso-ferric oxide particle is 0.5-1 times of chitosan；Dripping quality in mixing suspension is to mix the Arlacel-80 of suspension 3-5% and carry out ultrasound wave dispersion and emulsion, then first backward mixing suspension adds the glutaraldehyde that volume is mixing suspension 0.1-0.3% and the sodium hydroxide solution of the 4wt% that volume is mixing suspension 0.5-1 times and stirs, then adsorb with Magnet, separate after liquid, solid matter is carried out, prepares Magnetic Microspheres-Carrier after lyophilization；Described Magnetic Microspheres-Carrier is dispersed in the solution that compound enzyme content is 0.1-0.3wt%, at 25-35 DEG C stir 1-3h, formed immobilization magnetic coupling enzyme, with Magnet by immobilization magnetic coupling enzyme adsorbing separation, clean, be dried；Wherein, the quality of Magnetic Microspheres-Carrier is 0.1-0.4 times of compound enzyme quality.
The exquisite processing method of a kind of fish oil the most as claimed in claim 4, it is characterized in that, the preparation method of described composite aerogel granule is: mixed by furfural, water soluble phenol resin, sepiolite powder and water 4-6:1:0.4-0.6:100 in mass ratio, obtain mixed liquor after stirring, under agitation the ammonia that concentration is 0.5mol/L is added drop-wise in mixed liquor until mixed liquor is neutrality；Then at 55-65 DEG C, react 10-20h, obtain activated carbon composite colloidal sol；Activated carbon composite colloidal sol is mixed with TiO 2 sol 1:0.5-1.5 in mass ratio, mixed sols is obtained after stirring, after mixed sols is at room temperature stood aging 1-2 days, first with dehydrated alcohol, mixed sols solvent is replaced 12-24h, with normal hexane, mixed sols is carried out solvent displacement 6-12h again, after removing normal hexane, prepare pluralgel；Co 2 supercritical fluid is finally used i.e. to prepare composite aerogel granule to pulverizing after pluralgel dried.
The exquisite processing method of a kind of fish oil the most as claimed in claim 4, it is characterised in that described compound enzyme is the mixture of neutral protease, trypsin and papain.
The exquisite processing method of a kind of fish oil the most as claimed in claim 6, it is characterised in that the mass ratio of described neutral protease, trypsin and papain is 1:1-2:1.
The exquisite processing method of a kind of fish oil the most as claimed in claim 1, it is characterised in that in step b, adds the sodium chloride that quality is enzymolysis solution 4-6wt% in enzymolysis solution.
The exquisite processing method of a kind of fish oil the most as claimed in claim 1, it is characterised in that the internal diameter of described foam separation post is 40-50mm, in foam separation post, the loading height of oil water mixture is 40-50cm.
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