CN105907456B - A kind of purification processing method of fish oil - Google Patents

A kind of purification processing method of fish oil Download PDF

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Publication number
CN105907456B
CN105907456B CN201610294092.8A CN201610294092A CN105907456B CN 105907456 B CN105907456 B CN 105907456B CN 201610294092 A CN201610294092 A CN 201610294092A CN 105907456 B CN105907456 B CN 105907456B
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oil
fish oil
enzyme
fish
water mixture
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CN105907456A (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 present invention relates to fish product manufacture fields, disclose a kind of exquisite processing method of fish oil, comprising: a, carry out cleaning impurity elimination to fish internal organ, smash to pieces, blank is made；B, blank is added in the enzymolysis liquid containing immobilization magnetic coupling enzyme and is digested, immobilization magnetic coupling enzyme is recycled with magnet after enzymatic hydrolysis；C, to enzymolysis liquid filtering and removing slag, layering, isolated upper layer fish oil and lower layer's oil-water mixture are then allowed to stand；D, oil-water mixture is transferred in foam fraction factor column, is ventilated to the bottom of foam fraction factor column, oil-water mixture upper layer generates froth bed, and froth bed is separated with liquid in time；E, oil-water mixture is centrifuged, obtains upper layer fish oil；F, the upper layer fish oil for obtaining step c and step e mixes, and obtains fish oil.For the present invention for the processing method simple process of fish oil, extraction efficiency and recovery rate are high, and the fish oil purity is high that processing obtains, no fishy smell, color are pure.

Description

A kind of purification processing method of fish oil
Technical field
The present invention relates to the exquisite processing methods of fish product manufacture field more particularly to a kind of fish oil.
Background technique
Fish oil is one of important composition ingredient of fish, and fish oil has rich in a variety of unsaturated fatty acids such as EPA and DHA Blood pressure lowering eliminates fatigue, prevention cerebral thrombosis, improves the functions such as memory.Therefore fish oil is widely used in food, medical treatment, feed The fields such as industry.
The preparation method of fish oil is main at present are as follows: and 1, raw material is put into boiling water carries out boiling, then by upper layer floating Fish oil is extracted by centrifugation or by organic solvent.The fish oil purity extracted by the above method is not high, easily by water, albumen The impurity such as matter, colloid substance are brought into, need to carry out further Refining, are operated extremely complex.2, raw material is put into enzymolysis liquid In digested, upper layer fish oil is taken after enzymatic hydrolysis, then decolourized to fish oil, deodorant, removal of impurities processing.
Such as application No. is 201410468003.8 Chinese patent, to disclose a kind of decoloration of fish meal processing byproduct fish oil de- The method of raw meat decolourizes to low value fish oil using diatomite, can preferably remove fish meal processing byproduct fish oil color；Using ferment Female powder carries out the deodorant of fish meal processing byproduct fish oil, is successfully realized the removing of fish oil fishy smell.
Such as application No. is 200710031626.9 Chinese patents to disclose a kind of enzymatic isolation method extraction fish processing fent The technology of fish oil, method and step are pre-treatment: after the cleaning of fish processing fent, being blended；Protease hydrolytic: in use Property the double enzymes of protease and papain hydrolyze simultaneously；Water-oil separating: hydrolyzate removes slag through centrifugal filtration, filtrate through centrifuge into Row water-oil separating obtains fish oil and protein hydrolysate；Pyloric fat acid: fish oil obtains purification fish after degumming, depickling, decoloration and deodorization Oil.
Above two method has been all made of second method to prepare fish oil, and the purity that fish oil is made is pure compared with first method Du Genggao, but not ideal enough for the recovery rate of fish oil, and need to carry out subsequent decoloration, deodorant, removal of impurities processing, technique compared with Be it is cumbersome, influence production efficiency.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of exquisite processing methods of fish oil.The present invention is for fish The processing method simple process of oil, extraction efficiency and recovery rate are high, and the fish oil purity is high that processing obtains, no fishy smell, color It is pure.
The specific technical proposal of the invention is: a kind of exquisite processing method of fish oil, sequentially includes the following steps:
A, cleaning impurity elimination is carried out to fish internal organ, smashed to pieces, blank is made.
B, the blank is added in the enzymolysis liquid containing immobilization magnetic coupling enzyme and is digested, wherein blank, enzyme The mass ratio for solving liquid is 1:2.5-3.5, and the enzyme content in enzymolysis liquid is 0.05-0.2%, and hydrolysis temperature is 40-50 DEG C, when enzymatic hydrolysis Between 2-6h, enzymolysis liquid pH control in 6.5-7；The immobilization magnetic coupling enzyme is recycled with magnet after enzymatic hydrolysis.
Blank is digested using immobilization magnetic coupling enzyme, since enzyme is supported on carrier in immobilization magnetic coupling enzyme On, the fixed protection of carrier is received, is not easy to be protected from environmental and reduce enzymatic activity, therefore enzymolysis efficiency is higher；Another party It face, only need to be using magnetic field by immobilization magnetic coupling after the completion of enzymatic hydrolysis containing magnetic nuclear particle in immobilization magnetic coupling enzyme Enzyme is assembled, and is then separated and recovered, not only convenient separation, but also immobilization magnetic coupling enzyme can reuse, drop Low cost.It needs to carry out high temperature enzyme deactivation to enzymolysis liquid after enzymatic hydrolysis in conventional method, and for fish oil, high-temperature process In will lead to fish oil denaturation cracking, cause effective component to be lost, nutritive value decline.The method of the present invention is not necessarily to high temperature enzyme deactivation Journey can utmostly retain fish oil effective component.
In addition, the carrier in immobilization magnetic coupling enzyme of the invention, has complicated three-dimensional net structure, have very high Voidage, therefore adsorptivity is very strong, not only good to enzyme immobilizatio effect, but also while enzymatic hydrolysis, can be in fish Raw meat substance (amine substance) and pigment in dirty are adsorbed, so that fish oil is decolourized, taken off simultaneously in enzymolysis process Raw meat processing, a step are completed, and carry out relevant treatment again without subsequent, therefore the preparation efficiency of fish oil is higher.
C, to step b treated enzymolysis liquid filtering and removing slag, layering, isolated upper layer fish oil and lower layer's oil are then allowed to stand Water mixed liquid.
In this step, the fish oil purity on upper layer is very high, can directly be separated, and in the oil water mixture of lower layer, The stirring in presence and enzymolysis process, oscillation due to emulsion, form relatively stable oil-in-water emulsion systems, quiet It sets, centrifugal treating can not effectively separate grease.
D, the oil-water mixture is transferred in foam fraction factor column, is ventilated to the bottom of the foam fraction factor column, Oil-water mixture upper layer generates froth bed, and froth bed is separated with liquid in time；Wherein, Ventilation Rate 2-4L/min, The processing time is 10-30min, and oil-water mixture temperature is 20-30 DEG C, and oil-water mixture pH is controlled in 6-7.
Foam fraction factor is carried out to oil-water mixture, in the foaming process of foam fraction factor, due to emulsifying in oil-water mixture Substance has very strong surface tension, and the surface of foam is gas-liquid separation interface, therefore emulsifier can be gathered in foam table Face is collected separation to foam, so as to separate emulsifier from oil-water mixture.When in oil-water mixture After the content of emulsifier substantially reduces, the oil-in-water system in oil-water mixture is disintegrated, and water-oil separating difficulty substantially reduces.
E, by step d, treated that oil-water mixture is centrifuged, and obtains upper layer fish oil.
F, the upper layer fish oil for obtaining step c and step e mixes, and obtains fish oil.
Fish oil processing method of the invention, not only simple process, but also from the oil-water mixture for capableing of lower layer further Fish oil is extracted, the recovery rate of fish oil is higher, and fish oil purity is also higher, and without fishy smell, color is transparent pure.
Preferably, before carrying out step b, the blank is pre-processed into crossing: in excessive temperature being 30-40 DEG C by blank Water in dipping swelling 1-2h.
Dipping swelling treatment is carried out to blank before enzymatic hydrolysis, cell membrane is enabled to be in the state that swells, cell membrane more holds It is fragile, to be conducive to digest.
Preferably, while digesting to blank, carrying out supersonic oscillations processing to enzymolysis liquid in step b.? Supersonic oscillations processing is carried out in enzymolysis process, can speed up the breakage of cell membrane, improves enzymolysis efficiency.But it also brings simultaneously Disadvantage: supersonic oscillations processing can reinforce the emulsifying effectiveness of enzymolysis liquid, so that water-oil separating difficulty increases, but pass through this hair The foam fraction factor technique of bright subsequent process is able to solve this problem.
Preferably, the immobilization magnetic coupling enzyme the preparation method comprises the following steps: dissolving the chitosan in the second of 8-12wt% In acid solution, the chitosan solution that concentration is 2-3wt% is made；Composite aerogel particle and four oxygen are added into chitosan solution Change three iron particles, mixing suspension is made；Wherein, the quality of composite aerogel particle is 0.5-1.5 times of chitosan, four oxidations The quality of three iron particles is 0.5-1 times of chitosan；The department that quality is mixing suspension 3-5% is added dropwise into mixing suspension Disk -80 simultaneously carries out ultrasonic wave dispersion and emulsion, and then first addition volume is mixing suspension 0.1-0.3% in backward mixing suspension Glutaraldehyde and volume be 0.5-1 times of mixing suspension 4wt% sodium hydroxide solution and stir evenly, then use magnet into After separating liquid, Magnetic Microspheres-Carrier is made in row absorption after being cleaned, being freeze-dried to solid matter；The magnetism is micro- Balloon borne body is dispersed in the solution that complex enzyme content is 0.1-0.3wt%, and 1-3h is stirred at 25-35 DEG C, forms immobilization magnetic Property complex enzyme, with magnet by immobilization magnetic coupling enzyme adsorbing separation, cleaning, drying；Wherein, the quality of Magnetic Microspheres-Carrier is 0.1-0.4 times of complex enzyme quality.
The Magnetic Microspheres-Carrier of the method for the present invention preparation, by chitosan, composite aerogel particle and ferroso-ferric oxide particle Carry out it is compound, using ferroso-ferric oxide particle as magnetic core, with chitosan be coating carrier, composite aerogel particle be compound " inlaying " in chitosan, after the crosslinking by glutaraldehyde, compound fastness is higher, recently after the activation of sodium hydroxide, The Magnetic Microspheres-Carrier of formation has coating property well to enzyme material, and itself has very high porosity, can be right Raw meat substance, pigment, heavy metal ion in enzymolysis liquid are effectively adsorbed, and adsorption rate is high, and adsorption capacity is big, so as to one Step realizes enzymatic hydrolysis, deodorant, decolorization, improves extraction efficiency.
Preferably, the composite aerogel particle the preparation method comprises the following steps: by furfural, water soluble phenol resin, sepiolite Powder and water 4-6:1:0.4-0.6:100 in mass ratio mixing, obtain mixed liquor after mixing evenly, are by concentration under agitation The ammonium hydroxide of 0.5mol/L is added drop-wise in mixed liquor until mixed liquor is in neutrality；Then 10-20h is reacted at 55-65 DEG C, is answered Close charcoal colloidal sol；Activated carbon composite colloidal sol is mixed with TiO 2 sol 1:0.5-1.5 in mass ratio, obtains mixing after mixing evenly molten Glue, after mixed sols is stood aging 1-2 days at room temperature, first with dehydrated alcohol to mixed sols solvent displacement 12-24h, then Solvent displacement 6-12h is carried out to mixed sols with n-hexane, plural gel is made after removing n-hexane；Finally use carbon dioxide Supercritical fluid, which carries out crushing after being dried plural gel, obtains composite aerogel particle.
The composite aerogel particle of the method for the present invention preparation is charcoal/sepiolite/titanium dioxide composite aerogel, the compound gas Gel possesses the porosity of superelevation, and pore-size is different, distribution is wide, can adsorb to different substances, and adsorption efficiency is high, Deodorant, decoloration effectively can be carried out to enzymolysis liquid.And there is preferable hydrophily, fish oil will not be adsorbed.
Preferably, the complex enzyme is the mixture of neutral proteinase, trypsase and papain.Compound protein Enzyme can greatly improve enzymolysis efficiency.
Preferably, the mass ratio of the neutral proteinase, trypsase and papain is 1:1-2:1.
Preferably, adding the sodium chloride that quality is enzymolysis liquid 4-6wt% into enzymolysis liquid in step b.Sodium chloride adds Enter the separating degree that can increase grease, so that grease is more easily separated.
Preferably, the internal diameter of the foam fraction factor column is 40-50mm, the loading of oil water mixture is high in foam fraction factor column Degree is 40-50cm.The specification of foam fraction factor column of the invention is to can be improved bubble according to the specific setting of fish internal organ enzymolysis liquid Foam separative efficiency, farthest isolates emulsifier.
It is compared with the prior art, the beneficial effects of the present invention are: the present invention proposes the processing method simple process of fish oil Take efficiency and recovery rate high, and the fish oil purity is high that processing obtains, no fishy smell, color are pure.
Specific embodiment
The present invention will be further described with reference to the examples below.
Embodiment 1
Early period reagent preparation:
The preparation of composite aerogel particle: by furfural, water soluble phenol resin, sepiolite powder and water 5:1 in mass ratio: 0.5:100 mixing, obtains mixed liquor after mixing evenly, and the ammonium hydroxide that concentration is 0.5mol/L is added drop-wise to mixing under agitation Until mixed liquor is in neutrality in liquid；Then 15h is reacted at 60 DEG C, obtains activated carbon composite colloidal sol；By activated carbon composite colloidal sol and titanium dioxide Titanium colloidal sol 1:1 in mass ratio mixing, obtains mixed sols after mixing evenly, mixed sols is stood to aging 1.5 days at room temperature Afterwards, first with dehydrated alcohol to mixed sols solvent displacement 18h, then with n-hexane solvent displacement 9h is carried out to mixed sols, removed Plural gel is made after n-hexane；It is crushed i.e. after being finally dried using Co 2 supercritical fluid to plural gel Composite aerogel particle is made.
The preparation of immobilization magnetic coupling enzyme: dissolving the chitosan in the acetic acid solution of 10wt%, and obtained concentration is The chitosan solution of 2.5wt%；Composite aerogel particle and ferroso-ferric oxide particle are added into chitosan solution, and mixing is made Suspension；Wherein, the quality of composite aerogel particle is 1 times of chitosan, and the quality of ferroso-ferric oxide particle is chitosan 0.75 times；The Arlacel-80 that quality is mixing suspension 4% is added dropwise into mixing suspension and carries out ultrasonic wave dispersion and emulsion, so First addition volume is the glutaraldehyde of mixing suspension 0.2% in backward mixing suspension afterwards and volume is 0.75 times of mixing suspension 4wt% sodium hydroxide solution and stir evenly, then adsorbed with magnet, separate liquid after, to solid matter carry out Magnetic Microspheres-Carrier is made after cleaning, freeze-drying；It is 0.2wt%'s that the Magnetic Microspheres-Carrier, which is dispersed in complex enzyme content, In solution, stir 2h at 30 DEG C, form immobilization magnetic coupling enzyme, with magnet by immobilization magnetic coupling enzyme adsorbing separation, Cleaning, drying；Wherein, the quality of Magnetic Microspheres-Carrier is 0.25 times of complex enzyme quality.
Wherein, the complex enzyme is the mixture of neutral proteinase, trypsase and papain, and neutral protein The mass ratio of enzyme, trypsase and papain is 1:1.5:1.
A kind of exquisite processing method of fish oil, sequentially includes the following steps:
A, cleaning impurity elimination is carried out to fish internal organ, smashed to pieces, blank is made, by blank in the water that excessive temperature is 35 DEG C Dipping is swollen 1.5h, then spare.
B, the blank is added in the enzymolysis liquid containing immobilization magnetic coupling enzyme, under the conditions of supersonic oscillations into Row enzymatic hydrolysis, wherein blank, enzymolysis liquid mass ratio be 1:3, the enzyme content in enzymolysis liquid is 0.125%, and hydrolysis temperature is 45 DEG C, Enzymolysis time 4h, enzymolysis liquid pH are controlled in 6.5-7；The immobilization magnetic coupling enzyme is recycled with magnet after enzymatic hydrolysis.
C, to step b treated enzymolysis liquid filtering and removing slag, layering, isolated upper layer fish oil and lower layer's oil are then allowed to stand Water mixed liquid.
D, the oil-water mixture is transferred in foam fraction factor column, is ventilated to the bottom of the foam fraction factor column, Oil-water mixture upper layer generates froth bed, and froth bed is separated with liquid in time；Wherein, Ventilation Rate 3L/min, place The reason time is 20min, and oil-water mixture temperature is 25 DEG C, and oil-water mixture pH is controlled in 6-7.The internal diameter of the foam fraction factor column For 45mm, the loading height of oil water mixture is 45cm in foam fraction factor column.
E, by step d, treated that oil-water mixture is centrifuged, and obtains upper layer fish oil.
F, the upper layer fish oil for obtaining step c and step e mixes, and obtains fish oil.
Embodiment 2
Early period reagent preparation:
The preparation of composite aerogel particle: by furfural, water soluble phenol resin, sepiolite powder and water 4:1 in mass ratio: 0.4:100 mixing, obtains mixed liquor after mixing evenly, and the ammonium hydroxide that concentration is 0.5mol/L is added drop-wise to mixing under agitation Until mixed liquor is in neutrality in liquid；Then 20h is reacted at 55 DEG C, obtains activated carbon composite colloidal sol；By activated carbon composite colloidal sol and titanium dioxide Titanium colloidal sol 1:0.5 in mass ratio mixing, obtains mixed sols after mixing evenly, mixed sols is stood to aging 1 day at room temperature Afterwards, first with dehydrated alcohol to mixed sols solvent displacement 12h, then with n-hexane solvent displacement 12h is carried out to mixed sols, removed Plural gel is made after n-hexane；It is crushed i.e. after being finally dried using Co 2 supercritical fluid to plural gel Composite aerogel particle is made.
The preparation of immobilization magnetic coupling enzyme: dissolving the chitosan in the acetic acid solution of 8wt%, and obtained concentration is The chitosan solution of 2wt%；Composite aerogel particle and ferroso-ferric oxide particle are added into chitosan solution, and it is outstanding that mixing is made Turbid；Wherein, the quality of composite aerogel particle is 0.5 times of chitosan, and the quality of ferroso-ferric oxide particle is chitosan 0.5 times；The Arlacel-80 that quality is mixing suspension 3% is added dropwise into mixing suspension and carries out ultrasonic wave dispersion and emulsion, then First addition volume is the glutaraldehyde of mixing suspension 0.1% in backward mixing suspension and volume is 0.5 times of mixing suspension The sodium hydroxide solution of 4wt% simultaneously stirs evenly, and is then adsorbed with magnet, after separating liquid, carries out to solid matter clear Magnetic Microspheres-Carrier is made after washing, being freeze-dried；It is the molten of 0.1wt% that the Magnetic Microspheres-Carrier, which is dispersed in complex enzyme content, In liquid, 3h is stirred at 25 DEG C, form immobilization magnetic coupling enzyme, with magnet by immobilization magnetic coupling enzyme adsorbing separation, clear It washes, dry；Wherein, the quality of Magnetic Microspheres-Carrier is 0.1 times of complex enzyme quality.
Wherein, the complex enzyme is the mixture of neutral proteinase, trypsase and papain, and neutral protein The mass ratio of enzyme, trypsase and papain is 1:1:1.
A kind of exquisite processing method of fish oil, sequentially includes the following steps:
A, cleaning impurity elimination is carried out to fish internal organ, smashed to pieces, blank is made, by blank in the water that excessive temperature is 30 DEG C Dipping is swollen 2h, then spare.
B, the blank is added in the enzymolysis liquid containing immobilization magnetic coupling enzyme, quality is added into enzymolysis liquid is The sodium chloride of enzymolysis liquid 4wt%.Digested under the conditions of supersonic oscillations, wherein blank, enzymolysis liquid mass ratio be 1: 2.5, the enzyme content in enzymolysis liquid is 0.05%, and hydrolysis temperature is 40 DEG C, enzymolysis time 6h, enzymolysis liquid pH controls in 6.5-7；Enzyme Xie Houyong magnet recycles the immobilization magnetic coupling enzyme.
C, to step b treated enzymolysis liquid filtering and removing slag, layering, isolated upper layer fish oil and lower layer's oil are then allowed to stand Water mixed liquid.
D, the oil-water mixture is transferred in foam fraction factor column, is ventilated to the bottom of the foam fraction factor column, Oil-water mixture upper layer generates froth bed, and froth bed is separated with liquid in time；Wherein, Ventilation Rate 2L/min, place The reason time is 30min, and oil-water mixture temperature is 20 DEG C, and oil-water mixture pH is controlled in 6-7.The internal diameter of the foam fraction factor column For 40mm, the loading height of oil water mixture is 40cm in foam fraction factor column.
E, by step d, treated that oil-water mixture is centrifuged, and obtains upper layer fish oil.
F, the upper layer fish oil for obtaining step c and step e mixes, and obtains fish oil.
Embodiment 3
Early period reagent preparation:
The preparation of composite aerogel particle: by furfural, water soluble phenol resin, sepiolite powder and water 6:1 in mass ratio: 0.6:100 mixing, obtains mixed liquor after mixing evenly, and the ammonium hydroxide that concentration is 0.5mol/L is added drop-wise to mixing under agitation Until mixed liquor is in neutrality in liquid；Then 10h is reacted at 65 DEG C, obtains activated carbon composite colloidal sol；By activated carbon composite colloidal sol and titanium dioxide Titanium colloidal sol 1:1.5 in mass ratio mixing, obtains mixed sols after mixing evenly, mixed sols is stood to aging 2 days at room temperature Afterwards, first mixed sols solvent is replaced for 24 hours with dehydrated alcohol, then solvent displacement 6h is carried out to mixed sols with n-hexane, removed Plural gel is made after n-hexane；It is crushed i.e. after being finally dried using Co 2 supercritical fluid to plural gel Composite aerogel particle is made.
The preparation of immobilization magnetic coupling enzyme: dissolving the chitosan in the acetic acid solution of 12wt%, and obtained concentration is The chitosan solution of 3wt%；Composite aerogel particle and ferroso-ferric oxide particle are added into chitosan solution, and it is outstanding that mixing is made Turbid；Wherein, the quality of composite aerogel particle is 1.5 times of chitosan, and the quality of ferroso-ferric oxide particle is the 1 of chitosan Times；The Arlacel-80 that quality is mixing suspension 5% is added dropwise into mixing suspension and carries out ultrasonic wave dispersion and emulsion, then first Addition volume is the glutaraldehyde of mixing suspension 0.3% and the 4wt% that volume is 1 times of mixing suspension in backward mixing suspension Sodium hydroxide solution and stir evenly, then adsorbed with magnet, separate liquid after, solid matter is cleaned, is cold Dry rear obtained Magnetic Microspheres-Carrier is lyophilized；The Magnetic Microspheres-Carrier is dispersed in the solution that complex enzyme content is 0.3wt%, Stir 1h at 35 DEG C, form immobilization magnetic coupling enzyme, with magnet by immobilization magnetic coupling enzyme adsorbing separation, cleaning, do It is dry；Wherein, the quality of Magnetic Microspheres-Carrier is 0.4 times of complex enzyme quality.
Wherein, the complex enzyme is the mixture of neutral proteinase, trypsase and papain, and neutral protein The mass ratio of enzyme, trypsase and papain is 1:2:1.
A kind of exquisite processing method of fish oil, sequentially includes the following steps:
A, cleaning impurity elimination is carried out to fish internal organ, smashed to pieces, blank is made, by blank in the water that excessive temperature is 40 DEG C Dipping is swollen 1h, then spare.
B, the blank is added in the enzymolysis liquid containing immobilization magnetic coupling enzyme, quality is added into enzymolysis liquid is The sodium chloride of enzymolysis liquid 6wt%.Digested under the conditions of supersonic oscillations, wherein blank, enzymolysis liquid mass ratio be 1: 3.5, the enzyme content in enzymolysis liquid is 0.2%, and hydrolysis temperature is 50 DEG C, enzymolysis time 2h, enzymolysis liquid pH controls in 6.5-7；Enzyme Xie Houyong magnet recycles the immobilization magnetic coupling enzyme.
C, to step b treated enzymolysis liquid filtering and removing slag, layering, isolated upper layer fish oil and lower layer's oil are then allowed to stand Water mixed liquid.
D, the oil-water mixture is transferred in foam fraction factor column, is ventilated to the bottom of the foam fraction factor column, Oil-water mixture upper layer generates froth bed, and froth bed is separated with liquid in time；Wherein, Ventilation Rate 4L/min, place The reason time is 10min, and oil-water mixture temperature is 30 DEG C, and oil-water mixture pH is controlled in 6-7.The internal diameter of the foam fraction factor column For 50mm, the loading height of oil water mixture is 50cm in foam fraction factor column.
E, by step d, treated that oil-water mixture is centrifuged, and obtains upper layer fish oil.
F, the upper layer fish oil for obtaining step c and step e mixes, and obtains fish oil.
The recovery rate of fish oil made from embodiment 1-3, purity, fishy smell sense organ, color are as shown in the table:
Recovery rate 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 are as follows: without fishy smell 0, slightly fishy smell 1, fishy smell weaker 2, has fishy smell 3, fishy smell is general 4, fishy smell lays particular stress on 5, and fishy smell heavier 6, fishy smell weighs 7 very much.
Raw materials used in the present invention, equipment is unless otherwise noted the common raw material, equipment of this field；In the present invention Method therefor is unless otherwise noted the conventional method of this field.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way, it is all according to the present invention Technical spirit any simple modification, change and equivalent transformation to the above embodiments, still fall within the technology of the present invention side The protection scope of case.

Claims (7)

1. a kind of purification processing method of fish oil, it is characterised in that sequentially include the following steps:
A, cleaning impurity elimination is carried out to fish internal organ, smashed to pieces, blank is made；
B, the blank is added in the enzymolysis liquid containing immobilization magnetic coupling enzyme and is digested, matter is added into enzymolysis liquid Amount is the sodium chloride of enzymolysis liquid 4-6wt%；While digesting to blank, supersonic oscillations processing is carried out to enzymolysis liquid；Its Middle blank, enzymolysis liquid mass ratio be 1:2.5-3.5, the enzyme content in enzymolysis liquid is 0.05-0.2%, hydrolysis temperature 40-50 DEG C, enzymolysis time 2-6h, enzymolysis liquid pH are controlled in 6.5-7；The immobilization magnetic coupling enzyme is returned with magnet after enzymatic hydrolysis It receives；
C, to step b treated enzymolysis liquid filtering and removing slag, it is then allowed to stand layering, isolated upper layer fish oil and lower layer's grease are mixed Close liquid；
D, the oil-water mixture is transferred in foam fraction factor column, is ventilated to the bottom of the foam fraction factor column, grease Mixed liquor upper layer generates froth bed, and froth bed is separated with liquid in time；Wherein, Ventilation Rate 2-4L/min, processing Time is 10-30min, and oil-water mixture temperature is 20-30 DEG C, and oil-water mixture pH is controlled in 6-7；
E, by step d, treated that oil-water mixture is centrifuged, and obtains upper layer fish oil；
F, the upper layer fish oil for obtaining step c and step e mixes, and obtains fish oil.
2. a kind of purification processing method of fish oil as described in claim 1, which is characterized in that described before carrying out step b Blank is pre-processed into crossing: in excessive temperature being dipping swelling 1-2h in 30-40 DEG C of water by blank.
3. a kind of purification processing method of fish oil as described in claim 1, which is characterized in that the immobilization magnetic coupling Enzyme the preparation method comprises the following steps: dissolve the chitosan in the acetic acid solution of 8-12wt%, it is molten that the chitosan that concentration is 2-3wt% is made Liquid；Composite aerogel particle and ferroso-ferric oxide particle are added into chitosan solution, and mixing suspension is made；Wherein, compound The quality of aerogel particle is 0.5-1.5 times of chitosan, and the quality of ferroso-ferric oxide particle is 0.5-1 times of chitosan；To The Arlacel-80 that quality is mixing suspension 3-5% is added dropwise in mixing suspension and carries out ultrasonic wave dispersion and emulsion, it is then first backward Addition volume is the glutaraldehyde of mixing suspension 0.1-0.3% in mixing suspension and volume is 0.5-1 times of mixing suspension The sodium hydroxide solution of 4wt% simultaneously stirs evenly, and is then adsorbed with magnet, after separating liquid, carries out to solid matter clear Magnetic Microspheres-Carrier is made after washing, being freeze-dried；It is 0.1-0.3wt% that the Magnetic Microspheres-Carrier, which is dispersed in complex enzyme content, Solution in, stir 1-3h at 25-35 DEG C, form immobilization magnetic coupling enzyme, inhaled immobilization magnetic coupling enzyme with magnet Fufen is from, cleaning, dry；Wherein, the quality of Magnetic Microspheres-Carrier is 0.1-0.4 times of complex enzyme quality.
4. a kind of purification processing method of fish oil as claimed in claim 3, which is characterized in that the composite aerogel particle The preparation method comprises the following steps: furfural, water soluble phenol resin, sepiolite powder and water 4-6:1:0.4-0.6:100 in mass ratio are mixed Close, obtain mixed liquor after mixing evenly, under agitation by concentration be 0.5mol/L ammonium hydroxide be added drop-wise in mixed liquor until Mixed liquor is in neutrality；Then 10-20h is reacted at 55-65 DEG C, obtains activated carbon composite colloidal sol；By activated carbon composite colloidal sol and titanium dioxide Colloidal sol 1:0.5-1.5 in mass ratio mixing, obtains mixed sols after mixing evenly, mixed sols is stood to aging 1- at room temperature After 2 days, solvent displacement 6- first is carried out to mixed sols to mixed sols solvent displacement 12-24h, then with n-hexane with dehydrated alcohol Plural gel is made after removing n-hexane in 12h；Finally plural gel is dried using Co 2 supercritical fluid laggard Row crushes and obtains composite aerogel particle.
5. a kind of purification processing method of fish oil as claimed in claim 3, which is characterized in that the complex enzyme is neutral egg The mixture of white enzyme, trypsase and papain.
6. a kind of purification processing method of fish oil as claimed in claim 5, which is characterized in that the neutral proteinase, pancreas egg The mass ratio of white enzyme and papain is 1:1-2:1.
7. a kind of purification processing method of fish oil as described in claim 1, which is characterized in that the foam fraction factor column it is interior Diameter is 40-50mm, and the loading height of oil water mixture is 40-50cm in foam fraction factor column.
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