CN104388176B - Method for preparing euphausia superba oil, microcapsule of euphausia superba oil and low-fluorine euphausia superba peptide by using aqueous enzymatic method - Google Patents
Method for preparing euphausia superba oil, microcapsule of euphausia superba oil and low-fluorine euphausia superba peptide by using aqueous enzymatic method Download PDFInfo
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 30
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 27
- 239000011737 fluorine Substances 0.000 title claims abstract description 27
- 108090000765 processed proteins & peptides Proteins 0.000 title claims abstract description 20
- 238000006911 enzymatic reaction Methods 0.000 title claims abstract description 9
- 241000239370 Euphausia superba Species 0.000 title abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 29
- 239000000839 emulsion Substances 0.000 claims abstract description 24
- 238000010438 heat treatment Methods 0.000 claims abstract description 23
- 108010010803 Gelatin Proteins 0.000 claims abstract description 20
- 235000010489 acacia gum Nutrition 0.000 claims abstract description 20
- 239000001785 acacia senegal l. willd gum Substances 0.000 claims abstract description 20
- 229920000159 gelatin Polymers 0.000 claims abstract description 20
- 239000008273 gelatin Substances 0.000 claims abstract description 20
- 235000019322 gelatine Nutrition 0.000 claims abstract description 20
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000000919 ceramic Substances 0.000 claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- 239000012528 membrane Substances 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 238000001694 spray drying Methods 0.000 claims abstract description 8
- 241000239366 Euphausiacea Species 0.000 claims description 79
- 239000000243 solution Substances 0.000 claims description 38
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 210000000481 breast Anatomy 0.000 claims description 27
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 23
- 229940106134 krill oil Drugs 0.000 claims description 22
- 102000004190 Enzymes Human genes 0.000 claims description 18
- 108090000790 Enzymes Proteins 0.000 claims description 18
- MVORZMQFXBLMHM-QWRGUYRKSA-N Gly-His-Lys Chemical compound NCCCC[C@@H](C(O)=O)NC(=O)[C@@H](NC(=O)CN)CC1=CN=CN1 MVORZMQFXBLMHM-QWRGUYRKSA-N 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 18
- 108010038983 glycyl-histidyl-lysine Proteins 0.000 claims description 18
- 238000005119 centrifugation Methods 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 235000013305 food Nutrition 0.000 claims description 10
- 108091005658 Basic proteases Proteins 0.000 claims description 9
- 108091005804 Peptidases Proteins 0.000 claims description 9
- 239000004365 Protease Substances 0.000 claims description 9
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 230000001954 sterilising effect Effects 0.000 claims description 9
- 238000004659 sterilization and disinfection Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 102000035195 Peptidases Human genes 0.000 claims description 8
- 239000011162 core material Substances 0.000 abstract description 18
- 150000002632 lipids Chemical class 0.000 abstract description 11
- 238000000605 extraction Methods 0.000 abstract description 6
- 239000002904 solvent Substances 0.000 abstract description 5
- 239000000047 product Substances 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- 230000001804 emulsifying effect Effects 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 238000000194 supercritical-fluid extraction Methods 0.000 abstract description 2
- 230000002255 enzymatic effect Effects 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000413 hydrolysate Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 40
- 241000238557 Decapoda Species 0.000 description 16
- 150000003904 phospholipids Chemical class 0.000 description 12
- 238000011084 recovery Methods 0.000 description 12
- 239000000284 extract Substances 0.000 description 10
- 239000003960 organic solvent Substances 0.000 description 8
- 108060008539 Transglutaminase Proteins 0.000 description 7
- 230000001717 pathogenic effect Effects 0.000 description 7
- 102000003601 transglutaminase Human genes 0.000 description 7
- 230000007613 environmental effect Effects 0.000 description 6
- 235000015067 sauces Nutrition 0.000 description 6
- 230000002940 repellent Effects 0.000 description 4
- 239000005871 repellent Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- JEBFVOLFMLUKLF-IFPLVEIFSA-N Astaxanthin Natural products CC(=C/C=C/C(=C/C=C/C1=C(C)C(=O)C(O)CC1(C)C)/C)C=CC=C(/C)C=CC=C(/C)C=CC2=C(C)C(=O)C(O)CC2(C)C JEBFVOLFMLUKLF-IFPLVEIFSA-N 0.000 description 2
- 235000013793 astaxanthin Nutrition 0.000 description 2
- MQZIGYBFDRPAKN-ZWAPEEGVSA-N astaxanthin Chemical compound C([C@H](O)C(=O)C=1C)C(C)(C)C=1/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=CC1=C(C)C(=O)[C@@H](O)CC1(C)C MQZIGYBFDRPAKN-ZWAPEEGVSA-N 0.000 description 2
- 229940022405 astaxanthin Drugs 0.000 description 2
- 239000001168 astaxanthin Substances 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 235000019197 fats Nutrition 0.000 description 2
- 239000003495 polar organic solvent Substances 0.000 description 2
- 241000894007 species Species 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 1
- 230000003266 anti-allergic effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- -1 by weight 1:1~1:4 Substances 0.000 description 1
- 230000003293 cardioprotective effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- 235000020660 omega-3 fatty acid Nutrition 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
- 238000004809 thin layer chromatography Methods 0.000 description 1
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/043—Drying and spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
- B01J13/046—Making microcapsules or microballoons by physical processes, e.g. drying, spraying combined with gelification or coagulation
-
- 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
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P21/00—Preparation of peptides or proteins
- C12P21/06—Preparation of peptides or proteins produced by the hydrolysis of a peptide bond, e.g. hydrolysate products
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a method for preparing euphausia superba oil, a microcapsule of the euphausia superba oil and low-fluorine euphausia superba peptide by using an aqueous enzymatic method. The method comprises the following steps: thermally treating and homogenizing a euphausia superba raw material, subsequently performing enzymolysis and centrifuging, wherein the centrifuged enzymatic hydrolysate is divided into four layers, respectively including a free oil layer + an emulsion layer I, a water layer, an emulsion layer II and a residue layer from top to bottom; collecting the free oil layer + emulsion layer I and the emulsion layer II, taking the free oil layer + emulsion layer I and the emulsion layer II as core materials, heating and mixing Arabic gum and gelatin to obtain a mixed solution which is taken as a wall material, emulsifying, homogenizing and then performing spray-drying to obtain a euphausia superba microcapsule; filtering the water layer by a ceramic membrane, carrying out vacuum concentration on the filtrate and then spray-drying to obtain low-fluorine euphausia superba peptide powder. The method disclosed by the invention is green, friendly to environment and free of solvent residues, prevents unsafe factors such as solvent residues caused by a solvent method and overcomes the problem of incomplete extraction of lipid compositions in a supercritical fluid extraction method; moreover, the method disclosed by the invention is used for respectively preparing the euphausia superba oil, the euphausia superba microcapsule and the low-fluorine euphausia superba peptide, so that the variety of euphausia superba oil products is enriched.
Description
Technical field
The present invention relates to the deep process technology of Antarctic krill, more particularly, it relates to a kind of aqueous enzymatic method prepares Antarctic krill
Oil and its method for microcapsule and low fluorine Antarctic krill peptide.
Background technology
Antarctic krill (euphausia superba), is that on the earth, quantity is maximum, multiplies most successful single living resources
One of.The data announced according to FAO (Food and Agriculture Organization of the United Nation), hundred million tons of the Biomass about 1.25-7.25 of Antarctic krill, year can amount of fishing exist
More than 13000000 tons, be important potential fishery resources.In recent years, with the gradually exhaustion of worldwide traditional fishery resource, with
And the proposition of 200-nautical-mile exclusive economic zone, make huge Antarctic krill resource in antarctic waters be subject to some deep-sea fishings flourishing
The concern of country.China started Antarctic krill is carried out expedition from 2009, and the amount of fishing of 2013 is more than 20,000 tons.The South Pole
Krill development of resources has gone up as national strategy.Antarctic krill oil is rich in phosphatide type polyunsaturated fatty acid and astaxanthin, has
Suppression liver fatization, antiallergic, antioxidation, blood fat reducing, blood sugar lowering and Cardioprotective isoreactivity, have higher exploitation valency
Value.
The fat content of butt Antarctic krill, about between 10-20%, is rich in dha and epa as representative in shrimp sauce
Omega-3 polyunsaturated fatty acid.At present, to the exploitation of Antarctic krill resource with based on its protein, and to South Pole phosphorus
The exploitation of shrimp sauce are still insufficient, and antarctic krill oil product category is less.Extract the main method of antarctic krill oil at this stage
For solvent extraction method.When single organic solvent leaches, extraction efficiency is relatively low, abroad when extracting antarctic krill oil more than using a kind of
Highly polar organic solvent and a kind of weakly polar organic solvent collocation substep extract, and this method is referred to as " two-step method ".Though two-step method
So extracting efficiency can be improved, but there is also that operating process is loaded down with trivial details, organic solvent usage amount big, organic solvent separates, it is tired to reclaim
Difficult the problems such as.Additionally, the shrimp sauce that organic solvent extraction extracts generally requires high temperature in desolventizing, can destroy in the shrimp sauce of the South Pole
Thermal sensitivity functional active components astaxanthin structure, impact shrimp sauce quality.Except organic solvent extraction, also one kind is relatively
For the extracting method of environmental protection, supercritical co2Extraction, can not use organic solvent that antarctic krill oil is extracted,
But the shrimp sauce being carried with this method is based on the neutral fat such as triglyceride, the content of polarity oils and fatss phospholipid is very low, and phospholipid
The exactly featured function composition of antarctic krill oil, therefore merely using supercritical co2Extraction is difficult to realize Antarctic krill
The abundant extraction of oil.The present invention, also with a kind of green extraction method aqueous enzymatic method, extracts antarctic krill oil simultaneously from full shrimp
Prepare its microcapsule and low fluorine Antarctic krill peptide, this kind of method does not use organic solvent, environmental protection, no solvent residue, can be by
Phospholipid in Antarctic krill extracts.Antarctic krill can also be made full use of, obtain respectively by this method not only environmental protection
Antarctic krill oil, Antarctic krill microcapsule and low fluorine Antarctic krill peptide, the species of abundant krill oil product.
Content of the invention
It is an object of the invention to provide a kind of aqueous enzymatic method prepares antarctic krill oil and its microcapsule and low fluorine Antarctic krill
The method of peptide is it is intended to reach high excellent of the Antarctic krill oil recovery rate that safe and environment-friendly, flow process is simple, weight is stable, extract
Point.
In order to achieve the above object, the present invention provides a kind of aqueous enzymatic method to prepare antarctic krill oil and its microcapsule and low fluorine south
The method of pole krill peptide, comprises the steps:
(s1) with South Pole krill raw material, heat treatment 10-30min at 80～100 DEG C, homogenate；Or Antarctic krill is (whole
Shrimp) directly it is homogenized, more secondary homogenate after heat treatment 10-30min at 80～100 DEG C.Add the water of 1～4 times of weight by weight,
Stir.Adjust homogenate ph value to 8～10 with 1mol/l sodium hydroxide solution, add food stage alkaline protease
(ec3.4.21.62), enzyme dosage is 250～1000u/g krill raw material, digests 0.5～1.5h at a temperature of 40～60 DEG C.Enzymolysis
Liquid is heated to seething with excitement, and keeps fluidized state 10～30min with inactivated proteases.Enzymolysis solution is cooled to 10～30 DEG C, 8000
It is centrifuged 10～30min under～13500 × g centrifugal force.Enzymolysis solution after centrifugation can be divided into 4 layers, from top to bottom respectively free oil
Layer+newborn layer, water layer, newborn layer, residual layer.Wherein, free oil layer+breast layer is close together, and boundary is not very clear, limits
For one layer.
(s2) free oil layer+breast layer and newborn layer are collected, with it as core.Arabic gum and gelatin heating mixed solution
For wall material, by weight 1:1～1:4, arabic gum and gelatin are mixed, be dissolved in weight ratio in 1～3 times of 40～60 DEG C of water, system
Standby wall material aqueous solution；Core is added to weight than in 1～3 times of wall material aqueous solution, dispersion and emulsion；The ph value of adjustment emulsion
6.0, with T-5398 (ec 2.3.2.13) as firming agent, after 100～120 DEG C of sterilization 10～20min, 25mpa high pressure is equal
Matter 2～4 times；Homogenizing fluid drying tower inlet temperature be 150～180 DEG C, delivery temperature be 80～90 DEG C under the conditions of through spray dried
Dry prepared Antarctic krill oil microcapsule.
(s3) water layer is by the ceramic membrane filter in 8000-10000da molecular size range aperture, filtrate relative degree of vacuum-
0.05～-0.08mpa, being concentrated into solid content at 60～80 DEG C of temperature is 20%, then is 150～180 DEG C through inlet temperature,
Spray drying under the conditions of delivery temperature is 80～90 DEG C obtains low fluorine Antarctic krill Gly-His-Lys.
The inventive method extract antarctic krill oil and its microcapsule and Antarctic krill peptide, its oil recovery rate be 50% with
On, protein recovery is more than 40%；Phospholipid in lipid content reaches more than the 40% of lipid through rod thin layer chromatography detection；South
Pole krill Gly-His-Lys Oil repellent can be less than 300mg/kg；The embedding rate of Antarctic krill microcapsule is more than 80%, microcapsule diameter 200
Below μm.
The technological innovation of the present invention is: employs a kind of environment-friendly and green extracting method aqueous enzymatic method, extracts from full shrimp
Antarctic krill oil simultaneously prepares its microcapsule and low fluorine Antarctic krill peptide, and this kind of method does not use organic solvent, and environmental protection is no molten
Agent remains, and can extract the phospholipid in Antarctic krill.Both avoided the molten residual grade unsafe factor that solvent method causes, and gram
Take lipid composition in supercritical fluid extraction and extract incomplete problem.Not only environmental protection, can also be by Antarctic krill
It is fully utilized, obtain antarctic krill oil, Antarctic krill microcapsule and low fluorine Antarctic krill peptide, abundant krill oil product respectively
Species.The method safety, environmental protection, flow process is simple, and weight is stable, and the Antarctic krill oil recovery rate extracting is high.
Specific embodiment
The present invention, with South Pole krill raw material, digests after heat treatment, homogenate, the enzymolysis solution after centrifugation can be divided into 4 layers, by up to
It is respectively down free oil layer+breast layer, water layer, newborn layer, residual layer.Collect free oil layer+breast layer and newborn layer, with it as core
Material, arabic gum and gelatin heating mixed solution are wall material, through being spray-dried prepared Antarctic krill microcapsule after emulsifying, homogenizing.
, after ceramic membrane filter, filtrate is through concentrated in vacuo, then is spray-dried the low fluorine Antarctic krill Gly-His-Lys of acquisition for water layer.Instantiation is such as
Under:
Embodiment 1
(1) by Antarctic krill (whole shrimp) in 100 DEG C of water-bath heat treatment 30min, it is homogenized.
(2) add 1 times of water by weight, stir.Adjust homogenate ph value with 1mol/l sodium hydroxide solution to 8,
Add food stage alkaline protease (ec3.4.21.62), enzyme dosage is 250u/g krill raw material, digest at a temperature of 40 DEG C
0.5h.Enzymolysis solution is heated to seething with excitement, and keeps fluidized state 10min with inactivated proteases.Enzymolysis solution is cooled to 10 DEG C, 8000
It is centrifuged 10min under × g centrifugal force.Enzymolysis solution after centrifugation can be divided into 4 layers, from top to bottom respectively free oil layer+breast layer, water
Layer, newborn layer, residual layer.The free oil layer of gained+breast layer is 60.65 ± 2.07% with the oil recovery rate of newborn layer, phospholipid
Content accounts for the 51.62 ± 1.08% of lipid.
(3) free oil layer+breast layer and newborn layer are collected, with it as core, arabic gum and gelatin heating mixed solution are
Arabic gum and gelatin are mixed by weight 1:1, are dissolved in weight ratio in 1 times of 40 DEG C of water, prepare wall material aqueous solution by wall material；
Core is added to weight than in 1 times of wall material aqueous solution, dispersion and emulsion；The ph value 6.0 of adjustment emulsion, with transglutamin-ase 9
Enzyme (ec 2.3.2.13) is firming agent, 25mpa high pressure homogenize 2 times after 100 DEG C of sterilization 10min；Homogenizing fluid enters pathogenic wind-warm in drying tower
Spend for 150 DEG C, delivery temperature is spray-dried under the conditions of being 80 DEG C and Antarctic krill microcapsule is obtained.Gained Antarctic krill microcapsule
Embedding rate is 81.85%, below 200 μm of microcapsule diameter.
(4) ceramic membrane filter through 8000nmda molecular size range aperture for the water layer, filtrate in relative degree of vacuum -0.05mpa,
Being concentrated into solid content under temperature 60 C is 20%, then is 150 DEG C through inlet temperature, and delivery temperature is the spray under the conditions of 80 DEG C
Mist is dried and obtains low fluorine Antarctic krill Gly-His-Lys.In gained Antarctic krill Gly-His-Lys, protein recovery reaches 41.38%, and Oil repellent is
286mg/kg.
Embodiment 2
(1) by Antarctic krill (whole shrimp) in 100 DEG C of water-bath heat treatment 30min, it is homogenized.
(2) add 4 times of water by weight, stir.Adjust homogenate ph value with 1mol/l sodium hydroxide solution to 10,
Add food stage alkaline protease (ec3.4.21.62), enzyme dosage is 1000u/g krill raw material, digest at a temperature of 60 DEG C
2.5h.Enzymolysis solution is heated to seething with excitement, and keeps fluidized state 30min with inactivated proteases.Enzymolysis solution is cooled to 40 DEG C,
It is centrifuged 30min under 13500 × g centrifugal force.Enzymolysis solution after centrifugation can be divided into 4 layers, from top to bottom respectively free oil layer+breast layer
, water layer, newborn layer, residual layer.The free oil layer of gained+breast layer is 61.51+0.58% with the oil recovery rate of newborn layer,
Content of phospholipid accounts for the 61.11 ± 0.89% of lipid.
(3) free oil layer+breast layer and newborn layer are collected, with it as core, arabic gum and gelatin heating mixed solution are
Arabic gum and gelatin are mixed by weight 1:4, are dissolved in weight ratio in 3 times of 60 DEG C of water, prepare wall material aqueous solution by wall material；
Core is added to weight than in 3 times of wall material aqueous solutions, dispersion and emulsion；The ph value 6.0 of adjustment emulsion, with transglutamin-ase 9
Enzyme (ec 2.3.2.13) is firming agent, 25mpa high pressure homogenize 4 times after 120 DEG C of sterilization 20min；Homogenizing fluid enters pathogenic wind-warm in drying tower
Spend for 180 DEG C, delivery temperature is spray-dried under the conditions of being 90 DEG C and Antarctic krill microcapsule is obtained.Gained Antarctic krill microcapsule
Embedding rate is 82.33%, below 200 μm of microcapsule diameter.
(4) water layer is by the ceramic membrane filter in 10000da molecular size range aperture, filtrate in relative degree of vacuum 0.08mpa,
Being concentrated into solid content at 80 DEG C of temperature is 20%, then is 180 DEG C through inlet temperature, and delivery temperature is the spray under the conditions of 90 DEG C
Mist is dried and obtains low fluorine Antarctic krill Gly-His-Lys.In gained Antarctic krill Gly-His-Lys, the response rate of peptide reaches 48.59%, and Oil repellent is
238ug/g butt.
Embodiment 3
(1) by Antarctic krill (whole shrimp) in 100 DEG C of water-bath heat treatment 30min, it is homogenized.
(2) add 2 times of water by weight, stir.Adjust homogenate ph value with 1mol/l sodium hydroxide solution to 9,
Add food stage alkaline protease (ec3.4.21.62), enzyme dosage is 750u/g krill raw material, digest at a temperature of 50 DEG C
1.5h.Enzymolysis solution is heated to seething with excitement, and keeps fluidized state 20min with inactivated proteases.Enzymolysis solution is cooled to 20 DEG C,
It is centrifuged 15min under 13500 × g centrifugal force.Enzymolysis solution after centrifugation can be divided into 4 layers, from top to bottom respectively free oil layer+breast layer
, water layer, newborn layer, residual layer.The free oil layer of gained+breast layer is 64.77 ± 0.12% with the oil recovery rate of newborn layer,
Content of phospholipid accounts for the 65.58 ± 1.02% of lipid.
(3) free oil layer+breast layer and newborn layer are collected, with it as core, arabic gum and gelatin heating mixed solution are
Arabic gum and gelatin are mixed by weight 1:2, are dissolved in weight ratio in 2 times of 50 DEG C of water, prepare wall material aqueous solution by wall material；
Core is added to weight than in 2 times of wall material aqueous solutions, dispersion and emulsion；The ph value 6.0 of adjustment emulsion, with transglutamin-ase 9
Enzyme (ec 2.3.2.13) is firming agent, 25mpa high pressure homogenize 3 times after 110 DEG C of sterilization 15min；Homogenizing fluid enters pathogenic wind-warm in drying tower
Spend for 160 DEG C, delivery temperature is spray-dried under the conditions of being 90 DEG C and Antarctic krill microcapsule is obtained.Gained Antarctic krill microcapsule
Embedding rate is 86.86%, below 200 μm of microcapsule diameter.
(4) water layer is by the ceramic membrane filter in 10000da molecular size range aperture, filtrate relative degree of vacuum-
0.06mpa, being concentrated into solid content under temperature 70 C is 20%, then is 160 DEG C through inlet temperature, and delivery temperature is 90 DEG C of bars
Spray drying under part obtains low fluorine Antarctic krill Gly-His-Lys.In gained Antarctic krill Gly-His-Lys, the response rate of peptide reaches 49.57%, and fluorine contains
Measure as 228ug/g butt.
Embodiment 4
(1) Antarctic krill (whole shrimp) is first homogenized, in 100 DEG C of water-bath heat treatment 30min, secondary homogenate.
(2) add 3 times of water by weight, stir.With 1mol/l sodium hydroxide solution adjust homogenate ph value to
9.5, add food stage alkaline protease (ec3.4.21.62), enzyme dosage is 1000u/g krill raw material, enzyme at a temperature of 40 DEG C
Solution 1.0h.Enzymolysis solution is heated to seething with excitement, and keeps fluidized state 30min with the protease that goes out.Enzymolysis solution is cooled to 25 DEG C,
It is centrifuged 10min under 13500 × g centrifugal force.Enzymolysis solution after centrifugation can be divided into 4 layers, from top to bottom respectively free oil layer+breast layer
, water layer, newborn layer, residual layer.The free oil layer of gained+breast layer is 66.85 ± 0.77% with the oil recovery rate of newborn layer,
Content of phospholipid accounts for the 65.96 ± 1.27% of lipid.
(3) free oil layer+breast layer and newborn layer are collected, with it as core, arabic gum and gelatin heating mixed solution are
Arabic gum and gelatin are mixed by weight 1:3, are dissolved in weight ratio in 3 times of 60 DEG C of water, prepare wall material aqueous solution by wall material；
Core is added to weight than in 2 times of wall material aqueous solutions, dispersion and emulsion；The ph value 6.0 of adjustment emulsion, with transglutamin-ase 9
Enzyme (ec 2.3.2.13) is firming agent, 25mpa high pressure homogenize 3 times after 120 DEG C of sterilization 10min；Homogenizing fluid enters pathogenic wind-warm in drying tower
Spend for 180 DEG C, delivery temperature is spray-dried under the conditions of being 90 DEG C and Antarctic krill microcapsule is obtained.Gained Antarctic krill microcapsule
Embedding rate is 87.04%, below 200 μm of microcapsule diameter.
(4) water layer is by the ceramic membrane filter in 10000da molecular size range aperture, filtrate relative degree of vacuum-
0.08mpa, being concentrated into solid content under temperature 60 C is 20%, then is 180 DEG C through inlet temperature, and delivery temperature is 90 DEG C of bars
Spray drying under part obtains low fluorine Antarctic krill Gly-His-Lys.In gained Antarctic krill Gly-His-Lys, the response rate of peptide reaches 48.96%, and fluorine contains
Measure as 230ug/g butt.
Embodiment 5
(1) Antarctic krill (whole shrimp) is first homogenized, in 100 DEG C of water-bath heat treatment 30min, secondary homogenate.
(2) add 1 times of water by weight, stir.Adjust homogenate ph value with 1mol/l sodium hydroxide solution to 8,
Add food stage alkaline protease (ec3.4.21.62), enzyme dosage is 1000u/g krill raw material, digest at a temperature of 40 DEG C
1.5h.Enzymolysis solution is heated to seething with excitement, and keeps fluidized state 15min with inactivated proteases.Enzymolysis solution is cooled to 25 DEG C,
Enzymolysis solution after centrifugation 10min centrifugation under 13500 × g centrifugal force can be divided into 4 layers, respectively free oil layer+breast layer from top to bottom
, water layer, newborn layer, residual layer.The free oil layer of gained+breast layer is 67.69 ± 1.04% with the oil recovery rate of newborn layer,
Content of phospholipid accounts for more than the 66.01 ± 0.73% of lipid.
(3) free oil layer+breast layer and newborn layer are collected, with it as core, arabic gum and gelatin heating mixed solution are
Arabic gum and gelatin are mixed by weight 1:4, are dissolved in weight ratio in 2 times of 60 DEG C of water, prepare wall material aqueous solution by wall material；
Core is added to weight than in 2 times of wall material aqueous solutions, dispersion and emulsion；The ph value 6.0 of adjustment emulsion, with transglutamin-ase 9
Enzyme (ec 2.3.2.13) is firming agent, 25mpa high pressure homogenize 3 times after 120 DEG C of sterilization 10min；Homogenizing fluid enters pathogenic wind-warm in drying tower
Spend for 180 DEG C, delivery temperature is spray-dried under the conditions of being 90 DEG C and Antarctic krill microcapsule is obtained.Gained Antarctic krill microcapsule
Embedding rate is 87.11%, below 200 μm of microcapsule diameter.
(4) water layer is by the ceramic membrane filter in 10000da molecular size range aperture, filtrate relative degree of vacuum-
0.05mpa, being concentrated into solid content under temperature 70 C is 20%, then is 180 DEG C through inlet temperature, and delivery temperature is 90 DEG C of bars
Spray drying under part obtains low fluorine Antarctic krill Gly-His-Lys.In gained Antarctic krill Gly-His-Lys, the response rate of peptide is 50.26%, and fluorine contains
Measure as 225ug/g butt.
Embodiment 6
(1) Antarctic krill (whole shrimp) is first homogenized, in 100 DEG C of water-bath heat treatment 30min, secondary homogenate.
(2) add 4 times of water by weight, stir.Adjust homogenate ph value with 1mol/l sodium hydroxide solution to 8,
Add food stage alkaline protease (ec3.4.21.62), enzyme dosage is 1000u/g krill raw material, digest at a temperature of 60 DEG C
1.5h.Enzymolysis solution is heated to seething with excitement, and keeps fluidized state 30min with inactivated proteases.Enzymolysis solution is cooled to 30 DEG C,
It is centrifuged 10min under 13500 × g centrifugal force.Enzymolysis solution after centrifugation can be divided into 4 layers, from top to bottom respectively free oil layer+breast layer
, water layer, newborn layer, residual layer.The free oil layer of gained+breast layer is 69.74 ± 0.96% with the oil recovery rate of newborn layer,
Content of phospholipid accounts for the 67.58 ± 0.46% of lipid.
(3) free oil layer+breast layer and newborn layer are collected, with it as core, arabic gum and gelatin heating mixed solution are
Arabic gum and gelatin are mixed by weight 1:2, are dissolved in weight ratio in 2 times of 60 DEG C of water, prepare wall material aqueous solution by wall material；
Core is added to weight than in 3 times of wall material aqueous solutions, dispersion and emulsion；The ph value 6.0 of adjustment emulsion, with transglutamin-ase 9
Enzyme (ec 2.3.2.13) is firming agent, 25mpa high pressure homogenize 3 times after 120 DEG C of sterilization 10min；Homogenizing fluid enters pathogenic wind-warm in drying tower
Spend for 180 DEG C, delivery temperature is spray-dried under the conditions of being 90 DEG C and Antarctic krill microcapsule is obtained.Gained Antarctic krill microcapsule
Microencapsulated oil powder is 87.97%, and yield is 83.01%, and carrying capacity is 56.24%.
(4) pass through the ceramic membrane filter in 9000da molecular size range aperture, filtrate is in relative degree of vacuum -0.08mpa, temperature
Being concentrated into solid content at 60 DEG C is 20%, then is 180 DEG C through inlet temperature, and delivery temperature is the spray dried under the conditions of 90 DEG C
The low fluorine Antarctic krill Gly-His-Lys of dry acquisition.In gained Antarctic krill Gly-His-Lys, the response rate of peptide is 48.46%, and Oil repellent is 216ug/g
Butt.
Embodiment 7
(1) Antarctic krill (whole shrimp) is first homogenized, in 100 DEG C of water-bath heat treatment 30min, secondary homogenate.
(2) add 1 times of water by weight, stir.Adjust homogenate ph value with 1mol/l sodium hydroxide solution to 8,
Add food stage alkaline protease (ec3.4.21.62), enzyme dosage is 1000u/g krill raw material, digest at a temperature of 60 DEG C
1.5h.Enzymolysis solution is heated to seething with excitement, and keeps fluidized state 30min with inactivated proteases.Enzymolysis solution is cooled to 25 DEG C,
It is centrifuged 10min under 13500 × g centrifugal force.Enzymolysis solution after centrifugation can be divided into 4 layers, from top to bottom respectively free oil layer+breast layer
, water layer, newborn layer, residual layer.The free oil layer of gained+breast layer is 70.21 ± 0.45% with the oil recovery rate of newborn layer,
Content of phospholipid accounts for the 68.04 ± 1.18% of lipid.
(3) free oil layer+breast layer and newborn layer are collected, with it as core, arabic gum and gelatin heating mixed solution are
Arabic gum and gelatin are mixed by weight 1:2, are dissolved in weight ratio in 2 times of 60 DEG C of water, prepare wall material aqueous solution by wall material；
Core is added to weight than in 2 times of wall material aqueous solutions, dispersion and emulsion；The ph value 6.0 of adjustment emulsion, with transglutamin-ase 9
Enzyme (ec 2.3.2.13) is firming agent, 25mpa high pressure homogenize 3 times after 100 DEG C of sterilization 20min；Homogenizing fluid enters pathogenic wind-warm in drying tower
Spend for 180 DEG C, delivery temperature is spray-dried under the conditions of being 80 DEG C and Antarctic krill microcapsule is obtained.Gained Antarctic krill microcapsule
Embedding rate is 87.99%, below 200 μm of microcapsule diameter.
(4) water layer is by the ceramic membrane filter in 10000da molecular size range aperture, filtrate relative degree of vacuum-
0.06mpa, being concentrated into solid content at 80 DEG C of temperature is 20%, then is 180 DEG C through inlet temperature, and delivery temperature is 80 DEG C of bars
Spray drying under part obtains low fluorine Antarctic krill Gly-His-Lys.In gained Antarctic krill Gly-His-Lys, the response rate of peptide reaches 50.66%, and fluorine contains
Measure as 202ug/g butt.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope of present disclosure, technology according to the present invention scheme and its
Inventive concept equivalent or change in addition, all should be included within the scope of the present invention.
Claims (1)
1. a kind of aqueous enzymatic method prepares the method for antarctic krill oil and its microcapsule and low fluorine Antarctic krill peptide it is characterised in that wrapping
Include following steps
(s1) with Antarctic krill as raw material, heat treatment 10-30min at 80～100 DEG C, homogenate；Or, Antarctic krill is direct
Homogenate, then heat treatment 10-30min at 80～100 DEG C, secondary homogenate afterwards；
Add the water of 1～4 times of weight by weight, stir；Adjust ph value with 1mol/l sodium hydroxide solution to 8～10, plus
Enter food stage alkaline protease ec3.4.21.62, enzyme dosage is 250～1000u/g krill raw material, enzyme at a temperature of 40～60 DEG C
Solution 0.5～1.5h；Enzymolysis solution is heated to seething with excitement, and keeps fluidized state 10～30min with inactivated proteases；Enzymolysis solution is cooled to
10～30 DEG C, it is centrifuged 10～30min under 8000～13500 × g centrifugal force；Enzymolysis solution after centrifugation is divided into 4 layers, from top to bottom
It is respectively free oil layer+breast layer, water layer, newborn layer, residual layer；
(s2) free oil layer+breast layer and newborn layer are collected, with it as core；Arabic gum and gelatin heating mixed solution are wall
Arabic gum and gelatin are mixed by weight 1:1～1:4, are dissolved in weight ratio in 1～3 times of 40～60 DEG C of water, prepare wall by material
Material aqueous solution；Core is added to weight than in 1～3 times of wall material aqueous solution, dispersion and emulsion；The ph value 6.0 of adjustment emulsion,
With T-5398 ec 2.3.2.13 as firming agent, 25mpa high pressure homogenize 2～4 after 100～120 DEG C of sterilization 10～20min
Secondary；Homogenizing fluid is 150～180 DEG C in drying tower inlet temperature, and delivery temperature is spray-dried under the conditions of being 80～90 DEG C to be obtained
Antarctic krill oil microcapsule；
(s3) water layer passes through the ceramic membrane filter in 8000-10000da molecular size range aperture, and filtrate is in relative degree of vacuum -0.05
Being concentrated into solid content at～-0.08mpa, 60～80 DEG C of temperature is 20%, then is 150～180 DEG C through inlet temperature, aerofluxuss
Spray drying under the conditions of temperature is 80～90 DEG C obtains low fluorine Antarctic krill Gly-His-Lys.
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| CN104824651B (en) * | 2015-05-25 | 2017-06-16 | 武汉志邦化学技术有限公司 | The krill oil microcapsule and its preparation technology of a kind of high content |
| CN105433293B (en) * | 2015-12-07 | 2017-04-05 | 中国海洋大学 | The krill shrimp gruel of enrichment phosphatide and its production method |
| CN107095312A (en) * | 2017-03-30 | 2017-08-29 | 大连大学 | A kind of krill polypeptide formulations with reducing blood lipid ability and preparation method thereof |
| CN107874257B (en) * | 2017-11-09 | 2021-05-07 | 大连工业大学 | Preparation method of euphausia superba oil nanoparticles with high embedding rate and small particle size |
| CN107663473B (en) * | 2017-11-14 | 2021-02-26 | 广东环境保护工程职业学院 | Krill oil extraction method |
| CN109349416A (en) * | 2018-12-01 | 2019-02-19 | 浙江海洋大学 | A method of albumen powder is made using South Pole squama shrimp |
| CN109880871A (en) * | 2019-04-18 | 2019-06-14 | 威海市宇王集团海洋生物工程有限公司 | A method of small-molecular peptides are extracted by raw material of euphausia superba powder |
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