CN104388176A - 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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- C—CHEMISTRY; METALLURGY
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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 krill, more particularly, relate to a kind of method that aqueous enzymatic method prepares antarctic krill oil and microcapsule and low fluorine krill peptide.
Background technology
Krill (Euphausia superba) is that on the earth, quantity is maximum, multiplies one of the most successful single Biological resources.According to Food and Argriculture OrganizationFAO announce data, the biomass of krill is about 1.25-7.25 hundred million tons, year can amount of fishing more than 1,300 ten thousand tons, be important potential fishery resources.In recent years, along with the exhaustion gradually of worldwide traditional fishery resource, and the proposition of 200-nautical-mile exclusive economic zone, make krill resource huge in antarctic waters receive the concern of some sea going fisheries developed countries.China started from 2009 to carry out expedition to krill, and the amount of fishing of 2013 is more than 20,000 tons.Krill development of resources rises to national strategy.Antarctic krill oil is rich in phosphatide type polyunsaturated fatty acid and astaxanthin, has and suppresses liver fatization, antianaphylaxis, anti-oxidant, reducing blood-fat, hypoglycemic and Cardioprotective isoreactivity, have higher value of exploiting and utilizing.
The fat content of butt krill between 10-20%, the omega-3 polyunsaturated fatty acid that to be rich in DHA and EPA in shrimp sauce be representative.At present, to the exploitation of krill resource to utilize its protein, and still insufficient to the exploitation of antarctic krill oil, and antarctic krill oil product category is less.The main method that present stage extracts antarctic krill oil is solvent extraction method.When single organic solvent leaches, extraction efficiency is lower, and a kind of strong polar organic solvent of many employings and the lixiviate of a kind of weakly polar organic solvent collocation substep when lixiviate antarctic krill oil abroad, this method is called " two-step approach ".Although two-step approach can improve extracting efficiency, also there is the problems such as operating process is loaded down with trivial details, organic solvent usage quantity large, organic solvent is separated, recovery difficulty.In addition, the shrimp sauce that organic solvent extraction extracts generally needs high temperature when desolventizing, can destroy the structure of the thermo-sensitivity functional active components astaxanthin in the shrimp sauce of the South Pole, affect the quality of shrimp sauce.Except organic solvent extraction, also has a kind of extracting method of comparatively environmental protection, supercritical CO
2extraction process, can not with an organic solvent extract antarctic krill oil, but the shrimp sauce carried by this method is based on neutral grease such as triglyceride level, the content of polarity grease-phosphatide is very low, and the featured function composition of phosphatide antarctic krill oil exactly, therefore use supercritical CO merely
2extraction process is difficult to the abundant extraction realizing antarctic krill oil.The present invention utilizes a kind of green extraction method-aqueous enzymatic method equally, from full shrimp, extract antarctic krill oil and prepare its microcapsule and low fluorine krill peptide, this kind of method not with an organic solvent, environmental protection, no solvent residue, can extract the phosphatide in krill.Present method is environmental protection not only, krill can also be made full use of, and obtains antarctic krill oil, krill microcapsule and low fluorine krill peptide respectively, enriches the kind of krill oil product.
Summary of the invention
The object of the present invention is to provide a kind of aqueous enzymatic method to prepare the method for antarctic krill oil and microcapsule and low fluorine krill peptide, be intended to reach safety, environmental protection, flow process is simple, weight is stablized, the krill oil recovery rate that extracts is high advantage.
In order to achieve the above object, the invention provides a kind of method that aqueous enzymatic method prepares antarctic krill oil and microcapsule and low fluorine krill peptide, comprise the steps:
(S1) with South Pole krill raw material, thermal treatment 10-30min at 80 ~ 100 DEG C, homogenate; Or by krill (whole shrimp) directly homogenate, then secondary homogenate after thermal treatment 10-30min at 80 ~ 100 DEG C.Add the water of 1 ~ 4 times of weight by weight, stir.Regulate homogenate pH value to 8 ~ 10 with 1mol/L sodium hydroxide solution, add food grade Sumizyme MP (EC3.4.21.62), enzyme dosage is 250 ~ 1000U/g krill raw material, enzymolysis 0.5 ~ 1.5h at 40 ~ 60 DEG C of temperature.Enzymolysis solution is heated to boiling, and keeps boiling state 10 ~ 30min with inactivated proteases.Enzymolysis solution is cooled to 10 ~ 30 DEG C, centrifugal 10 ~ 30min under 8000 ~ 13500 × g centrifugal force.Enzymolysis solution after centrifugal can be divided into 4 layers, is respectively free oil layer+newborn layer I, water layer, newborn layer II, residual layer from top to bottom.Wherein, free oil layer+newborn layer I is close together, and boundary is not very clear, is defined as one deck.
(S2) free oil layer+newborn layer I and newborn layer II is collected, with it for core.Gum arabic and gelatin heating mixing solutions are wall material, by weight 1:1 ~ 1:4 by gum arabic and gelatin mixing, are dissolved in 40 ~ 60 DEG C of water of weight ratio 1 ~ 3 times, prepare the wall material aqueous solution; Core being joined weight ratio is in 1 ~ 3 times of wall material aqueous solution, dispersion and emulsion; The pH value 6.0 of adjustment emulsion, with trans-glutaminases (EC 2.3.2.13) for solidifying agent, high-pressure homogeneous 2 ~ 4 times of 25MPa after 100 ~ 120 DEG C of sterilization 10 ~ 20min; Homogenizing fluid is 150 ~ 180 DEG C in drying tower inlet temperature, and exhaust temperature is spray-dried obtained krill oil microcapsule under 80 ~ 90 DEG C of conditions.
(S3) water layer is by the ceramic membrane filter in 8000-10000Da molecular size range aperture, filtrate is at relative vacuum degree-0.05 ~-0.08Mpa, being concentrated into solid content at temperature 60 ~ 80 DEG C is 20%, be 150 ~ 180 DEG C through inlet temperature again, exhaust temperature is that the spraying dry under 80 ~ 90 DEG C of conditions obtains low fluorine krill Gly-His-Lys.
The antarctic krill oil that the inventive method is extracted and microcapsule and krill peptide, its oil recovery rate is more than 50%, and protein recovery is more than 40%; Phospholipid in lipid content detects through rod thin layer chromatography and reaches more than 40% of lipid; Krill Gly-His-Lys Oil repellent can lower than 300mg/kg; The embedding rate of krill microcapsule is more than 80%, microcapsule diameter less than 200 μm.
Technological innovation of the present invention is: have employed a kind of environment-friendly and green extracting method-aqueous enzymatic method, from full shrimp, extract antarctic krill oil and prepare its microcapsule and low fluorine krill peptide, this kind of method is not with an organic solvent, environmental protection, no solvent residue, can extract the phosphatide in krill.Both avoid the molten residual unsafe factor such as grade that solvent method causes, overcome again the incomplete problem of lipid composition extraction in supercritical fluid extraction.Not only environmental protection, can also be fully utilized krill, obtains antarctic krill oil, krill microcapsule and low fluorine krill peptide respectively, enriches the kind of krill oil product.The method safety, environmental protection, flow process is simple, and weight is stablized, and the krill oil recovery rate extracted is high.
Embodiment
The present invention is with South Pole krill raw material, and enzymolysis after thermal treatment, homogenate, the enzymolysis solution after centrifugal can be divided into 4 layers, is respectively free oil layer+newborn layer I, water layer, newborn layer II, residual layer from top to bottom.Collect free oil layer+newborn layer I and newborn layer II, with it for core, gum arabic and gelatin heating mixing solutions are wall material, obtain krill microcapsule after emulsification, homogeneous through spraying dry.Water layer is after ceramic membrane filter, and filtrate is through vacuum concentration, then spraying dry obtains low fluorine krill Gly-His-Lys.Specific examples is as follows:
Embodiment 1
(1) by krill (whole shrimp) at 100 DEG C of water-bath thermal treatment 30min, homogenate.
(2) add the water of 1 times by weight, stir.Regulate homogenate pH value to 8 with 1mol/L sodium hydroxide solution, add food grade Sumizyme MP (EC3.4.21.62), enzyme dosage is 250U/g krill raw material, enzymolysis 0.5h at 40 DEG C of temperature.Enzymolysis solution is heated to boiling, and keeps boiling state 10min with inactivated proteases.Enzymolysis solution is cooled to 10 DEG C, centrifugal 10min under 8000 × g centrifugal force.Enzymolysis solution after centrifugal can be divided into 4 layers, is respectively free oil layer+newborn layer I, water layer, newborn layer II, residual layer from top to bottom.Free oil layer+newborn the layer I of gained is 60.65 ± 2.07% with the oil recovery rate of newborn layer II, and phospholipids content accounts for 51.62 ± 1.08% of lipid.
(3) collect free oil layer+newborn layer I and newborn layer II, with it for core, gum arabic and gelatin heating mixing solutions are wall material, by weight 1:1 by gum arabic and gelatin mixing, are dissolved in 40 DEG C of water of weight ratio 1 times, prepare the wall material aqueous solution; Core being joined weight ratio is in 1 times of wall material aqueous solution, dispersion and emulsion; The pH value 6.0 of adjustment emulsion, with trans-glutaminases (EC 2.3.2.13) for solidifying agent, high-pressure homogeneous 2 times of 25MPa after 100 DEG C of sterilization 10min; Homogenizing fluid is 150 DEG C in drying tower inlet temperature, and exhaust temperature is that under 80 DEG C of conditions, spraying dry obtains krill microcapsule.The embedding rate of gained krill microcapsule is 81.85%, microcapsule diameter less than 200 μm.
(4) water layer is through the ceramic membrane filter in 8000nmDa molecular size range aperture, filtrate is at relative vacuum degree-0.05Mpa, being concentrated into solid content under temperature 60 C is 20%, be 150 DEG C through inlet temperature again, exhaust temperature is that the spraying dry under 80 DEG C of conditions obtains low fluorine krill Gly-His-Lys.In gained krill Gly-His-Lys, protein recovery reaches 41.38%, and Oil repellent is 286mg/kg.
Embodiment 2
(1) by krill (whole shrimp) at 100 DEG C of water-bath thermal treatment 30min, homogenate.
(2) add the water of 4 times by weight, stir.Regulate homogenate pH value to 10 with 1mol/L sodium hydroxide solution, add food grade Sumizyme MP (EC3.4.21.62), enzyme dosage is 1000U/g krill raw material, enzymolysis 2.5h at 60 DEG C of temperature.Enzymolysis solution is heated to boiling, and keeps boiling state 30min with inactivated proteases.Enzymolysis solution is cooled to 40 DEG C, centrifugal 30min under 13500 × g centrifugal force.Enzymolysis solution after centrifugal can be divided into 4 layers, is respectively free oil layer+newborn layer I, water layer, newborn layer II, residual layer from top to bottom.Free oil layer+newborn the layer I of gained is 61.51+0.58% with the oil recovery rate of newborn layer II, and phospholipids content accounts for 61.11 ± 0.89% of lipid.
(3) collect free oil layer+newborn layer I and newborn layer II, with it for core, gum arabic and gelatin heating mixing solutions are wall material, by weight 1:4 by gum arabic and gelatin mixing, are dissolved in 60 DEG C of water of weight ratio 3 times, prepare the wall material aqueous solution; Core being joined weight ratio is in 3 times of wall material aqueous solution, dispersion and emulsion; The pH value 6.0 of adjustment emulsion, with trans-glutaminases (EC 2.3.2.13) for solidifying agent, high-pressure homogeneous 4 times of 25MPa after 120 DEG C of sterilization 20min; Homogenizing fluid is 180 DEG C in drying tower inlet temperature, and exhaust temperature is that under 90 DEG C of conditions, spraying dry obtains krill microcapsule.The embedding rate of gained krill microcapsule is 82.33%, microcapsule diameter less than 200 μm.
(4) water layer is by the ceramic membrane filter in 10000Da molecular size range aperture, filtrate is at relative vacuum degree 0.08Mpa, being concentrated into solid content at temperature 80 DEG C is 20%, be 180 DEG C through inlet temperature again, exhaust temperature is that the spraying dry under 90 DEG C of conditions obtains low fluorine krill Gly-His-Lys.In gained krill Gly-His-Lys, the rate of recovery of peptide reaches 48.59%, and Oil repellent is 238ug/g butt.
Embodiment 3
(1) by krill (whole shrimp) at 100 DEG C of water-bath thermal treatment 30min, homogenate.
(2) add the water of 2 times by weight, stir.Regulate homogenate pH value to 9 with 1mol/L sodium hydroxide solution, add food grade Sumizyme MP (EC3.4.21.62), enzyme dosage is 750U/g krill raw material, enzymolysis 1.5h at 50 DEG C of temperature.Enzymolysis solution is heated to boiling, and keeps boiling state 20min with inactivated proteases.Enzymolysis solution is cooled to 20 DEG C, centrifugal 15min under 13500 × g centrifugal force.Enzymolysis solution after centrifugal can be divided into 4 layers, is respectively free oil layer+newborn layer I, water layer, newborn layer II, residual layer from top to bottom.Free oil layer+newborn the layer I of gained is 64.77 ± 0.12% with the oil recovery rate of newborn layer II, and phospholipids content accounts for 65.58 ± 1.02% of lipid.
(3) collect free oil layer+newborn layer I and newborn layer II, with it for core, gum arabic and gelatin heating mixing solutions are wall material, by weight 1:2 by gum arabic and gelatin mixing, are dissolved in 50 DEG C of water of weight ratio 2 times, prepare the wall material aqueous solution; Core being joined weight ratio is in 2 times of wall material aqueous solution, dispersion and emulsion; The pH value 6.0 of adjustment emulsion, with trans-glutaminases (EC 2.3.2.13) for solidifying agent, high-pressure homogeneous 3 times of 25MPa after 110 DEG C of sterilization 15min; Homogenizing fluid is 160 DEG C in drying tower inlet temperature, and exhaust temperature is that under 90 DEG C of conditions, spraying dry obtains krill microcapsule.The embedding rate of gained krill microcapsule is 86.86%, microcapsule diameter less than 200 μm.
(4) water layer is by the ceramic membrane filter in 10000Da molecular size range aperture, filtrate is at relative vacuum degree-0.06Mpa, being concentrated into solid content under temperature 70 C is 20%, be 160 DEG C through inlet temperature again, exhaust temperature is that the spraying dry under 90 DEG C of conditions obtains low fluorine krill Gly-His-Lys.In gained krill Gly-His-Lys, the rate of recovery of peptide reaches 49.57%, and Oil repellent is 228ug/g butt.
Embodiment 4
(1) by krill (whole shrimp) first homogenate, at 100 DEG C of water-bath thermal treatment 30min, secondary homogenate.
(2) add the water of 3 times by weight, stir.Regulate homogenate pH value to 9.5 with 1mol/L sodium hydroxide solution, add food grade Sumizyme MP (EC3.4.21.62), enzyme dosage is 1000U/g krill raw material, enzymolysis 1.0h at 40 DEG C of temperature.Enzymolysis solution is heated to boiling, and keeps boiling state 30min with the proteolytic enzyme that goes out.Enzymolysis solution is cooled to 25 DEG C, centrifugal 10min under 13500 × g centrifugal force.Enzymolysis solution after centrifugal can be divided into 4 layers, is respectively free oil layer+newborn layer I, water layer, newborn layer II, residual layer from top to bottom.Free oil layer+newborn the layer I of gained is 66.85 ± 0.77% with the oil recovery rate of newborn layer II, and phospholipids content accounts for 65.96 ± 1.27% of lipid.
(3) collect free oil layer+newborn layer I and newborn layer II, with it for core, gum arabic and gelatin heating mixing solutions are wall material, by weight 1:3 by gum arabic and gelatin mixing, are dissolved in 60 DEG C of water of weight ratio 3 times, prepare the wall material aqueous solution; Core being joined weight ratio is in 2 times of wall material aqueous solution, dispersion and emulsion; The pH value 6.0 of adjustment emulsion, with trans-glutaminases (EC 2.3.2.13) for solidifying agent, high-pressure homogeneous 3 times of 25MPa after 120 DEG C of sterilization 10min; Homogenizing fluid is 180 DEG C in drying tower inlet temperature, and exhaust temperature is that under 90 DEG C of conditions, spraying dry obtains krill microcapsule.The embedding rate of gained krill microcapsule is 87.04%, microcapsule diameter less than 200 μm.
(4) water layer is by the ceramic membrane filter in 10000Da molecular size range aperture, filtrate is at relative vacuum degree-0.08Mpa, being concentrated into solid content under temperature 60 C is 20%, be 180 DEG C through inlet temperature again, exhaust temperature is that the spraying dry under 90 DEG C of conditions obtains low fluorine krill Gly-His-Lys.In gained krill Gly-His-Lys, the rate of recovery of peptide reaches 48.96%, and Oil repellent is 230ug/g butt.
Embodiment 5
(1) by krill (whole shrimp) first homogenate, at 100 DEG C of water-bath thermal treatment 30min, secondary homogenate.
(2) add the water of 1 times by weight, stir.Regulate homogenate pH value to 8 with 1mol/L sodium hydroxide solution, add food grade Sumizyme MP (EC3.4.21.62), enzyme dosage is 1000U/g krill raw material, enzymolysis 1.5h at 40 DEG C of temperature.Enzymolysis solution is heated to boiling, and keeps boiling state 15min with inactivated proteases.Enzymolysis solution is cooled to 25 DEG C, under 13500 × g centrifugal force centrifugal 10min centrifugal after enzymolysis solution can be divided into 4 layers, be respectively free oil layer+newborn layer I, water layer, newborn layer II, residual layer from top to bottom.Free oil layer+newborn the layer I of gained is 67.69 ± 1.04% with the oil recovery rate of newborn layer II, and phospholipids content accounts for more than 66.01 ± 0.73% of lipid.
(3) collect free oil layer+newborn layer I and newborn layer II, with it for core, gum arabic and gelatin heating mixing solutions are wall material, by weight 1:4 by gum arabic and gelatin mixing, are dissolved in 60 DEG C of water of weight ratio 2 times, prepare the wall material aqueous solution; Core being joined weight ratio is in 2 times of wall material aqueous solution, dispersion and emulsion; The pH value 6.0 of adjustment emulsion, with trans-glutaminases (EC 2.3.2.13) for solidifying agent, high-pressure homogeneous 3 times of 25MPa after 120 DEG C of sterilization 10min; Homogenizing fluid is 180 DEG C in drying tower inlet temperature, and exhaust temperature is that under 90 DEG C of conditions, spraying dry obtains krill microcapsule.The embedding rate of gained krill microcapsule is 87.11%, microcapsule diameter less than 200 μm.
(4) water layer is by the ceramic membrane filter in 10000Da molecular size range aperture, filtrate is at relative vacuum degree-0.05Mpa, being concentrated into solid content under temperature 70 C is 20%, be 180 DEG C through inlet temperature again, exhaust temperature is that the spraying dry under 90 DEG C of conditions obtains low fluorine krill Gly-His-Lys.In gained krill Gly-His-Lys, the rate of recovery of peptide is 50.26%, and Oil repellent is 225ug/g butt.
Embodiment 6
(1) by krill (whole shrimp) first homogenate, at 100 DEG C of water-bath thermal treatment 30min, secondary homogenate.
(2) add the water of 4 times by weight, stir.Regulate homogenate pH value to 8 with 1mol/L sodium hydroxide solution, add food grade Sumizyme MP (EC3.4.21.62), enzyme dosage is 1000U/g krill raw material, enzymolysis 1.5h at 60 DEG C of temperature.Enzymolysis solution is heated to boiling, and keeps boiling state 30min with inactivated proteases.Enzymolysis solution is cooled to 30 DEG C, centrifugal 10min under 13500 × g centrifugal force.Enzymolysis solution after centrifugal can be divided into 4 layers, is respectively free oil layer+newborn layer I, water layer, newborn layer II, residual layer from top to bottom.Free oil layer+newborn the layer I of gained is 69.74 ± 0.96% with the oil recovery rate of newborn layer II, and phospholipids content accounts for 67.58 ± 0.46% of lipid.
(3) collect free oil layer+newborn layer I and newborn layer II, with it for core, gum arabic and gelatin heating mixing solutions are wall material, by weight 1:2 by gum arabic and gelatin mixing, are dissolved in 60 DEG C of water of weight ratio 2 times, prepare the wall material aqueous solution; Core being joined weight ratio is in 3 times of wall material aqueous solution, dispersion and emulsion; The pH value 6.0 of adjustment emulsion, with trans-glutaminases (EC 2.3.2.13) for solidifying agent, high-pressure homogeneous 3 times of 25MPa after 120 DEG C of sterilization 10min; Homogenizing fluid is 180 DEG C in drying tower inlet temperature, and exhaust temperature is that under 90 DEG C of conditions, spraying dry obtains krill microcapsule.The microencapsulated oil powder of gained krill microcapsule is 87.97%, and productive rate is 83.01%, and carrying capacity is 56.24%.
(4) by the ceramic membrane filter in 9000Da molecular size range aperture, filtrate is at relative vacuum degree-0.08Mpa, being concentrated into solid content under temperature 60 C is 20%, then is 180 DEG C through inlet temperature, and exhaust temperature is that the spraying dry under 90 DEG C of conditions obtains low fluorine krill Gly-His-Lys.In gained krill Gly-His-Lys, the rate of recovery of peptide is 48.46%, and Oil repellent is 216ug/g butt.
Embodiment 7
(1) by krill (whole shrimp) first homogenate, at 100 DEG C of water-bath thermal treatment 30min, secondary homogenate.
(2) add the water of 1 times by weight, stir.Regulate homogenate pH value to 8 with 1mol/L sodium hydroxide solution, add food grade Sumizyme MP (EC3.4.21.62), enzyme dosage is 1000U/g krill raw material, enzymolysis 1.5h at 60 DEG C of temperature.Enzymolysis solution is heated to boiling, and keeps boiling state 30min with inactivated proteases.Enzymolysis solution is cooled to 25 DEG C, centrifugal 10min under 13500 × g centrifugal force.Enzymolysis solution after centrifugal can be divided into 4 layers, is respectively free oil layer+newborn layer I, water layer, newborn layer II, residual layer from top to bottom.Free oil layer+newborn the layer I of gained is 70.21 ± 0.45% with the oil recovery rate of newborn layer II, and phospholipids content accounts for 68.04 ± 1.18% of lipid.
(3) collect free oil layer+newborn layer I and newborn layer II, with it for core, gum arabic and gelatin heating mixing solutions are wall material, by weight 1:2 by gum arabic and gelatin mixing, are dissolved in 60 DEG C of water of weight ratio 2 times, prepare the wall material aqueous solution; Core being joined weight ratio is in 2 times of wall material aqueous solution, dispersion and emulsion; The pH value 6.0 of adjustment emulsion, with trans-glutaminases (EC 2.3.2.13) for solidifying agent, high-pressure homogeneous 3 times of 25MPa after 100 DEG C of sterilization 20min; Homogenizing fluid is 180 DEG C in drying tower inlet temperature, and exhaust temperature is that under 80 DEG C of conditions, spraying dry obtains krill microcapsule.The embedding rate of gained krill microcapsule is 87.99%, microcapsule diameter less than 200 μm.
(4) water layer is by the ceramic membrane filter in 10000Da molecular size range aperture, filtrate is at relative vacuum degree-0.06Mpa, being concentrated into solid content at temperature 80 DEG C is 20%, be 180 DEG C through inlet temperature again, exhaust temperature is that the spraying dry under 80 DEG C of conditions obtains low fluorine krill Gly-His-Lys.In gained krill Gly-His-Lys, the rate of recovery of peptide reaches 50.66%, and Oil repellent is 202ug/g butt.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (1)
1. aqueous enzymatic method prepares a method for antarctic krill oil and microcapsule and low fluorine krill peptide, it is characterized in that, comprises the steps
(S1) take krill as raw material, thermal treatment 10-30min at 80 ~ 100 DEG C, homogenate; Or, by direct for krill homogenate, then at 80 ~ 100 DEG C thermal treatment 10-30min, secondary homogenate afterwards;
Add the water of 1 ~ 4 times of weight by weight, stir; With 1mol/L sodium hydroxide solution adjust ph to 8 ~ 10, add food grade Sumizyme MP EC3.4.21.62, enzyme dosage is 250 ~ 1000U/g krill raw material, enzymolysis 0.5 ~ 1.5h at 40 ~ 60 DEG C of temperature; Enzymolysis solution is heated to boiling, and keeps boiling state 10 ~ 30min with inactivated proteases; Enzymolysis solution is cooled to 10 ~ 30 DEG C, centrifugal 10 ~ 30min under 8000 ~ 13500 × g centrifugal force; Enzymolysis solution after centrifugal is divided into 4 layers, is respectively free oil layer+newborn layer I, water layer, newborn layer II, residual layer from top to bottom;
(S2) free oil layer+newborn layer I and newborn layer II is collected, with it for core; Gum arabic and gelatin heating mixing solutions are wall material, by weight 1:1 ~ 1:4 by gum arabic and gelatin mixing, are dissolved in 40 ~ 60 DEG C of water of weight ratio 1 ~ 3 times, prepare the wall material aqueous solution; Core being joined weight ratio is in 1 ~ 3 times of wall material aqueous solution, dispersion and emulsion; The pH value 6.0 of adjustment emulsion, with trans-glutaminases EC 2.3.2.13 for solidifying agent, high-pressure homogeneous 2 ~ 4 times of 25MPa after 100 ~ 120 DEG C of sterilization 10 ~ 20min; Homogenizing fluid is 150 ~ 180 DEG C in drying tower inlet temperature, and exhaust temperature is spray-dried obtained krill oil microcapsule under 80 ~ 90 DEG C of conditions;
(S3) water layer is by the ceramic membrane filter in 8000-10000Da molecular size range aperture, it is 20% that filtrate is concentrated into solid content at relative vacuum degree-0.05 ~-0.08Mpa, temperature 60 ~ 80 DEG C, be 150 ~ 180 DEG C through inlet temperature again, exhaust temperature is that the spraying dry under 80 ~ 90 DEG C of conditions obtains low fluorine krill Gly-His-Lys.
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