CN102524510B - Preparation method of low-fluorine Euphasia superb protein base stock - Google Patents
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- 108090000623 proteins and genes Proteins 0.000 title claims abstract description 60
- 102000004169 proteins and genes Human genes 0.000 title claims abstract description 60
- 229910052731 fluorine Inorganic materials 0.000 title claims abstract description 25
- 239000011737 fluorine Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 87
- 238000003756 stirring Methods 0.000 claims abstract description 69
- 239000002244 precipitate Substances 0.000 claims abstract description 56
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000000751 protein extraction Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 117
- 238000005119 centrifugation Methods 0.000 claims description 64
- 241000239366 Euphausiacea Species 0.000 claims description 57
- 230000001105 regulatory effect Effects 0.000 claims description 39
- 238000002386 leaching Methods 0.000 claims description 38
- 241000239370 Euphausia superba Species 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 33
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 28
- 239000001110 calcium chloride Substances 0.000 claims description 28
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 28
- 238000001556 precipitation Methods 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 26
- 239000000843 powder Substances 0.000 claims description 20
- 238000004321 preservation Methods 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 9
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 abstract description 105
- 208000035404 Autolysis Diseases 0.000 abstract description 5
- 206010057248 Cell death Diseases 0.000 abstract description 5
- 239000000047 product Substances 0.000 abstract description 5
- 230000028043 self proteolysis Effects 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000029983 protein stabilization Effects 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
- 238000010257 thawing Methods 0.000 abstract 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 75
- 235000018102 proteins Nutrition 0.000 description 44
- 239000012071 phase Substances 0.000 description 13
- 241000238557 Decapoda Species 0.000 description 12
- 235000019750 Crude protein Nutrition 0.000 description 7
- 230000005012 migration Effects 0.000 description 4
- 238000013508 migration Methods 0.000 description 4
- 101710172711 Structural protein Proteins 0.000 description 3
- MBLBDJOUHNCFQT-LXGUWJNJSA-N aldehydo-N-acetyl-D-glucosamine Chemical compound CC(=O)N[C@@H](C=O)[C@@H](O)[C@H](O)[C@H](O)CO MBLBDJOUHNCFQT-LXGUWJNJSA-N 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000003809 water extraction Methods 0.000 description 3
- 150000001413 amino acids Chemical class 0.000 description 2
- 235000015278 beef Nutrition 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 235000020247 cow milk Nutrition 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000050 nutritive effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 235000021120 animal protein Nutrition 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 150000003904 phospholipids Chemical class 0.000 description 1
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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Abstract
The invention discloses a preparation method of low-fluorine Euphasia superb protein base stock. The preparation method comprises the following steps of: 1, low-temperature autolysis: homogenizing fresh and alive Euphasia superb and treating through ultraviolet irradiation to realize autolysis; 2, protein extraction: adding water into homogenate, stirring and extracting, carrying out centrifugal separation to obtain an upper-layer liquid phase and precipitates; 3, protein stabilization: refrigerating the upper-layer liquid for storage or drying the upper-layer liquid before refrigerating the upper-layer liquid for storage; 4, protein preparation: thawing the refrigerated upper-layer liquid; adjusting pH value to 4.8-5.8 or heating for 10-30 minutes at 80-100 DEG C and then centrifuging to obtain precipitate products and carrying out spray drying to finally obtain the Euphasia superb protein base stock. The preparation method is simple to operate and is quite suitable for field operation on a fishing ship; through adoption of the preparation method, the protein recovery rate is up to 46%-51% and the fat recovery rate is up to 54%-60%; and in the prepared low-fluorine Euphasia superb protein base stock, the protein content is 70-78%/100g of dry base stock, the fat content is 25-31g/100g of dry base stock and the fluorine content is lower than 1.5 mcg./g of dry base stock.
Description
Technical field
The present invention relates to utilize krill to prepare the method for albumen base-material.
Background technology
Krill (Euphausia superba) is single one of living resources of planting maximum on the earth, the estimated value of its standing crop is about 4～1,500,000,000 tons, ripe shrimp annual production is 3～500,000,000 tons, and year can reach 100,000,000 tons of left and right by quantity of the catch, forms huge 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 deep-sea fishing developed countries.China also lists krill resource in one of main exploitation kind of Development for Distant Water Fishery from now on.
In krill, containing 11.9% to 15.4% albumen (wet basis), is one of available maximum protein resource of the mankind that it has been established that.Krill is described as the mankind's protein resource treasure-house, and this is that not only protein content is high due to krill, and the nutritive value of protein is also high.The World Health Organization once marked the amino acid comprehensive nutrient value ratio of krill, prawn, cow's milk and beef, and result krill gets a mark of 100, beef 96 minutes, cow's milk 91 minutes, prawn 71 minutes.According to one's analysis, necessary 8 seed amino acids of human body, all have in krill, and account for altogether the more than 40% of protein content.Therefore, krill can be used as the important high-quality animal protein resource of the mankind and is used.
That the Antarctic Continent is located in is remote, krill needs long period transportation, preservation after fishing for.The fluorine that contains high concentration in krill shell can pollute shrimp to shrimp migration in preserving process, affects the security of shrimp protein product.Meanwhile, in krill, be rich in polyunsaturated fatty acid, easily putrid and deteriorated.Therefore, original quality that krill is fished for is need be rapidly freezing, ultralow temperature is preserved guarantee shrimp, the transportation preservation cost that this has improved krill greatly, becomes the bottleneck of restriction krill resources development and utilization.The problem that solves krill transportation, preservation difficulty, best bet is processed krill to prepare rapidly albumen exactly after fishing for, but still lacks the processing on ship preparation method of krill albumen at present.
Summary of the invention
The present invention aims to provide a kind of simple and easy method and after krill is fished for, makes immediately the method for Euphasia superb protein base stock, has low fluorine characteristic, is especially applicable to operating on dredger, can provide technical support for the exploitation of krill.
In order to achieve the above object, the invention discloses a kind of preparation method of low fluorine Euphasia superb protein base stock, it is characterized in that, in turn include the following steps:
Step1, low temperature self-dissolving: the fresh and alive krill of fishing for is drained to rear direct homogenate and obtain homogenate, by the ultraviolet treatment with irradiation of 0.5～1 meter of 20～40 watts of power, wavelength 200～300 nanometers, distance 5～10 minutes, afterwards described homogenate is placed at 0～4 ℃ to self-dissolving 0.1～1 hour.
Step2, protein extraction: the water to adding in described homogenate with 1～4 times of volume, mix, under 0～4 ℃ of condition, stirring and leaching is 5～15 minutes, centrifugation, upper phase and precipitating for the first time for the first time.
Step3, albumen preparation: described upper phase is for the first time passed through to regulate pH value to 4.8～5.8, or at 80～100 ℃, heat centrifugal method after 10～30 minutes, upper phase and precipitating for the second time for the second time, by described, precipitate for the second time the spray-dried Euphausia superba protein base materials that obtains.
Under optimal way, in step Step2, when adding water to homogenate, adding final concentration is 0.01%～0.03% calcium chloride, to promote protein to dissolve.In addition in step Step2, before centrifugation, regulate, pH value to 2～3.5 of homogenate.
In order to improve the quality of Euphausia superba protein base materials, for precipitation for the second time, spray again after can further purifying and be dried.Specifically, in step Step3, can in described precipitation for the second time, add the water of 2～4 times of volumes, mix, regulating pH of mixed value is 4.8～5.8, and centrifugation obtains for the third time upper phase and precipitates for the third time, and described precipitation for the third time after spray-dried obtain Euphausia superba protein base materials.
Under optimal way, in step Step3, can be on dredger, for the first time upper phase frozen in-15 to-25 ℃ or spray-dried after frozen in-15 to-25 ℃ of preservations after dry powder; Then be transported to operation room, again described frozen upper phase is for the first time melted or described frozen dry powder is dissolved in the water of 2～4 times of volumes and revert to liquid state, as the completing steps Step3 of upper phase for the first time and the subsequent step in above-mentioned steps Step3.
In order to improve the output of Euphausia superba protein base materials, in step Step2, to described precipitation for the first time, add 0～4 ℃ of water of 2～4 times of volumes, be uniformly mixed, under 0～4 ℃ of condition, stirring and leaching is 5～15 minutes, and centrifugation obtains the 4th upper phase and the 4th precipitation; Described in mixing for the first time upper phase and described the 4th upper phase as the upper phase for the first time of using in step Step3.
In above-mentioned steps, regulate pH value can select HCl or the NaOH of 1～6M.In addition in Step1, " draining " object is that the water that fresh and alive krill is adhered to is removed, and drains rear shrimp itself and still keeps fresh shrimp state.
The whole preparation process of the present invention all completes at 0～4 ℃, this temperature is the antarctic average ambient temperature of catching season, operating procedure all can aboard ship complete, it is advantageous that the strong feature of fresh and alive krill self-dissolving ability of having utilized, increase the autolysis of structural proteins, improve the yield of water-solubility protein.In fresh and alive krill, fluorine mainly concentrates on shrimp shell, not yet, to shrimp migration, now with water extraction, gets, and fluorine is mainly distributed in precipitation, lighter to the pollution of water-soluble crude protein.In addition, the spray-dried rear transportation of water-soluble krill crude protein, increases transport capacity, saves cost of transportation.The present invention has the following advantages:
1, the operating process the present invention relates to is simple, does not need complicated equipment, and whole preparation process all completes at 0～4 ℃, and this temperature is the antarctic average ambient temperature of catching season, is adapted at the enterprising line operate of dredger.
2, the present invention utilizes the strong feature of fresh and alive krill self-dissolving ability, increases the autolysis of structural proteins, improves the yield of water-solubility protein.
3, the present invention drains rear direct homogenate by the fresh and alive krill of fishing for and operates, because fluorine in fresh and alive krill mainly concentrates on shrimp shell, not yet, to shrimp migration, now with water extraction, get, fluorine is mainly distributed in precipitation, has greatly reduced the pollution to water-soluble crude protein.
4, method of the present invention relates to the freeze-drying of water-soluble krill crude protein or spray-dired step, has increased the transport capacity to krill crude protein, saves cost of transportation.
Method of the present invention is simple and effective: the crude protein rate of recovery that can make krill is 46%～51%, and the thick lipid rate of recovery is 54%～60%.The low-fluorine Euphausia superba protein base materials fluorine content of preparation is lower than 1.5ug/g; Be of high nutritive value, in product, protein content is 70～78g/100g butt, and fat content is 25～31g/100g butt, and content of phospholipid is 400～440mg/g; Purposes is wide, is applicable to industrial applications, and the present invention can provide technical support for effective utilization of krill.
In addition, according to the technological parameter of the inventive method, can enhance productivity, product purity and quality are better simultaneously, have higher economic benefit.
The specific embodiment
Disclosure of the invention a kind of processing on ship preparation method of low fluorine Euphasia superb protein base stock, in turn include the following steps:
1, low temperature self-dissolving: the fresh and alive krill of fishing for is drained to rear direct homogenate, by the ultraviolet treatment with irradiation of 0.5～1 meter of 20～40 watts of power, wavelength 200～300 nanometers, distance 5～10 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.1～1 hour afterwards.This step has been utilized the strong feature of fresh and alive krill self-dissolving ability, increases the autolysis of structural proteins, improves the yield of water-solubility protein.
2, protein extraction: 0～4 ℃ of water to adding in the homogenate after low temperature self-dissolving with 1～4 times of volume, mix, under 0～4 ℃ of condition, stirring and leaching is 5～15 minutes, centrifugation, upper phase and precipitating for the first time for the first time.Because fluorine in fresh and alive krill mainly concentrates on shrimp shell, not yet, to shrimp migration, now with water extraction, to get, fluorine is mainly distributed in precipitation, lighter to the pollution of water-soluble crude protein.
3, stabilize proteins: by the upper phase for the first time obtaining in step 2 directly frozen or spray-dried after frozen after dry powder.This step has increased transport capacity, and saves cost of transportation.
4, albumen preparation: the cryopreserving liquid obtaining in step 3 is melted or described frozen dry powder is dissolved in the water of 2～4 times of volumes, by regulating pH value to 4.8～5.8, or at 80～100 ℃, heat centrifugal method after 10～30 minutes, be precipitated the spray-dried Euphausia superba protein base materials that obtains.
In above-mentioned steps 2, when adding water to homogenate, adding final concentration is 0.010%～0.030% calcium chloride.By regulating pH value to 2～3.5 of homogenate, increase albumen yield.
In above-mentioned steps 4, prepare method of protein, different according to the product of step 3, there are specifically following four kinds of situations:
Method 1: after frozen liquid phase is melted, regulating pH value is 4.8～5.8, stirs and evenly mixs latter standing 5～15 minutes, and centrifugation obtains precipitate A; Water to adding 2～4 times of volumes in precipitate A, stirs and evenly mixs, and regulating pH of mixed value is 4.8～5.8, stirs and evenly mixs latter standing 5～15 minutes, and centrifugation obtains precipitate B; After precipitate B is spray-dried, obtain Euphausia superba protein base materials.
Method 2: after frozen liquid phase is melted, heat 10～30 minutes at 80～100 ℃, stir and evenly mix latter standing 5～15 minutes, centrifugation obtains precipitate A; After precipitate A is spray-dried, obtain Euphausia superba protein base materials.
Method 3: frozen dry powder is dissolved in to the water of 2～4 times of volumes, regulating pH value is 4.8～5.8, stirs and evenly mixs latter standing 5～15 minutes, and centrifugation obtains precipitate A; The water that adds 2～4 times of volumes to precipitate A, stirs and evenly mixs, and regulating pH of mixed value is 4.8～5.8, stirs and evenly mixs latter standing 5～15 minutes, and centrifugation obtains precipitate B; After precipitate B is spray-dried, obtain Euphausia superba protein base materials.
Method 4: frozen dry powder is dissolved in to the water of 2～4 times of volumes, heats 10～30 minutes at 80～100 ℃, stir and evenly mix latter standing 5～15 minutes, centrifugation obtains precipitate A; After precipitate A is spray-dried, obtain Euphausia superba protein base materials.
Embodiment 1: the present invention be take krill as raw material, adopts the extraction and separation technology of modern protein, prepared the processing on ship preparation technology of low-fluorine Euphausia superba protein base materials.Fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 2～4 times of volumes, by the ultraviolet treatment with irradiation of 0.5～1 meter of 20～40 watts of power, wavelength 200～300 nanometers, distance 5～10 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.1～1 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.01%～0.03%, with 1～6M hydrochloric acid or NaOH, regulating the pH value of homogenate is 2～3.5, and under 0～4 ℃ of condition, stirring and leaching is 5～15 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 2～4 times of volumes to precipitate A, be uniformly mixed, to adding calcium chloride to make its final concentration in mixed liquor, be 0.01% to 0.03%, with 1M hydrochloric acid or NaOH, regulating the pH value of mixed liquor is 2～3.5, under 0～4 ℃ of condition, stirring and leaching is 5～15 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; To liquid phase C, adding 1M hydrochloric acid or NaOH to regulate pH value is 4.8～5.8, and the last stirring and evenly mixing under 0～4 ℃ of condition standing 5～15 minutes, centrifugation obtained deposit C; The water of 0～4 ℃ that adds 2～4 times of volumes to deposit C, stirs and evenly mixs, and to adding in mixed liquor 1M hydrochloric acid or NaOH to regulate pH value, is 4.8～5.8, stirs and evenly mixs afterwards under 0～4 ℃ of condition standing 5～15 minutes, and centrifugation must precipitate D; After precipitation D is spray-dried, obtain Euphausia superba protein base materials.
Embodiment 2: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 2 times of volumes, by the ultraviolet treatment with irradiation of 1 meter of 40 watts of power, wavelength 200 nanometers, distance 10 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 1 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.03%, with 6M hydrochloric acid or NaOH, regulating the pH value of homogenate is 3.5, and under 0～4 ℃ of condition, stirring and leaching is 15 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 4 times of volumes to precipitate A, being uniformly mixed, is 0.03% to adding calcium chloride to make its final concentration in mixed liquor, and with 6M hydrochloric acid or NaOH, regulating the pH value of mixed liquor is 3.5, under 0～4 ℃ of condition, stirring and leaching is 15 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; To liquid phase C, adding 6M hydrochloric acid or NaOH to regulate pH value is 5.8, and the last stirring and evenly mixing under 0～4 ℃ of condition standing 15 minutes, centrifugation obtained deposit C; The water of 0～4 ℃ that adds 4 times of volumes to deposit C, stirs and evenly mixs, and to adding in mixed liquor 6M hydrochloric acid or NaOH to regulate pH value, is 5.8, stirs and evenly mixs afterwards under 0～4 ℃ of condition standing 15 minutes, and centrifugation must precipitate D; After precipitation D is spray-dried, obtain Euphausia superba protein base materials.
Embodiment 3: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 2～4 times of volumes, by the ultraviolet treatment with irradiation of 0.8 meter of 30 watts of power, wavelength 250 nanometers, distance 7 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.5 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.02%, with 2M hydrochloric acid or NaOH, regulating the pH value of homogenate is 3, and under 0～4 ℃ of condition, stirring and leaching is 10 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 3 times of volumes to precipitate A, being uniformly mixed, is 0.02% to adding calcium chloride to make its final concentration in mixed liquor, and with 2M hydrochloric acid or NaOH, regulating the pH value of mixed liquor is 3, under 0～4 ℃ of condition, stirring and leaching is 10 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; To liquid phase C, adding 2M hydrochloric acid or NaOH to regulate pH value is 5, and the last stirring and evenly mixing under 0～4 ℃ of condition standing 10 minutes, centrifugation obtained deposit C; The water of 0～4 ℃ that adds 3 times of volumes to deposit C, stirs and evenly mixs, and to adding in mixed liquor 2M hydrochloric acid or NaOH to regulate pH value, is 5, stirs and evenly mixs afterwards under 0～4 ℃ of condition standing 10 minutes, and centrifugation must precipitate D; After precipitation D is spray-dried, obtain Euphausia superba protein base materials.
Embodiment 4: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 2 times of volumes, by the ultraviolet treatment with irradiation of 0.5 meter of 20 watts of power, wavelength 210 nanometers, distance 5 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.2 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.01%, with 1M hydrochloric acid or NaOH, regulating the pH value of homogenate is 2, and under 0～4 ℃ of condition, stirring and leaching is 5 minutes, and centrifugation obtains liquid phase A and precipitate A; To liquid phase A, adding 1M hydrochloric acid or NaOH to regulate pH value is 4.8, and the last stirring and evenly mixing under 0～4 ℃ of condition standing 5 minutes, centrifugation obtained precipitate B; The water of 0～4 ℃ that adds 2 times of volumes to precipitate B, stirs and evenly mixs, and to adding in mixed liquor 1M hydrochloric acid or NaOH to regulate pH value, is 4.8, stirs and evenly mixs afterwards under 0～4 ℃ of condition standing 5 minutes, and centrifugation obtains deposit C; After deposit C is spray-dried, obtain Euphausia superba protein base materials.
Embodiment 5: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 4 times of volumes, by the ultraviolet treatment with irradiation of 1 meter of 40 watts of power, wavelength 280 nanometers, distance 5 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.1 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.030%, with 4M hydrochloric acid or NaOH, regulating the pH value of homogenate is 3.5, and under 0～4 ℃ of condition, stirring and leaching is 15 minutes, and centrifugation obtains liquid phase A and precipitate A; To liquid phase A, adding 1M hydrochloric acid or NaOH to regulate pH value is 5.8, and the last stirring and evenly mixing under 0～4 ℃ of condition standing 15 minutes, centrifugation obtained precipitate B; The water of 0～4 ℃ that adds 4 times of volumes to precipitate B, stirs and evenly mixs, and to adding in mixed liquor 1M hydrochloric acid or NaOH to regulate pH value, is 5.2, stirs and evenly mixs afterwards under 0～4 ℃ of condition standing 15 minutes, and centrifugation obtains deposit C; After deposit C is spray-dried, obtain Euphausia superba protein base materials.
Embodiment 6: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 3 times of volumes, by the ultraviolet treatment with irradiation of 0.8 meter of 30 watts of power, wavelength 300 nanometers, distance 6 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.4 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.020%, with 2M hydrochloric acid or NaOH, regulating the pH value of homogenate is 3, and under 0～4 ℃ of condition, stirring and leaching is 10 minutes, and centrifugation obtains liquid phase A and precipitate A; To liquid phase A, adding 1M hydrochloric acid or NaOH to regulate pH value is 5, and the last stirring and evenly mixing under 0～4 ℃ of condition standing 10 minutes, centrifugation obtained precipitate B; The water of 0～4 ℃ that adds 3 times of volumes to precipitate B, stirs and evenly mixs, and to adding in mixed liquor 1M hydrochloric acid or NaOH to regulate pH value, is 5, stirs and evenly mixs afterwards under 0～4 ℃ of condition standing 10 minutes, and centrifugation obtains deposit C; After deposit C is spray-dried, obtain Euphausia superba protein base materials.
Embodiment 7: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 2 times of volumes, by the ultraviolet treatment with irradiation of 0.6 meter of 25 watts of power, wavelength 220 nanometers, distance 8 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.7 hour afterwards.Under 0～4 ℃ of condition, stirring and leaching is 6 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 3 times of volumes to precipitate A, is uniformly mixed, and under 0～4 ℃ of condition, stirring and leaching is 8 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; Liquid phase C is frozen in-15 ℃ of preservations; Melt cryopreserving liquid, regulate pH value to 4.8 rear centrifugal, be precipitated, precipitation spraying is drying to obtain to Euphausia superba protein base materials.
Embodiment 8: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 4 times of volumes, by the ultraviolet treatment with irradiation of 0.7 meter of 35 watts of power, wavelength 290 nanometers, distance 8 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.3 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.015%, with 1M hydrochloric acid or NaOH, regulating the pH value of homogenate is 2.4, and under 0～4 ℃ of condition, stirring and leaching is 11 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 2 times of volumes to precipitate A, being uniformly mixed, is 0.015% to adding calcium chloride to make its final concentration in mixed liquor, and with 1M hydrochloric acid or NaOH, regulating the pH value of mixed liquor is 2.5, under 0～4 ℃ of condition, stirring and leaching is 11 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; Liquid phase C is frozen in-20 ℃ of preservations; Melt cryopreserving liquid, regulate pH value to 5.2 rear centrifugal, be precipitated C, the water to adding 2 times of volumes in deposit C, stirs and evenly mixs, and regulating pH of mixed value is 5.2, and centrifugation obtains liquid phase D and precipitation D, after precipitation D is spray-dried, obtains Euphausia superba protein base materials.
Embodiment 9: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 3 times of volumes, by the ultraviolet treatment with irradiation of 0.8 meter of 35 watts of power, wavelength 255 nanometers, distance 6 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.4 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.025%, with 2M hydrochloric acid or NaOH, regulating the pH value of homogenate is 3, and under 0～4 ℃ of condition, stirring and leaching is 12 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 2～4 times of volumes to precipitate A, being uniformly mixed, is 0.025% to adding calcium chloride to make its final concentration in mixed liquor, and with 1M hydrochloric acid or NaOH, regulating the pH value of mixed liquor is 2, under 0～4 ℃ of condition, stirring and leaching is 12 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; Liquid phase C is frozen in-25 ℃ of preservations; Melt cryopreserving liquid, regulate pH value to 5 rear centrifugal, be precipitated the spray-dried Euphausia superba protein base materials that obtains.
Embodiment 10: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 2.5 times of volumes, by the ultraviolet treatment with irradiation of 0.9 meter of 28 watts of power, wavelength 230 nanometers, distance 8 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.5 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.010%, with 3M hydrochloric acid or NaOH, regulating the pH value of homogenate is 2.5, and under 0～4 ℃ of condition, stirring and leaching is 5 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 3 times of volumes to precipitate A, being uniformly mixed, is 0.010% to adding calcium chloride to make its final concentration in mixed liquor, and with 1M hydrochloric acid or NaOH, regulating the pH value of mixed liquor is 2.5, under 0～4 ℃ of condition, stirring and leaching is 5 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; Liquid phase C is frozen in-22 ℃ of preservations; Melt cryopreserving liquid, regulate pH value to 5.5 rear centrifugal, be precipitated C, the water to adding 4 times of volumes in deposit C, stirs and evenly mixs, and regulating pH of mixed value is 5.5, and centrifugation obtains liquid phase D and precipitation D, after precipitation D is spray-dried, obtains Euphausia superba protein base materials.
Embodiment 11: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 3.5 times of volumes, by the ultraviolet treatment with irradiation of 1 meter of 36 watts of power, wavelength 205 nanometers, distance 9 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.6 hour afterwards.Under 0～4 ℃ of condition, stirring and leaching is 15 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 2 times of volumes to precipitate A, is uniformly mixed, and under 0～4 ℃ of condition, stirring and leaching is 15 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; Obtain liquid phase C; After liquid phase C is spray-dried frozen in-21 ℃ of preservations after dry powder; Described frozen dry powder is dissolved in the water of 2 times of volumes, regulates pH value to 4.9 rear centrifugal, be precipitated the spray-dried Euphausia superba protein base materials that obtains.
Embodiment 12: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 2～4 times of volumes, by the ultraviolet treatment with irradiation of 0.8 meter of 30 watts of power, wavelength 245 nanometers, distance 8 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.7 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.030%, with 4M hydrochloric acid or NaOH, regulating the pH value of homogenate is 3, and under 0～4 ℃ of condition, stirring and leaching is 15 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 4 times of volumes to precipitate A, being uniformly mixed, is 0.030% to adding calcium chloride to make its final concentration in mixed liquor, and with 4M hydrochloric acid or NaOH, regulating the pH value of mixed liquor is 3, under 0～4 ℃ of condition, stirring and leaching is 15 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; After liquid phase C is spray-dried frozen in-18 ℃ of preservations after dry powder; Described frozen dry powder is dissolved in the water of 4 times of volumes, regulate pH value to 5.1 rear centrifugal, be precipitated C, to the water that adds 4 times of volumes in deposit C, stir and evenly mix, regulating pH of mixed value is 5.1, and centrifugation obtains liquid phase D and precipitation D, after precipitation D is spray-dried, obtains Euphausia superba protein base materials.
Embodiment 13: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 3 times of volumes, by the ultraviolet treatment with irradiation of 0.8 meter of 30 watts of power, wavelength 265 nanometers, distance 6 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.8 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.030%, with 5M hydrochloric acid or NaOH, regulating the pH value of homogenate is 3, and under 0～4 ℃ of condition, stirring and leaching is 15 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 2 times of volumes to precipitate A, being uniformly mixed, is 0.010% to adding calcium chloride to make its final concentration in mixed liquor, and with 5M hydrochloric acid or NaOH, regulating the pH value of mixed liquor is 3, under 0～4 ℃ of condition, stirring and leaching is 15 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; After liquid phase C is spray-dried frozen in-24 ℃ of preservations after dry powder; Described frozen dry powder is dissolved in the water of 2 times of volumes, regulates pH value to 5.0 rear centrifugal, be precipitated, precipitation spraying is drying to obtain to Euphausia superba protein base materials.
Embodiment 14: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 4 times of volumes, by the ultraviolet treatment with irradiation of 0.5 meter of 40 watts of power, wavelength 260 nanometers, distance 9 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.9 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.025%, with 1M hydrochloric acid or NaOH, regulating the pH value of homogenate is 2.5, and under 0～4 ℃ of condition, stirring and leaching is 15 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 4 times of volumes to precipitate A, being uniformly mixed, is 0.010% to adding calcium chloride to make its final concentration in mixed liquor, and with 1M hydrochloric acid or NaOH, regulating the pH value of mixed liquor is 2, under 0～4 ℃ of condition, stirring and leaching is 15 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; After liquid phase C is spray-dried frozen in-16 ℃ of preservations after dry powder; Described frozen dry powder is dissolved in the water of 2～4 times of volumes, regulate pH value to 5.8 rear centrifugal, be precipitated C, to the water that adds 2 times of volumes in deposit C, stir and evenly mix, regulating pH of mixed value is 5.0, and centrifugation obtains liquid phase D and precipitation D, after precipitation D is spray-dried, obtains Euphausia superba protein base materials.
Embodiment 15: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 2 times of volumes, by the ultraviolet treatment with irradiation of 0.5 meter of 30 watts of power, wavelength 275 nanometers, distance 9 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.2 hour afterwards.Under 0～4 ℃ of condition, stirring and leaching is 10 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 2 times of volumes to precipitate A, is uniformly mixed, and under 0～4 ℃ of condition, stirring and leaching is 5 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; Liquid phase C is frozen in-20 ℃ of preservations; Melt cryopreserving liquid, heat after 10 minutes at 100 ℃ centrifugally, be precipitated the spray-dried Euphausia superba protein base materials that obtains.
Embodiment 16: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 3 times of volumes, by the ultraviolet treatment with irradiation of 0.8 meter of 30 watts of power, wavelength 285 nanometers, distance 9 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.3 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.010%, with 1M hydrochloric acid or NaOH, regulating the pH value of homogenate is 2.5, and under 0～4 ℃ of condition, stirring and leaching is 10 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 2 times of volumes to precipitate A, being uniformly mixed, is 0.010% to adding calcium chloride to make its final concentration in mixed liquor, and with 1M hydrochloric acid or NaOH, regulating the pH value of mixed liquor is 2.5, under 0～4 ℃ of condition, stirring and leaching is 10 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; Liquid phase C is frozen in-19 ℃ of preservations; Melt cryopreserving liquid, heat after 30 minutes at 80 ℃ centrifugally, be precipitated the spray-dried Euphausia superba protein base materials that obtains.
Embodiment 17: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 2 times of volumes, by the ultraviolet treatment with irradiation of 0.5 meter of 20 watts of power, wavelength 295 nanometers, distance 8 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.6 hour afterwards.Under 0～4 ℃ of condition, stirring and leaching is 15 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 2 times of volumes to precipitate A, is uniformly mixed, and under 0～4 ℃ of condition, stirring and leaching is 10 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; Obtain liquid phase C; After liquid phase C is spray-dried frozen in-21 ℃ of preservations after dry powder; Described frozen dry powder is dissolved in the water of 2 times of volumes, heats after 20 minutes at 90 ℃ centrifugally, be precipitated the spray-dried Euphausia superba protein base materials that obtains.
Embodiment 18: the fresh and alive krill after fishing for drains away the water, homogenate after mixing with 0～4 ℃ of water of 4 times of volumes, by the ultraviolet treatment with irradiation of 40 watts of power, wavelength 225 nanometers, distance 0.5 8 minutes, homogenate is placed in fishes at area surroundings temperature self-dissolving 0.2 hour afterwards.To adding calcium chloride to make its final concentration in homogenate, be 0.010%, with 1M hydrochloric acid or NaOH, regulating the pH value of homogenate is 3.5, and under 0～4 ℃ of condition, stirring and leaching is 5 minutes, and centrifugation obtains liquid phase A and precipitate A; 0～4 ℃ of water that adds 2 times of volumes to precipitate A, being uniformly mixed, is 0.010% to adding calcium chloride to make its final concentration in mixed liquor, and with 1M hydrochloric acid or NaOH, regulating the pH value of mixed liquor is 3.5, under 0～4 ℃ of condition, stirring and leaching is 15 minutes, and centrifugation obtains liquid phase B and precipitate B; Merge liquid phase A and liquid phase B, obtain liquid phase C; After liquid phase C is spray-dried frozen in-23 ℃ of preservations after dry powder; Described frozen dry powder is dissolved in the water of 2 times of volumes, heats after 30 minutes at 85 ℃ centrifugally, be precipitated the spray-dried Euphausia superba protein base materials that obtains.
The above; it is only the preferably specific embodiment of the present invention; but protection scope of the present invention is not limited to this; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; according to technical scheme of the present invention and inventive concept thereof, be equal to replacement or changed, within all should being encompassed in protection scope of the present invention.
Claims (7)
1. a preparation method for low fluorine Euphasia superb protein base stock, is characterized in that, in turn includes the following steps:
S1, low temperature self-dissolving: the fresh and alive krill of fishing for is drained to rear homogenate and obtain homogenate, by the ultraviolet treatment with irradiation of 0.5～1 meter of 20～40 watts of power, wavelength 200～300 nanometers, distance 5～10 minutes, afterwards described homogenate is placed at 0～4 ℃ to self-dissolving 0.1～1 hour;
S2, protein extraction: the water to adding 1～4 times of volume in described homogenate, mix, under 0～4 ℃ of condition, stirring and leaching is 5～15 minutes, centrifugation, upper phase and precipitating for the first time for the first time;
S3, albumen preparation: described upper phase is for the first time heated 10～30 minutes by regulating at pH value to 4.8～5.8 or 80～100 ℃, then centrifugal method obtains for the second time upper phase and precipitation for the second time, by described, precipitates for the second time the spray-dried Euphausia superba protein base materials that obtains.
2. the preparation method of low fluorine Euphasia superb protein base stock as claimed in claim 1, is characterized in that: in step S2, when adding water to homogenate, adding final concentration is 0.01%～0.03% calcium chloride.
3. the preparation method of low fluorine Euphasia superb protein base stock as claimed in claim 2, is characterized in that: pH value to 2～3.5 that regulated described homogenate in step S2 before centrifugation.
4. the preparation method of low fluorine Euphasia superb protein base stock as claimed in claim 3, it is characterized in that: in step S3, by described, precipitate for the second time the spray-dried Euphausia superba protein base materials that obtains and be replaced by described precipitation for the second time and add the water of 2～4 times of volumes, mix, regulating pH of mixed value is 4.8～5.8, centrifugation obtains for the third time upper phase and precipitation for the third time, and described precipitation for the third time after spray-dried obtain Euphausia superba protein base materials.
5. the preparation method of low fluorine Euphasia superb protein base stock as claimed in claim 4, is characterized in that: in step S3, by described upper phase for the first time frozen in-15 to-25 ℃ or spray-dried after frozen in-15 to-25 ℃ of preservations after dry powder; Then be transported to after operation room, described frozen upper phase for the first time melted or described frozen dry powder is dissolved in the water of 2～4 times of volumes and revert to liquid state, completing steps S3 and subsequent step.
6. the preparation method of the low fluorine Euphasia superb protein base stock as described in as arbitrary in claim 1～5, it is characterized in that: 0～4 ℃ of water that adds 2～4 times of volumes in step S2 to described precipitation for the first time, be uniformly mixed, under 0～4 ℃ of condition, stirring and leaching is 5～15 minutes, centrifugation, obtains the 4th upper phase and the 4th precipitation; Upper phase and described the 4th upper phase for the first time described in mixing, the upper phase for the first time of using in alternative steps S3.
7. the preparation method of the low fluorine Euphasia superb protein base stock as described in as arbitrary in claim 1～5, is characterized in that: regulate pH value to select HCl or the NaOH of 1～6M.
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| CN104255898B (en) * | 2014-08-14 | 2016-03-09 | 淮阴工学院 | The preparation method of freshwater crayfish protein isolate |
| CN105029515A (en) * | 2015-06-26 | 2015-11-11 | 浙江海洋学院 | Processing method of euphausia superba low in fluorine |
| 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 |
| CN105454403B (en) * | 2015-12-07 | 2016-11-30 | 中国海洋大学 | A kind of low fluorine freezing Antarctic krill shrimp is rotten and preparation method thereof |
| CN107125492A (en) * | 2017-04-28 | 2017-09-05 | 广东越群海洋生物研究开发有限公司 | Application of the euphausia superba powder in terms of madai opening material is prepared |
| CN110229225B (en) * | 2019-06-12 | 2021-07-20 | 山东师范大学 | Preparation method of sulfur-rich and/or cesium-rich protein in antarctic krill |
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Inventor after: Zhou Dayong Inventor after: Zhu Beiwei Inventor after: Yang Jingfeng Inventor after: Chen Yuewen Inventor after: Wu Haitao Inventor after: Li Dongmei Inventor after: Li Ming Inventor before: Zhu Beiwei Inventor before: Yang Jingfeng Inventor before: Chen Yuewen Inventor before: Wu Haitao Inventor before: Li Dongmei Inventor before: Li Ming |
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