CN102224855A - Method for enriching lipid in Antarctic krill - Google Patents
Method for enriching lipid in Antarctic krill Download PDFInfo
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Abstract
The invention provides a method for enriching lipid in Antarctic krill, which comprises the following steps: (1) preprocessing the Antarctic krill serving as a raw material; (2) leaching the Antarctic krill obtained in the step (1) with a solvent to obtain a leaching liquid; (3) concentrating the leaching liquid obtained in the step (2) to a certain volume; (4) refining the concentrated leaching liquid obtained in the step (3); and (5) performing vacuum concentrating on the refined leaching liquid obtained in the step (4) until the residual volume of the solvent is 0.1% lower than the volume of the solvent used in the step (2) so as to obtain the lipid of Antarctic krill. According to the invention, the Antarctic krill or head capsule of Antarctic krill is preferentially used as a raw material, the lipid extraction efficiency is increased through the preprocessing, solvent leaching and refining methods, the lipid quality is improved, the comprehensive utilization rate of Antarctic krill is remarkably increased, the product quality is improved, and the obtained lipid in Antarctic krill is applied to healthcare foods.
Description
Technical field
The present invention relates to the enrichment method of lipid in a kind of biological raw material, relate in particular to the enrichment method of lipid in a kind of krill
Background technology
It is bigger that lipid extracting method in the biological raw material is extracted in solvent, the raw material influence of lipid content and moisture, generally be rich in the low moisture raw material of lipid, its lipid extracting method is comparatively simple, adopts traditional lipid extracting method such as chloroform methanol method can realize the extraction of lipid.In addition, can also adopt n-hexane, ether, benzinum, ethanol and isopropyl alcohol equal solvent to replace chloroform methanol to extract lipid in the biological raw material usually.Relatively fully still toxicity is bigger though adopt the chloroform methanol method to extract lipid, and is not only edible dangerous, and the harm health of operators; Though but the relative less extraction efficiency with benzinum toxicity of ether is lower, and if the raw material water content too high, can produce organic solvent and extract difficulty, consume the consequence that reagent too much causes cost to increase.Therefore, according to above-mentioned each side demand, proposing a kind of effective, cheap and safe extracting method is very to be necessary.
The krill resource is very abundant, and according to estimates, existing krill biomass is hundred million tons of 6.5-10.0.Because of its huge biomass and potential commercial value, and the special status in Antarctic ecosystems, krill is subject to people's attention day by day.Krill is aboundresources not only, and is of high nutritive value, and not only contains the protein of a large amount of high-qualitys, also contains the lipid of 2%-5%.Content of phospholipid is higher relatively in the krill lipid, and contains the polyunsaturated fatty acid of more ω-3 series, and as DHA and EPA, they all are the good health care raw-food materials, have exploitation prospect preferably.But higher, the relative lipid content of the moisture in the krill is lower, is a kind of high-moisture low fat biological raw material, for this class raw material, use traditional extraction process not only inefficiency, cost is too high but also have certain potential safety hazard.In addition, discussed above and adopted traditional lipid extracting method to tend to bring defective such as toxicity or extraction efficiency be on the low side, therefore, a kind of effective, cheap enrichment method that safely, is suitable for lipid in the novel krill of suitability for industrialized production is demanded exploitation urgently.
Summary of the invention
Technical problem to be solved by this invention is the enrichment method that is to provide lipid in a kind of low fat biological raw material that contains high-moisture, the enrichment method of lipid in a kind of krill especially is provided, efficient production and utilization with lipid resource in the low fat biological raw material of realizing containing high-moisture remedy the deficiency on the prior art.
In order to solve the problems of the technologies described above, the invention provides the enrichment method of lipid in a kind of krill, it is characterized in that, comprising:
The first step is with the krill pretreatment of raw material;
In second step, the pretreated described krill solvent lixiviate with the first step obtains obtains leaching liquor;
In the 3rd step, the described leaching liquor that second step was obtained is concentrated into certain volume;
The 4th step, with the 3rd step obtain concentrate after leaching liquor refining;
The 5th step, with the 4th step obtain refining after described leaching liquor further be concentrated into described solvent residues and be lower than 0.1%, obtain the lipid of described krill.
Because krill is of high nutritive value, a lot of countries as a kind of abundant fishery resources, fish for it, and be applied to market, therefore krill is a kind of product that can obtain on the market, all can buy from a lot of countries, in the coastal area of china city such as Qingdao, Dalian etc. all can buy.
Wherein, different conditions when the preliminary treatment of the krill in the described first step is taken according to it be preferably thaw, in shortening, drying, pulverizing etc. one or more, lower through the moisture in the pretreated krill, moisture in the preferred krill after treatment is lower than 10%, can remove moisture a large amount of in the krill like this, the low fat krill that contains high-moisture by original of dried krill be become contain low-moisture krill.
The krill that adopts in the described first step can be the dried product of krill or shrimp med, fresh or freezing krill, also can be the krill of integral body or the shrimp head capsule part of krill, wherein, when adopting freezing krill, described krill need through thaw, shortening and dry preliminary treatment.
Wherein, the further preferred shrimp head capsule of krill that adopts is as the raw material that obtains lipid, because the lipid that is rich in the shrimp head capsule of krill is howed a lot than the lipid of other body parts of krill.
Wherein, the solvent that uses in described second step is preferably a kind of solvent or several solvent in the ethanol, isopropyl alcohol, benzinum, ethyl acetate, ether, acetone, soybean extracting solvent no.6 (main component is a hexane) of n-hexane, 50%-100% etc., krill and described solvent quality are than preferred 1: 8-1: 18, the preferred 4-10 of extraction time hour, preferred 20 ℃-40 ℃ of extraction temperature.
Wherein, concentrate in described the 3rd step and being preferably decompression and concentrating, thickening temperature is preferably 30 ℃-55 ℃, and concentration time is preferably 30-50 minute, leaching liquor volume after concentrating is preferably the 1/20-1/10 of original leaching liquor volume, increases the concentration of residue leaching liquor with this.
Wherein, the refining method of residue leaching liquor in described the 4th step is preferably one or several in the refining material of filtration, freezing and crystallizing, high speed centrifugation and interpolation etc., and the temperature of described subtractive process is 20 to 40 ℃.
Wherein, described refining material is preferably micro alkaline solution, macroreticular resin etc.
Wherein, described macroreticular resin can be a macroreticular resin on sale on the normally used market, as D101 type macroreticular resin.
Wherein, concentrate in described the 5th step and being preferably decompression and concentrating, thickening temperature is preferably 30-55 ℃, and concentration time is preferably 30-50 minute, is concentrated into described solvent residues volume and is lower than 0.1% with respect to the solvent volume of using in second step.
The present invention also provides a kind of enrichment method of krill Prawn head capsule lipid, it is characterized in that, comprising:
The first step, the krill pretreatment of raw material, the moisture in the described krill after treatment is lower than 10%, gets shrimp head capsule part, pulverizes;
Second step, the shrimp head capsule solvent lixiviate of the pretreated described krill that the first step is obtained, obtain leaching liquor, described solvent is at least a in the ethanol, isopropyl alcohol, benzinum, ethyl acetate, ether, acetone, soybean extracting solvent no.6 (main component is a hexane) of n-hexane, 50%-100%, the shrimp head capsule of described krill and the mass ratio of described solvent are 1: 8 to 1: 18, extraction time is 4 to 10 hours, and extraction temperature is 20 ℃ to 40 ℃;
In the 3rd step, the described leaching liquor that second step was obtained concentrates, and described simmer down to decompression concentrates, and thickening temperature is 30 to 55 ℃, and concentration time is 30 to 50 minutes, and the described leaching liquor volume after concentrating is the 1/20-1/10 of the described leaching liquor volume before concentrating;
The 4th step, with the 3rd step obtain concentrate after described leaching liquor refining, described refining method is filtration, freezing and crystallizing, high speed centrifugation or adds in the refining material one or several that temperature of described subtractive process is 20 to 40 ℃;
The 5th step, with the 4th step obtain refining after described leaching liquor further be concentrated into described solvent residues volume and be lower than 0.1% with respect to the solvent volume of using in second step, obtain the lipid of the shrimp head capsule of described krill, described simmer down to decompression concentrates, thickening temperature is 30 to 55 ℃, and concentration time is 30 to 50 minutes.
The present invention also provides the lipid of the krill of the enrichment method acquisition of adopting lipid in the above-mentioned krill.
The present invention also provides the lipid of the krill shrimp head capsule of the enrichment method acquisition of adopting lipid in the above-mentioned krill shrimp head capsule.
The present invention also provides a kind of application of lipid in the preparation health food of adopting the enrichment method acquisition of lipid in the above-mentioned krill.
The present invention also provides a kind of application of lipid in the preparation health food of adopting the enrichment method acquisition of lipid in the above-mentioned krill shrimp head capsule.
The present invention also provides lipid that a kind of enrichment method that adopts lipid in the above-mentioned krill obtains as the application of unique health-care components in the preparation health food.
The present invention also provides lipid that a kind of enrichment method that adopts lipid in the above-mentioned krill shrimp head capsule obtains as the application of unique health-care components in the preparation health food.
Application in the process of the enrichment method that the present invention also provides lipid in above-mentioned krill lipid in extracting krill.
Application in the process of the enrichment method that the present invention also provides lipid in above-mentioned krill shrimp head capsule lipid in extracting krill shrimp head capsule.
The present invention also provides a kind of health food, and described health food comprises the lipid of the enrichment method acquisition of lipid in the above-mentioned krill.
The present invention also provides a kind of health food, and described health food comprises the lipid of the enrichment method acquisition of lipid in the above-mentioned krill shrimp head capsule.
The present invention also provides a kind of health food, wherein, the lipid that the enrichment method of lipid obtains in the above-mentioned krill in described health food as unique health-care components.
The present invention also provides a kind of health food, wherein, the lipid that the enrichment method of lipid obtains in the above-mentioned krill shrimp head capsule in described health food as unique health-care components.
The present invention is raw material with the krill, further preferred krill shrimp head capsule is a raw material, improved the extraction efficiency of lipid by preliminary treatment, solvent lixiviate and refining method, improved the quality of lipid, meet the security of food, can realize large-scale industrial production, greatly improve the comprehensive utilization ratio of krill.
The specific embodiment
Below adopt embodiment to describe embodiments of the present invention in detail, how the application technology means solve technical problem to the present invention whereby, and the implementation procedure of reaching technique effect can fully understand and implements according to this.
Because the krill resource is huge, be of high nutritive value, not only be rich in the protein of high-quality, and krill contains the lipid of 2%-5%, content of phospholipid is higher relatively and contain more DHA (DHA) and EPA (eicosapentaenoic acid) in the lipid, it is the good health care raw-food material, therefore following examples all adopt krill to carry out the lipid enrichment as biological raw material, but the present invention can be used for any enrichment method that contains the low fat biological raw material lipid of high-moisture, and is not limited to krill.
Assay method
With the content of triglycerides in the triglycerides kit measurement krill lipid, with the content of phosphatide in the GB GB/T5537-2008 molybdenum blue colorimetric method mensuration lipid, with the content of EPA and DHA in the gas chromatography determination lipid.Wherein the triglycerides kit is that Zhongsheng Beikong Biological Science ﹠ Technology Co., Ltd. produces, and gas chromatograph is that U.S. Agilent company produces.
Embodiment 1
The first step takes by weighing the freezing krill of the 10Kg back Steam Heating 5 minutes of thawing, and drains away the water to be dried to moisture and to be lower than 10%, obtains the krill of 1.91Kg;
Second step took by weighing 1Kg with the described krill that obtains in the first step, and with 12Kg (about 18 liters) n-hexane lixiviate 6 hours, extraction temperature was 30 ℃;
In the 3rd step, the leaching liquor that second step was obtained concentrates in 40 ℃ of decompressions, through 50 minutes, is concentrated into 900 milliliters;
The 4th step, filter behind the 3rd leaching liquor freezing and crystallizing that goes on foot after the concentrating of obtaining, remove the impurity such as solid granule in the leaching liquor, operating temperature is 20 ℃;
The 5th step, with the 4th step obtain refining after leaching liquor be evaporated to solvent residues and be lower than 0.1%, obtain quality krill lipid preferably.
With the content of triglycerides in the triglycerides kit measurement krill lipid, with the content of phosphatide in the GB GB/T5537-2008 molybdenum blue colorimetric method mensuration lipid, with the content of EPA and DHA in the gas chromatography determination lipid.Wherein the triglycerides kit is that Zhongsheng Beikong Biological Science ﹠ Technology Co., Ltd. produces, and gas chromatograph is that U.S. Agilent company produces.Through above assay determination, the 1Kg krill finally obtains 143g krill lipid after n-hexane lixiviate optimization, and wherein content of triglyceride is 52.4%, and content of phospholipid is 16.7%, and EPA and DHA content are 32.2%.
Embodiment 2
The first step took by weighing the fresh krill Steam Heating of 1800g 5 minutes, was dried to moisture after draining away the water and was lower than 10%.Dried krill decaptitated peel off, obtain the shrimp head capsule of 270g and the shrimp of 152g altogether, the shrimp head capsule that obtains is pulverized;
Second step took by weighing 200g with the krill shrimp head capsule of the pulverizing that obtains in the first step, and with the food grade ethanol lixiviate of 1.6Kg (about 2 liters) 95% 8 hours, extraction temperature was 25 ℃;
In the 3rd step, the leaching liquor that second step was obtained concentrates in 50 ℃ of decompressions, through 40 minutes, is concentrated into 120 milliliters;
The 4th step, high speed centrifugation behind the residue leaching liquor freezing and crystallizing that the 3rd step obtained, operating temperature is 20 ℃.The high speed centrifugation rotating speed is 8000-10000r/h, centrifugal 15-20 minute;
The 5th step, with the 4th step obtain refining after leaching liquor be evaporated to the solvent residues volume and be lower than 0.1% with respect to the solvent volume of using in second step, obtain the quality lipid of krill shrimp head capsule preferably.
With the content of triglycerides in the triglycerides kit measurement krill lipid, with the content of phosphatide in the GB GB/T5537-2008 molybdenum blue colorimetric method mensuration lipid, with the content of EPA and DHA in the gas chromatography determination lipid.Wherein the triglycerides kit is that Zhongsheng Beikong Biological Science ﹠ Technology Co., Ltd. produces, and gas chromatograph is that U.S. Agilent company produces.Through above assay determination, 200g krill shrimp head capsule finally obtains the lipid of 33.8g krill shrimp head capsule after 95% ethanol lixiviate optimization, and wherein content of triglyceride is 45.3%, and content of phospholipid is 23.4%, and EPA and DHA content are 41.1%.
Embodiment 3
The first step takes by weighing the freezing krill of the 2Kg back Steam Heating 5 minutes of thawing, and is dried to moisture after draining away the water and is lower than 10%, obtains the 367g krill, pulverizes krill;
Second step took by weighing 200g with the krill of the pulverizing that obtains in the first step, with 3Kg (about 4 liters) n-hexane/isopropyl alcohol (2: 1, V/V) lixiviate is 7 hours, extraction temperature is 25 ℃;
In the 3rd step, the leaching liquor that second step was obtained concentrates in 40 ℃ of decompressions, through 30 minutes, is concentrated into 200 milliliters;
The 4th step added 5 gram D101 type macroreticular resin resins (purchasing in Anhui Samsung resin Science and Technology Ltd.) as refining material behind the residue leaching liquor freezing and crystallizing that the 3rd step obtained, filter behind 30 ℃ of vibration 15min;
The 5th step, with the 4th step obtain refining after leaching liquor be evaporated to the solvent residues volume and be lower than 0.1% with respect to the solvent volume of using in second step, obtain quality krill lipid preferably.
With the content of triglycerides in the triglycerides kit measurement krill lipid, with the content of phosphatide in the GB GB/T5537-2008 molybdenum blue colorimetric method mensuration lipid, with the content of EPA and DHA in the gas chromatography determination lipid.Wherein the triglycerides kit is that Zhongsheng Beikong Biological Science ﹠ Technology Co., Ltd. produces, and gas chromatograph is that U.S. Agilent company produces.Through above assay determination, the 200g krill through n-hexane/isopropyl alcohol (2: 1, V/V) finally obtain 38.4g krill lipid after the lixiviate optimization, wherein content of triglyceride is 47.5%, content of phospholipid is 27.9%, EPA and DHA content are 41.3%.
This intellectual property of primary enforcement that all are above-mentioned is not set restriction this new product of other forms of enforcement and/or new method.Those skilled in the art will utilize this important information, and foregoing is revised, to realize similar implementation status.But all modifications or transformation belong to the right of reservation based on new product of the present invention.
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not break away to any simple modification, equivalent variations and remodeling that above embodiment did, still belongs to the protection domain of technical solution of the present invention according to technical spirit of the present invention.
Claims (10)
1. the enrichment method of lipid in the krill is characterized in that, comprising:
The first step, the krill pretreatment of raw material;
In second step, the pretreated described krill solvent lixiviate with the first step obtains obtains leaching liquor;
In the 3rd step, the described leaching liquor that second step was obtained is concentrated into certain volume;
The 4th step, with the 3rd step obtain concentrate after described leaching liquor refining;
The 5th step, with the 4th step obtain refining after described leaching liquor further be concentrated into described solvent residues and be lower than 0.1%, obtain the lipid of described krill.
2. enrichment method as claimed in claim 1 is characterized in that: the preliminary treatment in the described first step be thaw, in shortening, drying, pulverizing etc. one or more; The solvent that uses is at least a solvent in the ethanol of n-hexane, 50%-100%, isopropyl alcohol, benzinum, ethyl acetate, ether, acetone, the soybean extracting solvent no.6 solvent in described second step; The mass ratio of described krill and described solvent is about 1: 8 to about 1: 18, and extraction time is 4 to 10 hours, and extraction temperature is 20 ℃ to 40 ℃; The simmer down to decompression concentrates in described the 3rd step, and thickening temperature is 30 to 55 ℃, and concentration time is 30 to 50 minutes, and the leaching liquor volume after concentrating is the 1/20-1/10 of the leaching liquor volume before concentrating.
3. enrichment method as claimed in claim 1 or 2, it is characterized in that: the refining method of remaining described leaching liquor in described the 4th step is one or several in the refining material of filtration, freezing and crystallizing, high speed centrifugation and interpolation, the temperature of described subtractive process is 20 to 40 ℃, and described refining material is micro alkaline solution or macroreticular resin etc.; The simmer down to decompression concentrates in described the 5th step, and thickening temperature is 30 to 55 ℃, and concentration time is 30 to 50 minutes.
4. the enrichment method of lipid in the krill shrimp head capsule is characterized in that, comprising:
The first step, the krill pretreatment of raw material, the moisture in the described krill after treatment is lower than 10%, gets shrimp head capsule part, pulverizes;
Second step, the shrimp head capsule solvent lixiviate of the pretreated described krill that the first step is obtained, obtain leaching liquor, described solvent is at least a in the ethanol, isopropyl alcohol, benzinum, ethyl acetate, ether, acetone, soybean extracting solvent no.6 of n-hexane, 50%-100%, the shrimp head capsule of described krill and the mass ratio of described solvent are about 1: 8 to about 1: 18, extraction time is 4 to 10 hours, and extraction temperature is 20 ℃ to 40 ℃;
In the 3rd step, the described leaching liquor that second step was obtained concentrates, and described simmer down to decompression concentrates, and thickening temperature is 30 to 55 ℃, and concentration time is 30 to 50 minutes, and the described leaching liquor volume after concentrating is the 1/20-1/10 of the described leaching liquor volume before concentrating;
The 4th step, with the 3rd step obtain concentrate after described leaching liquor refining, described refining method is one or several in the refining material of filtration, freezing and crystallizing, high speed centrifugation or interpolation, the temperature of described subtractive process is 20 to 40 ℃, and described refining material is micro alkaline solution, macroreticular resin etc.;
The 5th step, with the 4th step obtain refining after described leaching liquor further be concentrated into described solvent residues volume and be lower than 0.1% with respect to the solvent volume of using in second step, obtain the lipid of the shrimp head capsule of described krill, described simmer down to decompression concentrates, thickening temperature is 30 to 55 ℃, and concentration time is 30 to 50 minutes.
5. the lipid that adopts the described enrichment method of claim 1 to 4 to obtain.
6. the application of lipid in the preparation health food of adopting the described enrichment method of claim 1 to 4 to obtain.
7. the lipid that adopts the described enrichment method acquisition of claim 1 to 4 is as the application of unique health-care components in the preparation health food.
8. adopt the application of the described enrichment method of claim 1 to 4 in the process of extracting the krill lipid.
9. health food is characterized in that: described health food comprises the lipid that the described enrichment method of claim 1 to 3 obtains.
10. health food is characterized in that: the lipid that the described enrichment method of claim 1 to 4 obtains in described health food as unique health-care components.
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| CN102559366A (en) * | 2012-02-21 | 2012-07-11 | 山东师范大学 | Method for preparing phosphatidyl ethanolamine-enriched Neptune krill oil |
| CN102732382A (en) * | 2012-07-18 | 2012-10-17 | 山东师范大学 | Method for extracting wax from Antarctic krill |
| CN102807518A (en) * | 2012-07-18 | 2012-12-05 | 山东师范大学 | Method for extracting astaxanthin and astaxanthin ester from Euphausia superba by using A beta-8 macroporous resin |
| CN102816638A (en) * | 2012-08-30 | 2012-12-12 | 辽宁省大连海洋渔业集团公司 | Method for extracting phospholipid-rich krill oil from antarctic krills |
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| CN102559366A (en) * | 2012-02-21 | 2012-07-11 | 山东师范大学 | Method for preparing phosphatidyl ethanolamine-enriched Neptune krill oil |
| CN102732382A (en) * | 2012-07-18 | 2012-10-17 | 山东师范大学 | Method for extracting wax from Antarctic krill |
| CN102807518A (en) * | 2012-07-18 | 2012-12-05 | 山东师范大学 | Method for extracting astaxanthin and astaxanthin ester from Euphausia superba by using A beta-8 macroporous resin |
| CN102732382B (en) * | 2012-07-18 | 2013-07-03 | 山东师范大学 | Method for extracting wax from Antarctic krill |
| CN102807518B (en) * | 2012-07-18 | 2014-08-27 | 山东师范大学 | Method for extracting astaxanthin and astaxanthin ester from Euphausia superba by using A beta-8 macroporous resin |
| CN102816638A (en) * | 2012-08-30 | 2012-12-12 | 辽宁省大连海洋渔业集团公司 | Method for extracting phospholipid-rich krill oil from antarctic krills |
| CN105062664A (en) * | 2015-07-23 | 2015-11-18 | 山东师范大学 | Method for preparing and detecting oleic acid in degreased euphausia superba |
| CN105085232A (en) * | 2015-07-23 | 2015-11-25 | 山东师范大学 | Method for extracting calcium stearate from euphausia superba and purifying calcium stearate |
| CN105419936A (en) * | 2015-11-04 | 2016-03-23 | 大连工业大学 | Preparation method of low fluorine content Euphausia superba oil |
| CN105419936B (en) * | 2015-11-04 | 2020-04-10 | 大连工业大学 | Preparation method of euphausia superba oil with low fluorine content |
| CN106479662A (en) * | 2016-12-29 | 2017-03-08 | 山东师范大学 | A kind of extracting method of the Antarctic krill oils and fatss rich in astaxanthin and its ester |
| CN106479662B (en) * | 2016-12-29 | 2020-03-27 | 山东师范大学 | Extraction method of antarctic krill grease rich in astaxanthin and esters thereof |
| CN108913352A (en) * | 2018-07-27 | 2018-11-30 | 山东鲁华海洋生物科技有限公司 | Low raw meat krill oil of a kind of de- amine and preparation method thereof |
| CN108913352B (en) * | 2018-07-27 | 2020-08-11 | 山东鲁华海洋生物科技有限公司 | Amine-removed low-fishy-smell krill oil and preparation method thereof |
| CN109207247A (en) * | 2018-09-25 | 2019-01-15 | 深圳先进技术研究院 | The preparation method of antarctic krill oil, deodorant antarctic krill oil and its application, food |
| CN112586624A (en) * | 2020-12-24 | 2021-04-02 | 日照职业技术学院 | Pet nutrition paste prepared from euphausia superba lipid and preparation method thereof |
| CN112602851A (en) * | 2020-12-24 | 2021-04-06 | 日照职业技术学院 | Multistage utilization method of euphausia superba powder |
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