CN105601666B - Method of phosphatide and products thereof is extracted in a kind of fish head from silver carp - Google Patents
Method of phosphatide and products thereof is extracted in a kind of fish head from silver carp Download PDFInfo
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- CN105601666B CN105601666B CN201610018681.3A CN201610018681A CN105601666B CN 105601666 B CN105601666 B CN 105601666B CN 201610018681 A CN201610018681 A CN 201610018681A CN 105601666 B CN105601666 B CN 105601666B
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- 241000251468 Actinopterygii Species 0.000 title claims abstract description 50
- 241000252234 Hypophthalmichthys nobilis Species 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 81
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 78
- 238000000605 extraction Methods 0.000 claims abstract description 21
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- 150000002632 lipids Chemical class 0.000 description 15
- TZCPCKNHXULUIY-RGULYWFUSA-N 1,2-distearoyl-sn-glycero-3-phosphoserine Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@H](COP(O)(=O)OC[C@H](N)C(O)=O)OC(=O)CCCCCCCCCCCCCCCCC TZCPCKNHXULUIY-RGULYWFUSA-N 0.000 description 10
- ZWZWYGMENQVNFU-UHFFFAOYSA-N Glycerophosphorylserin Natural products OC(=O)C(N)COP(O)(=O)OCC(O)CO ZWZWYGMENQVNFU-UHFFFAOYSA-N 0.000 description 10
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- 235000020669 docosahexaenoic acid Nutrition 0.000 description 9
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- 239000002253 acid Substances 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- JLPULHDHAOZNQI-JLOPVYAASA-N [(2r)-3-hexadecanoyloxy-2-[(9e,12e)-octadeca-9,12-dienoyl]oxypropyl] 2-(trimethylazaniumyl)ethyl phosphate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCC\C=C\C\C=C\CCCCC JLPULHDHAOZNQI-JLOPVYAASA-N 0.000 description 4
- 125000001931 aliphatic group Chemical group 0.000 description 4
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- WORJEOGGNQDSOE-UHFFFAOYSA-N chloroform;methanol Chemical compound OC.ClC(Cl)Cl WORJEOGGNQDSOE-UHFFFAOYSA-N 0.000 description 2
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- 150000008105 phosphatidylcholines Chemical class 0.000 description 2
- 150000008104 phosphatidylethanolamines Chemical class 0.000 description 2
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 2
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- JLPULHDHAOZNQI-ZTIMHPMXSA-N 1-hexadecanoyl-2-(9Z,12Z-octadecadienoyl)-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCC\C=C/C\C=C/CCCCC JLPULHDHAOZNQI-ZTIMHPMXSA-N 0.000 description 1
- 206010020466 Hunger Diseases 0.000 description 1
- 241000720946 Hypophthalmichthys molitrix Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
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- 239000000284 extract Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
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- 235000013305 food Nutrition 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
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- 238000000338 in vitro Methods 0.000 description 1
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- 230000002401 inhibitory effect Effects 0.000 description 1
- 235000015110 jellies Nutrition 0.000 description 1
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- 239000000178 monomer Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- -1 phospholipid lipid Chemical class 0.000 description 1
- 210000002706 plastid Anatomy 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 229940083466 soybean lecithin Drugs 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/10—Phosphatides, e.g. lecithin
- C07F9/103—Extraction or purification by physical or chemical treatment of natural phosphatides; Preparation of compositions containing phosphatides of unknown structure
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/10—Phosphatides, e.g. lecithin
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention belongs to the technical field of phosphatide is extracted for raw material with large cultivate fresh water fishes, and in particular to a kind of method that phosphatide is extracted in fish head from silver carp and products thereof, its step includes：1) clean silver carp fish head is minced into the fish head fragment of 1~2cm square；2) by ethanol that fish head fragment and volume fraction are 95% according to mass volume ratio 1：10~1：20 mixing, obtain pending thing；3) pending thing is carried out to the high-speed breakage of fish head fragment in homogenate extraction device, obtains slurries；4) slurries are filtered, obtains ethanol extract；5) ethanol extract is removed into ethanol, then with acetone according to mass volume ratio 1：5~1：10 are stirred mixing, and it is finished product that acetone supernatant is removed after centrifugation and is removed after residual acetone.For the present invention by extremely easy technical process, a use is easy to get very much and the extracting solution harmless to extract component, and coordinates efficient process control, you can realizes the high efficiency extraction of phosphatide in silver carp fish head.
Description
Technical field
The invention belongs to the technical field of phosphatide is extracted for raw material with large cultivate fresh water fishes, and in particular to a kind of from silver carp
Method of phosphatide and products thereof is extracted in fish head.
Background technology
China is one of fresh water fishery the most developed country in the world, and fresh-water fishes annual output is up to more than 15,000,000 tons；Silver carp
(Silver carp, Hypophthalmichthys molitrix) mainly cultivates fresh water fishes one of kind as China, adapts to
Property it is strong, growth is fast, annual output up to 3,000,000 tons or so, but due to being limited fresh-water fishes consumption habit by international, domestic market and
The factors such as fish processing characteristics in itself, flavor taste influence, its market value is relatively low, up for further utilization.
It is domestic studies have found that, the EPA (C20 of certain content are contained in the aliphatic acid composition of silver carp lipid:5,20 light dydrocarbons
Olefin(e) acid), DHA (C22:6, docosahexaenoic acid) etc. n-3 series polyunsaturated fatty acids, and sample segment data even with sea
Water fish is suitable, is a kind of resource for being worth further developing.And the also rare people's concern of the phospholipid lipid component in silver carp lipid.State
The molecule type of phosphatide, finds in outer 5 kinds of fish brains for originating in Hungary area for having researcher to count including silver carp
In the aliphatic acid composition of brain phosphatide, the EPA content average value of five kinds of fishes is that 1.8 ± 0.4%, DHA is 21.1 ± 2.5%, its
In the molecule type of main DHA phosphatide be 18:1/22:6、18:0/22:6 and 16:0/22:6 type diacyl phosphatidyl cholines (PC)
And phosphatidyl-ethanolamine (PE).
Being obtained out of various organisms has the function of the active phospholipid of specific structure sum, is always what functional lipids were studied
Important directions.In the aliphatic acid composition of marine organisms lipid, the characteristically more insatiable hungers of the n-3 such as EPA containing high level and DHA
And aliphatic acid, phosphatide concern of the researcher to wherein combining EPA and DHA are also more.There is researcher with 2-DHA-PC and 2-DHA-
2-DHA-PC/PS liposomes are made in PS (phosphatidyl serine), with soybean lecithin (being free of EPA, DHA) made of PC/PS lipids
Body has made comparative study.It was found that 2-DHA-PC/PS liposomes show the work with good anti-fibrosarcoma in Mice Body
Property, and Soybean PC/PS liposomes are then without any activity.In vitro test in terms of fibrosarcoma displays that 2-DHA-PC/PS
Liposome is better than Soybean PC/PS liposomes to the inhibitory activity of sarcoma Meth-A cells.Two lipoids are found by contrast test
Plastid is acted on for all unrestraints of macrophage class J744-1 cells, but 2-DHA-PC/PS liposomes and Soybean PC/PS liposomes
Compare, the phagocytic activity of J744-1 cell monomers can be advantageously promoted, while promote to participate in the cell proportion increase swallowed.From sight
The experimental phenomena observed is inferred：2-DHA-PC/PS liposomes can suppress fibrosarcoma cell growth at least partly cause
It can promote the phagocytic activity of macrophage at the same time since it directly suppresses the growth of tumour cell.The country has research to move marine products
The phosphatide in thing source has carried out molecule type and Analysis on Biological Activity, finds there is high-content in processing byproduct containing aquatic/marine animals
With reference to the phosphatide of EPA or DHA, wherein the phospholipid liposome rich in 2-DHA-PC, which has, suppresses S180 tumor-bearing mice tumour growths,
Adjust body specificity and non-specific immune function, thus it is speculated that DHA-PC phospholipid liposomes can by adjusting immune function,
Strengthen the function of T cell, B cell and macrophage, reach the effect for suppressing growth of tumour cell.
Silver carp is as one of important freshwater aquiculture fingerling in China, and it is light to become recent year for aboundresources and cost is relatively low
The important source material of water processing.Silver carp fish head accounts for overall 30% of silver carp, and based on bony structures, meat is less, and taste is bad,
Thus edible value is relatively low, in process through frequently as the processing of discarded object low value.The n-3 such as EPA, DHA in its body lipid
Polyunsaturated fatty acid ratio is higher, particularly contains more rich phosphatide in fish head, has higher active lipids exploitation profit
With value, but also lack the technology that effectively extraction processing is carried out to phosphatide in silver carp fish head both at home and abroad at present.
Domestic and foreign scholars have carried out the method for lipids extraction many researchs at present, and common lipids extraction method has：It is molten
Agent extraction method, supercritical extraction, membrane separation process, adsorption charomatography etc..Supercritical extraction, membrane separation process, adsorption charomatography
Etc. technology good separating effect, but production technology is more complicated, higher to equipment requirement, and running cost is high, and investment is larger, at present also
Be not suitable for large-scale production.Solvent extraction method is frequently with chloroform, methanol, ethanol, n-hexane, acetone, ethyl acetate, petroleum ether etc.
Organic solvent.Result of study shows, chloroform methanol method extraction lipid yield is high, and is suitable for the higher raw material of water content, can be with
As the standard extraction methods of aquatic products lipid content, but chloroform and higher with the toxicity of methanol, and chloroform methanol method extracts
Be lipid that a large amount of neutral fats are mixed with polar lipid.N-hexane, acetone, petroleum ether are only higher to the extraction efficiency of neutral fats,
And ethanol, ethyl acetate are higher to the extraction efficiency of polar lipid phosphatide.For ethanol, the cost of ethyl acetate is higher,
Therefore large-scale production generally carries out phosphatide extraction with 95% ethanol (industrial ethyl alcohol).Generally contain higher moisture in aquatic products
Content (generally more than 80%), the presence of moisture can influence the extraction effect of organic solvent, need to be general by raw material drying during extraction
Logical drying can cause the lipid oxidation in raw material, influence the quality of the phosphatide of extraction, and freeze-drying can keep former well
Cost is too high when expecting the quality of lipid, but applying in production.Also researcher is according to the different extraction properties of solvent, using two
The extracting mode of first mixed solvent system is to improve the recovery rate of phosphatide, but mixed solvent is less susceptible to separate and recover, production
In be difficult to realize recycle.
The content of the invention
The object of the present invention is to provide a kind of safety and environmental protection, it is easy to operate and be easily achieved large-scale industrial production from
Method of phosphatide and products thereof is extracted in silver carp fish head.
A kind of method that phosphatide is extracted in fish head from silver carp, comprises the following steps：
1) clean silver carp fish head is minced into the fish head fragment of 1~2cm square.
Wherein：
Specifically, the silver carp fish head is the fish head of the fresh removing fish gill, removes the fish head or solution freezed after the fish gill
The fish head of the fish gill is removed after jelly；
Preferably, the cleaning way of silver carp fish head is：Silver carp fish head is gone in the clear water after the cheek below 10 DEG C to soak repeatedly
Wash, it is 6.5~7 to embathe to immersion liquid pH value, then drainage.
2) ethanol that the fish head fragment for obtaining step 1) and volume fraction are 95% is according to mass volume ratio 1：10~1：
20 mixing, obtain pending thing.
3) the pending thing for obtaining step 2) carries out the high-speed breakage of fish head fragment in homogenate extraction device, is starched
Liquid.
Preferably, the operating temperature of homogenate extraction is 20~25 DEG C.
4) slurries for obtaining step 3) are filtered, and obtain ethanol extract.
Specifically, filter type is vacuum filtration or plate compression.
5) ethanol extract for obtaining step 4) obtains residue after isolating ethanol, and the residue is pressed with acetone
According to mass volume ratio 1：5~1：10 are stirred mixing, removed after centrifugation acetone supernatant obtain it is flaxen translucent sticky
The acetone insoluble matter precipitation of shape, then will be silver carp fish head phosphatide finished product after the acetone insoluble matter deposition removal residual acetone.
Wherein：
Specifically, the separate mode of ethanol evaporates for rotary evaporation in vacuo or thin film evaporator；
Specifically, the removing mode of residual acetone is rotary evaporation in vacuo.
Specifically, centrifugation is centrifuged for horizontal centrifuge or disc centrifuge centrifugation；
Preferably, the temperature conditionss being stirred are 20~25 DEG C；
Further, the ethanol that ethanol extract is isolated in step 5) can be mixed with 95% ethanol carries out step 2),
The ethanol and the amount ratio of 95% ethanol that ethanol extract is isolated are 1~3：1.
Present invention also offers the silver carp fish head phosphatide obtained according to the method that phosphatide is extracted in the above-mentioned fish head from silver carp
Finished product, the mass fraction of phosphatide are more than or equal to 90%.
The present invention is by extremely easy technical process, only using being easy to get very much and harmless to extract component in extraction process
Extracting solution, and coordinate efficient process control, you can realize the high efficiency extraction of phosphatide in silver carp fish head.And the present invention's is final
Product is after measured 90~95% containing phospholipid purity.The product has in fields such as biotechnology, health care and food industry
It is widely applied, there is important scientific value and economic benefit.During the ethanol that uses can recycle after reuse, pass through
Ji environmental protection.
Embodiment
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit
Determine the scope of the present invention.
Embodiment 1
Fresh silver carp fish head minces into the fragment of 1.5cm square, weighs 200g, by mass volume ratio 1:10(m:V, g/mL)
Add 95% ethanol 2000mL.Carry device using sudden strain of a muscle becomes pulpous state by the fish head fragment progress high-speed breakage 3min in ethanol,
Slurries are filtered by vacuum, obtain ethanol extract.Residue weight is weighed after ethanol extract rotary evaporation in vacuo is removed ethanol,
1 is added by mass volume ratio:5(m:V, g/ml) acetone centrifuged after being stirred using horizontal centrifuge, remove acetone supernatant
Acetone insoluble matter precipitation is obtained, to be removed by rotary evaporation in vacuo residual in flaxen translucent sticky mass, the precipitation
As silver carp fish head phosphatide finished product, its phospholipid purity is 93% after staying acetone.
Embodiment 2
Freezing silver carp fish head minces into the fragment of 2cm square, 10kg is weighed, by mass volume ratio 1:15(m:V, g/mL) plus
Enter 95% ethanol 150L.Carry device using sudden strain of a muscle becomes pulpous state by the fish head fragment progress high-speed breakage 5min in ethanol, will starch
Liquid is filtered using plate and frame filter press, obtains ethanol extract.After ethanol extract is used thin film evaporator evaporating ethanol
Residue weight is weighed, 1 is added by mass volume ratio:10(m:V, g/ml) acetone uses disc centrifuge point after being stirred
From, remove acetone supernatant obtain acetone insoluble matter precipitation, to pass through true in flaxen translucent sticky mass, the precipitation
It is silver carp fish head phosphatide finished product after empty rotary evaporation removing residual acetone, its phospholipid purity is 90%.
Embodiment 3
Freezing silver carp fish head minces into the fragment of 1.8cm square, 10kg is weighed, by mass volume ratio 1:20(m:V, g/mL)
Add 95% ethanol 200L.Carry device using sudden strain of a muscle becomes pulpous state by the fish head fragment progress high-speed breakage 5min in ethanol, will
Slurries are filtered using plate and frame filter press, obtain ethanol extract.Ethanol extract is used into thin film evaporator evaporating ethanol
After weigh residue weight, by mass volume ratio add 1:8(m:V, g/ml) acetone uses disc centrifuge point after being stirred
From, remove acetone supernatant obtain acetone insoluble matter precipitation, in flaxen translucent sticky mass, rotary evaporation in vacuo
As silver carp fish head phosphatide finished product, its phospholipid purity is 92% after removing residual acetone.
The foregoing is merely the better embodiment of the present invention, it is not intended to limit the invention, all spirit in the present invention
Within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention.
Claims (9)
1. the method for phosphatide is extracted in a kind of fish head from silver carp, it is characterised in that comprise the following steps：
1) clean silver carp fish head is minced into the fish head fragment of 1~2cm square；
2) ethanol that the fish head fragment for obtaining step 1) and volume fraction are 95% is according to mass volume ratio 1：10~1：20 is mixed
Close, obtain pending thing；
3) the pending thing for obtaining step 2) carries out the high-speed breakage of fish head fragment in homogenate extraction device, obtains slurries；
4) slurries for obtaining step 3) are filtered, and obtain ethanol extract；
5) ethanol extract for obtaining step 4) obtains residue after isolating ethanol, by the residue and acetone according to matter
Measure volume ratio 1：5~1：10 are stirred mixing, removed after centrifugation acetone supernatant obtain it is flaxen translucent thick
Acetone insoluble matter precipitates, then will be silver carp fish head phosphatide finished product after the acetone insoluble matter deposition removal residual acetone.
2. the method for phosphatide is extracted in the fish head according to claim 1 from silver carp, it is characterised in that：It is described in step 1)
Silver carp fish head for fresh the removings fish gill fish head, remove the fish head of the removing fish gill after the fish head that freezes after the fish gill or defrosting.
3. the method for phosphatide is extracted in the fish head according to claim 2 from silver carp, it is characterised in that：In step 1), silver carp
The cleaning way of fish head is：Silver carp fish head is gone in the clear water after the cheek below 10 DEG C to embathe repeatedly, embathes to immersion liquid pH value and is
6.5~7, then drainage.
4. the method for phosphatide is extracted in the fish head according to claim 1 from silver carp, it is characterised in that：It is flash in step 3)
The operating temperature of extraction is 20~25 DEG C.
5. the method for phosphatide is extracted in the fish head according to claim 1 from silver carp, it is characterised in that：In step 4), filtering
Mode is vacuum filtration or plate compression.
6. the method for phosphatide is extracted in the fish head according to claim 1 from silver carp, it is characterised in that；In step 5), ethanol
Separate mode evaporated for rotary evaporation in vacuo or thin film evaporator；The removing mode of residual acetone is rotary evaporation in vacuo.
7. the method for phosphatide is extracted in the fish head according to claim 1 from silver carp, it is characterised in that：In step 5), centrifugation
Mode is centrifuged for horizontal centrifuge or disc centrifuge centrifugation.
8. the method for phosphatide is extracted in the fish head according to claim 1 from silver carp, it is characterised in that：In step 5), stirring
The temperature conditionss of mixing are 20~25 DEG C.
9. the method for phosphatide is extracted in the fish head according to any one of claims 1 to 8 from silver carp, it is characterised in that：Step 5)
The ethanol that middle ethanol extract is isolated can be mixed with 95% ethanol carries out step 2), ethanol that ethanol extract is isolated with
The amount ratio of 95% ethanol is 1~3：1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610018681.3A CN105601666B (en) | 2016-01-12 | 2016-01-12 | Method of phosphatide and products thereof is extracted in a kind of fish head from silver carp |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610018681.3A CN105601666B (en) | 2016-01-12 | 2016-01-12 | Method of phosphatide and products thereof is extracted in a kind of fish head from silver carp |
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| CN107266494A (en) * | 2017-07-05 | 2017-10-20 | 武汉轻工大学 | Method of phosphatide and products thereof is extracted in a kind of fish head from grass carp |
| CN107535839A (en) * | 2017-09-26 | 2018-01-05 | 武汉轻工大学 | A kind of wet face of life of the phosphatide of head containing grass carp oil emulsion and preparation method thereof |
| CN109180723B (en) * | 2018-09-13 | 2021-03-30 | 武汉轻工大学 | Concentrated phospholipid and preparation method thereof |
| CN110862871A (en) * | 2019-11-13 | 2020-03-06 | 武汉轻工大学 | Method for efficiently enriching n-3PUFA lipid from aquatic product processing by-products |
| CN114432246A (en) * | 2021-11-19 | 2022-05-06 | 海南大学 | Liposome with neuroprotective effect and preparation method and application thereof |
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