CN103864841A - Method for extracting and refining phospholipid from egg of aquatic animal - Google Patents
Method for extracting and refining phospholipid from egg of aquatic animal Download PDFInfo
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- CN103864841A CN103864841A CN201410089039.5A CN201410089039A CN103864841A CN 103864841 A CN103864841 A CN 103864841A CN 201410089039 A CN201410089039 A CN 201410089039A CN 103864841 A CN103864841 A CN 103864841A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention provides a method for extracting and refining phospholipid from an egg of an aquatic animal. The extracting method comprises steps of firstly, drying the egg of the animal at a low temperature; secondly, smashing the egg dried in the first step; thirdly, mixing the smashed egg of the second step with a certain proportion of starch, then puffing and pelletizing the mixture; fourthly, putting the pelletized material of the third step into ethyl alcohol for extracting; fifthly, removing solvent of the leach liquor of the fourth step through reduced pressure vaporization; and sixthly, removing cholesterol of the extractive of the fifth step through CO2 supercritical extraction so as to refine the phospholipid. The method takes the egg of the aquatic animal as the raw material, the main component phospholipid in the egg of the aquatic animal is more effectively extracted through puffing and pelletizing, the extraction efficiency of the phospholipid in the egg of the animal is improved, the cholesterol is removed through CO2 supercritical extraction, so that the phospholipid in the extractive is refined, and effective development and utilization of low value animal egg are realized.
Description
Technical field
The present invention relates to a kind ofly from aquatic animal ovum, extract and the method for refined phosphatide.
Background technology
Phosphatide is that one has multiple bioactive lipid, and phosphatide is mainly to extract from soybean and yolk at present.
But in the animal ovum of low value, especially in aquatic animal ovum, be rich in abundant phosphatide.As contained a large amount of Yelkin TTS in fish-egg and squid ovum, the lipid acid in phosphatide is mainly EPA and DHA, and biological activity is different from plant phosphatide, and nutritive value is very abundant.If the extracting method of phosphatide in exploitation aquatic animal ovum, the efficient utilization of the low value thing that will realize.But, traditional phosphatide extracting method, as simple ethanol and acetone extraction method, extraction efficiency is low, and high cost can not be realized suitability for industrialized production, and it is high to extract the cholesterol level that the compound lipid that obtains contains.Therefore the extraction and the process for purification that, are suitable for phosphatide in the aquatic animal ovum of suitability for industrialized production are urgently developed.
Summary of the invention
Technical problem to be solved by this invention be to provide a kind of from aquatic animal ovum the method for purifying phosphatide, to realize effective extraction and efficient utilization of phosphatide in low-value aquatic product animal ovum, the deficiency on remedy technology.
In order to solve the problems of the technologies described above, the invention provides a kind of method of extracting phosphatide from aquatic animal ovum, it is characterized in that:
The first step, carries out cryodrying by aquatic animal ovum;
Second step, pulverizes dried ovum in the first step;
The 3rd step: the animal ovum of pulverizing in second step is mixed with certain ratio starch, then mixture is carried out to expanded granulation;
The 4th step: the material of the 3rd step granulation is put into alcohol and carry out lixiviate.
The 5th step: utilize the method for reduction vaporization to carry out desolventizing to the extracting solution in the 4th step, obtain mixing lipid;
The 6th step: utilize CO2 supercritical extraction to carry out cholesterol reduction to extracting lipid in the 5th step, thereby obtain refined phosphatide.
Wherein said aquatic animal egg follicle is drawn together fish-egg, squid ovum, sea urchin egg, shrimp ovum.Raw material is preferably fish-egg and squid ovum, owing to containing the contour biologically active substance nutritive substance of a large amount of Yelkin TTS in fish-egg and squid ovum, and fish-egg and squid ovum cheap, easily purchase and obtain, in Chinese coastal cities as Qingdao, Dalian, Shanghai etc. all can obtain.
Wherein, after described the first step cryodrying, the water content of gained aquatic animal ovum ovum powder is between 2-15%, and drying temperature is between 10-50 ℃;
Wherein, described second step is pulverized as utilizing pulverizer that dry ovum is pulverized;
Wherein, the aquatic animal ovum powder of described the 3rd step and starch blending ratio are 1: 0.1-1: between 3, expanded mode adopts extruding puffing;
Wherein, the ethanol concn that described the 4th step is used is 70-100%, and the time of lixiviate is between 2-10h, and the temperature of lixiviate is 10-60 ℃, and liquid ratio is 1-10l/kg fish-egg powder;
Wherein, the 5th step desolventizing is taked the method for reduction vaporization;
Wherein, described the 6th step SCF-CO 2 temperature is 35-50 ℃ of left and right, and extracting pressure is 20-30MPa, and extraction time is 1.5-3h.
The present invention also provides the application at protective foods of phosphatide that a kind of method that adopts above-mentioned side to extract phosphatide from aquatic animal ovum obtains.
Beneficial effect:
The present invention is take aquatic animal ovum as raw material, further preferred squid ovum and fish-egg, by the method for expanded granulation and CO2 supercritical extraction, the phosphatide in aquatic animal ovum is effectively extracted, improve the extraction yield of phosphatide, realize suitability for industrialized production, and can greatly improve raw material availability, reduce costs.It is more than 70% extracting with refining phosphatide extraction efficiency by the method for the invention, and cholesterol total lipid content is 6% effect, after refining, can remove more than 70%.
Embodiment
Below adopt embodiment to describe embodiments of the present invention in detail, to the present invention, how utilisation technology means solve technical problem whereby, and the implementation procedure of reaching technique effect can fully understand and implement according to this.
Choose respectively squid ovum, cod roe, mackerel ovum according to method extraction and the refined phosphatide of purifying phosphatide of the present invention, the line correlation of going forward side by side is measured.Measuring method: phosphatide adopts Agilent 1100HPLC high performance liquid chromatograph to measure.
Embodiment 1
Use of the present invention from squid ovum extract and refined phosphatide.
Extract with purification step and be:
The first step, gets 1Kg squid ovum, and 15 ℃ of cryodrying to moisture contents are 5%;
Second step, pulverizes dried squid ovum in the first step with pulverizer;
The 3rd step: the squid ovum of pulverizing in second step is mixed in the ratio of 1: 1 with starch, then mixture is carried out to expanded granulation;
The 4th step: the material after the 3rd step granulation is put into 90% spirit solvent, lixiviate 6h at 30 ℃.Wherein, liquid ratio is 10L/kg squid ovum powder;
The 5th step: utilize reduction vaporization method to carry out desolventizing to the extracting solution of the 4th step
The 6th step: the lipid of utilizing CO2 supercritical extraction to extract the 5th step is carried out cholesterol reduction, thereby refined phosphatide.Extraction temperature is 45 ℃ of left and right, and extracting pressure is 25MPa, and extraction time is 2h.
Measurement result: to the product analysis obtaining, its phospholipids content reaches 85.1%, cholesterol level 5.9% in total fat, has removed 80% after refining.
Embodiment 2
Use of the present invention from cod roe extract and refined phosphatide.
Extract with purification step and be:
The first step, gets 1Kg cod roe, and cryodrying to moisture content is 8%;
Second step, pulverizes dried squid ovum in the first step with pulverizer;
The 3rd step: the squid ovum of pulverizing in second step is mixed in the ratio of 1: 0.5 with starch, then mixture is carried out to expanded granulation;
The 4th step: the material after the 3rd step granulation is put into 95% spirit solvent, lixiviate 6h at 30 ℃.Wherein, liquid ratio is 8L/Kg squid ovum powder;
The 5th step: utilize reduction vaporization method to carry out desolventizing to the extracting solution of the 4th step;
The 6th step: the phosphatide that utilizes CO2 supercritical extraction to extract the 5th step carries out cholesterol reduction, thereby refined phosphatide.Extraction temperature is at 45 ℃, and extracting pressure is 25MPa, and extraction time is 3h.
Measurement result: to the product analysis obtaining, its phospholipids content reaches 88.0%, cholesterol level 6.4% in total fat, has removed 72% after refining.
Embodiment 3
Use of the present invention from mackerel ovum extract and refined phosphatide.
Extract with purification step and be:
The first step, gets 1Kg mackerel ovum, and cryodrying to moisture content is 6%;
Second step, pulverizes dried squid ovum in the first step with pulverizer;
The 3rd step: the squid ovum of pulverizing in second step is mixed in the ratio of 1: 0.1 with starch, then mixture is carried out to expanded granulation;
The 4th step: the material after the 3rd step granulation is put into 95% spirit solvent, lixiviate 6.5h at 30 ℃.Wherein, liquid ratio is 3L/Kg squid ovum powder;
The 5th step: utilize reduction vaporization method to carry out desolventizing to the extracting solution of the 4th step
The 6th step: the lipid of utilizing CO2 supercritical extraction to extract the 5th step is carried out cholesterol reduction, thereby refined phosphatide.Extraction temperature is at 45 ℃, and extracting pressure is 25MPa, and extraction time is 3h.
Measurement result: to the product analysis obtaining, its phospholipids content reaches 86.5%, cholesterol level 6% in total fat, has removed 75% after refining.
Squid ovum is worth cheap, and contain a large amount of phosphatide, especially contain abundant Yelkin TTS, it is good extraction raw material, but a kind of extraction of the present invention can be for the extraction of phosphatide in any aquatic animal ovum with the method for refined phosphatide, and be not limited to squid ovum, cod roe, mackerel ovum, also can be shrimp ovum, sea urchin egg etc.
All above-mentioned these intellecture properties of primary enforcement, do not set restriction this product innovation of other forms of enforcement and/or novel 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 product innovation of the present invention.
The above, be only preferred embodiment of the present invention, is not that the present invention is done to other forms of restriction, 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 depart from, any simple modification, equivalent variations and the remodeling above embodiment done according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.
Claims (5)
1. a method for extraction and refined phosphatide from aquatic animal ovum, is characterized in that: the step of described extraction and process for purification is:
The first step, gets a certain amount of aquatic animal ovum, carries out cryodrying;
Second step, pulverizes dried fish-egg in the first step with pulverizer;
The 3rd step: the aquatic animal ovum of pulverizing in second step is mixed with starch according to a certain percentage, then mixture is carried out to expanded granulation;
The 4th: the material after the 3rd step granulation is put into certain density spirit solvent and carry out lixiviate;
The 5th step: utilize the method for reduction vaporization to carry out desolventizing to the extracting solution of the 4th step, obtain mixing lipid;
The 6th step: the mixing fat that utilizes CO2 supercritical extraction to extract the 5th step carries out cholesterol reduction, thereby obtains refined phosphatide.
2. the method for a kind of extraction as claimed in claim 1 and refined phosphatide, is characterized in that: described the first step drying temperature is between 10 to 50 ℃, and the water content of dried product exhibited is between 2% to 15%; The aquatic animal ovum of described the 3rd step and starch blending ratio are 1: 0.1-1: between 3; The ethanol concn of described the 4th step is 70-100%, and the time of lixiviate is 2-10h, and the temperature of lixiviate is 10-60 ℃, and liquid ratio is 1-10l/kg fish-egg powder; Described the 6th step SCF-CO 2 temperature is 35-50 ℃ of left and right, and extracting pressure is 20-30MPa, and extraction time is 1.5-3h.
3. the method for a kind of extraction as claimed in claim 1 or 2 and refined phosphatide, is characterized in that: described the first step drying temperature is 15 ℃, and the water content of dried product exhibited is 5%; The aquatic animal ovum of described the 3rd step and starch blending ratio are between 1: 1; The ethanol concn of described the 4th step is 90%.
4. the method for a kind of extraction as claimed in claim 1 and refined phosphatide, is characterized in that: described aquatic animal ovum can be fish-egg, squid ovum, sea urchin egg, shrimp ovum.
5. the application of the prepared Yelkin TTS of method of a kind of extraction as claimed in claim 1 and refined phosphatide in protective foods.
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| CN201410089039.5A CN103864841A (en) | 2014-03-12 | 2014-03-12 | Method for extracting and refining phospholipid from egg of aquatic animal |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104479859A (en) * | 2014-11-27 | 2015-04-01 | 威海博宇食品有限公司 | Preparation method of roe extract |
| CN105265743A (en) * | 2014-07-02 | 2016-01-27 | 九三粮油工业集团有限公司 | Blend phospholipids composition |
| CN112779080A (en) * | 2020-12-17 | 2021-05-11 | 福州海锐黎思生物科技有限责任公司 | Equipment and method for extracting functional lipid from marine fish eggs |
| BE1029135B1 (en) * | 2021-08-25 | 2022-09-14 | First Inst Oceanography Mnr | Process for the separation and purification of active ingredients in sea urchins and its application |
Citations (4)
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| CN1252435A (en) * | 1998-10-22 | 2000-05-10 | 山东省粮油科学研究所 | Fish powder puffing, pelletizing and oil extracting technology |
| US6800299B1 (en) * | 1998-10-21 | 2004-10-05 | Universite De Sherbrooke | Method of extracting lipids from marine and aquatic animal tissues |
| CN101538278A (en) * | 2009-05-11 | 2009-09-23 | 江南大学 | High-purity egg yolk lecithin and production method and applications thereof |
| CN101812087A (en) * | 2010-05-07 | 2010-08-25 | 青岛海恩赐生物工程有限公司 | Method for extracting high-purity phospholipid from sleeve-fish-processing waste |
-
2014
- 2014-03-12 CN CN201410089039.5A patent/CN103864841A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6800299B1 (en) * | 1998-10-21 | 2004-10-05 | Universite De Sherbrooke | Method of extracting lipids from marine and aquatic animal tissues |
| CN1252435A (en) * | 1998-10-22 | 2000-05-10 | 山东省粮油科学研究所 | Fish powder puffing, pelletizing and oil extracting technology |
| CN101538278A (en) * | 2009-05-11 | 2009-09-23 | 江南大学 | High-purity egg yolk lecithin and production method and applications thereof |
| CN101812087A (en) * | 2010-05-07 | 2010-08-25 | 青岛海恩赐生物工程有限公司 | Method for extracting high-purity phospholipid from sleeve-fish-processing waste |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105265743A (en) * | 2014-07-02 | 2016-01-27 | 九三粮油工业集团有限公司 | Blend phospholipids composition |
| CN104479859A (en) * | 2014-11-27 | 2015-04-01 | 威海博宇食品有限公司 | Preparation method of roe extract |
| CN112779080A (en) * | 2020-12-17 | 2021-05-11 | 福州海锐黎思生物科技有限责任公司 | Equipment and method for extracting functional lipid from marine fish eggs |
| BE1029135B1 (en) * | 2021-08-25 | 2022-09-14 | First Inst Oceanography Mnr | Process for the separation and purification of active ingredients in sea urchins and its application |
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Application publication date: 20140618 |