CN102492538B - Method for extracting Antarctic krill oil with high phosphatide content from Antarctic krill - Google Patents
Method for extracting Antarctic krill oil with high phosphatide content from Antarctic krill Download PDFInfo
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Abstract
The invention relates to a method for extracting Antarctic krill oil with high phosphatide content from Antarctic krill, which takes fresh Antarctic krill as a raw material, the method comprises the following steps: heating, killing enzyme, disinfecting, removing moisture, drying and crushing, extracting Antarctic krill powder by an organic solvent, cutting and extracting in the extraction process, evaporating the separated extract, removing the residual organic solvent to obtain the Antarctic krill oil with the phosphatide content of 40%-45%. The invention has the advantages of simple operation and high phosphatide content of the final product, and can be the most available method for extracting grease, especially phosphatide-rich grease.
Description
Technical field
The present invention relates to a kind of method of extracting krill oil from the krill powder, particularly be rich in the extracting method of the krill oil of high phospholipid content.
Background technology
Krill is a kind of crustacean plankton that mainly is distributed in Southern Oceans, and standing stock are very surprising, approximately 6～1,000,000,000 tons.In krill, fat accounts for 2%～4% of weight in wet base.Main fatty acid type and content comprise: DHA9.3%～14.2%, and EPA15.0%～20.5%, linolic acid 2.4%～3.8%, linolenic acid 1.3%～3.7%, palmitinic acid 21.1%～23.2% etc., unsaturated fatty acids is in the great majority.Can make autolytic enzyme inactivation in krill by the heating enzyme that goes out, prevent krill self degraded.The krill oil that is rich in phosphatide has raising memory, and the prevention senile dementia plays an important role in prevention cardiovascular and cerebrovascular diseases and atherosclerosis.Therefore develop the extractive technique that is rich in the phosphatide krill oil of crucial importance.
At present, extraction research report about krill oil is less, Norway's general sieve Nova biomedical company is in the patent (CN101652462A) of application preparation marine phospholipids in 2007, and it adopts the mode of carbon dioxide upercritical fluid extraction to obtain marine phospholipids, but the supercritical extraction extraction yield is lower.The Rui Er of Shandong section biological products company extracts the process patent (CN102071101A) of krill oil in application in 2011 from krill, with freezing krill, the intensification of also will thawing, thawing also will be incubated self-dissolving, reheats insulation, then cooling and drying again, must being much higher than under the condition of normal temperature, need again a large amount of energy, complex technical process at the extraction dissolution process, waste energy, process length causes krill and the rotten minimizing of effective constituent.The finished product phospholipids content is lower, and phospholipids content is up to 34%.It is only 2.2% of material quantity that krill oil extracts weight.
Summary of the invention
The invention provides a kind of extracting method that obtains high phospholipid content krill oil, in the antarctic krill oil that the method obtains, phospholipids content up to 40%～45%, also contains the multiple elements useful to human body such as astaxanthin, unsaturated fatty acids, VITAMIN, trace element simultaneously.
Technical scheme of the present invention is: a kind of method of extracting high phospholipid content krill oil from krill, it is characterized by, and comprise the following steps:
(1) heating: heating under 50～120 ℃ after krill is fished for, be 3～20 minutes heat-up time;
(2) drying: the krill after heating carries out drying, and drying temperature is 20～90 ℃;
(3) pulverize: after dry, krill is pulverized, be ground into 5～100 purpose krill meals, grinding time can be controlled at 1～30 minute;
(4) soak: soak krill meal with the ethanolic soln organic solvent more than 90% under 15～35 ℃, solid-to-liquid ratio is 1: 2～1: 10, and the time is 0.5～2 hour;
(5) shear: the krill meal suspension liquid after immersion is sheared with the emulsification pretreatment machine and is extracted 2 times, shearing for the first time rotating speed is 4000～6000rpm, shear time is 1～10 minute, and shearing for the second time rotating speed is 7000～10000rpm, and shear time is 1～20 minute;
(6) extract: the krill meal suspension liquid of shearing after extracting is extracted, separation and Extraction liquid, again krill meal is extracted 2～4 times altogether, ethanolic soln organic solvent solid-to-liquid ratio more than krill meal and 90% is 1: 2～1: 10, preferably stirring at leaching process, stir and extracted 1～3 hour, temperature can be 4～30 ℃;
(7) solvent evaporates: united extraction liquid, with extracting solution 30～60 ℃ of temperature, vacuum tightness-0.05～-0.1MPa under rotary evaporation, removing and obtaining phospholipids content in extracting solution after organic solvent is 40%～45% antarctic krill oil.In order to ensure the not residual organic solvent that exceeds standard in shrimp sauce, pass in the antarctic krill oil that obtains gas remove shrimp sauce in residual organic solvent, make Determination of Residual Organic Solvents meet national standard.
Advantage of the present invention is just to carry out drying to after just fishing for the krill heating, has both utilized the energy of heating to accelerate dry process, has also saved energy; Keep corresponding with envrionment temperature at leaching process, needn't heat, also save a large amount of energy; Be particularly poach or pressurization during hot water bath under normal atmosphere to the krill type of heating, not only can guarantee the reliability of heat sterilization, after heating, isolated hot water is used for heating extracting solution, evaporative removal organic solvent, further effectively utilize the ability of heating, more saved a large amount of energy; These also all greatly reduce tooling cost.To just fishing for krill simultaneously, by heat and make autolytic enzyme inactivation in krill just fishing for krill at once, sterilization makes the spoilage organism in krill lose life condition, effectively keeps the krill oil of krill and extraction fresh strong, prevents enzymolysis and the conversion of corrupt sex change, effective constituent.The mode that also has the present invention to extract by shearing can effectively improve the content of phosphatide in krill oil, and the finished product also contain unsaturated fatty acids, astaxanthin, VITAMIN and various trace elements etc.
Embodiment
Embodiment 1
(1) heating: heating under 80 ℃ after krill is fished for, be 10 minutes heat-up time;
(2) drying: krill is carried out vacuum-drying; The vacuum-drying temperature is 50 ℃, and vacuum tightness is-0.05MPa;
(3) pulverize: after dry, krill is pulverized, and is crushed to 80 purpose krill meals, and grinding time is 5 minutes;
(4) soak: soak krill meal with ethanol under 30 ℃, solid-to-liquid ratio is 1: 8, and the time is 2 hours;
(5) shear: after soaking, the krill meal suspension liquid is sheared with the emulsification pretreatment machine and is extracted 2 times, and shearing for the first time rotating speed is 6000rpm, and shear time is 5 minutes, and shearing for the second time rotating speed is 7000rpm, and shear time is 5 minutes;
(6) extract: the krill meal suspension liquid of shearing after extracting is extracted, separation and Extraction liquid, then krill meal is extracted 1 time altogether, krill meal and ethanol solid-to-liquid ratio are 1: 8, stir and extract 3 hours, temperature is 30 ℃;
(7) solvent evaporates: united extraction liquid, at temperature 60 C, vacuum tightness is rotary evaporation under-0.05MPa with extracting solution, and removing and obtaining phospholipids content in extracting solution after ethanol is 45% antarctic krill oil.In order to ensure the not residual organic solvent that exceeds standard in shrimp sauce, pass in the antarctic krill oil that obtains carbon dioxide remove shrimp sauce in residual organic solvent, make Determination of Residual Organic Solvents meet national standard.
Embodiment 2
(1) heating: heating under 100 ℃ after krill is fished for, be 10 minutes heat-up time;
(2) drying: krill is carried out drying; The vacuum-drying temperature is 90 ℃, and vacuum tightness is-0.1MPa;
(3) pulverize: dried krill is pulverized, be crushed to 80 orders, grinding time is 5 minutes;
(4) soak: the ethanolic soln with 90% soaks krill meal under 30 ℃, solid-to-liquid ratio is 1: 8, and the time is 2 hours;
(5) shear: after soaking, the krill meal suspension liquid is sheared with the emulsification pretreatment machine and is extracted 2 times, and shearing for the first time rotating speed is 10000rpm, and shear time is 5 minutes, and shearing for the second time rotating speed is 4000rpm, and shear time is 5 minutes;
(6) extract: the krill meal suspension liquid of shearing after extracting is extracted, separation and Extraction liquid, then the krill meal that separates is extracted 1 time, krill meal is 1: 8 with 91% ethanolic soln organic solvent solid-to-liquid ratio, stirs extraction 3 hours, temperature is 30 ℃;
(7) solvent evaporates: united extraction liquid, at temperature 60 C, vacuum tightness is rotary evaporation under-0.1MPa with extracting solution, and removing and obtaining phospholipids content in extracting solution after the second alcohol and water is 42.5% antarctic krill oil.
Embodiment 3
(1) heating: heating under 50 ℃ after krill is fished for, be 20 minutes heat-up time;
(2) drying: krill is carried out drying; Drying temperature is 40 ℃, and vacuum tightness is-0.1MPa;
(3) pulverize: dried krill is crushed to 10 orders, and grinding time is 3 minutes;
(4) soak: the ethanolic soln with 95% soaks krill meal under 30 ℃, solid-to-liquid ratio is 1: 10, and the time is 0.5 hour;
(5) shear: the krill meal suspension liquid after soaking is sheared with the emulsification pretreatment machine extracted 2 times, shearing for the first time rotating speed is 6000rpm, and shear time is 5 minutes, and shearing for the second time rotating speed is 10000rpm, and shear time is 5 minutes;
(6) extract: the krill meal suspension liquid of shearing after extracting is extracted, separation and Extraction liquid, then the krill powder is extracted 3 times, krill meal is 1: 2 with 95% ethanolic soln organic solvent solid-to-liquid ratio, stirs extraction 3 hours, temperature is 30 ℃;
(7) solvent evaporates: united extraction liquid, at temperature 60 C, vacuum tightness is rotary evaporation under-0.08MPa with extracting solution, and removing and obtaining phospholipids content in extracting solution after the second alcohol and water is 40.5% antarctic krill oil.
Embodiment 4
(1) heating: heating under 120 ℃ after krill is fished for, be 8 minutes heat-up time;
(2) drying: krill is carried out vacuum-drying; The vacuum-drying temperature is 90 ℃, and vacuum tightness is-0.1MPa;
(3) pulverize: after dry, krill is pulverized, and is crushed to 100 purpose krill meals, and grinding time is 30 minutes;
(4) soak: the ethanolic soln with ethanol and 99% soaks krill meal under 35 ℃, solid-to-liquid ratio is 1: 2, and the time is 2 hours;
(5) shear: the krill meal suspension liquid after soaking is sheared with the emulsification pretreatment machine extracted 4 times, shearing for the first time rotating speed is 4000rpm, shear time is 10 minutes, shearing for the second time rotating speed is 6000rpm, shear time is 10 minutes, and shearing for the third time rotating speed is 6000rpm, and shear time is 10 minutes, the 4th time is sheared rotating speed is 10000rpm, and shear time is 10 minutes;
(6) extract: the krill meal suspension liquid of shearing after extracting is extracted, separation and Extraction liquid, then the krill powder is extracted 3 times, krill meal is 1: 10 with 98% ethanolic soln organic solvent solid-to-liquid ratio, stirs extraction 3 hours, temperature is 30 ℃;
(7) solvent evaporates: united extraction liquid, at temperature 60 C, vacuum tightness is rotary evaporation under-0.1MPa with extracting solution, and removing and obtaining phospholipids content in extracting solution after the second alcohol and water is 44.5% antarctic krill oil.
Claims (5)
1. method of extracting high phospholipid content krill oil from krill is characterized in that:
(1) heating: heating under 50～120 ℃ after krill is fished for, be 3～20 minutes heat-up time;
(2) drying: the krill after heating is dry, and drying temperature is 20～90 ℃;
(3) pulverize: after dry, krill is ground into krill meal, is crushed to 5～100 orders;
(4) soak: soak krill meal at the ethanolic soln organic solvent more than 90% with concentration under 4～30 ℃, solid-to-liquid ratio is 1:2～1:10, and the time is 0.5～2 hour;
(5) shear: the krill meal suspension liquid after immersion is sheared with the emulsification pretreatment machine and is extracted 1～4 time, and the shearing rotating speed is 4000～10000rpm, and shear time is 1～30 minute;
(6) extract: the krill meal suspension liquid of shearing after extracting is extracted, separation and Extraction liquid, then extract and separation and Extraction liquid 2～4 times, extract krill meal and concentration is 1:2～1:10 in the ethanolic soln organic solvent solid-to-liquid ratio more than 90% at every turn, extracted 1～3 hour, temperature is 4～30 ℃; Leaching process, shear with the emulsification pretreatment machine the krill meal suspension liquid after soaking and extract 1～4 time again, and the shearing rotating speed is 4000～10000rpm, and shear time is 1～30 minute;
(7) solvent evaporates: united extraction liquid, with extracting solution at 30～60 ℃, vacuum tightness-0.05～-evaporate under 0.1MPa, removing and obtaining phospholipids content in extracting solution after organic solvent is 40%～45% antarctic krill oil, pass into gas and remove organic solvent residual in shrimp sauce, make Determination of Residual Organic Solvents meet national standard.
2. extracting as described in claim 1 the method for high phospholipid content krill oil, it is characterized in that, is poach or microwave heating or steam heating or pressurized, heated to the krill type of heating.
3. the method for the extraction high phospholipid content krill oil described in claim 1 or 2, is characterized in that, drying mode is vacuum-drying or lyophilize.
4. the method for the extraction high phospholipid content krill oil described in claim 1 or 2, is characterized in that, grinding time was at 1～30 minute.
5. extracting as claimed in claim 1 the method for high phospholipid content krill oil, it is characterized in that, is poach or pressurization hot water bath under normal atmosphere to the krill type of heating, and after heating, isolated hot water is used for the heating extracting solution, the evaporation organic solvent.
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102766530B (en) * | 2012-08-08 | 2013-08-07 | 辽宁省大连海洋渔业集团公司 | Method for extracting phospholipid-rich krill oil from Antarctic krill |
| 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 |
| CN103141871B (en) * | 2013-04-03 | 2014-08-20 | 辽宁省大连海洋渔业集团公司 | Preparation method of euphausia superba powder |
| CN103320217A (en) * | 2013-07-11 | 2013-09-25 | 日照海大博远海洋生物科技有限公司 | Method for extracting krill oil rich in phospholipid from euphausia superba |
| CN104479859A (en) * | 2014-11-27 | 2015-04-01 | 威海博宇食品有限公司 | Preparation method of roe extract |
| CN104479850B (en) * | 2014-12-15 | 2015-10-21 | 中国水产科学研究院黄海水产研究所 | The method of high phospholipid content krill oil is extracted from fresh krill |
| CN105536275B (en) * | 2016-01-29 | 2017-12-05 | 山东鲁华海洋生物科技有限公司 | A kind of concentrating and separating method and apparatus of antarctic krill oil extract solution |
| CN105670779A (en) * | 2016-03-09 | 2016-06-15 | 湛江市博泰生物化工科技实业有限公司 | Method for extracting euphausia superba oil through nitrogen pressurizing water vapor |
| CN107904023B (en) * | 2017-12-21 | 2021-01-08 | 山东师范大学 | Method for extracting residual grease from degreased dried shrimp residues of Antarctic krill |
| WO2021194360A1 (en) * | 2020-03-27 | 2021-09-30 | Pharmazen Limited | Extraction method for bio-active fractions |
| CN114525168A (en) * | 2022-01-04 | 2022-05-24 | 中国水产科学研究院东海水产研究所 | Method for extracting antarctic krill oil from antarctic krill powder raw material |
| CN116286167A (en) * | 2023-05-22 | 2023-06-23 | 山东康境海洋生物工程有限公司 | Refining equipment for krill oil with high phospholipid content and processing method thereof |
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| US8829215B2 (en) * | 2008-05-15 | 2014-09-09 | Pronova Biopharma Norge As | Krill oil process |
| CN101313722A (en) * | 2008-06-28 | 2008-12-03 | 合肥工业大学 | Method for extracting lobster oil from lobster waste |
| CN102041166B (en) * | 2011-01-20 | 2012-05-23 | 山东师范大学 | Method for extracting shrimp oil with high phospholipid content from Antarctic krill |
| CN102071101B (en) * | 2011-01-21 | 2012-10-10 | 山东科芮尔生物制品有限公司 | Method for extracting phospholipid-enriched krill oil from Antarctic krill |
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Address after: 116113 No. 188 Dalian Bay Street, Ganjingzi District, Liaoning, Dalian Patentee after: Liaoning Fishery Group Co.,Ltd. Address before: 116060, No. 188 Dalian Bay Street, Dalian Bay, Ganjingzi District, Dalian, Liaoning Patentee before: Liaoning Dalian Ocean Fishery Group Co.,Ltd. |
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Effective date of registration: 20230327 Address after: 116000 No. 8-147, Dalian Bay Street, Ganjingzi District, Dalian City, Liaoning Province Patentee after: LIAOYU ANTARCTIC KRILL TECHNOLOGY DEVELOPMENT Co.,Ltd. Address before: 116113 No. 188 Dalian Bay Street, Ganjingzi District, Dalian City, Liaoning Province Patentee before: Liaoning Fishery Group Co.,Ltd. |