CN102492538A - 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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- CN102492538A CN102492538A CN2011103600314A CN201110360031A CN102492538A CN 102492538 A CN102492538 A CN 102492538A CN 2011103600314 A CN2011103600314 A CN 2011103600314A CN 201110360031 A CN201110360031 A CN 201110360031A CN 102492538 A CN102492538 A CN 102492538A
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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 from the krill powder, extracting krill oil, particularly be rich in the process for extracting of the krill oil of high phospholipid content.
Background technology
Krill is a kind of crustacean plankton that mainly is distributed in the Nanjing University ocean, and standing stock are very surprising, about 6～1,000,000,000 tons.Fat accounts for 2%～4% of weight in wet base in the krill.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 the autolytic enzyme inactivation in the krill through the heating enzyme that goes out, prevent krill self degraded.The krill oil that is rich in phosphatide has memory, and the prevention senile dementia is prevented cardiovascular and cerebrovascular diseases and prevented to play an important role in the atherosclerosis.Therefore it is of crucial importance to develop the extractive technique that is rich in the phosphatide krill oil.
At present; Extraction research report about krill oil is less; Norway general sieve Nova biological medicine 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 is to use the refrigerated krill in the process patent (CN102071101A) of application in 2011 extraction krill oil from krill, the intensification of also will thawing; Thawing also will be incubated self-dissolving, reheat insulation, cooling and drying again then; Must need lot of energy again, complex technical process being much higher than under the condition of normal temperature 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 only is 2.2% of material quantity that krill oil extracts weight.
Summary of the invention
The invention provides a kind of process for extracting that obtains high phospholipid content krill oil; Phospholipids content also contains multiple elements to the human body beneficial such as astaxanthin, unsaturated fatty acids, VITAMINs, trace element simultaneously up to 40%～45% in the krill oil that this method obtains.
Technical scheme of the present invention is: a kind of method of from krill, extracting high phospholipid content krill oil, it is characterized by, and may further comprise the steps:
(1) heating: krill is fished for the back 50～120 ℃ of heating down, and be 3～20 minutes heat-up time;
(2) drying: the krill after will heating carries out drying, and drying temperature is 20～90 ℃;
(3) pulverize: krill is pulverized in dry back, is ground into 5～100 purpose krill meals, and the pulverizing time can be controlled at 1～30 minute;
(4) soak: soak krill meal with the ethanolic soln organic solvent more than 90% down at 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 the immersion is sheared with the emulsification pretreatment machine and is extracted 2 times, and shearing rotating speed for the first time is 4000～6000rpm, and shear time is 1～10 minute, and shearing rotating speed for the second time is 7000～10000rpm, and shear time is 1～20 minute;
(6) extract: the krill meal suspension liquid to shearing after extracting extracts; Separation and Extraction liquid; Krill meal is extracted 2～4 times altogether, krill meal and 90% above ethanolic soln organic solvent solid-to-liquid ratio are 1: 2～1: 10, are preferably stirring at leaching process again; 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 the extracting solution behind the organic solvent is 40%～45% krill oil.In order to ensure the not residual organic solvent that exceeds standard in the shrimp sauce, in the krill oil that obtains, feed gas and remove residual organic solvent in the shrimp sauce, make the Determination of Residual Organic Solvents 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 quicken the exsiccant process, has also saved energy; Keep corresponding at leaching process, needn't heat, also save lot of energy with envrionment temperature; It is poach or pressurization poach when heating under the normal atmosphere particularly to the krill type of heating; Not only can guarantee the safety of heat sterilization, the isolated hot water in heating back is used for heating and extracting liquid, the evaporative removal organic solvent; Further effectively utilize the ability of heating, more saved lot of energy; These also all greatly reduce tooling cost.To just fishing for krill simultaneously; Through heat and make autolytic enzyme inactivation in the krill at once to just fishing for krill; Sterilization makes the spoilage organism in the krill lose life condition, effectively keeps the krill oil of krill and extraction fresh strong, prevents the enzymolysis and the conversion of corrupt sex change, effective constituent.Also have the present invention can effectively improve the content of phosphatide in krill oil through shearing the mode of extracting, the finished product also contain unsaturated fatty acids, astaxanthin, VITAMINs and various trace elements etc.
Embodiment
Embodiment 1
(1) heating: krill is fished for the back 80 ℃ of heating down, and 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: dry back krill is pulverized, and is crushed to 80 purpose krill meals, and the pulverizing time is 5 minutes;
(4) soak: soak krill meal with ethanol down at 30 ℃, solid-to-liquid ratio is 1: 8, and the time is 2 hours;
(5) shear: soak back krill meal suspension liquid and shear extraction 2 times with the emulsification pretreatment machine, shearing rotating speed for the first time is 6000rpm, and shear time is 5 minutes, and shearing rotating speed for the second time is 7000rpm, and shear time is 5 minutes;
(6) extract: the krill meal suspension liquid to shearing after extracting extracts, and separation and Extraction liquid extracts 1 time krill meal more altogether, and krill meal and ethanol solid-to-liquid ratio are 1: 8, stirs and extracts 3 hours, and temperature is 30 ℃;
(7) solvent evaporates: united extraction liquid, 60 ℃ of temperature, vacuum tightness is rotary evaporation under-0.05MPa with extracting solution, and removing and obtaining phospholipids content in the extracting solution behind the ethanol is 45% krill oil.In order to ensure the not residual organic solvent that exceeds standard in the shrimp sauce, in the krill oil that obtains, feed dioxide gas and remove residual organic solvent in the shrimp sauce, make the Determination of Residual Organic Solvents National standard.
Embodiment 2
(1) heating: krill is fished for the back 100 ℃ of heating down, and 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, the pulverizing time is 5 minutes;
(4) soak: the ethanolic soln with 90% soaks krill meal down at 30 ℃, and solid-to-liquid ratio is 1: 8, and the time is 2 hours;
(5) shear: soak back krill meal suspension liquid and shear extraction 2 times with the emulsification pretreatment machine, shearing rotating speed for the first time is 10000rpm, and shear time is 5 minutes, and shearing rotating speed for the second time is 4000rpm, and shear time is 5 minutes;
(6) extract: the krill meal suspension liquid to shearing after extracting extracts, and separation and Extraction liquid extracts 1 time isolating krill meal again, and krill meal is 1: 8 with 91% ethanolic soln organic solvent solid-to-liquid ratio, stirs extraction 3 hours, and temperature is 30 ℃;
(7) solvent evaporates: united extraction liquid, 60 ℃ of temperature, vacuum tightness is rotary evaporation under-0.1MPa with extracting solution, and removing and obtaining phospholipids content in the extracting solution behind the second alcohol and water is 42.5% krill oil.
Embodiment 3
(1) heating: krill is fished for the back 50 ℃ of heating down, and 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 the pulverizing time is 3 minutes;
(4) soak: the ethanolic soln with 95% soaks krill meal down at 30 ℃, and 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 rotating speed for the first time is 6000rpm, and shear time is 5 minutes, and shearing rotating speed for the second time is 10000rpm, and shear time is 5 minutes;
(6) extract: the krill meal suspension liquid to shearing after extracting extracts, and separation and Extraction liquid extracts 3 times the krill powder again, and krill meal is 1: 2 with 95% ethanolic soln organic solvent solid-to-liquid ratio, stirs extraction 3 hours, and temperature is 30 ℃;
(7) solvent evaporates: united extraction liquid, 60 ℃ of temperature, vacuum tightness is rotary evaporation under-0.08MPa with extracting solution, and removing and obtaining phospholipids content in the extracting solution behind the second alcohol and water is 40.5% krill oil.
Embodiment 4
(1) heating: krill is fished for the back 120 ℃ of heating down, and 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: dry back krill is pulverized, and is crushed to 100 purpose krill meals, and the pulverizing time is 30 minutes;
(4) soak: the ethanolic soln with ethanol and 99% soaks krill meal down at 35 ℃, and 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 rotating speed for the first time is 4000rpm, and shear time is 10 minutes; For the second time shearing rotating speed is 6000rpm; Shear time is 10 minutes, and shearing rotating speed for the third time 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 to shearing after extracting extracts, and separation and Extraction liquid extracts 3 times the krill powder again, and krill meal is 1: 10 with 98% ethanolic soln organic solvent solid-to-liquid ratio, stirs extraction 3 hours, and temperature is 30 ℃;
(7) solvent evaporates: united extraction liquid, 60 ℃ of temperature, vacuum tightness is rotary evaporation under-0.1MPa with extracting solution, and removing and obtaining phospholipids content in the extracting solution behind the second alcohol and water is 44.5% krill oil.
Claims (7)
1. method of from krill, extracting high phospholipid content krill oil is characterized in that:
(1) heating: krill is fished for the back 50～120 ℃ of heating down, and be 3～20 minutes heat-up time;
(2) drying: the krill after will heating is dry, and drying temperature is 20～90 ℃;
(3) pulverize: dry back is ground into krill meal to krill, is crushed to 5～100 orders;
(4) soak: down soak krill meal at the ethanolic soln organic solvent more than 90% at 4～30 ℃ with concentration, 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 the 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 to shearing after extracting extracts; Separation and Extraction liquid, extraction and separation and Extraction liquid are 2～4 times again, and 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 ℃;
(7) solvent evaporates: united extraction liquid; With extracting solution 30～60 ℃, vacuum tightness-0.05～-0.1MPa under evaporation; Removing and obtaining phospholipids content in the extracting solution behind the organic solvent is 40%～45% krill oil; Feed gas and remove residual organic solvent in the shrimp sauce, make the Determination of Residual Organic Solvents National standard.
2. the method for the extraction high phospholipid content krill oil described in claim 1 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; It is characterized in that leaching process is sheared extraction 1～4 time to the krill meal suspension liquid after soaking with the emulsification pretreatment machine again; The shearing rotating speed is 4000～10000rpm, and shear time is 1～30 minute.
4. 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 or membrane filtration is removed moisture or MSF is removed moisture.
5. the method for getting high phospholipid content krill oil described in claim 1 or 2 is characterized in that, the pulverizing time was at 1～30 minute.
6. described in claim 3, extracting the method for high phospholipid content krill oil, it is characterized in that, is poach or the heating of pressurization poach under the normal atmosphere to the krill type of heating, and the isolated hot water in heating back is used for heating and extracting liquid, the evaporative removal organic solvent.
7. described in claim 4, extract the method for high phospholipid content krill oil, it is characterized in that the pulverizing time was at 1～30 minute.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102766530A (en) * | 2012-08-08 | 2012-11-07 | 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 |
| CN103141871A (en) * | 2013-04-03 | 2013-06-12 | 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 |
| CN104479850A (en) * | 2014-12-15 | 2015-04-01 | 中国水产科学研究院黄海水产研究所 | Method for extracting krill oil with high phospholipid content from fresh Antarctic krill |
| CN104479859A (en) * | 2014-11-27 | 2015-04-01 | 威海博宇食品有限公司 | Preparation method of roe extract |
| CN105536275A (en) * | 2016-01-29 | 2016-05-04 | 山东鲁华海洋生物科技有限公司 | Method and device for concentrating and separating euphausia superb oil extraction liquid |
| 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 |
| CN107904023A (en) * | 2017-12-21 | 2018-04-13 | 山东师范大学 | A kind of method that remaining grease is extracted in the dry shrimp slag from krill degreasing |
| 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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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102766530A (en) * | 2012-08-08 | 2012-11-07 | 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 |
| CN103141871A (en) * | 2013-04-03 | 2013-06-12 | 辽宁省大连海洋渔业集团公司 | Preparation method of euphausia superba powder |
| 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 |
| CN104479850A (en) * | 2014-12-15 | 2015-04-01 | 中国水产科学研究院黄海水产研究所 | Method for extracting krill oil with high phospholipid content from fresh Antarctic krill |
| 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 |
| CN105536275A (en) * | 2016-01-29 | 2016-05-04 | 山东鲁华海洋生物科技有限公司 | Method and device for concentrating and separating euphausia superb oil extraction liquid |
| 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 |
| CN107904023A (en) * | 2017-12-21 | 2018-04-13 | 山东师范大学 | A kind of method that remaining grease is extracted in the dry shrimp slag from krill degreasing |
| 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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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. |