CN102888274A - Method for extracting crude fish oil from hairtail silvery fat - Google Patents
Method for extracting crude fish oil from hairtail silvery fat Download PDFInfo
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- CN102888274A CN102888274A CN2012103774236A CN201210377423A CN102888274A CN 102888274 A CN102888274 A CN 102888274A CN 2012103774236 A CN2012103774236 A CN 2012103774236A CN 201210377423 A CN201210377423 A CN 201210377423A CN 102888274 A CN102888274 A CN 102888274A
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Abstract
The invention discloses a method for extracting crude fish oil from hairtail silvery fat, which comprises the following steps: 1) adding water to the hairtail silvery fat; adding neutral protease again; processing enzyme for 2.5-3.5 hours at 45-52 degrees centigrade; 2) processing inactivation treatment of the neutral protease to acquired enzyme solution, adding petroleum ether, processing extraction for 25-35 minutes in warm bath at 38-42 degrees centigrade; 3) rotating and evaporating the petroleum ether located on an upper layer obtained in the step 2) so as to ventilate the petroleum ether, and acquiring the crude fish oil containing impurity; and 4) centrifuging the crude fish oil containing the impurity, separating acquired supernatant, wherein the supernatant is the crude fish oil. By dint of the invention, the crush fish oil with relatively high concentration can be acquired.
Description
Technical field
The present invention relates to a kind of method of processing extraction crude fish oil the residual silver-colored fat from hairtail.
Background technology
Along with the development research of marine food, the functional ingredient of fish oil more and more receives people's concern, and the application of fish oil is very extensive, and such as health care, medicine, food etc., world's fish oil output is very large, but at present the domestic fish oil output of China is lower.The hairtail aboundresources, however present hairtail is mainly used in the processing of fish product, can produce many tankage in the course of processing, these tankage added values are low, and the fish oil that the inside is contained fails to bring into play good effect.In addition, the fatty ingredient in the tankage is rich in polyunsaturated fatty acid, and easily oxidative rancidity is rotten.If these tankage are in time processed, not only cause the waste of resource, and can be to environment.
The silver-colored fat on hairtail top layer contains more unsaturated fatty acids, and fatty acid carbon chain is longer again, has reducing cholesterol, strengthens the skin surface cell viability, makes the delicate bright and clean effect of skin; Hairtail contains abundant Yelkin TTS, makes its more general fresh-water fishes have more the benefit brain function.
EPA and DHA have the functions such as the platelet aggregation of inhibition, antithrombotic, vasodilator, adjustment blood fat and raising biomembrane fluidity, at aspects such as treatment and prevention and cure of cardiovascular disease, diabetes, dermatitis, large intestinal ulcer and inhibition tumours preferably curative effect is arranged, discovered in recent years also has the physiological functions such as antidepressant, prevention rheumatic arthritis and senile dementia simultaneously.
Traditional fish oil production method has milling process, and solvent method etc., the raw material that this class methods are utilized are tankage or the band fish viscera of hairtail processing, but not only the extraction yield of crude fish oil is lower and also can destroy its original composition for these class methods.
Summary of the invention
Technical problem to be solved by this invention provides a kind of technique is simply extracted crude fish oil from hairtail silver fat method, adopts method of the present invention can obtain the higher crude fish oil of concentration.
In order to solve the problems of the technologies described above, the invention provides a kind of method of from hairtail silver fat, extracting crude fish oil, may further comprise the steps:
1), in 1g hairtail silver fat, add 1 ~ 3ml water, adds again neutral protease, in 45 ~ 52 ℃ of enzymolysis 2.5 ~ 3.5 hours; Neutral protease is that 1.5 ~ 3.2%(the best of hairtail silver fat weight is 3%);
2), the enzymolysis solution of step 1) gained carried out the inactivation treatment of neutral protease after, add again that 3.5 ~ 4.5ml(is best to be 4ml) sherwood oil, bathing extraction 25 ~ 35min(the best in 38 ~ 42 ℃ of lower temperature be to extract 30min in 40 ℃ of lower temperature baths);
3), with step 2) the petroleum ether extraction liquid (as organic phase) that is positioned at the upper strata of gained is in rotary evaporation (for example being 58 ~ 62 ℃), thereby sherwood oil is removed in volatilization, obtains containing the crude fish oil of impurity;
4), the crude fish oil that will contain impurity is the centrifugal 10min of 3000 r/min in the centrifugal 8 ~ 12min(the best of 2500 ~ 3500 r/min), separating obtained supernatant, this supernatant are crude fish oil.
As improvement of extracting the method for crude fish oil from hairtail silver fat of the present invention: it for example is 4 that the enzymolysis solution of step 1) gained is transferred pH to 3.9 ~ 4.1(), thus realize the inactivation treatment of centering proteolytic enzyme.
As the further improvements in methods of extracting crude fish oil from hairtail silver fat of the present invention: adopting concentration step 2) is for example 0.1mol/L of 0.08 ~ 0.12 mol/L() hydrochloric acid soln regulate the pH of enzymolysis solution.
As the further improvements in methods of extracting crude fish oil from hairtail silver fat of the present invention: step 1) is:
In 1g hairtail silver fat, add 1ml water, add again neutral protease, in 50 ℃ of enzymolysis 3 hours;
Neutral protease is 3% of hairtail silver fat weight.
Hairtail silver fat of the present invention is that hairtail is through processing the rear residual exterior skin silver fat such as the removal flesh of fish, fish-bone and internal organ.
In the present invention, neutral protease is conventional commercially available prod, for example the optional neutral protease of using the YY10511 of source, Shanghai leaf bio tech ltd production.
The crude fish oil of gained of the present invention can adopt conventional freezing preservation method to preserve.
Adopt method of the present invention, the yield of fish oil is 29.6%, and light yellow is comparatively transparent, has stronger fish oil fishy smell.
The lipid acid that adopts gc analysis to detect the crude fish oil of gained of the present invention forms, and it contains the material (following % is quality %) of following component:
The crude fish oil of gained of the present invention is refined into the higher refined fish oil of purity, for example can be according to the urea entraing method of routine
[1,2], molecular distillation method
[3,4], the crystallizing process under low temperature
[5], silver ion complexation
[6,7]Deng operating.
[1] Du Qiguang, Wang Zhixiang, field dragon. the technical study [J] of the EPA in the urea adduct method enrichment fish oil and DHA. print 2009,23 (9): 13-15 during chemical industry.
[2] He Jiandong, Wang Peng, Hu Ye etc. fish oil preparation and EPA and DHA enriching and purifying Research progress [J]. oil engineering, 2011 (7): 56-58.
[3] Fu Hong, fur coat like to chant. and molecular distillation method prepares fish oil polyunsaturated fatty acid [J]. Wuxi Light Industry Univ.'s journal, 2002,21 (6): 617-621.
[4] Fu Hong, Qiu Aiyong. molecular distillation method enrichment fish oil omega-fatty acid [J]. Chinese grain and oil journal, 2006,21 (3): 156-159.
[5] Lee and, Li Peiwen, Yang Yiping. the method [J] of EPA and DHA in the low temperature crystallization enrichment fish oil. Chinese Sea medicine, 1997 (4): 50-52.
[6] Tao Zunwei, Xie Hongwu, Liu Huizhi. the experimental study [J] of Silver Nitrate-water law purifying high content DHA and EPA. Chinese Sea medicine, 2004 (3): 28-30.
[7] Jiang Lili, Chen Jun. the EPA in the response surface method optimization silver ion complexation extraction fish oil and the technical study [J] of DHA. food science and technology, 2008 (5): 92-95.
Method of the present invention has following advantage and beneficial effect:
(1) the present invention utilizes neutral protease to come catalysis take water as medium, extracts under the condition of gentleness, has obtained enzymolysis solution, and then has utilized sherwood oil to extract, and after the centrifugation, obtains crude fish oil; Therefore have the characteristics such as technique is succinct, easy handling.
(2) the present invention leniently discharges fat in the residual silver-colored fat by zymolysis technique, thereby extracts fish oil more efficiently, obviously improves the fish oil extraction yield, also the drawback that traditional method can occur can not occur, and is residual etc. such as reagent.It is gentle that enzymolysis is carried the oil process reaction conditions, and parameter is easy to control, and is little to the loss that physiologically active ingredient causes, and also do not pollute the environment.
(3) enzymolysis solution that obtains behind the enzymolysis extracts again with sherwood oil, has greatly improved the extraction yield of crude fish oil.
(4) fatty acid component in the crude fish oil is carried out the analysis on the composition, for the comprehensive utilization with fish resource provides theoretical foundation, created added value of product.
(5) the present invention utilizes enzymolysis process, utilizes proteolytic enzyme to destroy the protein that combines with grease, and mild condition is polluted littlely, and the extraction object height is aided with solvent extraction again, more efficiently fish oil is extracted.
(6) the light yellow of the crude fish oil of gained is comparatively transparent, has stronger fish oil fishy smell.The yield of fish oil can be up to 29.6%, and the lipid acid that adopts gc analysis to detect crude fish oil forms, and records it and contains the multiple lipid acid such as EPA and DHA.
Embodiment
Hairtail of the present invention silver fat be hairtail through processing, remove residual exterior skin silver fat behind the flesh of fish, fish-bone and the internal organ.
Embodiment 1, a kind of method of from hairtail silver fat, extracting crude fish oil, carry out successively following steps:
1), in 15g hairtail silver fat, add 15ml water, add again the neutral protease of 0.3g, enzymolysis is 2.5 hours under 45 ℃ hydrolysis temperature;
2), to utilize concentration be the hydrochloric acid soln regulating step 1 of 0.1 mol/L) pH to 4 of the enzymolysis solution of gained, thereby realize the inactivation treatment of centering proteolytic enzyme; Then the sherwood oil that adds 60ml is bathed extraction 30min in 40 ℃ of lower temperature;
3), with step 2) the petroleum ether extraction liquid rotary evaporation (in 58 ~ 62 ℃) that is positioned at the upper strata of gained, thereby sherwood oil is removed in volatilization, obtains containing the crude fish oil of impurity;
4), the crude fish oil that will contain impurity is in the centrifugal 10min of 3000 r/min, separating obtained supernatant, supernatant are crude fish oil.
Get crude fish oil 3.615g, yield 24.1%.
In this crude fish oil, the content of DHA is that the content of 14%, EPA is 7%.
Embodiment 2, a kind of method of from hairtail silver fat, extracting crude fish oil, carry out successively following steps:
1), in 15g hairtail silver fat, add 15ml water, add again the neutral protease of 0.45g, enzymolysis is 3 hours under 50 ℃ hydrolysis temperature;
2), to utilize concentration be the hydrochloric acid soln regulating step 1 of 0.1 mol/L) pH to 4 of the enzymolysis solution of gained, thereby realize the inactivation treatment of centering proteolytic enzyme; Then the sherwood oil that adds 60ml is bathed extraction 30min in 40 ℃ of lower temperature;
3), with step 2) the petroleum ether extraction liquid rotary evaporation (in 58 ~ 62 ℃) that is positioned at the upper strata of gained, thereby sherwood oil is removed in volatilization, obtains containing the crude fish oil of impurity;
4), the crude fish oil that will contain impurity is in the centrifugal 10min of 3000 r/min, separating obtained supernatant, supernatant are crude fish oil.
Get crude fish oil 4.44g, yield 29.6%.
In this crude fish oil, the content of DHA is that the content of 14%, EPA is 7%.
Embodiment 3, a kind of method of from hairtail silver fat, extracting crude fish oil, carry out successively following steps:
1), in 15g hairtail silver fat, add 30ml water, add again the neutral protease of 0.3g, enzymolysis is 3 hours under 45 ℃ hydrolysis temperature;
2), to utilize concentration be the hydrochloric acid soln regulating step 1 of 0.1 mol/L) pH to 4 of the enzymolysis solution of gained, thereby realize the inactivation treatment of centering proteolytic enzyme; Then the sherwood oil that adds 60ml is bathed extraction 30min in 40 ℃ of lower temperature;
3), with step 2) the petroleum ether extraction liquid rotary evaporation (in 58 ~ 62 ℃) that is positioned at the upper strata of gained, thereby sherwood oil is removed in volatilization, obtains containing the crude fish oil of impurity;
4), the crude fish oil that will contain impurity is in the centrifugal 10min of 3000 r/min, separating obtained supernatant, supernatant are crude fish oil.
Get crude fish oil 3.66g, yield 24.4%.
In this crude fish oil, the content of DHA is that the content of 14%, EPA is 7%.
Embodiment 4, a kind of method of from hairtail silver fat, extracting crude fish oil, carry out successively following steps:
1), in 15g hairtail silver fat, add 45ml water, add again the neutral protease of 0.225g, enzymolysis is 3 hours under 45 ℃ hydrolysis temperature;
2), to utilize concentration be the hydrochloric acid soln regulating step 1 of 0.1 mol/L) pH to 4 of the enzymolysis solution of gained, thereby realize the inactivation treatment of centering proteolytic enzyme; Then the sherwood oil that adds 60ml is bathed extraction 30min in 40 ℃ of lower temperature;
3), with step 2) the petroleum ether extraction liquid rotary evaporation (in 58 ~ 62 ℃) that is positioned at the upper strata of gained, thereby sherwood oil is removed in volatilization, obtains containing the crude fish oil of impurity;
4), the crude fish oil that will contain impurity is in the centrifugal 10min of 3000 r/min, separating obtained supernatant, supernatant are crude fish oil.
Get crude fish oil 3.975g, yield 26.5%.
In this crude fish oil, the content of DHA is that the content of 14%, EPA is 7%.
Embodiment 5, a kind of method of from hairtail silver fat, extracting crude fish oil, carry out successively following steps:
1), in 15g hairtail silver fat, add 45ml water, add again the neutral protease of 0.45g, enzymolysis is 2.5 hours under 40 ℃ hydrolysis temperature;
2), to utilize concentration be the hydrochloric acid soln regulating step 1 of 0.1 mol/L) pH to 4 of the enzymolysis solution of gained, thereby realize the inactivation treatment of centering proteolytic enzyme; Then the sherwood oil that adds 60ml is bathed extraction 30min in 40 ℃ of lower temperature;
3), with step 2) the petroleum ether extraction liquid rotary evaporation (in 58 ~ 62 ℃) that is positioned at the upper strata of gained, thereby sherwood oil is removed in volatilization, obtains containing the crude fish oil of impurity;
4), the crude fish oil that will contain impurity is in the centrifugal 10min of 3000 r/min, separating obtained supernatant, supernatant are crude fish oil.
Get crude fish oil 3.69g, yield 24.6%.
In this crude fish oil, the content of DHA is that the content of 14%, EPA is 7%.
At last, it is also to be noted that, what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (4)
1. from hairtail silver fat, extract the method for crude fish oil, it is characterized in that may further comprise the steps:
1), in 1g hairtail silver fat, add 1 ~ 3ml water, adds again neutral protease, in 45 ~ 52 ℃ of enzymolysis 2.5 ~ 3.5 hours;
Described neutral protease is 1.5 ~ 3.2% of hairtail silver fat weight;
2), the enzymolysis solution of step 1) gained carried out the inactivation treatment of neutral protease after, add again the sherwood oil of 3.5 ~ 4.5ml, bathe extraction 25 ~ 35min in 38 ~ 42 ℃ of lower temperature;
3), with step 2) the petroleum ether extraction liquid rotary evaporation that is positioned at the upper strata of gained, thereby sherwood oil is removed in volatilization, obtains containing the crude fish oil of impurity;
4), the crude fish oil that will contain impurity is in the centrifugal 8 ~ 12min of 2500 ~ 3500 r/min, separating obtained supernatant, described supernatant are crude fish oil.
2. the method for extracting crude fish oil from hairtail silver fat according to claim 1 is characterized in that: the enzymolysis solution of step 1) gained is transferred pH to 3.9 ~ 4.1, thereby realize the inactivation treatment of centering proteolytic enzyme.
3. the method for extracting crude fish oil from hairtail silver fat according to claim 2 is characterized in that: adopting concentration described step 2) is the pH that the hydrochloric acid soln of 0.08 ~ 0.12 mol/L is regulated enzymolysis solution.
4. according to claim 1, the 2 or 3 described methods of from hairtail silver fat, extracting crude fish oil, it is characterized in that: described step 1) is:
In 1g hairtail silver fat, add 1ml water, add again neutral protease, in 50 ℃ of enzymolysis 3 hours;
Described neutral protease is 3% of hairtail silver fat weight.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105132122A (en) * | 2015-09-11 | 2015-12-09 | 江苏锦宇环境工程有限公司 | Method of preparing biodiesel by utilizing grass carp visceral fat |
| CN107320497A (en) * | 2017-07-24 | 2017-11-07 | 武汉轻工大学 | Purposes of the sturgeon extract oil in lowering fat and protecting liver health food or medicine is prepared |
| CN111826236A (en) * | 2020-07-13 | 2020-10-27 | 昆山全亚冠环保科技有限公司 | Method for recovering fish oil and silver from silver-containing fish oil waste liquid |
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Patent Citations (6)
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105132122A (en) * | 2015-09-11 | 2015-12-09 | 江苏锦宇环境工程有限公司 | Method of preparing biodiesel by utilizing grass carp visceral fat |
| CN107320497A (en) * | 2017-07-24 | 2017-11-07 | 武汉轻工大学 | Purposes of the sturgeon extract oil in lowering fat and protecting liver health food or medicine is prepared |
| CN111826236A (en) * | 2020-07-13 | 2020-10-27 | 昆山全亚冠环保科技有限公司 | Method for recovering fish oil and silver from silver-containing fish oil waste liquid |
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