CN103981021A - Method for refining krill oil from Antarctic krill powder - Google Patents
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Abstract
The invention relates to a method for refining krill oil from Antarctic krill powder, belonging to the technical field of deep processing of Antarctic krill. Acccording to the invention, the solvent ethanol and a small part of water in the extracting solution are removed not directly by one-step reduced pressure distillation, but are removed by the following steps: removing part of the solvent, adding deionized water, concentrating phospholipid, unsaturated fatty acids, krill astaxanthin and other effective substances by utilizing the characteristics of phospholipid, adding anhydrous ethanol to remove most of polysaccharides, proteins and salts, and finally, distilling under reduced pressure to remove the solvent and water. By using the refinement technique, the contents of the phospholipid DHA, EPA and other unsaturated fatty acids, astaxanthin and other effective components in the obtained krill oil are obviously enhanced, and the quality (flowability and transparency) of the obtained krill oil is obviously improved.
Description
Technical field
The present invention relates to a kind of method of refining krill oil from krill powder, belong to the deep process technology field of krill.
Background technology
Krill is perched in the marine site, the South Pole on the south the convergence zone of the South Pole, is a kind of marine crustacean.It plays an important role in Southern Oceans food chain, is the food of sea dog, whale and penguin, is also important Living marine resources.Krill is precious from head to foot, in its body, be rich in phosphatide, lipid acid, phosphorus astaxanthin, low temperature active enzyme, biologically active peptides, chitin isoreactivity material, can be in field widespread uses such as medicine, chemical industry, agricultural, aquatic products, and krill marine stock biomass is abundant, therefore huge to its comprehensive deep development utility value.
The phosphatide that comprises abundant polyunsaturated fatty acid (DHA and EPA) combination the krill oil extracting from krill, therefore antarctic krill oil has the basic function of mental, stable nerve of the enhancing of phosphatide, balance internal secretion, raising immunizing power and regeneration power, removing toxic substances diuresis, blood clean, vigorous and graceful skin concurrently, and effect of the prophylactic treatment cardiovascular disorder of polyunsaturated fatty acid, the pain that reduces inflammation, alleviate premenstrual syndrome and dysmenorrhoea, reduction prostate cancer morbidity.In addition, be rich in phosphorus astaxanthin, VITAMIN and flavonoid in antarctic krill oil, therefore edible antarctic krill oil is not only of value to brain health, for anti-oxidant, remove free radical and delay senility and there is equally good effect.Antarctic krill oil becomes the upgrading products of human health day by day, will start new era of functional nutrient food industries.
The method of extracting at present antarctic krill oil is mainly organic solvent extraction method and the supercritical carbon dioxide extraction method that adopts normal hexane, No. 6 gasoline, sherwood oil etc.Organic solvent extraction method, refers to the krill oil in organic solvent soaking extraction krill, then adopts the mode of heating decompression by organic solvent evaporation, thereby obtains krill oil.But this method exists the content of the unsaturated fatty acids such as phosphatide, DHA, EPA, phosphorus astaxanthin, vitamin A, E, animal Protoapigenone, trace element of the krill oil extracting low, the problem that organic solvent residual is high.And supercritical carbon dioxide extraction method, also lower problem of phospholipids content in the lower and krill oil that extracts of the product extraction yield that exists.
Summary of the invention
Extract the existing above-mentioned technical problem of krill oil in order to solve organic solvent extraction method, contriver attempts using South Pole krill meal as raw material, using ethanol as solvent extraction krill oil; Described krill powder is to be pulverized and formed by krill.The steps include: krill powder ethanol fully to dissolve acquisition leaching liquid, then leaching liquid is directly adopted to the ethanol that remove side of underpressure distillation, thereby obtain krill oil.But adopt the krill oil of preparation in this way, the foreign matter contents such as the krill oil free fatty acid obtaining, polysaccharide, albumen, salt are high, and the content of the unsaturated fatty acidss such as phosphatide, DHA, EPA is low.In any case change underpressure distillation condition, in krill oil, the content of phosphatide is all the time below 40%.
For this reason, contriver provides a kind of unsaturated fatty acid contents such as phosphatide, DHA, EPA in krill oil quality and krill oil that can effectively improve, from the krill powder method of refining krill oil by further research.
Method of refining krill oil from krill powder of the present invention; Comprise the steps:
(1) 90-100% ethanol leaching for krill powder, obtains extracting solution; Then remove part ethanol in extracting solution, obtaining extractive content is 10-20% concentrated solution;
(2) by the concentrated solution heating in water bath to 50 DEG C of step 1, then in slurry tank, add deionized water and mix, leave standstill to layering, collect subnatant;
(3) subnatant of step (2) is mixed in slurry tank to rear leaving standstill with dehydrated alcohol, then bleed off undissolved throw out, retain lysate;
(4) lysate of step 3 is put into scraper concentrator and heated underpressure distillation and remove second alcohol and water wherein, obtain refining krill oil; Heating underpressure distillation condition: temperature is no more than 62 DEG C, vacuum tightness-0.09MPa.
In step (1), extract refers to thick oil, comprises effective constituent: the unsaturated fatty acidss such as phosphatide, DHA, EPA etc.; Also comprise impurity free fatty acids, polysaccharide, albumen, salt etc., by distilling dry detection.
In step (2), the stratification time used is generally 3-4 hour.
The present invention directly removes etoh solvent and the small part water in extracting solution by the mode of a underpressure distillation, but first remove partial solvent, then add deionized water to utilize the characteristic of phosphatide, the active substances such as the mode concentrated phosphatide by physics sedimentation and unsaturated fatty acids, phosphorus astaxanthin, add dehydrated alcohol to go out most of polysaccharide, albumen and salinity, solvent and water are removed in last underpressure distillation again.Adopt this process for refining, the effective constituents such as unsaturated fatty acids and astaxanthin such as phosphatide DHA, EPA in the krill oil obtaining obviously improve, and the quality of the krill oil obtaining (mobility and transparency) obviously improves.
The height of step (1) alcohol concn can affect quality, the extraction yield of krill oil, the content of active substance, along with the reduction of alcohol concn, extraction yield improves, phospholipids content improves, but phosphorus astaxanthin, transparency reduce, and viscosity increased, after alcohol concn is lower than 90%, krill oil poor quality, most preferred ethanol concentration is 95% or 100%.
Step (1) concentrated solution concentration is that 10-20% is one of gordian technique of this technique, lower than this numerical value, will increase production cost, will affect the quality of krill oil higher than this numerical value, and most preferable concentrations is 15%.
Step (2) order that physics sedimentation and step (3) add the sedimentation of ethanol physics that adds water can not be put upside down, if put upside down, with respect to the method for existing direct underpressure distillation, the active substance content of krill oil does not obviously change.
The add water consumption of water in physics settling process of step (2) can affect the quality of extraction yield and krill oil; The consumption of water is determined according to different starting material, is preferably the 40-70wt% of concentrated solution.In this amount ranges, oil extracting rate is higher, and in gained krill oil, phospholipids content is higher.General water is most preferred is 58 wt% of concentrated solution.
The consumption that step (3) adds dehydrated alcohol in ethanol physics settling process can affect the quality of production cost and krill oil; So the consumption of dehydrated alcohol is preferably 1.5-2.5 times of subnatant quality.In this amount ranges, oil extracting rate is higher, and in gained krill oil, phospholipids content is higher, and production cost is minimum.Dehydrated alcohol is most preferred is 2 times of subnatant quality.
When step (4) scraper concentrator final evaporation moisture, temperature can not be too high, and exceeding 70 DEG C of phosphatide will gelatinization, and krill oil darkens, and unsaturated fatty acids and phosphorus astaxanthin are destroyed, affect krill oil quality.
Aforesaid method, in step (1), " krill powder for 90-100% ethanol leaching " and " removing part ethanol in extracting solution " can adopt any operating method realization of the prior art, as long as can " obtaining extractive content is 10-20% concentrated solution ".But, as well known to a person skilled in the art be, the concrete operations mode difference of " 90-100% ethanol leaching for krill powder ", the content difference of extract in extracting solution, concentrated needed time and energy consumption are also different.In order to improve content, shortening concentration time, the reduction energy consumption of extract in extracting solution, " krill powder leaches with ethanol " preferably adopts following concrete operations mode:
The first step: get krill powder, repeatedly leach n time with ethanol, obtain respectively the 1st ..., n extracting solution; No. the 1st extracting solution is for concentrated;
Second step: get krill powder, repeatedly leach n time; Obtain respectively the 1st ..., n extracting solution;
Wherein, the 1st leaching adopts No. the 2nd extracting solution of previous step as solvent, and the n-1 time leaching adopts the n time extracting solution of previous step as solvent, and the n time leaching adopts ethanol as solvent; No. the 1st extracting solution that this step obtains is for concentrated, and the n time extracting solution leaches for the n-1 time of next step;
In the time of n=3, the n-1 time extracting solution that this step obtains leaches for the n-2 time of next step;
Constantly repeat second step;
N value in each step is identical, n=2 or 3; The leaching condition of each step is: feed liquid weight ratio is 1:3-4, and 10-40 DEG C of temperature condition soaks after 0.5-2 hour and filter.
Adopt aforesaid way leaching krill powder, in each step, only add ethanol one time, thereby reduce the consumption of ethanol, reduce raw materials cost; In the 1st leaching liquid obtaining in each step, the content of extract, for up to 5-8%, has improved the content of extract, shortens concentration time.In addition, adopt aforesaid operations mode, although the consumption of solvent reduces, the leaching amount of krill oil does not reduce, and can not cause disadvantageous effect to the productive rate of krill oil.
Aforesaid method, " krill powder leaches with ethanol " can also adopt the mode of countercurrent extraction to complete: krill powder and ethanol are utilized to counterflow extraction apparatus, under 10-40 DEG C of condition, extract continuously, control solid-liquid ratio is 1:5-8, extraction time 0.5-2 hour.
Aforesaid method, the concrete operations of " removing part ethanol in extracting solution " are: extracting solution is put into single-action or double-effect evaporator, to-0.09MPa condition, heat reduction vaporization at vacuum tightness-0.06MPa, remove partial solvent in extracting solution, obtaining extractive content is 15% concentrated extracting solution, carry out classified filtering, and be finally that 0.22-0.45um strainer is removed impurity by aperture.
Beneficial effect
In the prepared antarctic krill oil of the present invention, phospholipids content is more than 52%, and contains the multiple nutritive elements useful to human body such as the abundant unsaturated fatty acids such as DHA, EPA, phosphorus astaxanthin, vitamin A, E, animal Protoapigenone, trace element; The foreign matter contents such as free fatty acids, polysaccharide, albumen, salt are low; Good fluidity, the transparency of krill oil are high;
The extraction yield (calculating taking South Pole krill meal as radix) of krill oil is as 5-18%(is because of the different variations to some extent of krill powder oleaginousness);
The peculiar fragrance of antarctic krill oil and beautiful redness are kept.
Embodiment
Embodiment 1.1-1.13
Prepare krill oil crude extract
(1) getting 1 part of krill powder adds the ethanol that 3-4 times of weight part food grade mass concentration is M to put into extractor, soak at ambient temperature 2 hours, then adopt classified filtering, the strainer that is finally 0.45um by aperture, obtaining extractive content is No. the 1st extracting solution and the filter residue of 3-5%.Filter residue is added to the ethanol that the food grade mass concentration of its 3 times of weight parts is M again, soak at ambient temperature 2 hours, then adopt classified filtering, the strainer that is finally 0.45um by aperture, obtains extracting solution and filter residue No. the 2nd time.Filter residue is added to the ethanol that the food grade mass concentration of its 3 times of weight parts is M again, soak at ambient temperature 2 hours, then adopt classified filtering, the strainer that is finally 0.45um by aperture, obtains extracting solution and filter residue No. the 3rd time.
(2) again get No. the 2nd extracting solution that 1 part of krill powder adds the step (1) of its 3 times of weight parts, soak at ambient temperature 2 hours, then adopt classified filtering, the strainer that is finally 0.45um by aperture, obtains extractive content and is No. the 1st extracting solution and the filter residue a of 5-8%.No. the 3rd extracting solution that filter residue a is added again to the step (1) of its 3 times of weight parts, soaks 2 hours at ambient temperature, then adopts classified filtering, and the strainer that is finally 0.45um by aperture obtains No. the 2nd extracting solution and filter residue b.Filter residue b is added to the ethanol that the food grade mass concentration of its 3 times of weight parts is M again, soak at ambient temperature 2 hours, then adopt classified filtering, the strainer that is finally 0.45um by aperture, obtains No. the 3rd extracting solution and filter residue c.Constantly repeating step (2), No. the 2nd, 3 extracting solutions of gained are for next leaching process.No. the 1st extracting solution of leaching process gained is krill oil crude extract each time.
Refining krill oil
(3) krill oil crude extract is put into single-action or double-effect evaporator, to-0.08MPa condition, heat reduction vaporization in vacuum tightness-0.06, remove partial solvent in extracting solution, obtain the concentrated extracting solution that extractive content is N (N refers to the mass content of extract with respect to concentrated extracting solution); Then carry out classified filtering, and be finally that 0.22-0.45um strainer is removed impurity by aperture, obtain concentrated solution.
(4), by concentrated solution heating in water bath to 50 DEG C, then add its weight x(x to refer to and will add the amount of deionized water and the mass percent of concentrated solution) water mix, leave standstill to layering (being generally 4 hours), collect subnatant;
(5) subnatant of step (4) being collected mixes with the dehydrated alcohol of its y times weight, and standing sedimentation bleeds off undissolved throw out after 2 hours, retains lysate;
(6) lysate is put into scraper plate or decompression concentrator, controlled outlet temperature and be no more than 62 DEG C, under vacuum tightness-0.09MPa condition, heat reduction vaporization, remove second alcohol and water wherein, obtain refining krill oil.In above-mentioned preparation process, the value of M, N, x, y is as table 1.
Embodiment 2
Krill powder and food grade 95% ethanol are utilized to counterflow extraction apparatus, extract continuously at ambient temperature, control solid-liquid ratio is 1:5-8, extraction time 0.5-2 hour, and collecting extracting solution is krill oil crude extract.Adopt the method steps of embodiment 1.1-1.13 " refining krill oil " to refine krill oil crude extract, obtain refining krill oil.
Comparative example 1
Step (1), (2), (3) are identical with step, the parameter of embodiment 1.1;
(4) concentrated solution is mixed with the dehydrated alcohol of its y times weight, standing sedimentation bleeds off undissolved throw out after 2 hours, retains lysate;
(5) by lysate heating in water bath to 50 DEG C, then add the water of its weight 58% to mix, leave standstill 4 hours (now layering completely), collect subnatant;
(6) subnatant is put into scraper plate or decompression concentrator, controlled outlet temperature and be no more than 62 DEG C, under vacuum tightness-0.09MPa condition, heat reduction vaporization, remove second alcohol and water wherein, obtain refining krill oil.
Comparative example 2
Get 1 part of krill powder and add 3-4 part food grade 95% ethanol, soak at ambient temperature 2 hours, then adopt classified filtering, the strainer that is finally 0.45um by aperture, obtains extracting solution and filter residue No. the 1st time.Food grade 95% ethanol that filter residue is added again to its 3 times of weight parts, soaks 2 hours at ambient temperature, then adopts classified filtering, and the strainer that is finally 0.45um by aperture, obtains extracting solution and filter residue No. the 2nd time.Food grade 95% ethanol that filter residue is added again to its 3 times of weight parts soaks 2 hours under room temperature DEG C condition, then adopts classified filtering, and the strainer that is finally 0.45um by aperture, obtains extracting solution No. the 3rd time.No. the 1st, 2,3 extracting solutions are merged, put into single-action or double-effect evaporator, to-0.08MPa condition, heat reduction vaporization in vacuum tightness-0.06, remove the second alcohol and water in extracting solution, obtain krill oil.
Above-described embodiment and the prepared krill oil of comparative example are detected, and detected result is as table 1.
In table 1, the implication of krill oil oil extracting rate is obtained krill oil and the mass ratio of the krill powder for extracting krill oil, and in form, data show that more greatly extraction yield is higher;
Phospholipids content, DHA/EPA content, content astaxanthin, adopt national standard to detect;
Mobility and the transparency of the prepared krill oil of visual inspection, comparative example and comparative example, draw " fine, good, general, poor, very poor " different comment.
Table 1:
。Data analysis in his-and-hers watches 1 draws to draw a conclusion:
Embodiment 1.1 is preferred embodiments;
Embodiment 1.2-1.4 is compared with embodiment 1.1, and only in step 1, alcohol concn changes, and when embodiment 1.4 alcohol concn are during lower than the scope of protection of present invention, its phosphorus content astaxanthin is low, and krill oil mobility is very poor, poor transparency;
Embodiment 1.5-1.7 is compared with embodiment 1.1, and only in step 3, in concentrated extracting solution, the content of extract changes; When the content of embodiment 1.7 extracts is 25%, while exceeding the scope of protection of present invention, phospholipids content is lower, and phosphorus content astaxanthin is lower, krill oil poor fluidity, and transparency is very poor;
Embodiment 1.8-1.10 is compared with embodiment 1.1, and only in step 4, the consumption of water changes; When the consumption of embodiment 1.10 water is 80%, while exceeding the scope of protection of present invention, phospholipids content is lower, and phosphorus content astaxanthin is lower, and krill oil mobility is very poor, and transparency is very poor;
Embodiment 1.11-1.13 is compared with embodiment 1.1, and only in step 5, the consumption of dehydrated alcohol changes; In the time that the consumption of embodiment 1.13 dehydrated alcohols is 1 times, during lower than the scope of protection of present invention, phospholipids content is lower, and phosphorus content astaxanthin is lower, and transparency is very poor.
Claims (10)
1. a method for refining krill oil from krill powder, is characterized in that, comprises the steps:
(1) 90-100% ethanol leaching for krill powder, obtains extracting solution; Then remove part ethanol in extracting solution, obtaining extractive content is 10-20% concentrated solution;
(2) by the concentrated solution heating in water bath to 50 DEG C of step 1, then in slurry tank, add deionized water and mix, leave standstill to layering, collect subnatant;
(3) subnatant of step (2) is mixed in slurry tank to rear leaving standstill with dehydrated alcohol, then bleed off undissolved throw out, retain lysate;
(4) lysate of step 3 is put into scraper concentrator and heated underpressure distillation and remove second alcohol and water wherein, obtain refining krill oil; Heating underpressure distillation condition: temperature is no more than 62 DEG C, vacuum tightness-0.09MPa.
2. method according to claim 1, is characterized in that, step (1) alcohol concn is 95% or 100%.
3. method according to claim 1, is characterized in that, step (1) concentrated solution concentration is 15%.
4. method according to claim 1, is characterized in that, in step (2), the stratification time used is 3-4 hour.
5. method according to claim 1, is characterized in that, step (2) 40-70wt% that the consumption of water is concentrated solution in physics settling process that adds water.
6. method according to claim 1, is characterized in that, the consumption that step (3) adds dehydrated alcohol in ethanol physics settling process be subnatant quality 1.5-2.5 doubly.
7. method according to claim 5, is characterized in that, step (2) 58wt% that the consumption of water is concentrated solution in physics settling process that adds water.
8. method according to claim 6, is characterized in that, the consumption that step (3) adds dehydrated alcohol in ethanol physics settling process is 2 times of subnatant quality.
9. method according to claim 1, is characterized in that, in step (1), " for krill powder, 90-100% ethanol leaches " adopts following operating method:
Mode one:
The first step: get krill powder, repeatedly leach n time with ethanol, obtain respectively the 1st ..., n extracting solution; No. the 1st extracting solution is for concentrated;
Second step: get krill powder, repeatedly leach n time; Obtain respectively the 1st ..., n extracting solution;
Wherein, the 1st leaching adopts No. the 2nd extracting solution of previous step as solvent, and the n-1 time leaching adopts the n time extracting solution of previous step as solvent, and the n time leaching adopts ethanol as solvent; No. the 1st extracting solution that this step obtains is for concentrated, and the n time extracting solution leaches for the n-1 time of next step;
In the time of n=3, the n-1 time extracting solution that this step obtains leaches for the n-2 time of next step;
Constantly repeat second step;
N value in each step is identical, n=2 or 3; The leaching condition of each step is: feed liquid weight ratio is 1:3-4, and 10-40 DEG C of temperature condition soaks after 0.5-2 hour and filter;
Or, mode two:
Adopt the mode of countercurrent extraction to complete: krill powder and ethanol are utilized to counterflow extraction apparatus, under 10-40 DEG C of condition, extract continuously, control solid-liquid ratio is 1:5-8, extraction time 0.5-2 hour.
10. method according to claim 1, it is characterized in that, the concrete operations of " removing part ethanol in extracting solution " are: extracting solution is put into single-action or double-effect evaporator, to-0.09MPa condition, heat reduction vaporization at vacuum tightness-0.06MPa, remove partial solvent in extracting solution, obtaining extractive content is 15% concentrated extracting solution, carries out classified filtering, and is finally that 0.22-0.45um strainer is removed impurity by aperture.
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