CN109439430A - A kind of method of refining of antarctic krill oil - Google Patents
A kind of method of refining of antarctic krill oil Download PDFInfo
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- CN109439430A CN109439430A CN201811231008.3A CN201811231008A CN109439430A CN 109439430 A CN109439430 A CN 109439430A CN 201811231008 A CN201811231008 A CN 201811231008A CN 109439430 A CN109439430 A CN 109439430A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/12—Production of fats or fatty oils from raw materials by melting out
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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/115—Fatty acids or derivatives thereof; Fats or oils
- A23L33/12—Fatty acids or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
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Abstract
The invention discloses a kind of method of refining of antarctic krill oil, the following steps are included: step S1: the rehydration solution for being equivalent to 1~6 times of quality of phosphatide mass content in antarctic krill oil being added into antarctic krill oil, then heat while stirring 30min~120min, to 45 DEG C~70 DEG C, it is cooling later, stand, sedimentation separation or be centrifugated to obtain krill oil triglycerides and antarctic krill oil phospholipid solution；Wherein, the rehydration solution is the aqueous solution for being 1.5%~6% citric acid containing mass concentration；Step S2: the isolated antarctic krill oil phospholipid solution of step S1 is concentrated and dried, moisture removal is removed, antarctic krill oil phosphatide must be dehydrated.Benefit of the invention is that can be realized being sufficiently separated for triglycerides and phosphatide, and save the function component in separation product from damage not lose, product after separation has the advantages that purity is high, functional, property stabilization, free from admixture, it can be used as function component to be added in health food, improve the utilization rate of krill.
Description
Technical field
The present invention relates to oil and fat refining fields, more particularly, to a kind of method of refining of antarctic krill oil.
Background technique
Krill is one of maximum single biology of stock number on the earth.It is estimated that the biomass of krill is about
Hundred million tons of 6.5-10.Krill it is annual can amount of fishing be about 60,000,000 to 100,000,000 tons, be equivalent to global 1 year marine fishes and first
The total output of shell class fishing.Krill is the fourth-largest resource of the earth after grain, petroleum, coal, and krill with
Grain is all renewable resource.Krill has high nutritive value, is increasingly subject to the attention of people.
Antarctic krill oil is the upgrading products of human health, has and prevents and assist in the treatment of cardiovascular and cerebrovascular diseases, diabetes, resists
Aging, it is anti-oxidant, remove free radical, effectively reduce the functions such as arthritic symptom, control premenstrual syndrome and dysmenorrhea, auxiliary is reduced
Treating hyperactivity, the immunity for improving people, the physical strength for enhancing people and vigor etc. has apparent effect, it has filled up the country
The blank of health care market Related product will be started new era of domestic functional nutrient food industries.
Antarctic krill oil is widely paid close attention to as a kind of novel oceanic functional grease, it is also krill phase
The product that nutritive effect, added value are all relatively high in product is closed, this krill for also becoming most development prospect produces
One of product.
Main component in antarctic krill oil includes phosphatide and triglycerides, wherein content of phospholipid is greater than 45%, and phosphorus
The unsaturated fatty acids such as a large amount of EPA and DHA are combined on rouge, be in current nature uniquely with phosphatide combination of shape and state EPA,
The molecular structure of DHA, it is easier to absorption of human body, therefore be 15-20 times of fish oil effect the effect of krill oil, meanwhile, glycerol three
Ester combination high-content function ingredients astaxanthin has preferable inoxidizability.
Summary of the invention
The purpose of the present invention is to provide a kind of method of refining of antarctic krill oil, further separate in antarctic krill oil
Phosphatide and triglycerides, and utmostly retain the function ingredients in phosphatide and triglycerides, improve the utilization of krill
Rate, production surcharge height, functional stronger health care product.
To achieve the above object, technical scheme is as follows:
A kind of method of refining of antarctic krill oil, which comprises the following steps:
Step S1: the water for being equivalent to 1~6 times of quality of phosphatide mass content in antarctic krill oil is added into antarctic krill oil
Change solution, then heat while stirring 30min~120min, cooling later, stand until 45 DEG C~70 DEG C, sedimentation separation or from
The heart separates to obtain krill oil triglycerides and antarctic krill oil phospholipid solution；Wherein, the rehydration solution is containing mass concentration
For the aqueous solution of 1.5%~6% citric acid；
Step S2: the isolated antarctic krill oil phospholipid solution of step S1 is concentrated and dried, moisture removal is removed, obtains de-
Water antarctic krill oil phosphatide.
Further, in the step S1, agitation revolution is 50r/min~100r/min.
Further, in the step S1, the process of the cooling be cooled in 30min~120min 40 DEG C with
Under.
Further, in the step S2, described be concentrated and dried is true under the conditions of -20 DEG C~-50 DEG C, 5pa~10pa
Empty frozen drying for 24 hours~72h.
Further, the quality of the rehydration solution is 3~5 times of phosphatide mass content in antarctic krill oil.
Further, the quality of the rehydration solution is 4 times of phosphatide mass content in antarctic krill oil.
Further, the rehydration solution is the aqueous solution for being 1.5%~3% citric acid containing mass concentration.
Further, it in the step S1, is heated using water-bath.
It can be seen from the above technical proposal that the present invention is by using the rehydration solution of addition citric acid electrolyte certain
Under reaction condition, the separation of triglycerides and phospholipid composition in antarctic krill oil is realized, and has saved functional group thereon from damage
Part is not lost, and product purity height, functional, property stabilization, free from admixture after separation can be used as function component and be added to guarantor
In health food, the utilization rate of krill is improved.
Detailed description of the invention
Fig. 1 is the flow diagram of the method for refining of antarctic krill oil of the invention.
Specific embodiment
With reference to the accompanying drawing, specific embodiments of the present invention will be described in further detail.
The method of existing aquation degumming is applied to always in the production of vegetable oil, and phospholipid in lipid used in degumming
Content be below 5%, it is rare to be used for animal fat, and the phosphatide in existing animal and plant fat is only used as individually
Body, and content of phospholipid is greater than 45% in antarctic krill oil, and has also combined EPA and DHA, increases the difficulty of aquation degumming.
The method of existing grease aquation degumming are as follows: hydrophilic radical and water knot after heating water in hot oil, in phospholipid molecule
It closes, is converted into hydrated phospholipid molecular structure, to be precipitated from oil, is dissolved in hot water, belong to physics hydration process, aquation is molten
The temperature of liquid is generally equal to or the temperature of a little higher than hot oil.Aquation degumming effect is heavily dependent on the phosphorus formed after water suction
The stability of rouge micelle.
Influence aquation degumming because being known as: 1) amount of water, suitable amount of water could form stable micelle structure, water
Deficiency, aquation is incomplete, and micelle flocculation is poor；Hypervolia, water/oil or oil/water emulsion easy to form, it is difficult to separate；2)
Hydration temperature, hydration temperature is related with amount of water, and amount of water is bigger, and micelle granularity is bigger, and hydration temperature is higher；3) mixing intensity
With action time, mechanical mixture makes water droplet form enough dispersion degrees, and cannot form stable oil/water or water/oil emulsifying
State.Therefore, amount of water, hydration temperature, stirring intensity require suitable range, could utmostly realize antarctic krill oil
The separation of middle phosphatide and triglycerides meets the requirements the phosphatide residual volume in triglycerides.
Refering to fig. 1, the present invention advanced optimizes reaction condition on the basis of existing aquation Degumming method, specifically include with
Lower step:
Step S1: the water for being equivalent to 1~6 times of quality of phosphatide mass content in antarctic krill oil is added into antarctic krill oil
Change solution, then heat while stirring 30min~120min, until 45 DEG C~70 DEG C, low temperature hydrated degumming in progress.The step with
The method of " water is heated in hot oil " in existing hydration method is different, and antarctic krill oil and the aquation of addition are molten in the present invention
The temperature of liquid is all room temperature, and heating while stirring is the heating process of a milder, can utmostly avoid EPA, DHA,
The functional activities component such as astaxanthin is lost at high temperature, in addition, lasting stirring limits the rapid growth of phospholipid particles size, is reduced
The critical hydrolysis temperature of phosphatide, that is, generate the temperature of cotton-shaped phosphatide, further avoid the functional activities such as EPA, DHA, astaxanthin
Component is lost at high temperature.Preferably, agitation revolution is 50r/min~100r/min.Preferably, it is heated using water-bath,
Temperature is further controlled, avoids temperature excessively high, causes the loss of EPA and DHA.
It is cooling later, stand, sedimentation separation or be centrifugated to obtain krill oil triglycerides and antarctic krill oil phosphatide
Solution.Phosphatide water suction becomes to flocculate micelle when being dissolved in aqueous solution, that is, the process of aquation occurs, at this time temperature highest.In order to the greatest extent
Amount avoids loss of the high temperature to function ingredients, and the agitating and heating time cannot continue too long, preferably in 30~120min, terminates stirring
After heating, due to having surplus heat, in order to reduce the loss of function ingredients, Ying Jinliang reduces temperature, cooling procedure within a short period of time
40 DEG C or less are preferably cooled in 30min~120min.
Since temperature is room temperature when rehydration solution is added, reduce the effect of aquation degumming, in addition can not degumming, in order to increase
Strong degumming effect increases a small amount of electrolyte in rehydration solution, considers that electrolyte is preferably citric acid from edible angle.In addition,
It is not soluble in water due to also containing hydrophilic weaker acid, such as phosphatidic acid in antarctic krill oil phosphatide, therefore, the addition of electrolyte
Hydrophilic weaker acid can also be changed into hydrophilic stronger acid, as far as possible separate triglycerides with phosphatide, reduce glycerol
The residual volume of phosphatide in three esters.Preferably, the mass concentration of citric acid is preferably 1.5%~6%, and citric acid can promote non-aqueous
Change phosphatide and is transformed into hydrophily phosphatide.
Step S2: the isolated antarctic krill oil phospholipid solution of step S1 is concentrated and dried, moisture removal is removed, obtains de-
Water antarctic krill oil phosphatide, in order to avoid the loss of function ingredients, the condition of concentrate drying preferably -20 DEG C~-50 DEG C,
Vacuum and low temperature is freeze-dried for 24 hours~72h under the conditions of 5pa~10pa.
Embodiment 1
Using water bath heating device, the rehydration solution (tool of its 3 times of quality of phosphatide mass content is added into antarctic krill oil
Body is 1.5% citric acid solution), it heats while stirring, 50r/min stirs 30min, until 60 DEG C, it is cooled in 1h under 40 DEG C,
Standing sedimentation 4h obtains the phospholipid solution positioned at the triglycerides on upper layer and positioned at lower layer, separates up to high astaxanthin type south
Pole krill oil triglycerides and high EPA/DHA type antarctic krill oil phospholipid solution.
Components identification, isolated high astaxanthin type krill oil triglycerides Prawn are carried out to above-mentioned separation product
The content of green element is 895.43ppm, and phosphatide residual volume is 98ppm.In high EPA/DHA type antarctic krill oil phospholipid solution, phosphatide
Content be 22.94%, EPA and DHA content be respectively 79.82mg/g and 56.12mg/g, with separate before in antarctic krill oil
Astaxanthin, the EPA contained is compared with DHA content, astaxanthin, phosphatide, EPA and DHA loss late be respectively 4.56%,
8.25%, 0.73% and 0.96%.
By high EPA/DHA type antarctic krill oil phospholipid solution under the conditions of -50 DEG C, 10pa cryogenic vacuum drying and dehydrating 48h
Up to high EPA/DHA type antarctic krill oil phospholipid powder (water content is lower than 2%).
Embodiment 2
Using water bath heating device, the rehydration solution of its 4 times of quality of content of phospholipid is added into antarctic krill oil (specially
1.5% citric acid solution), 30min is stirred through 60 DEG C, 50r/min, is cooled under 40 DEG C in 1h, standing sedimentation 4h is obtained in place
Triglycerides in upper layer and the phospholipid solution positioned at lower layer, separate up to high astaxanthin type krill oil triglycerides and
High EPA/DHA type antarctic krill oil phospholipid solution.
Wherein, the content of the green element of high astaxanthin type krill oil triglycerides Prawn is 881.35ppm, phosphatide residual volume
For 75ppm.In high EPA/DHA type antarctic krill oil phospholipid solution, the content of phosphatide is the content point of 19.97%, EPA and DHA
Not Wei 69.52mg/g and 48.93mg/g, astaxanthin, phosphatide, EPA and DHA loss late be respectively 6.06%, 0.15%,
0.54% and 0.80%.
By high EPA/DHA type antarctic krill oil phospholipid solution under the conditions of -50 DEG C, 10pa cryogenic vacuum drying and dehydrating 72h
Up to high EPA/DHA type antarctic krill oil phospholipid powder (water content is lower than 2%).
Embodiment 3
Using water bath heating device, the rehydration solution of its 1 times of quality of content of phospholipid is added into antarctic krill oil (specially
1.5% citric acid solution), 30min is stirred through 60 DEG C, 50r/min, is cooled under 40 DEG C in 1h, standing sedimentation 4h is obtained in place
Triglycerides in upper layer and the phospholipid solution positioned at lower layer, separate up to high astaxanthin type krill oil triglycerides and
High EPA/DHA type antarctic krill oil phospholipid solution.
Wherein, the content of the green element of high astaxanthin type krill oil triglycerides Prawn is 857.58ppm, and phosphatide remnants contain
Amount is 186ppm.In high EPA/DHA type antarctic krill oil phospholipid solution, the content of phosphatide is the content of 45.63%, EPA and DHA
Respectively 152.13mg/g and 106.86mg/g, astaxanthin, phosphatide, EPA and DHA loss late be respectively 8.59%, 8.74%,
4.88% and 5.19%.
By high EPA/DHA type antarctic krill oil phospholipid solution, drying and dehydrating is for 24 hours under the conditions of -20 DEG C, 10pa cryogenic vacuum
Up to high EPA/DHA type antarctic krill oil phospholipid powder (water content is lower than 2%).
Embodiment 4
Using water bath heating device, the rehydration solution of its 5 times of quality of content of phospholipid is added into antarctic krill oil (specially
1.5% citric acid solution), 30min is stirred through 60 DEG C, 50r/min, is cooled under 40 DEG C in 1h, standing sedimentation 4h is obtained in place
Triglycerides in upper layer and the phospholipid solution positioned at lower layer, separate up to high astaxanthin type krill oil triglycerides and
High EPA/DHA type antarctic krill oil phospholipid solution.
Wherein, the content of the green element of high astaxanthin type krill oil triglycerides Prawn is 869.36ppm, and phosphatide remnants contain
Amount is 127ppm.In high EPA/DHA type antarctic krill oil phospholipid solution, the content of phosphatide is the content of 16.63%, EPA and DHA
Respectively 57.82mg/g and 40.61mg/g, astaxanthin, phosphatide, EPA and DHA loss late be respectively 7.34%, 0.22%,
0.81% and 1.14%.
By high EPA/DHA type antarctic krill oil phospholipid solution, drying and dehydrating 48h is under the conditions of -50 DEG C, 5pa cryogenic vacuum
Obtain high EPA/DHA type antarctic krill oil phospholipid powder (water content is lower than 2%).
Embodiment 5
The rehydration solution of its 6 times of quality of content of phospholipid is added into antarctic krill oil using water bath heating device (specially
1.5% citric acid solution), 30min is stirred through 60 DEG C, 50r/min, is cooled under 40 DEG C in 1h, standing sedimentation 4h is obtained in place
Triglycerides in upper layer and the phospholipid solution positioned at lower layer, separate up to high astaxanthin type krill oil triglycerides and
High EPA/DHA type antarctic krill oil phospholipid solution.
The content of the green element of high astaxanthin type krill oil triglycerides Prawn is 827.16ppm, and phosphatide residual content is
133ppm.In high EPA/DHA type antarctic krill oil phospholipid solution, the content that the content of phosphatide is 13.93%, EPA and DHA is distinguished
For 47.93mg/g and 33.75mg/g, astaxanthin, phosphatide, EPA and DHA loss late be respectively 11.84%, 2.49%,
1.84% and 1.91%.
By high EPA/DHA type antarctic krill oil phospholipid solution, drying and dehydrating 72h is under the conditions of -50 DEG C, 5pa cryogenic vacuum
Obtain high EPA/DHA type antarctic krill oil phospholipid powder (water content is lower than 2%).
Embodiment 6
Using water bath heating device, the rehydration solution of its 4 times of quality of content of phospholipid is added into antarctic krill oil (specially
2% citric acid solution), 30min is stirred through 60 DEG C, 50r/min, is cooled under 40 DEG C in 1h, standing sedimentation 4h is located at
The triglycerides on upper layer and phospholipid solution positioned at lower layer separate up to high astaxanthin type krill oil triglycerides and height
EPA/DHA type antarctic krill oil phospholipid solution.
The content of the green element of high astaxanthin type krill oil triglycerides Prawn is 872.61ppm, and phosphatide residual content is
94ppm.In high EPA/DHA type antarctic krill oil phospholipid solution, the content that the content of phosphatide is 19.36%, EPA and DHA is distinguished
For 67.43mg/g and 47.43mg/g, astaxanthin, phosphatide, EPA and DHA loss late be respectively 6.99%, 3.2%, 0.63%
With 0.81%.
By high EPA/DHA type antarctic krill oil phospholipid solution, drying and dehydrating 72h is under the conditions of -20 DEG C, 5pa cryogenic vacuum
Obtain high EPA/DHA type antarctic krill oil phospholipid powder (water content is lower than 2%).
Embodiment 7
Using water bath heating device, the rehydration solution of its 4 times of quality of content of phospholipid is added into antarctic krill oil (specially
3% citric acid solution), 30min is stirred through 60 DEG C, 50r/min, is cooled under 40 DEG C in 1h, standing sedimentation 4h is located at
The triglycerides on upper layer and phospholipid solution positioned at lower layer separate up to high astaxanthin type krill oil triglycerides and height
EPA/DHA type antarctic krill oil phospholipid solution.
The content of the green element of high astaxanthin type krill oil triglycerides Prawn is 830.42ppm, and phosphatide residual content is
86ppm.In high EPA/DHA type antarctic krill oil phospholipid solution, the content that the content of phosphatide is 19.41%, EPA and DHA is distinguished
For 67.54mg/g and 47.57mg/g, astaxanthin, phosphatide, EPA and DHA loss late be respectively 11.49%, 2.95%,
0.73% and 0.78%.
By high EPA/DHA type antarctic krill oil phospholipid solution, drying and dehydrating 48h is under the conditions of -20 DEG C, 5pa cryogenic vacuum
Obtain high EPA/DHA type antarctic krill oil phospholipid powder (water content is lower than 2%).
Embodiment 8
Using water bath heating device, the rehydration solution of its 4 times of quality of content of phospholipid is added into antarctic krill oil (specially
4.5% citric acid solution), 30min is stirred through 60 DEG C, 50r/min, is cooled under 40 DEG C in 1h, standing sedimentation 4h is obtained in place
Triglycerides in upper layer and the phospholipid solution positioned at lower layer, separate up to high astaxanthin type krill oil triglycerides and
High EPA/DHA type antarctic krill oil phospholipid solution.
The content of the green element of high astaxanthin type krill oil triglycerides Prawn is 817.63ppm, and phosphatide residual content is
118ppm.In high EPA/DHA type antarctic krill oil phospholipid solution, the content that the content of phosphatide is 18.62%, EPA and DHA is distinguished
For 64.64mg/g and 45.50mg/g, astaxanthin, phosphatide, EPA and DHA loss late be respectively 12.85%, 6.9%, 0.96%
With 1.06%.
By high EPA/DHA type antarctic krill oil phospholipid solution under the conditions of -20 DEG C, 10pa cryogenic vacuum drying and dehydrating 72h
Up to high EPA/DHA type antarctic krill oil phospholipid powder (water content is lower than 2%).
Embodiment 9
Using water bath heating device, the rehydration solution of its 4 times of quality of content of phospholipid is added into antarctic krill oil (specially
6% citric acid solution), 30min is stirred through 60 DEG C, 50r/min, is cooled under 40 DEG C in 1h, standing sedimentation 4h is located at
The triglycerides on upper layer and phospholipid solution positioned at lower layer separate up to high astaxanthin type krill oil triglycerides and height
EPA/DHA type antarctic krill oil phospholipid solution.
The content of the green element of high astaxanthin type krill oil triglycerides Prawn is 823.55ppm, and phosphatide residual content is
142ppm.In high EPA/DHA type antarctic krill oil phospholipid solution, the content that the content of phosphatide is 18.35%, EPA and DHA is distinguished
For 63.62mg/g and 44.81mg/g, astaxanthin, phosphatide, EPA and DHA loss late be respectively 12.22%, 8.25%,
1.09% and 1.13%.
By high EPA/DHA type antarctic krill oil phospholipid solution under the conditions of -20 DEG C, 10pa cryogenic vacuum drying and dehydrating 48h
Up to high EPA/DHA type antarctic krill oil phospholipid powder (water content is lower than 2%).
Embodiment 10
Using water bath heating device, the rehydration solution of its 4 times of quality of content of phospholipid is added into antarctic krill oil (specially
1.5% citric acid solution), 30min is stirred through 60 DEG C, 70r/min, is cooled under 40 DEG C in 1h, standing sedimentation 4h is obtained in place
Triglycerides in upper layer and the phospholipid solution positioned at lower layer, separate up to high astaxanthin type krill oil triglycerides and
High EPA/DHA type antarctic krill oil phospholipid solution.
The content of the green element of high astaxanthin type krill oil triglycerides Prawn is 863.85ppm, and phosphatide residual content is
105ppm.In high EPA/DHA type antarctic krill oil phospholipid solution, the content that the content of phosphatide is 19.36%, EPA and DHA is distinguished
For 67.36mg/g and 47.48mg/g, astaxanthin, phosphatide, EPA and DHA loss late be respectively 7.92%, 3.2%, 0.74%
With 0.71%.
By high EPA/DHA type antarctic krill oil phospholipid solution, drying and dehydrating is for 24 hours under the conditions of -50 DEG C, 10pa cryogenic vacuum
Up to high EPA/DHA type antarctic krill oil phospholipid powder (water content is lower than 2%).
Embodiment 11
Using water bath heating device, the rehydration solution of its 4 times of quality of content of phospholipid is added into antarctic krill oil (specially
1.5% citric acid solution), 30min is stirred through 60 DEG C, 100r/min, is cooled under 40 DEG C in 1h, standing sedimentation 4h is obtained
Triglycerides positioned at upper layer and the phospholipid solution positioned at lower layer separate up to high astaxanthin type krill oil triglycerides
With high EPA/DHA type antarctic krill oil phospholipid solution.
The content of the green element of high astaxanthin type krill oil triglycerides Prawn is 883.46ppm, and phosphatide residual content is
105ppm.In high EPA/DHA type antarctic krill oil phospholipid solution, the content that the content of phosphatide is 19.50%, EPA and DHA is distinguished
For 67.88mg/g and 47.78mg/g, astaxanthin, phosphatide, EPA and DHA loss late be respectively 5.83%, 2.5%, 0.69%
With 0.80%.
By high EPA/DHA type antarctic krill oil phospholipid solution, drying and dehydrating is for 24 hours under the conditions of -50 DEG C, 5pa cryogenic vacuum
Obtain high EPA/DHA type antarctic krill oil phospholipid powder (water content is lower than 2%).
Table 1: embodiment response parameter and Comparative result
Reference table 1, be comprehensively compared Examples 1 to 5 it can be concluded that, when rehydration solution quality be antarctic krill oil in phosphatide
At 3~5 times of mass content, aquation degumming effect is preferable, and the separation of triglycerides and phosphatide is more abundant, and function component shrimp
Green element, phosphatide, the loss late of EPA and DHA are lower, wherein when the quality of rehydration solution contains for phosphatide quality in antarctic krill oil
Amount 4 times when, aquation degumming effect is best, and function ingredients loss late is minimum.
Be comprehensively compared embodiment 2,6~9 it can be concluded that, the content of electrolyte citric acid be not it is The more the better, preferably
Range is 1.5%~3%.
Be comprehensively compared embodiment 2,10,11 it can be concluded that, agitation revolution is preferably 50~100r/min.
Above-mentioned data are comprehensively compared and obtain optimal reaction condition are as follows: the quality of rehydration solution is phosphatide in antarctic krill oil
4 times of mass content, wherein the content of electrolyte citric acid is 1.5%, and speed of agitator is 50~100r/min.
Control group 1
60 DEG C of acidification 15min of citric acid powder of shrimp sauce phosphatide quality 4.5% are added in antarctic krill oil, then cool down
To 40 DEG C hereinafter, adding the deionized water that 3 times of quality of content of phospholipid are preheated to 70 °, 30min is reacted, cooling and standings later are heavy
It drops 4h or more, separates to obtain krill oil triglycerides and phospholipid solution (rehydration solution is selected as deionized water)
In this comparative example, it is with embodiment difference: the solid powder of citric acid is first added, adds deionized water,
Acidification and hydration process are separated, and the temperature of deionized water is higher, experiments have shown that this reaction degumming separating effect is bad, only
Small part triglycerides can be obtained, the phospholipid layer of lower layer contains a large amount of triglycerides, and emulsion occurs, poor fluidity,
It is difficult to separate, also, function component loss late is high, the content of the green element of obtained krill oil triglycerides Prawn is
641.92ppm, in antarctic krill oil phospholipid solution, the content of phosphatide is 16.30%.The total content of EPA/DHA is 48.59mg/g
And 30.43mg/g, astaxanthin, phosphatide, EPA and DHA loss late be respectively 50%, 34.8%, 14.95% and 24.42%.
Control group 2
The deionized water that 3 times of quality of shrimp sauce content of phospholipid are preheated to 70 ° is added in antarctic krill oil, reacts 30min, so
It is cooled to 40 DEG C afterwards hereinafter, adding the citric acid powder of phosphatide quality 4.5%, 60 DEG C of acidification 15min, later cooling and standings are sunk
4h or more is dropped, is then separated.
In this comparative example, be with embodiment difference: deionized water and citric acid are that substep is added, and krill
Oil differs larger with the temperature difference of deionized water, and the results show this comparative example degumming separating effect is bad, only few part
Triglycerides is precipitated, and emulsion occurs completely, can not carry out degumming process for lower layer.
Control group 3
Antarctic krill oil and rehydration solution (specially 1.5% citric acid solution) are preheating to 70 ° respectively, then to the South Pole
The rehydration solution of its 3 times of quality of phosphatide mass content is added in krill oil, 60 ° of temperature, 50r/min stirs 30min, cooling in 1h
To under 40 DEG C, standing sedimentation 4h obtains the phospholipid solution positioned at the triglycerides on upper layer and positioned at lower layer, separates up to high
Astaxanthin type krill oil triglycerides and high EPA/DHA type antarctic krill oil phospholipid solution.
The content of the green element of high astaxanthin type krill oil triglycerides Prawn is 428.69ppm, and phosphatide residual volume is
139ppm.In high EPA/DHA type antarctic krill oil phospholipid solution, the content that the content of phosphatide is 22.48%, EPA and DHA is distinguished
For 69.85mg/g and 48.83mg/g, astaxanthin, phosphatide, EPA and DHA loss late be respectively 54.31%, 10.08%,
11.35% and 12.05%.
In this comparative example, be with embodiment difference: antarctic krill oil adds mutually synthermal aquation after being heated
Solution, identical as aquation scouring processes in the prior art, the loss late of the results show EPA, DHA and astaxanthin is higher.
Control group 4
The deionized water of its 3 times of quality of phosphatide mass content is added into antarctic krill oil, heats while stirring, 50r/
Min stirs 30min, until 60 DEG C, it is cooled in 1h under 40 DEG C, then standing sedimentation 4h is separated.
In this comparative example, it is with embodiment difference: electrolyte is not added in rehydration solution, the experimental results showed that this is right
Ratio does not have the effect of any degumming separation, and emulsion occurs completely for rehydration solution and shrimp sauce, can not multi_layer extraction.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of method of refining of antarctic krill oil, which comprises the following steps:
Step S1: into antarctic krill oil be added be equivalent to 1~6 times of quality of phosphatide mass content in antarctic krill oil aquation it is molten
Liquid, then heat while stirring 30min~120min, until 45 DEG C~70 DEG C, cooling later, standing, sedimentation separation or centrifugation divide
From krill oil triglycerides and antarctic krill oil phospholipid solution；Wherein, the rehydration solution is to be containing mass concentration
The aqueous solution of 1.5%~6% citric acid；
Step S2: the isolated antarctic krill oil phospholipid solution of step S1 is concentrated and dried, moisture removal is removed, south must be dehydrated
Pole krill oil phosphatide.
2. the method for refining of antarctic krill oil according to claim 1, which is characterized in that in the step S1, stirring turns
Number is 50r/min~100r/min.
3. the method for refining of antarctic krill oil according to claim 1, which is characterized in that described cold in the step S1
But process is that 40 DEG C or less are cooled in 30min~120min.
4. the method for refining of antarctic krill oil according to claim 1, which is characterized in that described dense in the step S2
Contracting is dry for vacuum and low temperature freeze-drying for 24 hours~72h under the conditions of -20 DEG C~-50 DEG C, 5pa~10pa.
5. the method for refining of antarctic krill oil according to claim 1, which is characterized in that the quality of the rehydration solution is
3~5 times of phosphatide mass content in antarctic krill oil.
6. the method for refining of antarctic krill oil according to claim 1, which is characterized in that the quality of the rehydration solution is
4 times of phosphatide mass content in antarctic krill oil.
7. the method for refining of antarctic krill oil according to claim 1, which is characterized in that the rehydration solution is containing quality
Concentration is the aqueous solution of 1.5%~3% citric acid.
8. the method for refining of antarctic krill oil according to claim 1, which is characterized in that in the step S1, using water
Bath is heated.
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