CN107760439A - A kind of method that ultrasonic assistant ethanol extraction prepares antarctic krill oil - Google Patents
A kind of method that ultrasonic assistant ethanol extraction prepares antarctic krill oil Download PDFInfo
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- CN107760439A CN107760439A CN201711058789.6A CN201711058789A CN107760439A CN 107760439 A CN107760439 A CN 107760439A CN 201711058789 A CN201711058789 A CN 201711058789A CN 107760439 A CN107760439 A CN 107760439A
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- ethanol
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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
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/106—Production of fats or fatty oils from raw materials by extracting using ultra-sounds
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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
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
Abstract
The present invention relates to the preparation method of antarctic krill oil, and in particular to the method that ultrasonic assistant ethanol extraction prepares antarctic krill oil.This method only can be obtained the higher krill oil product of yield with an ethanol extraction, be extracted without multiple ethanol, antarctic krill oil yield is higher, has saved cost and workload using efficient, green batch (-type) ultrasonic assistant ethanol extraction；Meanwhile the antarctic krill oil obtained after measured contains higher phosphatide, unrighted acid and astaxanthin, there is high antioxidation biology active function.The coproduct ethanol obtained by rotary distillation is repeatable simultaneously utilizes, and has saved the energy.
Description
Technical field
The present invention relates to the preparation method of antarctic krill oil, and in particular to a kind of ultrasonic assistant ethanol extraction prepares the South Pole
The method of krill oil.
Background technology
Krill is most living marine resources of Development volue in the world now, is distributed widely in South Pole marine site,
Its biological total amount is up to hundred million tons of 6.5-10, and its year highest allows amount of fishing up to ten thousand tons of 4000-6000.Krill is because of its high egg
White and high bioactivity shrimp sauce and by people's concern.Numerous studies show antarctic krill oil have reduce cardiovascular incidence,
Mitigate allergy and inflammation, promote brain growth, protection eyesight, reduce the biological functions such as diabetes incidence, and because its high phospholipid,
High unsaturated fatty acid and high astaxanthin are significantly better than deep sea fish oil containing reason, its biological activity.
The method of production antarctic krill oil mainly is organic solvent extractionprocess, enzymatic isolation method and supercritical carbon dioxide at present
Extraction, wherein, because of organic solvent extractionprocess simple process, cost is relatively low, yield is higher and utilization is the most universal.In view of peace
Full property and Cost Problems, ethanol are the most frequently used organic solvents of organic solvent extractionprocess extraction antarctic krill oil.Such as patent " one
The method that kind extracts high phospholipid content krill oil from fresh krill ", publication number CN104479850A, is entered using 95% ethanol
2-4 extraction of row；Such as patent " a kind of method that high phospholipid content krill oil is extracted from krill " again, publication number
CN102492538A, using more than 90% ethanol extract under 2-4 shearing force, obtain the South Pole phosphorus of high phospholipid content
Shrimp sauce product；Such as patent " method that the shrimp sauce of high phospholipid content is extracted from krill " again, the patent No.
CN102041166A, krill is extracted 3 times using non-polar solvens such as n-hexanes, recycles ethanol polar solvent to south
Pole krill oil is enriched with, and obtains krill oil product.It is above-mentioned to obtain shrimp using the organic solvents such as ethanol extraction krill
Oil, to improve yield, it is necessary to carry out multiplicating extraction, process is more complicated, and the dosage of ethanol is also corresponding larger, to extracting
Journey and the process operation workload of later separation ethanol and lipid are larger.
The content of the invention
In order to solve the problems, such as that prior art is present, extracted the invention provides a kind of ultrasonic assistant ethanol and prepare the South Pole
The method of krill oil.This method is extracted using efficient, green batch (-type) ultrasonic assistant ethanol, is only with an ethanol extraction
The higher krill oil product of yield can be obtained, is extracted without multiple ethanol, is saved the dosage of ethanol, greatly reduce
Workload, is a kind of extraction process of efficient, quick, simple antarctic krill oil.
A kind of method that ultrasonic assistant ethanol extraction prepares antarctic krill oil, comprises the following steps：
1) to freeze krill as raw material, drain away the water, weigh after defrosting, it is even using refiner to add 95% ethanol
Slurry, obtains homogenate；
2) 95% ethanol for adding 1-4 times of homogenate volume is stirred at room temperature under state and carries out extractive reaction, during extraction
Between 2-8h, during which every 1h carry out ultrasound-assisted extraction；
3) the extraction solution after extracting first uses 3 layers of filtered through gauze, then with the filterings of 3 layers of filter paper, a small amount of 95% ethanol of filter residue
With 3 layers of filtered through gauze after being cleaned, then filtered with 3 layers of filter paper, after merging filtrate, then filtered with 3 layers of filter paper；
4) ethanol is removed using low pressure revolving, coproduct ethanol is repeatable to be utilized, and the grease of acquisition adds anhydrous sodium sulfate
Excessive moisture is removed, then the ethanol in grease is volatilized using carbon dioxide bottom purge, with except being dissolved in degreasing
Ethanol, and unrighted acid in oxygen-free environment in pre- grease-proof etc. occur oxidation reaction, finally obtain krill
Oil product.
Preferably, the krill and the w/v of 95% ethanol that are drained away the water after being thawed described in step 1)
For 1:2(g/mL).
Preferably, it be 5~20min to carry out ultrasound-assisted extraction processing time every 1h in the step 2), it is ultrasonic
Sound field intensity is 30~50W/cm2, supersonic frequency is 20~25kHz.
Preferably, 95% ethanol in the step 1), step 2) and step 3) is edible ethanol.
Preferably, extraction time is 6-8 hours in the step 2).
Preferably, the low pressure revolving temperature in the step 4) is 45-50 DEG C.
Preferably, the mass ratio of the anhydrous sodium sulfate amount and grease in the step 4) is 1:5.
Preferably, the carbon dioxide bottom purge time in the step 4) is 10-15min.
The present invention is to utilize batch (-type) ultrasonic assistant ethanol extraction antarctic krill oil, it is not necessary to repeats to extract using ethanol
Higher shrimp sauce yield is can be obtained by, has saved cost and workload.Meanwhile the antarctic krill oil obtained after measured contains
Higher phosphatide, unrighted acid and astaxanthin, there is high antioxidation biology active function.Rotary distillation institute simultaneously
The repeatable utilization of coproduct ethanol obtained, has saved the energy.
Embodiment
Reagent used in the present invention has no particular limits, and can use commercially available conventional reagent.
As 95% edible ethanol is bought in Kate's biochemical industry Co., Ltd of Guangxi pingguo in embodiment.
Carbon dioxide is bought in hundred million foreign gas companies of Zhoushan.
Anhydrous sodium sulfate is bought in Shanghai Bang Jing Industrial Co., Ltd.s.
Krill is freezed in the present embodiment to be provided by Zhejiang Hailisheng Group Co., Ltd..
Embodiment 1
1) to freeze krill 300g as raw material, drain away the water to obtain krill 264g after defrosting, adds product 528mL's
95% ethanol is homogenized using refiner, obtains homogenate 661mL；
2) 95% ethanol for adding 1 times of homogenate volume is stirred at room temperature under state and carries out extractive reaction, extraction time
5h, during which carry out ultrasound-assisted extraction every 1h；It is 20min every 1h progress ultrasound-assisted extraction processing times, ultrasound
Sound field intensity is 30W/cm2, supersonic frequency 25kH；
3) the extraction solution after extracting first uses 3 layers of filtered through gauze, then with the filterings of 3 layers of filter paper, a small amount of 95% ethanol of filter residue
With 3 layers of filtered through gauze after being cleaned, then filtered with 3 layers of filter paper, after merging filtrate, then filtered with 3 layers of filter paper, obtain filtrate
1225mL；
4) ethanol is removed using low pressure revolving under the conditions of 45 DEG C, obtains grease 10.75g, added anhydrous sodium sulfate 2.15g and remove
Excessive moisture is removed, then uses carbon dioxide bottom purge 10min with except the ethanol dissolved in degreasing, final acquisition south
Pole krill oil product 9.86g, its index of correlation measurement result such as table 1.
Table 1
Embodiment 2
1) to freeze krill 500g as raw material, drain away the water to obtain krill 441g after defrosting, adds product 882mL's
95% ethanol is homogenized using refiner, obtains homogenate 1103mL；
2) 95% ethanol for adding 4 times of homogenate volumes is stirred at room temperature under state and carries out extractive reaction, extraction time
6h, during which carry out ultrasound-assisted extraction every 1h；It is 20min every 1h progress ultrasound-assisted extraction processing times, ultrasound
Sound field intensity is 30W/cm2, supersonic frequency 20kHz；
3) the extraction solution after extracting first uses 3 layers of filtered through gauze, then with the filterings of 3 layers of filter paper, a small amount of 95% ethanol of filter residue
With 3 layers of filtered through gauze after being cleaned, then filtered with 3 layers of filter paper, after merging filtrate, then filtered with 3 layers of filter paper, obtain filtrate
5243mL；
4) ethanol is removed using low pressure revolving under the conditions of 45 DEG C, obtains grease 17.85g, added anhydrous sodium sulfate 3.57g and remove
Excessive moisture is removed, then uses carbon dioxide bottom purge 10min with except the ethanol dissolved in degreasing, final acquisition south
Pole krill oil product 16.92g, its index of correlation measurement result such as table 2.
Table 2
Embodiment 3
1) to freeze krill 1kg as raw material, drain away the water to obtain krill 881g after defrosting, adds product 1762mL's
95% ethanol is homogenized using refiner, obtains homogenate 2206mL；
2) 95% ethanol for adding 4 times of homogenate volumes is stirred at room temperature under state and carries out extractive reaction, extraction time
4h, during which carry out ultrasound-assisted extraction every 1h；It is 20min every 1h progress ultrasound-assisted extraction processing times, ultrasound
Sound field intensity is 50W/cm2, supersonic frequency 25kH；
3) the extraction solution after extracting first uses 3 layers of filtered through gauze, then with the filterings of 3 layers of filter paper, a small amount of 95% ethanol of filter residue
With 3 layers of filtered through gauze after being cleaned, then filtered with 3 layers of filter paper, after merging filtrate, then filtered with 3 layers of filter paper, obtain filtrate
10747mL；
4) ethanol is removed using low pressure revolving under the conditions of 45 DEG C, obtains grease 34.75g, added anhydrous sodium sulfate 6.95g and remove
Excessive moisture is removed, then uses carbon dioxide bottom purge 15min with except the ethanol dissolved in degreasing, final acquisition south
Pole krill oil product 33.26g, its index of correlation measurement result such as table 3.
Table 3
Embodiment 4
1) to freeze krill 1.5kg as raw material, drain away the water to obtain krill 1328g after defrosting, adds product
2565mL 95% ethanol is homogenized using refiner, obtains homogenate 3311mL；
2) 95% ethanol for adding 3 times of homogenate volumes is stirred at room temperature under state and carries out extractive reaction, extraction time
6h, during which carry out ultrasound-assisted extraction every 1h；It is 20min every 1h progress ultrasound-assisted extraction processing times, ultrasound
Sound field intensity is 35W/cm2, supersonic frequency 25kH；
3) the extraction solution after extracting first uses 3 layers of filtered through gauze, then with the filterings of 3 layers of filter paper, a small amount of 95% ethanol of filter residue
With 3 layers of filtered through gauze after being cleaned, then filtered with 3 layers of filter paper, after merging filtrate, then filtered with 3 layers of filter paper, obtain filtrate
12659mL；
4) ethanol is removed using low pressure revolving under the conditions of 45 DEG C, obtains grease 52.24g, add anhydrous sodium sulfate 10.45g
Excessive moisture is removed, then uses carbon dioxide bottom purge 10min with except the ethanol dissolved in degreasing, final acquisition
Krill oil product 50.65g, its index of correlation measurement result such as table 4.
Table 4
Embodiment 5
1) to freeze krill 2kg as raw material, drain away the water to obtain krill 1760g after defrosting, adds product 3520mL
95% ethanol using refiner be homogenized, obtain homogenate 4405mL；
2) 95% ethanol for adding 2 times of homogenate volumes is stirred at room temperature under state and carries out extractive reaction, extraction time
8h, during which carry out ultrasound-assisted extraction every 1h；It is 10min every 1h progress ultrasound-assisted extraction processing times, ultrasound
Sound field intensity is 40W/cm2, supersonic frequency 25kH；
3) the extraction solution after extracting first uses 3 layers of filtered through gauze, then with the filterings of 3 layers of filter paper, a small amount of 95% ethanol of filter residue
With 3 layers of filtered through gauze after being cleaned, then filtered with 3 layers of filter paper, after merging filtrate, then filtered with 3 layers of filter paper, obtain filtrate
12468mL；
4) ethanol is removed using low pressure revolving under the conditions of 50 DEG C, obtains grease 67.25g, add anhydrous sodium sulfate 13.45g
Excessive moisture is removed, then uses carbon dioxide bottom purge 12min with except the ethanol dissolved in degreasing, final acquisition
Krill oil product 65.61g, its index of correlation measurement result such as table 5.
Table 5
Embodiment 6
1) to freeze krill 5kg as raw material, drain away the water to obtain krill 4398g after defrosting, adds product 8796mL
95% ethanol using refiner be homogenized, obtain homogenate 10047mL；
2) 95% ethanol for adding 3 times of homogenate volumes is stirred at room temperature under state and carries out extractive reaction, extraction time
8h, during which carry out ultrasound-assisted extraction every 1h；It is 5min to carry out ultrasound-assisted extraction processing time every 1h, ultrasonic sound
Field intensity is 50W/cm2, supersonic frequency 20kH；
3) the extraction solution after extracting first uses 3 layers of filtered through gauze, then with the filterings of 3 layers of filter paper, a small amount of 95% ethanol of filter residue
With 3 layers of filtered through gauze after being cleaned, then filtered with 3 layers of filter paper, after merging filtrate, then filtered with 3 layers of filter paper, obtain filtrate
42927mL；
4) ethanol is removed using low pressure revolving under the conditions of 45 DEG C, obtains grease 171.66g, add anhydrous sodium sulfate 34.33g
Excessive moisture is removed, then uses carbon dioxide bottom purge 15min with except the ethanol dissolved in degreasing, final acquisition
Krill oil product 165.95g, its index of correlation measurement result such as table 6.
Table 6
This place embodiment is in place of the claimed non-limit of technical scope midrange and in embodiment technology
The new technical scheme that equal replacement in scheme to single or multiple technical characteristics is formed, equally all in application claims
In the range of protection；Simultaneously the present invention program it is all enumerate or unrequited embodiment in, in the same embodiment each
Parameter is merely representative of an example (i.e. a kind of feasible scheme) for its technical scheme, and between parameters and in the absence of strict
Cooperation and qualified relation, wherein each parameter can be replaced mutually when stating and asking without prejudice to axiom and the present invention, special declaration
Except.
Technological means disclosed in the present invention program is not limited only to the technological means disclosed in above-mentioned technological means, in addition to
Formed technical scheme is combined by above technical characteristic.Described above is the embodiment of the present invention, should be referred to
Go out, for those skilled in the art, under the premise without departing from the principles of the invention, can also make some
Improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (8)
1. a kind of method that ultrasonic assistant ethanol extraction prepares antarctic krill oil, it is characterised in that comprise the following steps：
1) to freeze krill as raw material, drain away the water, weigh after defrosting, add 95% ethanol and be homogenized using refiner, obtained
Homogenate；
2) 95% ethanol for adding 1-4 times of homogenate volume is stirred at room temperature under state and carries out extractive reaction, extraction time 2-
8h, during which carry out ultrasound-assisted extraction every 1h；
3) the extraction solution after extracting first uses 3 layers of filtered through gauze, then is carried out with the filterings of 3 layers of filter paper, filter residue with a small amount of 95% ethanol
With 3 layers of filtered through gauze after cleaning, then filtered with 3 layers of filter paper, after merging filtrate, then filtered with 3 layers of filter paper；
4) ethanol is removed using low pressure revolving, coproduct ethanol is repeatable to be utilized, and the grease of acquisition adds anhydrous sodium sulfate and removed
Excessive moisture, then the ethanol in grease is set to volatilize using carbon dioxide bottom purge, with except the second dissolved in degreasing
Alcohol, and oxidation reaction occurs for unrighted acid in oxygen-free environment in pre- grease-proof etc., it is final to obtain antarctic krill oil production
Product.
2. the method that a kind of ultrasonic assistant ethanol extraction according to claim 1 prepares antarctic krill oil, its feature exist
The krill and the w/v of 95% ethanol to be drained away the water after being thawed described in step 1) is 1:2(g/mL).
3. the method that a kind of ultrasonic assistant ethanol extraction according to claim 1 prepares antarctic krill oil, its feature exist
It is 5~20min to carry out ultrasound-assisted extraction processing time every 1h in the step 2), ultrasonic sound field intensity for 30~
50W/cm2, supersonic frequency is 20~25kHz.
4. the method that a kind of ultrasonic assistant ethanol extraction according to claim 1 prepares antarctic krill oil, its feature exist
95% ethanol in the step 1), step 2) and step 3) is edible ethanol.
5. the method that a kind of ultrasonic assistant ethanol extraction according to claim 1 prepares antarctic krill oil, its feature exist
Extraction time is 6-8 hours in the step 2).
6. the method that a kind of ultrasonic assistant ethanol extraction according to claim 1 prepares antarctic krill oil, its feature exist
Low pressure revolving temperature in the step 4) is 45-50 DEG C.
7. the method that a kind of ultrasonic assistant ethanol extraction according to claim 1 prepares antarctic krill oil, its feature exist
The mass ratio of anhydrous sodium sulfate amount and grease in the step 4) is 1:5.
8. the method that a kind of ultrasonic assistant ethanol extraction according to claim 1 prepares antarctic krill oil, its feature exist
The carbon dioxide bottom purge time in the step 4) is 10-15min.
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Application publication date: 20180306 |