CN107663473B - Krill oil extraction method - Google Patents

Krill oil extraction method Download PDF

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CN107663473B
CN107663473B CN201711118852.0A CN201711118852A CN107663473B CN 107663473 B CN107663473 B CN 107663473B CN 201711118852 A CN201711118852 A CN 201711118852A CN 107663473 B CN107663473 B CN 107663473B
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krill oil
iii
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treatment
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CN107663473A (en
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刘慧燕
张少敏
贾洪信
张志平
潘兆广
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Shandong Hailongyuan Biotechnology Co ltd
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Guangdong Vocational College of Environmental Protection Engineering
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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
    • 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
    • C11B1/02—Pretreatment
    • 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
    • C11B1/02—Pretreatment
    • C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
    • 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
    • C11B1/06—Production of fats or fatty oils from raw materials by pressing
    • 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
    • C11B1/16—Production of fats or fatty oils from raw materials by melting out with steam
    • 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
    • C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
    • 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
    • C11B3/006—Refining fats or fatty oils by extraction

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Microbiology (AREA)
  • Biochemistry (AREA)
  • Meat, Egg Or Seafood Products (AREA)
  • Medicines Containing Material From Animals Or Micro-Organisms (AREA)
  • Fats And Perfumes (AREA)
  • Edible Oils And Fats (AREA)

Abstract

The invention discloses a krill oil extraction method, which comprises the following steps: drying the body surface moisture of the Antarctic krill, repeating the freezing-microwave thawing treatment, and collecting a liquid II; preparing antarctic krill into antarctic krill quick-frozen powder, uniformly mixing the antarctic krill quick-frozen powder with the liquid I, and performing ultrasonic crushing treatment to obtain a mixture II; centrifuging the mixture II to obtain a residue I and a liquid III; carrying out flash evaporation treatment on the residue I under the instantaneous pressure difference to obtain a liquid IV and a residue II; squeezing the residue II to obtain primary krill oil and residue III; mixing the residue III, the liquid II and the liquid III to obtain a mixture III, carrying out enzymolysis and centrifugal treatment to obtain an enzymolysis liquid, and extracting with an organic solvent to obtain secondary krill oil; and mixing the secondary krill oil, the liquid IV and the primary krill oil, centrifuging to remove impurities and remove water, and refining the krill oil. The extraction rate of the krill oil is high, the active ingredients in the krill oil can be effectively reserved, and the finally obtained product is high in nutritive value and free of organic solvent residues.

Description

Krill oil extraction method
Technical Field
The invention relates to the technical field of production formulas of bioactive substances and functional foods, in particular to a krill oil extraction method.
Background
Antarctic krill is abundant in resources, and the growth environment is free of industrial pollution. Krill oil is lipid extracted from Antarctic krill (Euphausiasuperba) and comprises the following main components: glycerides, phospholipids, astaxanthin, sterols, and the like. Meanwhile, the krill oil contains natural antioxidant astaxanthin, the content of the natural antioxidant astaxanthin can reach 100 mg/kg-300 mg/kg, the antioxidant capacity of the natural krill oil is far higher than that of substances such as vitamin E, lycopene and the like, and the natural krill oil is called as a natural substance with the strongest antioxidant activity. Existing studies have demonstrated that krill oil is rich in a variety of unsaturated fatty acids, with long chain omega-3 polyunsaturated fatty acids EPA and DHA content as high as 15.86%. Unlike the omega-3 triglyceride forms of fish and cod liver oils, the omega-3 fatty acids of krill oil are attached to phospholipids, and the bioactive complex molecules of the long chain polyunsaturated fatty acid phospholipids can directly enter the small intestine to be completely absorbed after passing through the stomach, so that the bioavailability is increased, and finally the ratio of omega-3 to omega-6 fatty acids is increased. But also astaxanthin, a natural strong antioxidant inherent in krill oil, is attached to phospholipids, resulting in a more stable and long lasting antioxidant effect. According to experiments, the bioavailability of the krill oil bioactive complex is 95% -98%, while the bioavailability of the fish oil is only 61% -64%, mainly because the krill oil contains phospholipid fatty acid, and the fish oil contains almost 100% triglyceride. The research shows that: the krill oil (2g/d) can increase the concentration of EPA and DHA in blood of obese people, and the effect is obviously higher than the increase of taking herring oil (2g/d) and taking olive oil (2g/d), which indicates that the krill oil has good absorptivity in human body; and the krill oil is determined to have no toxic or side effect.
The extraction method of the krill oil at home and abroad mainly comprises the following steps: compared with other methods, the organic solvent method has the advantages of simple process, high extraction efficiency, low cost and the like, and is still the most commonly used method for industrialization, but the method for extracting the shrimp sauce by taking the whole shrimps as the raw materials and adopting the organic solvent has the following problems: the problem of solvent residue exists in the process of organic solvent extraction, the utilization of krill proteins is influenced, other nutritional ingredients are damaged, and the full utilization of krill resources is influenced.
Disclosure of Invention
An object of the present invention is to solve at least the above problems and to provide at least the advantages described later.
Still another object of the present invention is to provide a krill oil extraction method, which has a high extraction rate of krill oil, can effectively retain active ingredients in krill oil, and can obtain a product with high nutritional value and no organic solvent residue.
To achieve these objects and other advantages in accordance with the present invention, there is provided a krill oil extraction method comprising the steps of:
step one, blow-drying body surface moisture of euphausia superba within 3 hours after the euphausia superba is caught, and collecting blown liquid I;
freezing the euphausia superba subjected to body surface blow-drying, then performing microwave thawing treatment, and repeating the freezing and microwave thawing treatment for 2-3 times;
collecting a liquid II evaporated and cooled in the microwave thawing treatment process;
step four, quickly freezing the euphausia superba obtained in the step three, and then crushing to obtain quick-frozen euphausia superba powder;
step five, adding liquid I into the quick-frozen antarctic krill powder according to the volume ratio of 2:1-2, uniformly mixing to obtain a mixture I, and performing ultrasonic crushing treatment on the mixture I to obtain a mixture II;
step six, performing centrifugal treatment on the mixture II to obtain a residue I and a liquid III;
performing flash evaporation treatment on the residue I under the instantaneous pressure difference to obtain liquid IV and residue II, wherein the flash evaporation temperature under the instantaneous pressure difference is not more than 95 ℃;
step eight, squeezing the residue II to obtain primary krill oil and residue III;
step nine, fully mixing the residue III, the liquid II and the liquid III according to the volume ratio of 1-2:1:1 to obtain a mixture III, heating the mixture III to 35-45 ℃, adding a proper amount of protease into the mixture III, uniformly mixing the mixture III, standing the mixture for 30-50min, and centrifuging the mixture III to obtain an enzymolysis liquid; wherein the addition amount of the protease is 1 percent of the mass of the mixture III;
step ten, fully mixing the enzymatic hydrolysate with an organic solvent to extract secondary krill oil;
and eleventh, after recovering the organic solvent in the secondary krill oil, mixing the secondary krill oil, the liquid IV and the primary krill oil, centrifuging to remove impurities and water, and refining the krill oil.
Preferably, the first step further comprises the following steps:
a. uniformly laying the Antarctic krill on a plurality of layers of drying nets distributed from top to bottom, wherein the plurality of layers of drying nets are arranged in a relatively closed drying device;
b. introducing dry nitrogen into the drying device from the bottom of the drying device, wherein the temperature of the nitrogen is 50-60 ℃;
c. after passing through the multilayer drying net, the nitrogen is discharged from an outlet of the drying device;
d. and (4) carrying out water-vapor separation on the discharged nitrogen with water vapor to obtain liquid I.
Preferably, the specific conditions of the microwave thawing treatment in the second step are as follows: the time of the primary microwave thawing is 10-20s, and the temperature in the antarctic krill is kept not to exceed 90 ℃ in the microwave thawing process.
Preferably, in the second step, the in vivo temperature of the frozen antarctic krill is-6 to-2 ℃.
Preferably, the liquid I, the liquid II and the liquid III are stored in a sealed tank for later use, and the sealed tank is filled with nitrogen.
Preferably, in the fifth step, the frequency of the ultrasonic wave is 20-25KHz, the total time of the ultrasonic wave treatment is 4-8min, the ultrasonic wave treatment is carried out once every 2-4s, the time of one time is 10-15s, and the sound power of the ultrasonic wave is 3-5W/cm2。
Preferably, the seventh step further comprises the steps of:
e. vacuumizing a sealing cavity of the instantaneous differential pressure treatment device containing the residues I;
f. introducing hot steam into the sealed cavity until the internal temperature is not higher than 95 ℃ and the pressure is 0.15-0.25Mpa, and then carrying out pressure maintaining treatment for 20-40 s;
g. the pressure in the sealing cavity is relieved within 3s to 5-6 kpa;
h. repeating the steps a, b and c once every 30-45s, and repeating the steps 2-3 times in total.
Preferably, in f, hot steam is introduced into the sealing cavity until the internal temperature is 93 ℃ and the pressure is 0.25MPa, and then the pressure is maintained for 35 s.
Preferably, in the step f, the step a, the step b and the step c are repeated once and 3 times in total.
Preferably, in the step eight, the residue ii is put into a screw extruder to be pressed, and the pressing treatment comprises primary pressing and secondary pressing:
the screw extruder is correspondingly provided with two primary squeezing cylinders and two secondary squeezing cylinders, wherein the bottoms of outer shells I of the two primary squeezing cylinders are connected, and screws in the two primary squeezing cylinders are not in contact, so that the two primary squeezing cylinders form an included angle smaller than 90 degrees;
and the upper end of the shell of the second-stage squeezing cylinder is connected to the joint of the bottoms of the shell bodies II of the two first-stage squeezing cylinders, and the maximum diameter of the shell bodies II is smaller than 1.5 times of the minimum diameter of the shell body I.
The invention at least comprises the following beneficial effects:
according to the extraction method of the krill oil, the Antarctic krill is subjected to body surface blow drying and then the krill oil is extracted, so that the mass percentage concentration of oil in the primary pressing process is improved;
the antarctic krill is subjected to freezing-microwave thawing cyclic treatment for 2-3 times, during the freezing process, the ice crystals in cells form cutting damage cell membranes, and the cell membranes are damaged after thawing, so that primary freezing-thawing membrane breaking treatment can be performed on the cells of the antarctic krill, in addition, the microwave thawing temperature is kept not to exceed 95 ℃, and the nutrient components in the antarctic krill are preserved to the maximum extent without being damaged;
after the antarctic krill subjected to membrane breaking treatment is quickly frozen and crushed, the antarctic krill is subjected to low-power ultrasonic treatment, so that the nutritional ingredients in the antarctic krill including a part of krill oil can be released preliminarily, and a liquid III is obtained through centrifugal treatment;
performing instantaneous differential pressure flash evaporation treatment on the residue I to obtain a liquid IV, so that most of water and krill oil in the Antarctic krill are instantaneously flushed out from the krill powder to obtain the liquid IV, and performing centrifugal treatment to obtain separated krill oil;
further squeezing the residue II to obtain primary krill oil and residue III, so as to further separate the grease in the Antarctic krill;
the mixture III is subjected to enzymolysis to thoroughly collect grease (krill oil) in the antarctic krill, and in the process, because the grease of the antarctic krill powder in the mixture III is basically separated, the grease of the antarctic krill powder can be thoroughly extracted only by a very small amount of organic solvent, so that waste is avoided, the use of the organic solvent is greatly reduced, and the residue of the organic solvent can be ignored.
In conclusion, the method provided by the invention has the advantages that the extraction rate of the krill oil is high, the active ingredients in the krill oil can be effectively reserved, the finally obtained product has high nutritional value, and no organic solvent residue exists.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The present invention is further described in detail below with reference to examples so that those skilled in the art can practice the invention with reference to the description.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1
A krill oil extraction method comprises the following steps:
step one, blow-drying body surface moisture of euphausia superba within 3 hours after the euphausia superba is caught, and collecting blown liquid I; wherein, the step one also comprises the following steps: a. uniformly laying the Antarctic krill on a plurality of layers of drying nets distributed from top to bottom, wherein the plurality of layers of drying nets are arranged in a relatively closed drying device; b. introducing dry nitrogen into the drying device from the bottom of the drying device, wherein the temperature of the nitrogen is 50 ℃; c. after passing through the multilayer drying net, the nitrogen is discharged from an outlet of the drying device; d. the discharged nitrogen with water vapor is subjected to water-vapor separation to obtain liquid I;
freezing the euphausia superba subjected to body surface blow-drying, then performing microwave thawing treatment, and repeating the freezing and microwave thawing treatment for 2 times; the in vivo temperature of the frozen antarctic krill is-6 ℃; the time of primary microwave thawing is 10-20s, and the temperature in the antarctic krill is kept at 90 ℃ in the microwave thawing process;
collecting a liquid II evaporated and cooled in the microwave thawing treatment process;
step four, quickly freezing the euphausia superba obtained in the step three, and then crushing to obtain quick-frozen euphausia superba powder;
step five, adding liquid I into the quick-frozen antarctic krill powder according to the volume ratio of 2:1, uniformly mixing to obtain a mixture I, and performing ultrasonic crushing treatment on the mixture I to obtain a mixture II; wherein the frequency of the ultrasonic wave is 20KHz, the total time of ultrasonic wave treatment is 4min, the time of ultrasonic wave treatment is 10s every 2s, and the sound power of the ultrasonic wave is 3W/cm2；
Step six, performing centrifugal treatment on the mixture II to obtain a residue I and a liquid III;
performing flash evaporation treatment on the residue I under the instantaneous pressure difference to obtain liquid IV and residue II, wherein the flash evaporation temperature under the instantaneous pressure difference is 95 ℃; wherein, still include the following step: e. vacuumizing a sealing cavity of the instantaneous differential pressure treatment device containing the residues I; f. introducing hot steam into the sealed cavity until the internal temperature is 95 ℃ and the pressure is 0.25Mpa, and then carrying out pressure maintaining treatment for 20 s; g. the pressure in the sealing cavity is relieved to 5kpa within 3 s; h. repeating the steps a, b and c once every 30s, and repeating the steps for 2 times in total;
step eight, squeezing the residue II to obtain primary krill oil and residue III; and step eight, putting the residue II into a screw extruder for squeezing treatment, wherein the squeezing treatment comprises first-stage squeezing and second-stage squeezing: the screw extruder is correspondingly provided with two primary squeezing cylinders and two secondary squeezing cylinders, wherein the bottoms of outer shells I of the two primary squeezing cylinders are connected, and screws in the two primary squeezing cylinders are not in contact, so that the two primary squeezing cylinders form an included angle smaller than 90 degrees; the upper end of the shell of the second-stage squeezing cylinder is connected to the joint of the bottoms of the shell II of the two first-stage squeezing cylinders, and the maximum diameter of the shell II is smaller than 1.5 times of the minimum diameter of the shell I;
step nine, fully mixing the residue III, the liquid II and the liquid III according to the volume ratio of 1:1:1 to obtain a mixture III, heating the mixture III to 35 ℃, adding a proper amount of protease into the mixture III, uniformly mixing the mixture III, standing the mixture for 30min, and centrifuging the mixture III to obtain an enzymolysis liquid; wherein the addition amount of the protease is 1 percent of the mass of the mixture III;
step ten, fully mixing the enzymatic hydrolysate with an organic solvent to extract secondary krill oil; the organic solvent is ethanol or acetone with the mass fraction of 95 percent;
and eleventh, after recovering the organic solvent in the secondary krill oil, mixing the secondary krill oil, the liquid IV and the primary krill oil, centrifuging to remove impurities and water, and refining the krill oil.
Wherein, liquid I, liquid II and liquid III are all put into the seal pot and keep for later use, and fill nitrogen gas in the seal pot.
Example 2
A krill oil extraction method comprises the following steps:
step one, blow-drying body surface moisture of euphausia superba within 2.5 hours after the euphausia superba is caught, and collecting blown liquid I; wherein, the step one also comprises the following steps: a. uniformly laying the Antarctic krill on a plurality of layers of drying nets distributed from top to bottom, wherein the plurality of layers of drying nets are arranged in a relatively closed drying device; b. introducing dry nitrogen into the drying device from the bottom of the drying device, wherein the temperature of the nitrogen is 55 ℃; c. after passing through the multilayer drying net, the nitrogen is discharged from an outlet of the drying device; d. the discharged nitrogen with water vapor is subjected to water-vapor separation to obtain liquid I;
freezing the euphausia superba subjected to body surface blow-drying, then performing microwave thawing treatment, and repeating the freezing and microwave thawing treatment for 3 times; the in vivo temperature of the frozen antarctic krill is-4 ℃; the time of primary microwave thawing is 15s, and the temperature in the antarctic krill is kept at 88 ℃ in the microwave thawing process;
collecting a liquid II evaporated and cooled in the microwave thawing treatment process;
step four, quickly freezing the euphausia superba obtained in the step three, and then crushing to obtain quick-frozen euphausia superba powder;
step five, adding liquid I into the quick-frozen antarctic krill powder according to the volume ratio of 1:1, uniformly mixing to obtain a mixture I, and performing ultrasonic crushing treatment on the mixture I to obtain a mixture II; wherein the frequency of the ultrasonic wave is 25KHz, the total time of ultrasonic wave treatment is 6min, the ultrasonic wave treatment is carried out once every 4s, the time of one time is 15s, and the sound power of the ultrasonic wave is 5W/cm2；
Step six, performing centrifugal treatment on the mixture II to obtain a residue I and a liquid III;
performing flash evaporation treatment on the residue I under the instantaneous pressure difference to obtain liquid IV and residue II, wherein the flash evaporation temperature under the instantaneous pressure difference is 90 ℃; wherein, still include the following step: e. vacuumizing a sealing cavity of the instantaneous differential pressure treatment device containing the residues I; f. introducing hot steam into the sealed cavity until the internal temperature is 90 ℃ and the pressure is 0.20Mpa, and then carrying out pressure maintaining treatment for 30 s; g. the pressure in the sealing cavity is relieved to 6kpa within 3 s; h. repeating the steps a, b and c once every 35s, and repeating the steps 3 times in total;
step eight, squeezing the residue II to obtain primary krill oil and residue III; and step eight, putting the residue II into a screw extruder for squeezing treatment, wherein the squeezing treatment comprises first-stage squeezing and second-stage squeezing: the screw extruder is correspondingly provided with two primary squeezing cylinders and two secondary squeezing cylinders, wherein the bottoms of outer shells I of the two primary squeezing cylinders are connected, and screws in the two primary squeezing cylinders are not in contact, so that the two primary squeezing cylinders form an included angle smaller than 90 degrees; the upper end of the shell of the second-stage squeezing cylinder is connected to the joint of the bottoms of the shell II of the two first-stage squeezing cylinders, and the maximum diameter of the shell II is smaller than 1.5 times of the minimum diameter of the shell I;
step nine, fully mixing the residue III, the liquid II and the liquid III according to the volume ratio of 2:1:1 to obtain a mixture III, heating the mixture III to 45 ℃, adding a proper amount of protease into the mixture III, uniformly mixing the mixture III, standing the mixture for 50min, and centrifuging the mixture III to obtain an enzymolysis liquid; wherein the addition amount of the protease is 2 percent of the mass of the mixture III;
step ten, fully mixing the enzymatic hydrolysate with an organic solvent to extract secondary krill oil; the organic solvent is ethanol or acetone with the mass fraction of 95 percent;
and eleventh, after recovering the organic solvent in the secondary krill oil, mixing the secondary krill oil, the liquid IV and the primary krill oil, centrifuging to remove impurities and water, and refining the krill oil.
Wherein, liquid I, liquid II and liquid III are all put into the seal pot and keep for later use, and fill nitrogen gas in the seal pot.
Example 3
A krill oil extraction method comprises the following steps:
step one, blow-drying body surface moisture of euphausia superba within 2 hours after the euphausia superba is caught, and collecting blown liquid I; wherein, the step one also comprises the following steps: a. uniformly laying the Antarctic krill on a plurality of layers of drying nets distributed from top to bottom, wherein the plurality of layers of drying nets are arranged in a relatively closed drying device; b. introducing dry nitrogen into the drying device from the bottom of the drying device, wherein the temperature of the nitrogen is 60 ℃; c. after passing through the multilayer drying net, the nitrogen is discharged from an outlet of the drying device; d. the discharged nitrogen with water vapor is subjected to water-vapor separation to obtain liquid I;
freezing the euphausia superba subjected to body surface blow-drying, then performing microwave thawing treatment, and repeating the freezing and microwave thawing treatment for 3 times; the in vivo temperature of the frozen antarctic krill is-2 ℃; the time of primary microwave thawing is 20s, and the temperature in the antarctic krill is kept at 85 ℃ in the microwave thawing process;
collecting a liquid II evaporated and cooled in the microwave thawing treatment process;
step four, quickly freezing the euphausia superba obtained in the step three, and then crushing to obtain quick-frozen euphausia superba powder;
step five, adding liquid I into the quick-frozen antarctic krill powder according to the volume ratio of 1:1, uniformly mixing to obtain a mixture I, and performing ultrasonic crushing treatment on the mixture I to obtain a mixture II; wherein the frequency of the ultrasonic wave is 25KHz, and the total time of the ultrasonic wave treatmentThe length is 8min, ultrasonic treatment is carried out once every 4s, the time length of one time is 15s, and the sound power of ultrasonic is 5W/cm2；
Step six, performing centrifugal treatment on the mixture II to obtain a residue I and a liquid III;
performing flash evaporation treatment on the residue I under the instantaneous pressure difference to obtain liquid IV and residue II, wherein the flash evaporation temperature under the instantaneous pressure difference is not more than 95 ℃; wherein, still include the following step: e. vacuumizing a sealing cavity of the instantaneous differential pressure treatment device containing the residues I; f. introducing hot steam into the sealed cavity until the internal temperature is 93 ℃ and the pressure is 0.25Mpa, and then carrying out pressure maintaining treatment for 35 s; g. the pressure in the sealing cavity is relieved to 6kpa within 3 s; h. repeating the step a, the step b and the step c once every 30-45s, and repeating for 3 times in total;
step eight, squeezing the residue II to obtain primary krill oil and residue III; and step eight, putting the residue II into a screw extruder for squeezing treatment, wherein the squeezing treatment comprises first-stage squeezing and second-stage squeezing: the screw extruder is correspondingly provided with two primary squeezing cylinders and two secondary squeezing cylinders, wherein the bottoms of outer shells I of the two primary squeezing cylinders are connected, and screws in the two primary squeezing cylinders are not in contact, so that the two primary squeezing cylinders form an included angle smaller than 90 degrees; the upper end of the shell of the second-stage squeezing cylinder is connected to the joint of the bottoms of the shell II of the two first-stage squeezing cylinders, and the maximum diameter of the shell II is smaller than 1.5 times of the minimum diameter of the shell I;
step nine, fully mixing the residue III, the liquid II and the liquid III according to the volume ratio of 1:1:1 to obtain a mixture III, heating the mixture III to 45 ℃, adding a proper amount of protease into the mixture III, uniformly mixing the mixture III, standing the mixture for 50min, and centrifuging the mixture III to obtain an enzymolysis liquid; wherein the addition amount of the protease is 3 percent of the mass of the mixture III;
step ten, fully mixing the enzymatic hydrolysate with an organic solvent to extract secondary krill oil; the organic solvent is ethanol or acetone with the mass fraction of 95 percent;
and eleventh, after recovering the organic solvent in the secondary krill oil, mixing the secondary krill oil, the liquid IV and the primary krill oil, centrifuging to remove impurities and water, and refining the krill oil.
Wherein, liquid I, liquid II and liquid III are all put into the seal pot and keep for later use, and fill nitrogen gas in the seal pot.
The krill oil prepared by the method of the above example 1-3 is used as an experimental group 1, an experimental group 2 and an experimental group 3, and three groups of control groups are respectively set as a control group 1, a control group 2 and a control group 3 corresponding to the examples 1-3, wherein the processing time of the euphausia superba after being caught is the same, and the euphausia superba is directly subjected to quick freezing → crushing → homogenizing → organic solvent extraction → vacuum rotary evaporation → the processing process of refined krill oil after being dried on the body surface.
The physical and chemical properties of krill oil of experimental group 1, experimental group 2, experimental group 3, control group 1, control group 2 and control group 3 were measured by the following methods:
1) and (3) calculating yield: the yield of krill oil/% -krill oil mass (g)/dried krill meal mass (g) × 100%
2) Measurement of EPA and DHA content A sample of krill oil was sent to Standard technical service (Shanghai) Co., Ltd and entrusted to detection instead. According to the determination of total fat, saturated fat (acid) and unsaturated fat (acid) in GB/T22223-2008 food, the EPA and DHA content in the shrimp sauce is determined by adopting hydrolysis extraction-gas chromatography.
3) Content determination of vitamin E and astaxanthin content: reference is made to the method for determination of vitamin E content (AOCSOfficial method 8-89, 1998). The sample (0.05g) was dissolved in 10mL heptane and the extract was analyzed by HPLC-FLD, 4.6X 150mm silica gel column; the mobile phase is heptane: isopropanol (100:0.4) at a flow rate of 1 mL/min; the detection of the tocopherol adopts fluorescence detection, the wavelength of excitation light is 290nm, and the wavelength of emission light is 330 nm; the astaxanthin content is determined by the method of F.S.H.Lu and the like (the detection result is shown in the following table 1).
TABLE 1 Krill oil yield and physicochemical Properties
Figure GDA0002746329030000091
As can be seen from table 1 above, the experimental group 1, the experimental group 2 and the experimental group 3 all obtained higher krill oil yield and higher contents of phospholipids, VE, astaxanthin, EPA and DHA than the control group 1, the control group 2 and the control group 3, and the active ingredients of the krill oil were retained; in addition, the organic solvents used in examples 1 to 3 corresponding to experimental group 1, experimental group 2 and experimental group 3 were very small in content and almost no organic solvent remained.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable to various fields of endeavor for which the invention may be embodied with additional modifications as would be readily apparent to those skilled in the art, and the invention is therefore not limited to the details given herein and to the embodiments shown and described without departing from the generic concept as defined by the claims and their equivalents.

Claims (6)

1. A krill oil extraction method is characterized by comprising the following steps:
step one, blow-drying body surface moisture of euphausia superba within 3 hours after the euphausia superba is caught, and collecting blown liquid I;
freezing the euphausia superba subjected to body surface blow-drying, then performing microwave thawing treatment, and repeating the freezing and microwave thawing treatment for 2-3 times; the specific conditions of the microwave thawing treatment are as follows: the time of primary microwave thawing is 10-20s, and the temperature in the antarctic krill is kept not to exceed 90 ℃ in the microwave thawing process;
collecting a liquid II evaporated and cooled in the microwave thawing treatment process;
step four, quickly freezing the euphausia superba obtained in the step three, and then crushing to obtain quick-frozen euphausia superba powder;
step five, adding liquid I into the quick-frozen antarctic krill powder according to the volume ratio of 2:1-2, uniformly mixing to obtain a mixture I, and performing ultrasonic crushing treatment on the mixture I to obtain a mixture II; the frequency of ultrasonic wave is 20-25KHz, the total time of ultrasonic treatment is 4-8min, ultrasonic treatment is carried out once every 2-4s, the time of one time is 10-15s, and the sound power of ultrasonic wave is 3-5W/cm2；
Step six, performing centrifugal treatment on the mixture II to obtain a residue I and a liquid III;
performing flash evaporation treatment on the residue I under the instantaneous pressure difference to obtain liquid IV and residue II, wherein the flash evaporation temperature under the instantaneous pressure difference is not more than 95 ℃;
step eight, squeezing the residue II to obtain primary krill oil and residue III;
step nine, fully mixing the residue III, the liquid II and the liquid III according to the volume ratio of 1-2:1:1 to obtain a mixture III, heating the mixture III to 35-45 ℃, adding a proper amount of protease into the mixture III, uniformly mixing the mixture III, standing the mixture for 30-50min, and centrifuging the mixture III to obtain an enzymolysis liquid; wherein the addition amount of the protease is 1 percent of the mass of the mixture III;
step ten, fully mixing the enzymatic hydrolysate with an organic solvent to extract secondary krill oil;
step eleven, after recovering the organic solvent in the secondary krill oil, mixing the secondary krill oil, the liquid IV and the primary krill oil, centrifuging to remove impurities and water, and refining the krill oil;
wherein, the step one also comprises the following steps:
a. uniformly laying the Antarctic krill on a plurality of layers of drying nets distributed from top to bottom, wherein the plurality of layers of drying nets are arranged in a relatively closed drying device;
b. introducing dry nitrogen into the drying device from the bottom of the drying device, wherein the temperature of the nitrogen is 50-60 ℃;
c. after passing through the multilayer drying net, the nitrogen is discharged from an outlet of the drying device;
d. the discharged nitrogen with water vapor is subjected to water-vapor separation to obtain liquid I;
in addition, the seventh step further comprises the steps of:
e. vacuumizing a sealing cavity of the instantaneous differential pressure treatment device containing the residues I;
f. introducing hot steam into the sealed cavity until the internal temperature is not higher than 95 ℃ and the pressure is 0.15-0.25Mpa, and then carrying out pressure maintaining treatment for 20-40 s;
g. the pressure in the sealing cavity is relieved within 3s to 5-6 kpa;
h. repeating the steps a, b and c once every 30-45s, and repeating the steps 2-3 times in total.
2. The krill oil extraction method according to claim 1, wherein the in vivo temperature of the frozen Euphausia superba is in the range of-6 to-2 ℃ in the second step.
3. A process for extracting krill oil according to claim 1, wherein the liquid I, the liquid II and the liquid III are kept in a sealed tank and the sealed tank is filled with nitrogen.
4. A process for extracting krill oil according to claim 1, wherein the hot steam is introduced into the sealed chamber to an internal temperature of 93 ℃ and a pressure of 0.25MPa, and then the pressure is maintained for 35 s.
5. A process for extracting krill oil according to claim 1, wherein step a, step b and step c are repeated once, for a total of 3 times, in f, into the sealed chamber.
6. The krill oil extraction method according to claim 1, wherein the residue II is fed into a screw extruder to be subjected to a pressing process in step eight, and the pressing process comprises a primary pressing and a secondary pressing:
the screw extruder is correspondingly provided with two primary squeezing cylinders and two secondary squeezing cylinders, the bottoms of outer shells I of the two primary squeezing cylinders are connected, and screws in the two primary squeezing cylinders are not in contact, so that the two primary squeezing cylinders form an included angle smaller than 90 degrees;
and the upper end of the shell of the second-stage squeezing cylinder is connected to the joint of the bottoms of the shell bodies II of the two first-stage squeezing cylinders, and the maximum diameter of the shell bodies II is smaller than 1.5 times of the minimum diameter of the shell body I.
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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011051743A1 (en) * 2009-10-30 2011-05-05 Tharos Ltd. Solvent-free process for obtaining phospholipids and neutral enriched krill oils
CN102311868A (en) * 2011-04-29 2012-01-11 塞拉斯有限责任公司 Method for extracting krill oil rich in phospholipids and neutral lipid without using solvent
CN102559369A (en) * 2010-12-14 2012-07-11 大连工业大学 Preparation method of antarctic krill oil
CN102942991A (en) * 2012-12-04 2013-02-27 深圳国能环保节能科技有限公司 Microalgae oil extraction method
CN104388176A (en) * 2014-11-10 2015-03-04 大连工业大学 Method for preparing euphausia superba oil, microcapsule of euphausia superba oil and low-fluorine euphausia superba peptide by using aqueous enzymatic method
CN104479850A (en) * 2014-12-15 2015-04-01 中国水产科学研究院黄海水产研究所 Method for extracting krill oil with high phospholipid content from fresh Antarctic krill
CN105670779A (en) * 2016-03-09 2016-06-15 湛江市博泰生物化工科技实业有限公司 Method for extracting euphausia superba oil through nitrogen pressurizing water vapor
TW201635910A (en) * 2015-04-14 2016-10-16 陳淑德 One processing method for krill oil
CN106235123A (en) * 2016-08-15 2016-12-21 中国农业科学院农产品加工研究所 Utilize the method that instantaneous differential pressure flash process produces apple crisp slices

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011051743A1 (en) * 2009-10-30 2011-05-05 Tharos Ltd. Solvent-free process for obtaining phospholipids and neutral enriched krill oils
CN102559369A (en) * 2010-12-14 2012-07-11 大连工业大学 Preparation method of antarctic krill oil
CN102311868A (en) * 2011-04-29 2012-01-11 塞拉斯有限责任公司 Method for extracting krill oil rich in phospholipids and neutral lipid without using solvent
CN102942991A (en) * 2012-12-04 2013-02-27 深圳国能环保节能科技有限公司 Microalgae oil extraction method
CN104388176A (en) * 2014-11-10 2015-03-04 大连工业大学 Method for preparing euphausia superba oil, microcapsule of euphausia superba oil and low-fluorine euphausia superba peptide by using aqueous enzymatic method
CN104479850A (en) * 2014-12-15 2015-04-01 中国水产科学研究院黄海水产研究所 Method for extracting krill oil with high phospholipid content from fresh Antarctic krill
TW201635910A (en) * 2015-04-14 2016-10-16 陳淑德 One processing method for krill oil
CN105670779A (en) * 2016-03-09 2016-06-15 湛江市博泰生物化工科技实业有限公司 Method for extracting euphausia superba oil through nitrogen pressurizing water vapor
CN106235123A (en) * 2016-08-15 2016-12-21 中国农业科学院农产品加工研究所 Utilize the method that instantaneous differential pressure flash process produces apple crisp slices

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