CN115109649B - Euphausia superba oil refining process - Google Patents

Euphausia superba oil refining process Download PDF

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Publication number
CN115109649B
CN115109649B CN202211036577.9A CN202211036577A CN115109649B CN 115109649 B CN115109649 B CN 115109649B CN 202211036577 A CN202211036577 A CN 202211036577A CN 115109649 B CN115109649 B CN 115109649B
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oil
antarctic krill
crude
krill oil
stirring
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CN115109649A (en
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周芳
刘丽
李凯
冯蕾
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Fengshi Qingdao Ocean Technology Co ltd
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Fengshi Qingdao Ocean Technology Co ltd
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Priority to JP2023120287A priority patent/JP7343952B1/en
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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
    • 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
    • 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
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • C11B3/04—Refining fats or fatty oils by chemical reaction with acids
    • 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
    • C11B3/02—Refining fats or fatty oils by chemical reaction
    • C11B3/06—Refining fats or fatty oils by chemical reaction with bases
    • 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
    • C11B3/10—Refining fats or fatty oils by adsorption
    • 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
    • C11B3/16—Refining fats or fatty oils by mechanical means
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/74—Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

Abstract

The application discloses euphausia superba oil refining process belongs to krill oil preparation technical field. The refining process of the antarctic krill oil comprises the following steps: mixing the crude Antarctic krill oil with n-hexane in a ratio of 1: (2-4) mixing in a mass ratio, adding sodium silicate, and stirring and reacting in an ultrasonic water bath at 40-60 ℃ for 30-80min to obtain crude oil A; adding active zeolite into crude oil A, dearsenicating in 40-60 deg.C constant temperature water bath for 3-4 hr, and supplying air of 2-4m by blowing microporous aeration 3 Nitrogen gas/m 3 Filtering the crude oil A to obtain crude oil B; maintaining the temperature of the crude oil B below 50 deg.C, adding adsorbent, charging nitrogen, stirring for 20-40min, cooling, filtering, and collecting supernatant. According to the refining process of the antarctic krill oil, the crude product of the antarctic krill oil is refined step by step through the steps of deacidification, dearsenification and decoloration, bad substances are removed, the purity of the antarctic krill oil is improved, and the quality of the antarctic krill oil is improved.

Description

Euphausia superba oil refining process
Technical Field
The application relates to a refining process of antarctic krill oil, and belongs to the technical field of krill oil preparation.
Background
The Antarctic krill oil is a product with high nutritional efficacy and high added value in related products of Antarctic krill. The main active ingredients of the antarctic krill oil are phospholipid, astaxanthin, DHA, EPA and the like. Research shows that the euphausia superba oil has certain effects of preventing cardiovascular and cerebrovascular diseases, promoting brain development, resisting oxidation, relieving gout, rheumatoid arthritis and the like. Therefore, the Antarctic krill oil can be widely applied to industries such as food, health food, biomedicine and the like, and has high deep development and application values.
The Antarctic krill oil extracted in the rough way contains more free fatty acids (about 5-10%), unsaponifiable matters (2-7%) mainly containing cholesterol, insoluble impurities (1-4%) and arsenic enriched in the krill oil, and the like, which influence the color and quality of the Antarctic krill oil, cause certain eating problems and are not beneficial to subsequent production and sale.
Disclosure of Invention
In order to solve the problems, the antarctic krill oil refining process is provided, and the antarctic krill oil crude product is refined step by step through the steps of deacidification, dearsenification and decoloration, so that bad substances are removed, the purity of the antarctic krill oil is improved, and the quality of the antarctic krill oil is improved.
The invention adopts the following technical scheme:
a refining process of antarctic krill oil comprises the following steps:
(1) Mixing the crude Antarctic krill oil with n-hexane in a ratio of 1: (2-4) uniformly mixing the components in a mass ratio, then adding sodium silicate, placing the mixture in an ultrasonic water bath at the temperature of 40-60 ℃, and stirring and reacting for 30-80min to obtain crude oil A;
(2) Adding active zeolite into crude oil A, stirring in 40-60 deg.C constant temperature water bath for dearsenication for 3-4 hr, and aerating with blowing micropore with air supply of 2-4m 3 Nitrogen gas/m 3 Filtering the crude oil A to obtain crude oil B;
(3) Maintaining the temperature of the crude oil B below 50 deg.C, adding adsorbent, charging nitrogen, stirring for reaction for 20-40min, cooling to room temperature, centrifuging, filtering, and collecting supernatant.
Preferably, in the step (1), the adding mass of the sodium silicate is 20-40% of the crude antarctic krill oil.
Preferably, in the step (1), the ultrasonic power is 200-400W.
Preferably, in the step (2), the mass ratio of the crude oil A to the active zeolite is 1: (0.2-0.4).
Preferably, in the step (2), the active zeolite is a sodium zeolite, a calcium zeolite or a hydrogen ion type zeolite.
Preferably, in the step (3), the added mass of the adsorbent is 1-3% of that of the crude oil B.
Preferably, in the step (3), the adsorbent is activated carbon, activated clay or a mixture of the activated carbon and the activated clay.
Preferably, in the step (3), the centrifugal speed is 7000-9000r/min, and the centrifugal time is 8-15min.
Preferably, the method further comprises a step of extracting the crude euphausia superba oil, and specifically comprises the following steps:
uniformly mixing antarctic krill powder with absolute ethyl alcohol, performing stirring extraction for 0.7-1.2h, performing suction filtration, performing stirring extraction on filter residues with the absolute ethyl alcohol for 20-40min, performing suction filtration on extract, combining filtrate, and drying to obtain a crude antarctic krill oil product;
wherein the mass ratio of the antarctic krill powder to the absolute ethyl alcohol is 1: (8-12).
Preferably, the method further comprises a step of enriching the supernatant oil obtained in the step (3), and specifically comprises the following steps:
mixing the supernatant oil obtained in the step (3) with citric acid, stirring and reacting at 50-70 ℃ for 20-40min, standing in a separating funnel for 3-5h, separating to obtain a lower-layer phospholipid solution and an upper-layer triglyceride, and drying the phospholipid solution at low temperature in vacuum to obtain antarctic krill oil;
wherein the mass fraction of the citric acid is 1-3%, and the mass ratio of the supernatant oil to the citric acid is 1: (2-6), and the stirring speed is 50-70r/min.
As used herein, "room temperature" means in the range of 20-30 ℃.
Benefits of the present application include, but are not limited to:
1. in the refining process of the Antarctic krill oil, the sodium silicate is a weakly alkaline salt, can perform a neutralization reaction with acidic free fatty acid in a crude Antarctic krill oil product, simultaneously avoids a water washing process, does not cause phospholipid which is easy to absorb water and swell in the krill oil to be lost, and reduces the discharge of waste water; the ultrasonic cavitation effect of the ultrasonic waves can promote the reaction of the sodium silicate and the free fat in the krill oil, reduce the using amount of the sodium silicate, shorten the deacidification time, reduce the energy consumption and improve the deacidification efficiency and effect; adopt deacidification condition in this application can make in the krill oil free fatty acid's desorption rate reach more than 60%, and can not generate the nigre, the shrimp sauce can not become muddy, guarantees the shrimp sauce quality.
2. According to the refining process of the antarctic krill oil, the active zeolite is selected to remove arsenic elements in the crude antarctic krill oil product, the active zeolite has a natural porous loose layer structure, the specific surface area is large, the adsorption capacity for arsenic is strong, and high-valence metal ions which easily cause oil body turbidity and precipitation are prevented from being introduced in the removing process; during the process, air in the crude antarctic krill oil is removed through blowing micropore aeration, the oxidation of unsaturated fatty acid and astaxanthin in the crude antarctic krill oil is slowed down, a large number of bubbles are generated at the same time, the contact area and the contact frequency of the crude antarctic krill oil and active zeolite are increased, and the dearsenization efficiency and the dearsenization effect are improved; arsenic content in the Antarctic krill oil obtained by arsenic removal condition treatment in the application is remarkably reduced, and most of arsenic exists in the form of organic arsenic, so that the food safety of the krill oil is high.
3. According to the refining process of the Antarctic krill oil, pigment substances in the Antarctic krill oil are removed through the adsorbent, so that the color and the quality of oil are improved, and meanwhile, the adsorbent can adsorb free fatty acid remained in the previous step to obtain high-purity Antarctic krill oil; the color of the krill oil obtained under the decolorizing condition is orange red, clear and high in transparency, and the food safety of the euphausia superba oil is improved.
4. In the refining process of the antarctic krill oil, absolute ethyl alcohol is selected as an organic solvent in the extraction step, so that safe and high-efficiency extraction of the antarctic krill oil is realized; citric acid is selected as the reaction solution in the enrichment step, so that the layering is obvious, and functional components in the phospholipid solution and the triglyceride obtained by the separation are hardly influenced.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The raw materials or instruments used are not indicated by manufacturers, and are all conventional products which can be obtained by commercial purchase.
In this application, antarctic krill powder obtains after the preliminary treatment, and specific preliminary treatment step is: unfreezing frozen antarctic krill shrimp bricks with running water, cooking to inactivate enzyme, freeze-drying in vacuum, and pulverizing to obtain antarctic krill powder; wherein, the antarctic krill shrimp brick is purchased from Dalian ocean fishery group company of Liaoning province and is frozen at-20 ℃ for standby.
Example 1
A refining process of antarctic krill oil comprises the following steps:
(1) Mixing Antarctic krill powder with absolute ethyl alcohol according to the ratio of 1: uniformly mixing the mixture according to the mass ratio of 10, performing suction filtration after stirring and extracting for 1h, and then mixing the filter residue with absolute ethyl alcohol according to the mass ratio of 1: uniformly mixing the raw materials according to the mass ratio of 10, stirring and extracting for 30min, performing suction filtration on the extracting solution, combining the filtrate, and drying to obtain a crude product of the euphausia superba oil;
(2) Mixing the crude Antarctic krill oil with n-hexane in a ratio of 1:3, then adding sodium silicate accounting for 30 percent of the mass of the crude Antarctic krill oil, placing the mixture into an ultrasonic water bath at 50 ℃, stirring and reacting for 60min, wherein the ultrasonic power is set to be 300W, and obtaining crude oil A;
(3) Adding sodium type zeolite into crude oil A, wherein the mass ratio of the crude oil A to the sodium type zeolite is 1:0.3 stirring in a constant temperature water bath at 50 ℃ for dearsenifying for 3.5h, and aerating by blowing micropores at the period of time, wherein the air supply amount is 3m 3 Nitrogen gas/m 3 Filtering the crude oil A to obtain crude oil B;
(4) Maintaining the temperature of the crude oil B at 30 ℃, adding activated carbon and activated clay with the mass ratio of 1 to 2 percent of the total mass of the added activated carbon and activated clay, charging nitrogen, stirring for reaction for 30min, cooling to room temperature, centrifuging and filtering, wherein the centrifugal speed is 8000r/min, the centrifugal time is 10min, and taking supernatant oil;
(5) Mixing the supernatant oil with 2% citric acid according to the mass percentage of 1: mixing at a mass ratio of 4, stirring at 60 ℃ for 30min, reacting at a stirring speed of 60r/min, standing in a separating funnel for 4h, separating to obtain a lower-layer phospholipid solution and an upper-layer triglyceride, and drying the phospholipid solution at low temperature in vacuum to obtain the antarctic krill oil.
Example 2
A refining process of antarctic krill oil comprises the following steps:
(1) Mixing Antarctic krill powder with absolute ethyl alcohol according to the ratio of 1:8, stirring and extracting for 1.2h, then carrying out suction filtration, and mixing the filter residue with absolute ethyl alcohol according to a ratio of 1:8, uniformly mixing the raw materials in a mass ratio of 8, stirring and extracting for 40min, performing suction filtration on an extracting solution, combining filtrates, and drying to obtain a crude product of the euphausia superba oil;
(2) Mixing the crude Antarctic krill oil with n-hexane in a ratio of 1:2, uniformly mixing, adding sodium silicate accounting for 20% of the mass of the crude Antarctic krill oil, placing the mixture into an ultrasonic water bath at 40 ℃, and stirring for reacting for 80min, wherein the ultrasonic power is set to be 200W, so as to obtain crude oil A;
(3) Adding hydrogen ion type zeolite into crude oil A, wherein the mass ratio of the crude oil A to the hydrogen ion type zeolite is 1:0.2 stirring in 40 deg.C constant temperature water bath for dearsenifying for 4 hr, aerating by blowing microporous aeration with air supply amount of 2m 3 Nitrogen gas/m 3 Filtering the crude oil A to obtain crude oil B;
(4) Maintaining the temperature of the crude oil B at 20 ℃, adding activated carbon, wherein the adding mass of the activated carbon is 1% of that of the crude oil B, charging nitrogen, stirring for reaction for 40min, cooling to room temperature, centrifuging and filtering, wherein the centrifugal rotating speed is 7000r/min, the centrifugal time is 15min, and taking supernatant oil;
(5) Mixing the supernatant oil with 1% citric acid according to a mass ratio of 1:2, stirring at 50 ℃ for 40min, standing in a separating funnel for 5h, separating to obtain a lower layer of phospholipid solution and an upper layer of triglyceride, and drying the phospholipid solution in vacuum at low temperature to obtain the antarctic krill oil.
Example 3
A refining process of antarctic krill oil comprises the following steps:
(1) Mixing Antarctic krill powder with absolute ethyl alcohol according to the ratio of 1:12, stirring and extracting for 0.7h, then carrying out suction filtration, and mixing the filter residue with absolute ethyl alcohol according to a ratio of 1: uniformly mixing the raw materials according to the mass ratio of 12, stirring and extracting for 20min, performing suction filtration on an extracting solution, combining filtrates, and drying to obtain a crude product of the euphausia superba oil;
(2) Mixing the crude Antarctic krill oil with n-hexane in a ratio of 1:4, uniformly mixing, adding sodium silicate accounting for 40% of the mass of the crude Antarctic krill oil, placing the mixture into an ultrasonic water bath at 60 ℃, stirring and reacting for 30min, wherein the ultrasonic power is set to be 400W, and obtaining crude oil A;
(3) Adding calcium type zeolite into the crude oil A, wherein the mass ratio of the crude oil A to the calcium type zeolite is 1:0.4 stirring in a constant temperature water bath at 60 ℃ for dearsenifying for 3 hours, and aerating by blowing micropores at the period of time, wherein the air supply amount is 4m 3 Nitrogen gas/m 3 Filtering the crude oil A to obtain crude oil B;
(4) Maintaining the temperature of the crude oil B at 40 ℃, adding activated clay, wherein the adding mass of the activated clay is 3% of that of the crude oil B, charging nitrogen, stirring for reaction for 20min, cooling to room temperature, centrifuging and filtering, wherein the centrifugal rotating speed is 9000r/min, the centrifugal time is 8min, and taking supernatant oil;
(5) Mixing the supernatant oil with 3% citric acid according to the mass percent of 1: and 6, mixing according to the mass ratio, stirring at 70 ℃ for 20min, reacting at the stirring speed of 50r/min, standing in a separating funnel for 3h, separating to obtain a lower-layer phospholipid solution and an upper-layer triglyceride, and drying the phospholipid solution in vacuum at a low temperature to obtain the antarctic krill oil.
Comparative example 1
A refining process of antarctic krill oil comprises the following steps:
(1) Mixing Antarctic krill powder with absolute ethyl alcohol according to the ratio of 1: uniformly mixing the materials according to a mass ratio of 10, performing suction filtration after stirring and extracting for 1h, and then mixing the filter residue with absolute ethyl alcohol according to a ratio of 1: uniformly mixing the raw materials according to the mass ratio of 10, stirring and extracting for 30min, performing suction filtration on the extracting solution, combining the filtrate, and drying to obtain a crude product of the euphausia superba oil;
(2) Mixing the crude Antarctic krill oil with n-hexane in a ratio of 1:3, uniformly mixing, adding sodium silicate accounting for 30% of the mass of the crude Antarctic krill oil, placing the mixture into an ultrasonic water bath at 50 ℃, and stirring to react for 60min, wherein the ultrasonic power is set to be 300W, so as to obtain crude oil A;
(3) Maintaining the temperature of the crude oil A at 30 ℃, adding activated carbon and activated clay with the mass ratio of 1 to 2 percent of the total mass of the added activated carbon and activated clay, charging nitrogen, stirring for reaction for 30min, cooling to room temperature, centrifuging and filtering, wherein the centrifugal speed is 8000r/min, the centrifugal time is 10min, and taking supernatant oil;
(4) Mixing the supernatant oil with 2% citric acid according to the mass percentage of 1: mixing at a mass ratio of 4, stirring at 60 ℃ for 30min, reacting at a stirring speed of 60r/min, standing in a separating funnel for 4h, separating to obtain a lower-layer phospholipid solution and an upper-layer triglyceride, and drying the phospholipid solution at low temperature in vacuum to obtain the antarctic krill oil.
Comparative example 2
A refining process of antarctic krill oil comprises the following steps:
(1) Mixing Antarctic krill powder with absolute ethyl alcohol according to the ratio of 1: uniformly mixing the mixture according to the mass ratio of 10, performing suction filtration after stirring and extracting for 1h, and then mixing the filter residue with absolute ethyl alcohol according to the mass ratio of 1: uniformly mixing the raw materials according to the mass ratio of 10, stirring and extracting for 30min, performing suction filtration on the extracting solution, combining the filtrate, and drying to obtain a crude product of the euphausia superba oil;
(2) Mixing the crude Antarctic krill oil with n-hexane in a ratio of 1:3, uniformly mixing, adding sodium silicate accounting for 30% of the mass of the crude Antarctic krill oil, placing the mixture into an ultrasonic water bath at 50 ℃, and stirring to react for 60min, wherein the ultrasonic power is set to be 300W, so as to obtain crude oil A;
(3) Adding sodium type zeolite into crude oil A, wherein the mass ratio of the crude oil A to the sodium type zeolite is 1:0.3, stirring in a constant temperature water bath at 50 ℃ for dearsenization for 3.5 hours, and aerating by blowing micropores at the period of time, wherein the air supply amount is 3m 3 Nitrogen gas/m 3 Filtering the crude oil A to obtain crude oil B;
(4) Mixing the crude oil B with 2% of citric acid according to the mass fraction of 1: mixing at a mass ratio of 4, stirring at 60 ℃ for 30min, reacting at a stirring speed of 60r/min, standing in a separating funnel for 4h, separating to obtain a lower-layer phospholipid solution and an upper-layer triglyceride, and drying the phospholipid solution at low temperature in vacuum to obtain the antarctic krill oil.
Comparative example 3
The difference from example 1 is that: replacing the step (2) with: mixing the crude Antarctic krill oil with n-hexane in a ratio of 1:3, then adding sodium silicate accounting for 30 percent of the mass of the crude Antarctic krill oil, placing the mixture into a thermostatic water bath at 50 ℃, stirring and reacting for 60min to obtain crude oil A.
Comparative example 4
The difference from example 1 is that: replacing the step (3) with: adding sodium type zeolite into crude oil A, wherein the mass ratio of the crude oil A to the sodium type zeolite is 1:0.3, stirring in a constant-temperature water bath at 50 ℃ for 3.5 hours to remove arsenic, and filtering to obtain crude oil B.
Comparative example 5
The difference from example 1 is that: sodium zeolite was replaced with montmorillonite.
Comparative example 6
The difference from example 1 is that: the activated carbon and the activated clay with the mass ratio of 1.
Comparative example 7
The difference from example 1 is that: citric acid was replaced by sodium silicate.
The performance of the antarctic krill oil obtained by the above examples 1-3 and comparative examples 1-7 was tested and the results are shown in table 1; wherein, the arsenic detection refers to GB 5009.11-2014 'determination of total arsenic and inorganic arsenic in food', and the dearsenification rate = arsenic content in zeolite/arsenic content in krill oil x 100%.
Calculation formula of acid removal rate (%): free fatty acid removal rate (%) = (A1-A2)/A1X 100%
In the formula: a1 is the content (%) of free fatty acid in the raw shrimp oil; a2 is the content (%) of free fatty acid in the treated shrimp sauce.
The determination of the phospholipid content of the Antarctic krill oil is disclosed in GB/T5537-2008 'determination of phospholipid content in grain oil inspection'.
TABLE 1
Figure DEST_PATH_IMAGE001
As can be seen from table 1, compared with comparative examples 1 to 7, the antarctic krill oil refining process of examples 1 to 3 is adopted to refine the antarctic krill oil crude product step by step through the steps of deacidification, dearsenification and decoloration, so that bad substances are removed, the purity of the antarctic krill oil is improved, and the quality of the antarctic krill oil is improved.
The above description is only an example of the present application, and the protection scope of the present application is not limited by these specific examples, but is defined by the claims of the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the technical idea and principle of the present application should be included in the protection scope of the present application.

Claims (6)

1. A refining process of antarctic krill oil is characterized by comprising the following steps:
(1) Mixing the crude Antarctic krill oil with n-hexane in a ratio of 1: (2-4) uniformly mixing the components in a mass ratio, then adding sodium silicate, placing the mixture in an ultrasonic water bath at 50 ℃, and stirring and reacting for 60min to obtain crude oil A;
(2) Adding active zeolite into crude oil A, stirring in 40-60 deg.C constant temperature water bath for dearsenication for 3-4 hr, and aerating with blowing micropore with air supply of 3m 3 Nitrogen gas/m 3 Filtering the crude oil A to obtain crude oil B;
(3) Maintaining the temperature of the crude oil B below 50 ℃, adding an adsorbent, charging nitrogen, stirring for reaction for 20-40min, cooling to room temperature, centrifuging, filtering, and taking supernatant oil;
(4) Mixing the supernatant oil obtained in the step (3) with citric acid, stirring and reacting at 50-70 ℃ for 20-40min, standing in a separating funnel for 3-5h, separating to obtain a lower-layer phospholipid solution and an upper-layer triglyceride, and drying the phospholipid solution at low temperature in vacuum to obtain the antarctic krill oil;
wherein the mass fraction of the citric acid is 1-3%, and the mass ratio of the supernatant oil to the citric acid is 1: (2-6), wherein the stirring speed is 50-70r/min;
in the step (1), the ultrasonic power is 300W;
in the step (3), the adding mass of the adsorbent is 1-3% of that of the crude oil B, and the adsorbent is activated carbon, activated clay or a mixture of the activated carbon and the activated clay.
2. The refining process of antarctic krill oil according to claim 1, wherein in the step (1), the added mass of sodium silicate is 20-40% of the crude antarctic krill oil.
3. The refining process of antarctic krill oil according to claim 1, wherein in the step (2), the mass ratio of the crude oil A to the active zeolite is 1: (0.2-0.4).
4. The refining process of antarctic krill oil according to claim 1, wherein in the step (2), the active zeolite is sodium type zeolite, calcium type zeolite or hydrogen ion type zeolite.
5. The refining process of antarctic krill oil according to claim 1, wherein in step (3), the centrifugal rotation speed is 7000-9000r/min and the centrifugal time is 8-15min.
6. The antarctic krill oil refining process according to claim 1, further comprising a step of extracting the crude antarctic krill oil, specifically comprising the steps of:
uniformly mixing antarctic krill powder with absolute ethyl alcohol, performing stirring extraction for 0.7-1.2h, performing suction filtration, performing stirring extraction on filter residues with the absolute ethyl alcohol for 20-40min, performing suction filtration on extract, combining filtrate, and drying to obtain a crude antarctic krill oil product;
wherein the mass ratio of the antarctic krill powder to the absolute ethyl alcohol is 1: (8-12).
CN202211036577.9A 2022-08-29 2022-08-29 Euphausia superba oil refining process Active CN115109649B (en)

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Application Number Priority Date Filing Date Title
CN202211036577.9A CN115109649B (en) 2022-08-29 2022-08-29 Euphausia superba oil refining process
JP2023120287A JP7343952B1 (en) 2022-08-29 2023-07-24 Antarctic krill oil refining process
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