CN109439430B - Euphausia superba oil refining method - Google Patents
Euphausia superba oil refining method Download PDFInfo
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- CN109439430B CN109439430B CN201811231008.3A CN201811231008A CN109439430B CN 109439430 B CN109439430 B CN 109439430B CN 201811231008 A CN201811231008 A CN 201811231008A CN 109439430 B CN109439430 B CN 109439430B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/12—Production of fats or fatty oils from raw materials by melting out
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/115—Fatty acids or derivatives thereof; Fats or oils
- A23L33/12—Fatty acids or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
Abstract
The invention discloses a method for refining antarctic krill oil, which comprises the following steps: step S1: adding a hydration solution which is 1-6 times of the mass content of phospholipid in the antarctic krill oil into the antarctic krill oil, heating while stirring for 30-120 min to 45-70 ℃, cooling, standing, and performing sedimentation separation or centrifugal separation to obtain antarctic krill oil triglyceride and antarctic krill oil phospholipid solution; wherein the hydration solution is an aqueous solution containing citric acid with the mass concentration of 1.5-6%; step S2: and (4) concentrating and drying the euphausia superba oil phospholipid solution separated in the step (S1), and removing water to obtain the dehydrated euphausia superba oil phospholipid. The method has the advantages that the triglyceride and the phospholipid can be fully separated, the loss of functional components on the separated product is avoided, the separated product has the advantages of high purity, strong functionality, stable property and no impurities, and the separated product can be used as a functional component to be added into health food, so that the utilization rate of the euphausia superba is improved.
Description
Technical Field
The invention relates to the field of oil refining, and in particular relates to a method for refining antarctic krill oil.
Background
Antarctic krill is one of the largest resource single organisms on earth. It is estimated that the biomass of antarctic krill is about 6.5-10 million tons. The annual fishing amount of the antarctic krill is about 6000 million to 1 hundred million tons, which is equivalent to the total yield of marine fishes and crustaceans in one year around the world. The Antarctic krill is the fourth most resource of the earth after grains, petroleum and coal, and the Antarctic krill and the grains are renewable resources. Antarctic krill has extremely high nutritional value and is increasingly valued by people.
The euphausia superba oil is an upgraded product for human health, has the functions of preventing and assisting in treating cardiovascular and cerebrovascular diseases and diabetes, resisting aging and oxidation, eliminating free radicals, effectively reducing arthritis symptoms and the like, has obvious effects on reducing premenstrual syndrome and dysmenorrhea, assisting in treating hyperactivity, improving human immunity, enhancing human physical strength and vitality and the like, fills the blank of related products in the domestic health-care market, and will create a new era of the domestic functional nutritional food industry.
Antarctic krill oil is widely concerned as a novel marine functional oil, and is a product with relatively high nutritional efficacy and added value in related products of Antarctic krill, so that the Antarctic krill oil becomes one of the Antarctic krill products with the greatest development prospect.
The main components of the antarctic krill oil comprise phospholipid and triglyceride, wherein the content of phospholipid is more than 45%, and a large amount of unsaturated fatty acids such as EPA and DHA are combined on the phospholipid, so that the phospholipid is the only molecular structure combining EPA and DHA in a phospholipid form in the natural world at present and is easy to absorb by a human body, therefore, the effect of the krill oil is 15-20 times that of fish oil, and meanwhile, the triglyceride is combined with a high-content functional component astaxanthin, so that the antarctic krill oil has better oxidation resistance.
Disclosure of Invention
The invention aims to provide a method for refining antarctic krill oil, which is used for further separating phospholipid and triglyceride from the antarctic krill oil, retaining functional components in the phospholipid and the triglyceride to the maximum extent, improving the utilization rate of the antarctic krill and producing a health-care product with high added value and stronger functionality.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a refining method of antarctic krill oil is characterized by comprising the following steps:
step S1: adding a hydration solution which is 1-6 times of the mass content of phospholipid in the antarctic krill oil into the antarctic krill oil, heating while stirring for 30-120 min to 45-70 ℃, cooling, standing, and performing sedimentation separation or centrifugal separation to obtain antarctic krill oil triglyceride and antarctic krill oil phospholipid solution; wherein the hydration solution is an aqueous solution containing citric acid with the mass concentration of 1.5-6%;
step S2: and (4) concentrating and drying the euphausia superba oil phospholipid solution separated in the step (S1), and removing water to obtain the dehydrated euphausia superba oil phospholipid.
Further, in the step S1, the stirring rotation number is 50 to 100 r/min.
Further, in the step S1, the cooling process is to cool the mixture to below 40 ℃ within 30-120 min.
Further, in the step S2, the concentration and drying are carried out for 24 to 72 hours under the conditions of-20 to-50 ℃ and 5 to 10pa of vacuum low-temperature freeze drying.
Furthermore, the quality of the hydration solution is 3-5 times of the content of phospholipid in the antarctic krill oil.
Further, the quality of the hydration solution is 4 times of the content of phospholipid in the antarctic krill oil.
Further, the hydration solution is an aqueous solution containing citric acid with the mass concentration of 1.5-3%.
Further, in step S1, heating is performed using a water bath.
According to the technical scheme, the method realizes the separation of triglyceride and phospholipid components in the antarctic krill oil under certain reaction conditions by adopting the hydration solution added with the citric acid electrolyte, keeps the functional components on the antarctic krill oil from losing, has high purity, strong functionality, stable property and no impurity of the separated product, can be used as the functional components to be added into health-care food, and improves the utilization rate of the antarctic krill.
Drawings
Fig. 1 is a schematic flow diagram of a method for refining antarctic krill oil according to the present invention.
Detailed Description
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
The existing hydration degumming method is always applied to the production of vegetable oil, the phospholipid content in the oil used for degumming is lower than 5%, the phospholipid content is rarely used for animal oil, the phospholipid content in the existing animal and vegetable oil is only used as a single individual, the phospholipid content in the antarctic krill oil is higher than 45%, EPA and DHA are combined, and the difficulty of hydration degumming is increased.
The existing method for hydration degumming of grease comprises the following steps: after heating water in hot oil, hydrophilic groups in phospholipid molecules are combined with water and converted into a hydrated phospholipid molecular structure, so that the phospholipid molecules are separated out of the oil and dissolved in the hot water, which belongs to a physical hydration process, and the temperature of a hydration solution is usually equal to or slightly higher than that of the hot oil. The hydration degumming effect depends to a large extent on the stability of the phospholipid micelles formed after water absorption.
Factors influencing hydration degumming include: 1) adding water, wherein a stable micelle structure can be formed only by adding a proper amount of water, and the water is insufficient, the hydration is incomplete, and the flocculation of colloidal particles is poor; excessive water easily forms water/oil or oil/water emulsification phenomenon, and is difficult to separate; 2) the hydration temperature is related to the water adding amount, and the larger the water adding amount is, the larger the micelle granularity is, and the higher the hydration temperature is; 3) the mixing intensity and action time, and the mechanical mixing can make the water drops form enough dispersion, and can not form stable oil/water or water/oil emulsion state. Therefore, the water addition amount, the hydration temperature and the stirring strength need to have proper ranges so as to maximally separate the phospholipids from the triglyceride in the antarctic krill oil and enable the residual amount of the phospholipids in the triglyceride to meet the requirements.
Referring to fig. 1, the present invention further optimizes the reaction conditions based on the existing hydration degumming method, and specifically comprises the following steps:
step S1: and adding a hydration solution which is 1-6 times of the mass content of phospholipid in the Antarctic krill oil into the Antarctic krill oil, heating and stirring for 30-120 min to 45-70 ℃, and carrying out medium-low temperature hydration degumming. The method is different from the method of heating water in hot oil in the existing hydration method, the temperature of the antarctic krill oil and the added hydration solution is normal temperature, heating and stirring are a milder heating process, loss of functional active components such as EPA, DHA, astaxanthin and the like at high temperature can be avoided to the greatest extent, in addition, continuous stirring limits rapid increase of phospholipid particle size, the critical hydrolysis temperature of phospholipid is reduced, namely the temperature of flocculent phospholipid is generated, and loss of the functional active components such as EPA, DHA, astaxanthin and the like at high temperature is further avoided. Preferably, the stirring speed is 50r/min to 100 r/min. Preferably, a water bath is adopted for heating, the temperature is further controlled, and the loss of EPA and DHA caused by overhigh temperature is avoided.
And then cooling, standing, and carrying out sedimentation separation or centrifugal separation to obtain the antarctic krill oil triglyceride and the antarctic krill oil phospholipid solution. When phospholipid absorbs water to become flocculation micelle and is dissolved in water solution, a hydration process occurs, and the temperature is highest. In order to avoid the loss of the functional components caused by high temperature as much as possible, the stirring and heating time cannot last too long, preferably 30-120 min, after the stirring and heating are finished, the temperature is reduced as much as possible within a short time due to the residual heat in order to reduce the loss of the functional components, and the cooling process is preferably cooled to below 40 ℃ within 30-120 min.
Because the temperature of the hydration solution is room temperature when the hydration solution is added, the hydration degumming effect is weakened, even degumming can not be realized, in order to enhance the degumming effect, a small amount of electrolyte is added in the hydration solution, and the electrolyte is preferably citric acid from the edible point of view. In addition, because antarctic krill oil phospholipid also contains acid with weak hydrophilicity, such as phosphatidic acid, which is not dissolved in water, the addition of the electrolyte can also convert the acid with weak hydrophilicity into acid with strong hydrophilicity, so that triglyceride can be separated from the phospholipid as much as possible, and the residual amount of the phospholipid in the triglyceride is reduced. Preferably, the mass concentration of the citric acid is 1.5-6%, and the citric acid can promote the non-hydrated phospholipid to be converted into the hydrophilic phospholipid.
Step S2: and (4) concentrating and drying the antarctic krill oil phospholipid solution separated in the step (S1) to remove water to obtain dehydrated antarctic krill oil phospholipid, wherein in order to avoid loss of functional components, the concentrating and drying conditions are preferably vacuum low-temperature freeze drying for 24-72 h under the conditions of-20-50 ℃ and 5-10 pa.
Example 1
Adding a hydration solution (specifically a 1.5% citric acid solution) with the phospholipid mass content being 3 times that of the krill oil into the krill oil by adopting a water bath heating device, heating while stirring, stirring at 50r/min for 30min, cooling to 60 ℃, cooling to below 40 ℃ within 1h, standing and settling for 4h to obtain triglyceride at the upper layer and phospholipid solution at the lower layer, and separating to obtain the high-astaxanthin type antarctic krill oil triglyceride and high-EPA/DHA type antarctic krill oil phospholipid solution.
And (3) carrying out component identification on the separated product, wherein the content of astaxanthin in the triglyceride of the high-astaxanthin type antarctic krill oil obtained by separation is 895.43ppm, and the residual content of phospholipid is 98 ppm. In the phospholipid solution of the high EPA/DHA type antarctic krill oil, the content of phospholipid is 22.94%, the content of EPA and DHA is 79.82mg/g and 56.12mg/g respectively, and compared with the content of astaxanthin, EPA and DHA in the antarctic krill oil before separation, the loss rates of astaxanthin, phospholipid, EPA and DHA are 4.56%, 8.25%, 0.73% and 0.96% respectively.
And (3) drying and dehydrating the high EPA/DHA type antarctic krill oil phospholipid solution at the temperature of 50 ℃ below zero and the low temperature of 10pa for 48 hours to obtain the high EPA/DHA type antarctic krill oil phospholipid powder (the water content is lower than 2%).
Example 2
Adding a hydration solution (specifically a 1.5% citric acid solution) with 4 times of phospholipid by mass into the Euphausia superba oil by adopting a water bath heating device, stirring at 60 ℃ and 50r/min for 30min, cooling to below 40 ℃ within 1h, standing and settling for 4h to obtain triglyceride at the upper layer and phospholipid solution at the lower layer, and separating to obtain the high-astaxanthin type Euphausia superba oil triglyceride and the high-EPA/DHA type Euphausia superba oil phospholipid solution.
Wherein the content of astaxanthin in the triglyceride of the euphausia superba oil with high astaxanthin content is 881.35ppm, and the residue content of phospholipid is 75 ppm. In the high EPA/DHA type antarctic krill oil phospholipid solution, the content of phospholipid is 19.97%, the content of EPA and DHA is 69.52mg/g and 48.93mg/g respectively, and the loss rates of astaxanthin, phospholipid, EPA and DHA are 6.06%, 0.15%, 0.54% and 0.80% respectively.
And (3) drying and dehydrating the high EPA/DHA type antarctic krill oil phospholipid solution for 72h at the temperature of 50 ℃ below zero and under the low-temperature vacuum condition of 10pa to obtain the high EPA/DHA type antarctic krill oil phospholipid powder (the water content is lower than 2%).
Example 3
Adding a hydration solution (specifically a 1.5% citric acid solution) with the phospholipid content being 1 time of the mass of the oil into the oil of the euphausia superba by adopting a water bath heating device, stirring the oil at 60 ℃ and 50r/min for 30min, cooling the oil to below 40 ℃ within 1h, standing and settling the oil for 4h to obtain triglyceride positioned at the upper layer and a phospholipid solution positioned at the lower layer, and separating the triglyceride and the phospholipid solution to obtain the high-astaxanthin type antarctic krill oil and the high-EPA/DHA type antarctic krill oil phospholipid solution.
Wherein the content of astaxanthin in the high-astaxanthin type antarctic krill oil triglyceride is 857.58ppm, and the content of phospholipid residue is 186 ppm. In the high EPA/DHA type antarctic krill oil phospholipid solution, the content of phospholipid is 45.63%, the content of EPA and DHA is 152.13mg/g and 106.86mg/g respectively, and the loss rates of astaxanthin, phospholipid, EPA and DHA are 8.59%, 8.74%, 4.88% and 5.19% respectively.
And (3) drying and dehydrating the high EPA/DHA type antarctic krill oil phospholipid solution at the temperature of-20 ℃ and the low temperature of 10pa for 24 hours to obtain the high EPA/DHA type antarctic krill oil phospholipid powder (the water content is lower than 2%).
Example 4
Adding a hydration solution (specifically a 1.5% citric acid solution) with phospholipid content 5 times of the mass of the krill oil into the krill oil by adopting a water bath heating device, stirring at 60 ℃ and 50r/min for 30min, cooling to below 40 ℃ within 1h, standing and settling for 4h to obtain triglyceride at the upper layer and phospholipid solution at the lower layer, and separating to obtain the high-astaxanthin type antarctic krill oil triglyceride and the high-EPA/DHA type antarctic krill oil phospholipid solution.
Wherein the content of astaxanthin in the high-astaxanthin type antarctic krill oil triglyceride is 869.36ppm, and the content of phospholipid residue is 127 ppm. In the high EPA/DHA type antarctic krill oil phospholipid solution, the content of phospholipid is 16.63%, the content of EPA and DHA is 57.82mg/g and 40.61mg/g respectively, and the loss rates of astaxanthin, phospholipid, EPA and DHA are 7.34%, 0.22%, 0.81% and 1.14% respectively.
And (3) drying and dehydrating the high EPA/DHA type antarctic krill oil phospholipid solution at the temperature of 50 ℃ below zero and the low temperature of 5pa for 48 hours to obtain the high EPA/DHA type antarctic krill oil phospholipid powder (the water content is lower than 2%).
Example 5
Adding a hydration solution (specifically a 1.5% citric acid solution) with phospholipid content 6 times the mass of the antarctic krill oil into the antarctic krill oil by adopting a water bath heating device, stirring for 30min at 60 ℃ at 50r/min, cooling to below 40 ℃ within 1h, standing and settling for 4h to obtain triglyceride at the upper layer and a phospholipid solution at the lower layer, and separating to obtain the high-astaxanthin type antarctic krill oil triglyceride and the high-EPA/DHA type antarctic krill oil phospholipid solution.
The content of astaxanthin in the triglyceride of the high-astaxanthin type antarctic krill oil is 827.16ppm, and the residual content of phospholipid is 133 ppm. In the high EPA/DHA type antarctic krill oil phospholipid solution, the content of phospholipid is 13.93%, the content of EPA and DHA is 47.93mg/g and 33.75mg/g respectively, and the loss rates of astaxanthin, phospholipid, EPA and DHA are 11.84%, 2.49%, 1.84% and 1.91% respectively.
And (3) drying and dehydrating the high EPA/DHA type antarctic krill oil phospholipid solution at the temperature of 50 ℃ below zero and the low temperature of 5pa for 72 hours to obtain the high EPA/DHA type antarctic krill oil phospholipid powder (the water content is lower than 2%).
Example 6
Adding a hydration solution (specifically a 2% citric acid solution) with 4 times of phospholipid by mass into the Euphausia superba oil by adopting a water bath heating device, stirring for 30min at 60 ℃ at 50r/min, cooling to below 40 ℃ within 1h, standing and settling for 4h to obtain triglyceride at the upper layer and a phospholipid solution at the lower layer, and separating to obtain the high-astaxanthin type Euphausia superba oil triglyceride and the high-EPA/DHA type Euphausia superba oil phospholipid solution.
The content of astaxanthin in the triglyceride of the euphausia superba oil with high astaxanthin type is 872.61ppm, and the residual content of phospholipid is 94 ppm. In the high EPA/DHA type antarctic krill oil phospholipid solution, the content of phospholipid is 19.36%, the content of EPA and DHA is 67.43mg/g and 47.43mg/g respectively, and the loss rates of astaxanthin, phospholipid, EPA and DHA are 6.99%, 3.2%, 0.63% and 0.81% respectively.
And (3) drying and dehydrating the high EPA/DHA type antarctic krill oil phospholipid solution at the temperature of-20 ℃ and the low temperature of 5pa for 72h to obtain the high EPA/DHA type antarctic krill oil phospholipid powder (the water content is lower than 2%).
Example 7
Adding a hydration solution (specifically a 3% citric acid solution) with 4 times of phospholipid by mass into the Euphausia superba oil by adopting a water bath heating device, stirring for 30min at 60 ℃ at 50r/min, cooling to below 40 ℃ within 1h, standing and settling for 4h to obtain triglyceride at the upper layer and a phospholipid solution at the lower layer, and separating to obtain the high-astaxanthin type Euphausia superba oil triglyceride and the high-EPA/DHA type Euphausia superba oil phospholipid solution.
The content of astaxanthin in the triglyceride of the high-astaxanthin type antarctic krill oil is 830.42ppm, and the content of phospholipid residues is 86 ppm. In the high EPA/DHA type antarctic krill oil phospholipid solution, the content of phospholipid is 19.41%, the content of EPA and DHA is 67.54mg/g and 47.57mg/g respectively, and the loss rates of astaxanthin, phospholipid, EPA and DHA are 11.49%, 2.95%, 0.73% and 0.78% respectively.
And (3) drying and dehydrating the high EPA/DHA type antarctic krill oil phospholipid solution at the temperature of-20 ℃ and the low temperature of 5pa for 48 hours to obtain the high EPA/DHA type antarctic krill oil phospholipid powder (the water content is lower than 2%).
Example 8
Adding a hydration solution (specifically 4.5% citric acid solution) with 4 times of phospholipid content into the Euphausia superba oil by adopting a water bath heating device, stirring at 60 ℃ and 50r/min for 30min, cooling to below 40 ℃ within 1h, standing and settling for 4h to obtain triglyceride at the upper layer and phospholipid solution at the lower layer, and separating to obtain the high-astaxanthin type Euphausia superba oil triglyceride and high-EPA/DHA type Euphausia superba oil phospholipid solution.
The content of astaxanthin in the triglyceride of the high-astaxanthin type antarctic krill oil is 817.63ppm, and the content of phospholipid residues is 118 ppm. In the high EPA/DHA type antarctic krill oil phospholipid solution, the content of phospholipid is 18.62%, the content of EPA and DHA is 64.64mg/g and 45.50mg/g respectively, and the loss rates of astaxanthin, phospholipid, EPA and DHA are 12.85%, 6.9%, 0.96% and 1.06% respectively.
And (3) drying and dehydrating the high EPA/DHA type antarctic krill oil phospholipid solution for 72h at the temperature of-20 ℃ and under the low-temperature vacuum condition of 10pa to obtain the high EPA/DHA type antarctic krill oil phospholipid powder (the water content is lower than 2%).
Example 9
Adding a hydration solution (specifically a 6% citric acid solution) with 4 times of phospholipid by mass into the Euphausia superba oil by adopting a water bath heating device, stirring for 30min at 60 ℃ at 50r/min, cooling to below 40 ℃ within 1h, standing and settling for 4h to obtain triglyceride at the upper layer and a phospholipid solution at the lower layer, and separating to obtain the high-astaxanthin type Euphausia superba oil triglyceride and the high-EPA/DHA type Euphausia superba oil phospholipid solution.
The content of astaxanthin in the triglyceride of the high-astaxanthin type antarctic krill oil is 823.55ppm, and the content of phospholipid residues is 142 ppm. In the high EPA/DHA type antarctic krill oil phospholipid solution, the content of phospholipid is 18.35%, the content of EPA and DHA is 63.62mg/g and 44.81mg/g respectively, and the loss rates of astaxanthin, phospholipid, EPA and DHA are 12.22%, 8.25%, 1.09% and 1.13% respectively.
And (3) drying and dehydrating the high EPA/DHA type antarctic krill oil phospholipid solution at the temperature of-20 ℃ and the low temperature of 10pa for 48 hours to obtain the high EPA/DHA type antarctic krill oil phospholipid powder (the water content is lower than 2%).
Example 10
Adding a hydration solution (specifically a 1.5% citric acid solution) with 4 times of phospholipid by mass into the Euphausia superba oil by adopting a water bath heating device, stirring at 60 ℃ and 70r/min for 30min, cooling to below 40 ℃ within 1h, standing and settling for 4h to obtain triglyceride at the upper layer and phospholipid solution at the lower layer, and separating to obtain the high-astaxanthin type Euphausia superba oil triglyceride and the high-EPA/DHA type Euphausia superba oil phospholipid solution.
The content of astaxanthin in the triglyceride of the high-astaxanthin type antarctic krill oil is 863.85ppm, and the residual content of phospholipid is 105 ppm. In the high EPA/DHA type antarctic krill oil phospholipid solution, the content of phospholipid is 19.36%, the content of EPA and DHA is 67.36mg/g and 47.48mg/g respectively, and the loss rates of astaxanthin, phospholipid, EPA and DHA are 7.92%, 3.2%, 0.74% and 0.71% respectively.
And (3) drying and dehydrating the high EPA/DHA type antarctic krill oil phospholipid solution at the temperature of 50 ℃ below zero and the low temperature of 10pa for 24 hours to obtain the high EPA/DHA type antarctic krill oil phospholipid powder (the water content is lower than 2%).
Example 11
Adding a hydration solution (specifically a 1.5% citric acid solution) with 4 times of phospholipid by mass into the Euphausia superba oil by adopting a water bath heating device, stirring at 60 ℃ and 100r/min for 30min, cooling to below 40 ℃ within 1h, standing and settling for 4h to obtain triglyceride at the upper layer and phospholipid solution at the lower layer, and separating to obtain the high-astaxanthin type Euphausia superba oil triglyceride and the high-EPA/DHA type Euphausia superba oil phospholipid solution.
The content of astaxanthin in the triglyceride of the high-astaxanthin type antarctic krill oil is 883.46ppm, and the residual content of phospholipid is 105 ppm. In the high EPA/DHA type antarctic krill oil phospholipid solution, the content of phospholipid is 19.50%, the content of EPA and DHA is 67.88mg/g and 47.78mg/g respectively, and the loss rates of astaxanthin, phospholipid, EPA and DHA are 5.83%, 2.5%, 0.69% and 0.80% respectively.
And (3) drying and dehydrating the high EPA/DHA type antarctic krill oil phospholipid solution at the temperature of 50 ℃ below zero and the low temperature of 5pa for 24 hours to obtain the high EPA/DHA type antarctic krill oil phospholipid powder (the water content is lower than 2%).
Table 1: examples reaction parameters and comparison of results
Referring to table 1, it can be seen from the comprehensive comparison of examples 1 to 5 that when the mass of the hydration solution is 3 to 5 times of the content of phospholipids in the antarctic krill oil, the hydration degumming effect is better, the separation of triglycerides from phospholipids is more sufficient, and the loss rates of the functional components astaxanthin, phospholipids, EPA and DHA are lower, wherein when the mass of the hydration solution is 4 times of the content of phospholipids in the antarctic krill oil, the hydration degumming effect is the best, and the loss rate of the functional components is the lowest.
The comprehensive comparison of examples 2 and 6 to 9 shows that the more the content of the citric acid electrolyte is, the better the content is, and the preferable range is 1.5 to 3%.
The stirring speed is preferably 50 to 100r/min, as can be seen by combining comparative examples 2, 10 and 11.
The optimal reaction conditions obtained by comprehensively comparing the data are as follows: the mass of the hydration solution is 4 times of the content of phospholipid in the antarctic krill oil, wherein the content of electrolyte citric acid is 1.5%, and the stirring speed is 50-100 r/min.
Control group 1
Adding citric acid powder with 4.5% of phospholipid of krill oil into Antarctic krill oil, acidifying at 60 deg.C for 15min, cooling to below 40 deg.C, adding deionized water with phospholipid content 3 times the mass and preheating to 70 deg.C, reacting for 30min, cooling, standing, settling for more than 4 hr, and separating to obtain triglyceride and phospholipid solution (water solution is deionized water)
In this comparative example, the points of difference from the examples are: the solid powder of citric acid is added firstly, deionized water is added, the acidification process and the hydration process are separated, and the temperature of the deionized water is higher, experiments prove that the reaction degumming separation effect is poor, only a small amount of triglyceride can be obtained, the lower phospholipid layer contains a large amount of triglyceride, an emulsification phenomenon occurs, the fluidity is poor, the separation is difficult, the loss rate of functional components is high, the content of astaxanthin in the obtained antarctic krill oil triglyceride is 641.92ppm, and the content of phospholipid in the antarctic krill oil phospholipid solution is 16.30%. The total content of EPA/DHA was 48.59mg/g and 30.43mg/g, and the loss rates of astaxanthin, phospholipids, EPA and DHA were 50%, 34.8%, 14.95% and 24.42%, respectively.
Control group 2
Adding deionized water with 3 times of phospholipid content of krill oil and preheated to 70 ℃ in mass into Antarctic krill oil, reacting for 30min, cooling to below 40 ℃, adding citric acid powder with 4.5% of phospholipid mass, acidifying at 60 ℃ for 15min, cooling, standing, settling for more than 4h, and separating.
In this comparative example, the points of difference from the examples are: the deionized water and the citric acid are added step by step, the temperature difference between the Antarctic krill oil and the deionized water is large, experimental results prove that the degumming separation effect of the comparative example is poor, only a few parts of triglyceride are separated out, the lower layer is completely emulsified, and degumming treatment cannot be carried out.
Control group 3
Preheating the antarctic krill oil and the hydration solution (specifically 1.5% citric acid solution) to 70 degrees respectively, then adding the hydration solution with the phospholipid mass content being 3 times of that of the antarctic krill oil into the antarctic krill oil, stirring for 30min at the temperature of 60 degrees and at the speed of 50r/min, cooling to below 40 ℃ within 1h, standing and settling for 4h to obtain triglyceride positioned at the upper layer and phospholipid solution positioned at the lower layer, and separating to obtain the high-astaxanthin type antarctic krill oil triglyceride and high-EPA/DHA type antarctic krill oil phospholipid solution.
The content of astaxanthin in the triglyceride of the euphausia superba oil with high astaxanthin content is 428.69ppm, and the residual content of phospholipid is 139 ppm. In the phospholipid solution of the antarctic krill oil with high EPA/DHA content, the phospholipid content is 22.48%, the EPA and DHA content is 69.85mg/g and 48.83mg/g respectively, and the loss rates of astaxanthin, phospholipid, EPA and DHA are 54.31%, 10.08%, 11.35% and 12.05% respectively.
In this comparative example, the points of difference from the examples are: the antarctic krill oil is heated and then added with the hydration solution with the same temperature, the hydration degumming process is the same as that in the prior art, and the experimental result proves that the loss rate of EPA, DHA and astaxanthin is higher.
Control group 4
Adding deionized water with the phospholipid mass content being 3 times of that of Antarctic krill oil, heating while stirring, stirring at 50r/min for 30min, cooling to 60 deg.C within 1h, cooling to below 40 deg.C, standing for settling for 4h, and separating.
In this comparative example, the points of difference from the examples are: electrolyte is not added into the hydration solution, and experimental results show that the comparative example has no degumming and separation effect, and the hydration solution and the shrimp sauce are completely emulsified and cannot be separated in a layering way.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (4)
1. A refining method of antarctic krill oil is characterized by comprising the following steps:
step S1: adding a hydration solution which is 4-5 times of the mass content of phospholipid in the Antarctic krill oil into the Antarctic krill oil, heating while stirring, stirring at 60 ℃ and 50r/min for 30min, cooling to below 40 ℃ within 1h, standing and settling for 4h to obtain Antarctic krill oil triglyceride and Antarctic krill oil phospholipid solution; wherein the hydration solution is an aqueous solution containing citric acid with the mass concentration of 1.5%;
step S2: and (4) concentrating and drying the euphausia superba oil phospholipid solution separated in the step (S1), and removing water to obtain the dehydrated euphausia superba oil phospholipid.
2. The refining method of antarctic krill oil according to claim 1, wherein in the step S2, the concentration and drying is performed by vacuum low-temperature freeze drying at-20 ℃ to-50 ℃ for 24h to 72h under 5pa to 10 pa.
3. The refining method for antarctic krill oil according to claim 1, wherein the quality of the hydration solution is 4 times the content of phospholipids in the antarctic krill oil.
4. The refining method of antarctic krill oil according to claim 1, wherein in step S1, heating is performed by using a water bath.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4162260A (en) * | 1976-09-10 | 1979-07-24 | Lever Brothers Company | Oil purification by adding hydratable phosphatides |
| EP0269277A2 (en) * | 1986-11-13 | 1988-06-01 | The Cambrian Engineering Group Limited | Process for degumming triglyceride oils |
| CN1096686A (en) * | 1993-06-24 | 1994-12-28 | 北京召福新技术发展公司 | A kind of production method of high nutrient phosphatide oral liquid |
| US6147237A (en) * | 1995-06-12 | 2000-11-14 | Lipton, Inc. | Mild refining of triglyceride oil |
| CN101445764A (en) * | 2007-10-26 | 2009-06-03 | 油籽生物精炼公司 | Emulsification-free degumming of oil |
| WO2011137160A2 (en) * | 2010-04-30 | 2011-11-03 | U.S. Nutraceuticals, Llc D/B/A Valensa International | Composition and method to improve blood lipid profiles and optionally reduce low density lipoprotein (ldl) per-oxidation in humans |
| CN102813209A (en) * | 2012-08-09 | 2012-12-12 | 浙江大学 | Health-care food containing egg yolk lecithin, and preparation method thereof |
| CN102919512A (en) * | 2012-09-26 | 2013-02-13 | 内蒙古金达威药业有限公司 | DHA (docosahexaenoic acid)-rich microalgae powder and preparation method thereof |
| CN103305335A (en) * | 2013-06-27 | 2013-09-18 | 日照海大博远海洋生物科技有限公司 | Low-temperature countercurrent extraction method of euphausia superba sauce |
| CN108179053A (en) * | 2018-01-26 | 2018-06-19 | 日照职业技术学院 | A kind of preparation method of high quality Antarctic krill oil |
-
2018
- 2018-10-22 CN CN201811231008.3A patent/CN109439430B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4162260A (en) * | 1976-09-10 | 1979-07-24 | Lever Brothers Company | Oil purification by adding hydratable phosphatides |
| EP0269277A2 (en) * | 1986-11-13 | 1988-06-01 | The Cambrian Engineering Group Limited | Process for degumming triglyceride oils |
| CN1096686A (en) * | 1993-06-24 | 1994-12-28 | 北京召福新技术发展公司 | A kind of production method of high nutrient phosphatide oral liquid |
| US6147237A (en) * | 1995-06-12 | 2000-11-14 | Lipton, Inc. | Mild refining of triglyceride oil |
| CN101445764A (en) * | 2007-10-26 | 2009-06-03 | 油籽生物精炼公司 | Emulsification-free degumming of oil |
| WO2011137160A2 (en) * | 2010-04-30 | 2011-11-03 | U.S. Nutraceuticals, Llc D/B/A Valensa International | Composition and method to improve blood lipid profiles and optionally reduce low density lipoprotein (ldl) per-oxidation in humans |
| CN102813209A (en) * | 2012-08-09 | 2012-12-12 | 浙江大学 | Health-care food containing egg yolk lecithin, and preparation method thereof |
| CN102919512A (en) * | 2012-09-26 | 2013-02-13 | 内蒙古金达威药业有限公司 | DHA (docosahexaenoic acid)-rich microalgae powder and preparation method thereof |
| CN103305335A (en) * | 2013-06-27 | 2013-09-18 | 日照海大博远海洋生物科技有限公司 | Low-temperature countercurrent extraction method of euphausia superba sauce |
| CN108179053A (en) * | 2018-01-26 | 2018-06-19 | 日照职业技术学院 | A kind of preparation method of high quality Antarctic krill oil |
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