CN108659947B - Method for preparing antarctic krill oil and protein powder from antarctic krill, and antarctic krill oil and protein powder - Google Patents

Method for preparing antarctic krill oil and protein powder from antarctic krill, and antarctic krill oil and protein powder Download PDF

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CN108659947B
CN108659947B CN201810603425.XA CN201810603425A CN108659947B CN 108659947 B CN108659947 B CN 108659947B CN 201810603425 A CN201810603425 A CN 201810603425A CN 108659947 B CN108659947 B CN 108659947B
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antarctic krill
shrimp
mixed
krill oil
protein powder
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CN108659947A (en
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柳玉平
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Shandong Lanao Biotech Co ltd
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Shandong Lanao Biotech Co ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23JPROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J1/00Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
    • A23J1/04Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from fish or other sea animals
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B3/00Refining fats or fatty oils
    • C11B3/001Refining fats or fatty oils by a combination of two or more of the means hereafter
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

Abstract

The invention provides a method for preparing antarctic krill oil and protein powder by using antarctic krill, which comprises the following steps: mixing and soaking the cooked euphausia superba meat paste with ethyl acetate, and centrifuging to obtain a mixed solution and a shrimp meat paste; enabling the mixed solution to pass through an ultrafiltration membrane with the aperture of 200-300 daltons to obtain mixed ester liquid, drying the centrifuged shrimp meat paste and grinding to obtain shrimp powder; mixing the shrimp meal with a mixed oil engine solvent obtained by mixing petroleum ether and ethanol, adding the mixture into a homogenizer for homogenization to obtain a homogenized mixed shrimp liquid, and filtering the homogenized mixed shrimp liquid to obtain a filtrate and shrimp meat paste; mixing the filtrate with the mixed ester solution, and distilling twice to obtain antarctic krill oil; and drying the shrimp paste to obtain the protein powder. The method has the advantages that the extraction rate of the Antarctic krill oil is high, the total arsenic content of the prepared Antarctic krill oil is low, and the shrimp paste is prepared into protein powder, so that the resource waste is avoided. The invention also provides the antarctic krill oil and the protein powder prepared by the method.

Description

Method for preparing antarctic krill oil and protein powder from antarctic krill, and antarctic krill oil and protein powder
Technical Field
The invention relates to the technical field of health product preparation, and particularly relates to a method for preparing antarctic krill oil and protein powder from antarctic krill, the antarctic krill oil and the protein powder.
Background
Antarctic krill (Euphausia superba) belongs to the small crustacean class of the Krill order of the Crustacea. The antarctic krill is also called euphausia superba or euphausia superba, has the body length of 40 mm and 60 mm, is relatively transparent, has reddish brown spots and is favorable for living. The euphausia superba biological deposits are key species of an antarctic ecosystem, the euphausia superba biological deposits are abundant and remarkable, the estimated biological deposits of the euphausia superba are conservative estimated to be 4-10 hundred million tons, the annual sustainable capture amount is more than 0.7 hundred million tons, and the total annual capture amount is equivalent to the sum of annual capture amounts of primary and other aquatic products all over the world at present.
The antarctic krill not only has amazing storage amount, but also has extremely high nutritional value. The krill protein is the highest protein-containing organism found by people today, and the protein content and the fat content in the meat of the Antarctic krill are high, so that the krill is an ideal food for human beings, and is similar to a future protein resource warehouse of the human beings.
The Antarctic krill oil is oil extracted from Antarctic krill, and contains unsaturated fatty acids eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA), and is rich in vitamin E, vitamin A, astaxanthin, phospholipids, flavonoids, etc. Antarctic krill oil has been receiving increasing attention and interest for its significant effects in reducing the incidence of cardiovascular diseases, alleviating allergic and inflammatory conditions, assisting brain development and maintaining normal vision. It is known that antarctic krill oil contains non-toxic organic arsenic, but long-term intake of organic arsenic may not benefit human health. In addition, the extraction rate of the antarctic krill oil in the existing extraction method of the antarctic krill oil is still to be improved.
In view of this, the present application is specifically made.
Disclosure of Invention
The invention provides a method for preparing antarctic krill oil and protein powder by using antarctic krill, and aims to improve the extraction rate of the antarctic krill oil and reduce the total arsenic content in the obtained antarctic krill oil.
The invention also provides euphausia superba oil which is high in purity and low in total arsenic content.
The invention also provides protein powder which has higher nutritional value.
The invention is realized by the following steps:
a method for preparing antarctic krill oil and protein powder by using antarctic krill comprises the following steps: mixing and soaking the cooked minced meat of the Antarctic krill with ethyl acetate for 5-70 min, and centrifuging to obtain the minced meat of the Antarctic krill and a mixed solution after liquid removal; passing the mixed solution through an ultrafiltration membrane with the aperture of 200-300 daltons to obtain a intercepted mixed ester solution; drying and grinding the shrimp meat paste after liquid removal to obtain shrimp powder; adding the shrimp powder and the mixed organic solvent into a homogenizer, homogenizing for 10-60 min under the pressure of 10.8-20.6 MPa to obtain a homogenized mixed shrimp liquid, filtering the homogenized mixed shrimp liquid to obtain a filtrate and shrimp paste, wherein the dosage ratio of the shrimp powder to the mixed organic solvent is 1g: 1-7 mL of mixed organic solvent, wherein the mixed organic solvent comprises petroleum ether and ethanol solution with the mass concentration of more than 95% in a volume ratio of 1.5-3: 1; mixing the filtrate and the mixed ester solution, carrying out primary purification at the temperature of 30-70 ℃, the pressure of 0.01-0.1 MPa and the extraction time of 60-180 min to obtain a concentrated solution and a steam condensate, and filtering the concentrated solution through 400-500-mesh filter cloth to obtain first antarctic krill oil; carrying out secondary purification on the steam condensate under the conditions of 55-85 ℃, 0.01-0.08 MPa of pressure and 30-120 min of extraction time to obtain second Antarctic krill oil, and mixing the first Antarctic krill oil and the second Antarctic krill oil to obtain Antarctic krill oil; and drying the shrimp paste to obtain the protein powder.
Antarctic krill oil is prepared by the method for preparing the Antarctic krill oil and protein powder by using the Antarctic krill.
The protein powder is prepared by adopting the method for preparing the antarctic krill oil and the protein powder by using the antarctic krill.
The invention has the beneficial effects that: according to the method for preparing the antarctic krill oil and the protein powder by using the antarctic krill, which is designed, in the preparation process, the ethyl acetate is mixed with the minced meat of the antarctic krill, and the mixture is soaked for a proper time and then filtered by the ultrafiltration membrane to remove organic arsenic and other small molecular impurities, so that the total arsenic content in the prepared antarctic krill oil is reduced; the shrimp meal and the mixed oil machine solvent of ethanol and petroleum ether with a reasonable proportion are uniformly mixed in the homogenizer, so that the krill oil contained in the shrimp meal is fully contacted with the organic solvent and enters the organic solvent no matter the polarity is strong or weak, and the extraction rate of the antarctic krill is effectively improved; the water in the euphausia superba meat is removed in a centrifugal mode in the liquid removing process, so that the subsequent extraction is facilitated, and compared with the existing squeezing and dewatering mode, the liquid removing process is not easy to cause the oil of the euphausia superba in the euphausia superba to be lost; and the subsequent two times of evaporation and concentration after the liquid removal are finished ensure that the ethanol, the petroleum ether and partial water are completely evaporated under proper evaporation conditions, so that the purity of the Antarctic krill oil is ensured, meanwhile, the shrimp paste produced in the extraction is dried to obtain the protein powder, so that the raw material waste is avoided, and the protein powder is defatted protein powder and has higher nutritional value.
The antarctic krill oil obtained by the design has high purity and low total arsenic content.
According to the protein powder obtained by the design, the raw material is shrimp paste left in the antarctic krill oil production process, and the protein powder has high nutritional value.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The following provides a specific description of a method for preparing antarctic krill oil and protein powder by using antarctic krill.
A method for preparing antarctic krill oil and protein powder by using antarctic krill comprises the following steps:
s1, mixing and soaking the cooked minced euphausia superba meat with ethyl acetate for 5-70 min, and centrifuging to obtain the minced euphausia superba meat after liquid removal.
Fresh antarctic krill can be selected, and the antarctic krill which is frozen and then thawed by microwave can also be selected as the raw material. And then placing the selected antarctic krill in a cooking device with the temperature of 70-100 ℃, and heating and cooking for 5-20 min. The heating temperature of the euphausia superba is not too high, partial nutrient substances in the euphausia superba are lost due to the too high temperature, the temperature is not too low, the sterilization effect is difficult to achieve due to the low temperature, the cooking efficiency is reduced, and when the heating temperature is within the range, the heating time is preferably 5-20min in order to ensure the cooking efficiency and complete sterilization of the shrimp meat.
After being cooked, the euphausia superba is subjected to shelling treatment to obtain shrimp meat and a shrimp shell, and the shrimp shell can be recycled for preparing protein powder. Mincing the shrimp meat into the minced antarctic krill meat in a meat mincer. And mixing the obtained minced meat of the antarctic krill with ethyl acetate, placing the mixture into a stirring device, and soaking for 5-70 min under the stirring condition to dissolve out part of phospholipid and arsenic betaine in the antarctic krill meat. Then centrifuging and removing liquid to obtain the shrimp meat paste and mixed ester liquid. Preferably, before centrifugation, soaking the Antarctic krill meat paste with ethyl acetate, filtering, wherein the filtrate is an ethyl acetate mixed solution, the ethyl acetate mixed solution is a mixture of ethyl acetate, phospholipid, organic arsenic and the like, the filter residue is the Antarctic krill meat paste, washing the Antarctic krill meat paste in clear water to remove the residual ethyl acetate and the water-soluble organic arsenic in the krill meat paste, centrifuging the mixed solution of the Antarctic krill meat paste and the clear water in a centrifuge to obtain the deliquored krill meat paste and a centrifugate, and mixing the centrifugate and the ethyl acetate mixed solution to obtain a mixed solution.
Preferably, in order to enable the ethyl acetate to sufficiently react with the minced antarctic krill meat to achieve a better dissolution effect of the organic arsenic without excessively low extraction efficiency, the using ratio of the minced antarctic krill meat to the ethyl acetate is 1g: 5-17 ml.
Further preferably, during washing, the mass ratio of the clear water to the filter residue of the minced meat of antarctic krill is 2.5-3.5: 1, so that the washing effect is better.
And S2, passing the mixed solution through an ultrafiltration membrane with the aperture of 200-300 daltons to obtain the intercepted mixed ester solution.
Filtering the mixed solution by using an ultrafiltration membrane with the aperture of 200-300 daltons to remove organic arsenic with small molecular weight, partial heavy metal ions and ethyl acetate, and intercepting phospholipid which is mutually soluble with the ethyl acetate and other macromolecular esters with strong polarity on the ultrafiltration membrane to obtain mixed ester solution.
And S3, drying the shrimp meat paste after liquid removal and grinding to obtain shrimp powder.
And (4) drying the shrimp paste subjected to liquid removal and prepared in the S1 for 5-60 min at the temperature of 60-100 ℃ to obtain a brownish red powder. To reduce the moisture in the shrimp paste and increase the extraction rate. The temperature in the drying process is not suitable to be too high or too low, the nutrient components in the shrimp meat paste can be damaged due to too high temperature, and the drying speed can be reduced due to too low temperature. The moisture removal rate is higher with longer drying time, but too long drying time can also cause the nutrient components in the shrimp paste to be destroyed. And when the drying temperature is 60-100 ℃, the drying time cannot be less than 5min, and the drying time is less than 5min, so that the moisture content of the prepared shrimp meal is still high due to insufficient drying of the shrimp meat paste.
S4, adding the shrimp meal and the mixed organic solvent into a homogenizer, homogenizing for 10-60 min under the pressure of 10.8-20.6 MPa to obtain a homogenized mixed shrimp liquid, filtering the homogenized mixed shrimp liquid to obtain a filtrate and shrimp paste, wherein the dosage ratio of the shrimp meal to the mixed organic solvent is 1g: 1-7 mL, wherein the mixed organic solvent comprises petroleum ether and ethanol solution with the mass concentration of more than 95% in a volume ratio of 1.5-3: 1.
Specifically, firstly, petroleum ether and ethanol solution with the mass concentration of more than 95% are mixed according to the volume ratio of 1.5-3: 1 to obtain mixed organic solvent, and the shrimp meal obtained in the step S3 is added into the mixed organic solvent under the condition of adding the shrimp meal while stirring, so that the phenomenon that all the shrimp meal is added into the ethanol solution to form lumps is prevented. The dosage ratio of the added shrimp meal to the ethanol solution is 1g: 1-7 mL.
After putting the shrimp meal into the ethanol solution, adding the mixed solution of the shrimp meal and the ethanol solution into a homogenizer, and homogenizing at the normal temperature of 20-40 ℃ and under the pressure of 10.8-20.6 MPa for 10-60 min to obtain the homogenized and mixed shrimp solution. Under the homogeneous condition, the shrimp meal can be uniformly distributed in the mixed organic solvent, so that the mixed organic solvent is fully contacted with the shrimp oil contained in the shrimp meal, and the extraction rate of the krill oil is improved. The petroleum ether belongs to an organic solvent with weaker polarity, the ethanol belongs to an organic solvent with stronger polarity, the oil in the krill can be extracted by matching the petroleum ether with the ethanol, so that the oil with stronger polarity and the oil with weaker polarity in the krill can be fully extracted, and the extraction effect is best when the ratio of the petroleum ether to the ethanol is 1.5-3: 1.
And filtering the obtained homogenized and mixed shrimp liquid after homogenization to obtain filtrate and shrimp paste. Preferably, the shrimp paste is mixed with the mixed organic solvent (the mixed organic solvent may be a filtrate obtained by primary filtration or an unused mixed organic solvent), and the mixture is put into the homogenizer again, homogenized for 10-60 min under the same homogenization condition, filtered, and repeatedly extracted for at least 2 times, and the obtained multiple filtrates are mixed with the primary filtrate to obtain a total filtrate, and then the total filtrate is subjected to the next operation.
S5, mixing the filtrate and the mixed ester solution, carrying out primary purification at the temperature of 30-70 ℃, the pressure of 0.01-0.1 MPa and the extraction time of 60-180 min to obtain a concentrated solution and a steam condensate, and filtering the concentrated solution through 400-500-mesh filter cloth to obtain the first antarctic krill oil.
Specifically, the filtrate or the total filtrate obtained in the step S4 is mixed with the mixed ester solution, primary purification is carried out by adopting a distillation mode under the conditions that the temperature is 30-70 ℃, the pressure is 0.01-0.1 MPa and the extraction time is 60-180 min, so that the ethanol and the water in the filtrate are completely evaporated, and a concentration tank capable of recycling steam is adopted to condense the steam to obtain a concentrated solution and a steam condensate. Filtering the concentrated solution through 400-500-mesh filter cloth to obtain first antarctic krill oil so as to remove shrimp meat possibly remaining.
S5, carrying out secondary purification on the steam condensate under the conditions of 55-85 ℃, 0.01-0.08 MPa of pressure and 30-120 min of extraction time to obtain second Antarctic krill oil, and mixing the first Antarctic krill oil and the second Antarctic krill mixed oil to obtain the Antarctic krill oil.
Specifically, the steam condensate obtained from S4 is subjected to secondary purification by distillation under the conditions of 55-85 ℃, 0.01-0.08 MPa of pressure and 30-120 min of extraction time, so as to extract part of Antarctic krill oil carried away by ethanol steam. And (3) obtaining second antarctic krill oil after secondary purification, and mixing the first antarctic krill oil and the second antarctic krill mixed oil to obtain the antarctic krill oil provided by the invention.
S6, drying the shrimp paste to obtain protein powder.
And (3) drying the shrimp paste obtained after one or more extractions in the step S3 until the moisture content is lower than 8%, so as to obtain the protein powder provided by the invention.
The method for preparing the antarctic krill oil and the protein powder by using the antarctic krill, the antarctic krill oil and the protein powder provided by the invention are specifically described in the following with reference to specific examples.
Example 1
The embodiment provides a method for preparing antarctic krill oil and protein powder by using antarctic krill and the antarctic krill oil and protein powder prepared by the method.
The method for preparing the antarctic krill oil and the protein powder by using the antarctic krill comprises the following steps: placing the antarctic krill unfrozen by microwave in a cooking device, heating and cooking at 70 ℃ for 20min to obtain cooked antarctic krill, then placing the cooked antarctic krill in a huller to hull to obtain the krill meat and the krill shells, recycling the krill shells, placing the krill meat in a meat grinder to stir into antarctic krill meat paste, mixing the obtained antarctic krill meat paste with ethyl acetate, and placing the mixture in a stirring device, wherein the use ratio of the antarctic krill meat paste to the ethyl acetate is 1g: the volume of the mixture is 8ml, soaking for 5min under the stirring condition, then filtering to obtain mixed liquid of the Antarctic krill meat emulsion filter residue and ethyl acetate, cleaning the Antarctic krill meat emulsion filter residue by using clear water, wherein the mass ratio of the clear water to the filter residue is 2.5:1, placing the mixed liquid of the Antarctic krill meat emulsion and the clear water in a centrifuge for centrifugation, obtaining bottom Antarctic krill meat emulsion and centrifugate after centrifugation, and mixing the centrifugate and the mixed liquid of the ethyl acetate to obtain the mixed liquid.
Filtering the mixed solution by an ultrafiltration membrane with the aperture of 200 daltons, and recovering the mixed ester solution which does not pass through the membrane pores.
Drying the minced meat of the Antarctic krill obtained after centrifugation for 60min at the temperature of 60 ℃ to obtain shrimp meal, putting the shrimp meal into a mixed organic solvent obtained by mixing petroleum ether with the volume ratio of 1.5:1 and ethanol with the mass percentage content of more than 95%, wherein the dosage ratio of the shrimp meal to the mixed organic solvent is 1g: 1mL, adding the shrimp powder into the mixed organic solvent completely, adding the mixed solution of the shrimp powder and the mixed organic solvent into a homogenizer, and homogenizing for 60min at 40 ℃ under the pressure of 10.8MPa to obtain the homogenized and mixed shrimp liquid. And then filtering the homogenized and mixed shrimp liquid to obtain filtrate and shrimp paste, mixing the shrimp paste with ethanol repeatedly according to the conditions for homogenizing for 2 times, and drying the finally obtained shrimp paste to obtain the protein powder. Mixing the obtained multistage filtrates, mixing the mixed filtrate with mixed ester solution, desolventizing and dehydrating at 30 ℃ and under the pressure of 0.1MPa, extracting for 60min to obtain concentrated solution and steam condensate, and filtering the concentrated solution through 400-mesh filter cloth to obtain the first antarctic krill oil. And (3) carrying out secondary purification on the steam condensate at the temperature of 55 ℃ and under the pressure of 0.08MPa, extracting for 30min to obtain second Antarctic krill oil, and mixing the second Antarctic krill oil with the first Antarctic krill oil to obtain the Antarctic krill oil provided by the invention.
Example 2
The embodiment provides a method for preparing antarctic krill oil and protein powder by using antarctic krill and the antarctic krill oil and protein powder prepared by the method.
The method for preparing the antarctic krill oil and the protein powder by using the antarctic krill comprises the following steps: placing the antarctic krill thawed by microwave in a cooking device, heating and cooking at 100 deg.C for 5min to obtain cooked antarctic krill, then placing the cooked antarctic krill in a huller to hull to obtain the krill meat and the krill shells, recycling the krill shells, placing the krill meat in a meat grinder to stir into antarctic krill meat paste, mixing the obtained antarctic krill meat paste with ethyl acetate, and placing the mixture in a stirring device, wherein the use ratio of the antarctic krill meat paste to the ethyl acetate is 1g: the volume of the mixture is 17ml, soaking for 70min under the stirring condition, then filtering to obtain mixed liquid of the Antarctic krill meat emulsion filter residue and ethyl acetate, cleaning the Antarctic krill meat emulsion filter residue by using clear water, wherein the mass ratio of the clear water to the filter residue is 3.5:1, placing the mixed liquid of the Antarctic krill meat emulsion and the clear water in a centrifuge for centrifugation, obtaining bottom Antarctic krill meat emulsion and centrifugate after centrifugation, and mixing the centrifugate and the mixed liquid of the ethyl acetate to obtain the mixed liquid.
Filtering the mixed solution by an ultrafiltration membrane with the aperture of 300 daltons, and recovering the mixed ester solution which does not pass through the membrane pores.
Drying the minced meat of the Antarctic krill obtained after centrifugation for 5min at the temperature of 100 ℃ to obtain shrimp meal, putting the shrimp meal into a mixed organic solvent obtained by mixing petroleum ether with the volume ratio of 3:1 and ethanol with the mass percentage content of more than 95%, wherein the dosage ratio of the shrimp meal to the mixed organic solvent is 1g: 7mL, adding the shrimp powder into the mixed organic solvent completely, adding the mixed solution of the shrimp powder and the mixed organic solvent into a homogenizer, and homogenizing at 20 ℃ and 20.6MPa for 10min to obtain a homogenized and mixed shrimp solution. And then filtering the homogenized and mixed shrimp liquid to obtain filtrate and shrimp paste, mixing the shrimp paste with ethanol repeatedly according to the conditions for homogenizing for 1 time, and drying the finally obtained shrimp paste to obtain the protein powder. Mixing the obtained multistage filtrates, mixing the mixed filtrate with mixed ester solution, desolventizing and dehydrating at 70 ℃ and under the pressure of 0.01MPa, extracting for 180min to obtain concentrated solution and steam condensate, and filtering the concentrated solution through 500-mesh filter cloth to obtain the first antarctic krill oil. And (3) carrying out secondary purification on the steam condensate at the temperature of 85 ℃ and under the pressure of 0.01MPa, extracting for 120min to obtain second Antarctic krill oil, and mixing the second Antarctic krill oil with the first Antarctic krill oil to obtain the Antarctic krill oil provided by the invention.
Example 3
The embodiment provides a method for preparing antarctic krill oil and protein powder by using antarctic krill and the antarctic krill oil and protein powder prepared by the method.
The method for preparing the antarctic krill oil and the protein powder by using the antarctic krill comprises the following steps: placing the antarctic krill thawed by microwave in a cooking device, heating and cooking at 80 deg.C for 8min to obtain cooked antarctic krill, then placing the cooked antarctic krill in a huller to hull to obtain the krill meat and the krill shells, recycling the krill shells, placing the krill meat in a meat grinder to stir into antarctic krill meat paste, mixing the obtained antarctic krill meat paste with ethyl acetate, and placing the mixture in a stirring device, wherein the use ratio of the antarctic krill meat paste to the ethyl acetate is 1g:5ml of the mixture is added into the reaction kettle, soaking for 10min under the stirring condition, then filtering to obtain mixed liquid of the Antarctic krill meat emulsion filter residue and ethyl acetate, cleaning the Antarctic krill meat emulsion filter residue by using clear water, wherein the mass ratio of the clear water to the filter residue is 3:1, placing the mixed liquid of the Antarctic krill meat emulsion and the clear water in a centrifuge for centrifugation, obtaining bottom Antarctic krill meat emulsion and centrifugate after centrifugation, and mixing the centrifugate and the mixed liquid of the ethyl acetate to obtain the mixed liquid.
Filtering the mixed solution by an ultrafiltration membrane with the aperture of 250 daltons, and recovering the mixed ester solution which does not pass through the membrane pores.
Drying the minced meat of the Antarctic krill obtained after centrifugation for 10min at the temperature of 70 ℃ to obtain shrimp meal, putting the shrimp meal into a mixed organic solvent obtained by mixing petroleum ether with the volume ratio of 2:1 and ethanol with the mass percentage content of more than 95%, wherein the dosage ratio of the shrimp meal to the mixed organic solvent is 1g: 2mL, adding the shrimp powder into the mixed organic solvent completely, adding the mixed solution of the shrimp powder and the mixed organic solvent into a homogenizer, and homogenizing for 20min at the temperature of 30 ℃ and under the pressure of 12.8MPa to obtain a homogenized and mixed shrimp solution. And then filtering the homogenized and mixed shrimp liquid to obtain filtrate and shrimp paste, mixing the shrimp paste with ethanol repeatedly according to the conditions for 3 times, and drying the finally obtained shrimp paste to obtain the protein powder. Mixing the obtained multistage filtrates, mixing the mixed filtrate with mixed ester solution, desolventizing and dehydrating at 30 ℃ and under the pressure of 0.1MPa, extracting for 60min to obtain concentrated solution and steam condensate, and filtering the concentrated solution through 450-mesh filter cloth to obtain the first antarctic krill oil. And (3) carrying out secondary purification on the steam condensate at the temperature of 65 ℃ and under the pressure of 0.03MPa, extracting for 50min to obtain second Antarctic krill oil, and mixing the second Antarctic krill oil with the first Antarctic krill oil to obtain the Antarctic krill oil provided by the invention.
Example 4
The embodiment provides a method for preparing antarctic krill oil and protein powder by using antarctic krill and the antarctic krill oil and protein powder prepared by the method.
The method for preparing the antarctic krill oil and the protein powder by using the antarctic krill comprises the following steps: placing the antarctic krill thawed by microwave in a cooking device, heating and cooking at 90 deg.C for 12min to obtain cooked antarctic krill, then placing the cooked antarctic krill in a huller to hull to obtain the krill meat and the krill shells, recycling the krill shells, placing the krill meat in a meat grinder to stir into antarctic krill meat paste, mixing the obtained antarctic krill meat paste with ethyl acetate, and placing the mixture in a stirring device, wherein the use ratio of the antarctic krill meat paste to the ethyl acetate is 1g:10ml of the mixture is added into the reaction kettle, soaking for 8min under the stirring condition, then filtering to obtain mixed liquid of the Antarctic krill meat emulsion filter residue and ethyl acetate, cleaning the Antarctic krill meat emulsion filter residue by using clear water, wherein the mass ratio of the clear water to the filter residue is 2.8:1, placing the mixed liquid of the Antarctic krill meat emulsion and the clear water in a centrifuge for centrifugation after cleaning, obtaining bottom Antarctic krill meat emulsion and centrifugate, and mixing the centrifugate and the mixed liquid of the ethyl acetate to obtain the mixed liquid.
Filtering the mixed solution by an ultrafiltration membrane with the aperture of 200 daltons, and recovering the mixed ester solution which does not pass through the membrane pores.
Drying the minced meat of the Antarctic krill obtained after centrifugation for 30min at the temperature of 80 ℃ to obtain shrimp meal, putting the shrimp meal into a mixed organic solvent obtained by mixing petroleum ether with the volume ratio of 1.8:1 and ethanol with the mass percentage content of more than 95%, wherein the dosage ratio of the shrimp meal to the mixed organic solvent is 1g: 3mL, adding the shrimp powder into the mixed organic solvent completely, adding the mixed solution of the shrimp powder and the mixed organic solvent into a homogenizer, and homogenizing at 25 ℃ under the pressure of 15MPa for 30min to obtain a homogenized and mixed shrimp liquid. And then filtering the homogenized and mixed shrimp liquid to obtain filtrate and shrimp paste, mixing the obtained filtrate with the mixed ester liquid, desolventizing and dehydrating at the temperature of 50 ℃ and under the pressure of 0.03MPa, extracting for 90min to obtain concentrated solution and steam condensate, and filtering the concentrated solution through 400-mesh filter cloth to obtain the first antarctic krill oil. And (3) carrying out secondary purification on the steam condensate at the temperature of 75 ℃ and under the pressure of 0.03MPa, extracting for 60min to obtain second Antarctic krill oil, and mixing the second Antarctic krill oil with the first Antarctic krill oil to obtain the Antarctic krill oil provided by the invention.
Example 5
The embodiment provides a method for preparing antarctic krill oil and protein powder by using antarctic krill and the antarctic krill oil and protein powder prepared by the method.
The method for preparing the antarctic krill oil and the protein powder by using the antarctic krill comprises the following steps: placing the Antarctic krill thawed by microwaves in a cooking device, heating and cooking for 18min at the temperature of 95 ℃ to obtain cooked Antarctic krill, then placing the cooked Antarctic krill in a huller to hull, obtaining krill meat and a krill shell, recycling the krill shell, placing the krill in a meat grinder to grind into Antarctic krill meat paste, mixing the obtained Antarctic krill meat paste with ethyl acetate, placing the mixture in a stirring device, soaking the Antarctic krill meat paste and the ethyl acetate for 60min under the stirring condition, filtering to obtain a mixed solution of Antarctic krill meat paste filter residue and ethyl acetate, recycling ethyl acetate filtrate, cleaning the Antarctic krill meat paste filter residue with clear water, wherein the mass ratio of the clear water to the filter residue is 3.2:1, placing the mixed solution of the Antarctic krill meat paste and the clear water in a centrifugal machine, centrifuging, and obtaining bottom krill paste and Antarctic liquid after centrifuging, and mixing the centrifugate and the mixed solution of ethyl acetate to obtain a mixed solution.
Filtering the mixed solution by an ultrafiltration membrane with the aperture of 200 daltons, and recovering the mixed ester solution which does not pass through the membrane pores.
Drying the minced meat of the Antarctic krill obtained after centrifugation for 40min at the temperature of 65 ℃ to obtain shrimp meal, putting the shrimp meal into a mixed organic solvent obtained by mixing petroleum ether with the volume ratio of 2.5:1 and ethanol with the mass percentage content of more than 95%, wherein the dosage ratio of the shrimp meal to the mixed organic solvent is 1g: and 6mL, completely adding the shrimp powder into the mixed organic solvent, adding the mixed solution of the shrimp powder and the mixed organic solvent into a homogenizer, and homogenizing at 40 ℃ under the pressure of 19MPa for 45min to obtain the homogenized and mixed shrimp liquid. And then filtering the homogenized and mixed shrimp solution to obtain filtrate and shrimp meat paste, mixing the filtrate and the mixed ester solution, desolventizing and dehydrating at the temperature of 65 ℃ and under the pressure of 0.06MPa, extracting for 120min to obtain concentrated solution and steam condensate, and filtering the concentrated solution through 500-mesh filter cloth to obtain first antarctic krill oil. And (3) carrying out secondary purification on the steam condensate at the temperature of 80 ℃ and under the pressure of 0.06MPa, extracting for 30min to obtain second Antarctic krill oil, and mixing the second Antarctic krill oil with the first Antarctic krill oil to obtain the Antarctic krill oil provided by the invention.
Example 6
The embodiment provides a method for preparing antarctic krill oil and protein powder by using antarctic krill and the antarctic krill oil and protein powder prepared by the method.
The method for preparing the antarctic krill oil and the protein powder by using the antarctic krill comprises the following steps: placing the antarctic krill thawed by microwave in a cooking device, heating and cooking at 85 deg.C for 9min to obtain cooked antarctic krill, then placing the cooked antarctic krill in a huller to hull to obtain the krill meat and the krill shells, recycling the krill shells, placing the krill meat in a meat grinder to stir into antarctic krill meat paste, mixing the obtained antarctic krill meat paste with ethyl acetate, and placing the mixture in a stirring device, wherein the use ratio of the antarctic krill meat paste to the ethyl acetate is 1g: the volume of the mixture is 16ml, soaking for 40min under the stirring condition, then filtering to obtain mixed liquid of the Antarctic krill meat emulsion filter residue and ethyl acetate, cleaning the Antarctic krill meat emulsion filter residue by using clear water, wherein the mass ratio of the clear water to the filter residue is 3.1:1, placing the mixed liquid of the Antarctic krill meat emulsion and the clear water in a centrifuge for centrifugation, obtaining bottom Antarctic krill meat emulsion and centrifugate after centrifugation, and mixing the centrifugate and the mixed liquid of the ethyl acetate to obtain the mixed liquid.
Filtering the mixed solution by an ultrafiltration membrane with the aperture of 200 daltons, and recovering the mixed ester solution which does not pass through the membrane pores.
Drying the minced meat of the Antarctic krill obtained after centrifugation for 50min at the temperature of 85 ℃ to obtain shrimp meal, putting the shrimp meal into a mixed organic solvent obtained by mixing petroleum ether with the volume ratio of 2.8:1 and ethanol with the mass percentage content of more than 95%, wherein the dosage ratio of the shrimp meal to the mixed organic solvent is 1g: and 5mL, completely adding the shrimp powder into the mixed organic solvent, adding the mixed solution of the shrimp powder and the mixed organic solvent into a homogenizer, and homogenizing at 35 ℃ under the pressure of 16MPa for 35min to obtain a homogenized and mixed shrimp liquid. And then filtering the homogenized and mixed shrimp liquid to obtain filtrate and shrimp paste, mixing the filtrate and the mixed ester liquid, desolventizing and dehydrating at the temperature of 45 ℃ and under the pressure of 0.05MPa, extracting for 150min to obtain concentrated liquid and steam condensate, and filtering the concentrated liquid through 400-mesh filter cloth to obtain first antarctic krill oil. And (3) carrying out secondary purification on the steam condensate at 70 ℃ and under the pressure of 0.04MPa, extracting for 100min to obtain second Antarctic krill oil, and mixing the second Antarctic krill oil with the first Antarctic krill oil to obtain the Antarctic krill oil provided by the invention.
Example 7
The embodiment provides a method for preparing antarctic krill oil and protein powder by using antarctic krill and the antarctic krill oil and protein powder prepared by the method.
The method for preparing the antarctic krill oil and the protein powder by using the antarctic krill comprises the following steps: placing the antarctic krill thawed by microwave in a cooking device, heating and cooking at 72 deg.C for 15min to obtain cooked antarctic krill, then placing the cooked antarctic krill in a huller to hull to obtain the krill meat and the krill shells, recycling the krill shells, placing the krill meat in a meat grinder to stir into antarctic krill meat paste, mixing the obtained antarctic krill meat paste with ethyl acetate, and placing the mixture in a stirring device, wherein the use ratio of the antarctic krill meat paste to the ethyl acetate is 1g: the volume of the mixture is 6ml, soaking for 20min under the stirring condition, then filtering to obtain mixed liquid of the Antarctic krill meat emulsion filter residue and ethyl acetate, cleaning the Antarctic krill meat emulsion filter residue by using clear water, wherein the mass ratio of the clear water to the filter residue is 2.9:1, placing the mixed liquid of the Antarctic krill meat emulsion and the clear water in a centrifuge for centrifugation, obtaining bottom Antarctic krill meat emulsion and centrifugate after centrifugation, and mixing the centrifugate and the mixed liquid of the ethyl acetate to obtain the mixed liquid.
Filtering the mixed solution by an ultrafiltration membrane with the aperture of 200 daltons, and recovering the mixed ester solution which does not pass through the membrane pores.
Drying the minced meat of the Antarctic krill obtained after centrifugation for 15min at the temperature of 65 ℃ to obtain shrimp meal, putting the shrimp meal into a mixed organic solvent obtained by mixing petroleum ether with the volume ratio of 2.2:1 and ethanol with the mass percentage content of more than 95%, wherein the dosage ratio of the shrimp meal to the mixed organic solvent is 1g: 3mL, adding the shrimp powder into the mixed organic solvent completely, adding the mixed solution of the shrimp powder and the mixed organic solvent into a homogenizer, and homogenizing at 35 ℃ under the pressure of 13MPa for 18min to obtain a homogenized and mixed shrimp liquid. And then filtering the homogenized and mixed shrimp solution to obtain filtrate and shrimp meat paste, mixing the filtrate and the mixed ester solution, desolventizing and dehydrating at the temperature of 35 ℃ and under the pressure of 0.09MPa, extracting for 80min to obtain concentrated solution and steam condensate, and filtering the concentrated solution through 500-mesh filter cloth to obtain first antarctic krill oil. And (3) carrying out secondary purification on the steam condensate at the temperature of 60 ℃ and under the pressure of 0.02MPa, extracting for 50min to obtain second Antarctic krill oil, and mixing the second Antarctic krill oil with the first Antarctic krill oil to obtain the Antarctic krill oil provided by the invention.
Comparative example 1
The comparative example is basically the same as the example 1, except that the comparative example 1 does not react with ethyl acetate and is filtered by an ultrafiltration membrane before the meat paste of the antarctic krill is dried, and the meat paste is directly dried and ground by adopting a mixed organic solvent for extraction.
Comparative example 2
This comparative example is substantially the same as example 4, except that the mixing of shrimp meal and ethanol was not carried out in a homogenizer, and was left for 30min after direct mixing.
Comparative example 3
This comparative example is substantially the same as example 4 except that the centrifugal draining was replaced with press draining.
Comparative example 4
This comparative example is substantially the same as example 4 except that the mixed organic solvent was replaced with petroleum ether.
Comparative example 5
This comparative example is substantially the same as example 4, except that the mixed organic solvent is replaced with an ethanol solution having a mass percentage of 95% or more.
Examples of the experiments
60 kg of antarctic krill was selected and divided into 10 portions on average, and each portion was subjected to extraction of antarctic krill oil according to the methods provided in examples 1-7 and comparative examples 1-5. And (4) measuring the extraction rate and the total arsenic content in the obtained antarctic krill oil. And the results of the measurements are recorded in table 1. Examples 1-7 and comparative examples 1-5 are numbered in series as groups 1-12.
The extraction rate is the ratio of the weight of the obtained antarctic krill oil to the raw material of the antarctic krill.
The total arsenic content in krill oil is detected by national standard for food safety of GB 5009.11-2014.
Table 1 shows the extraction yield (%) and the total arsenic (ppm) content in Euphausia superba oil
Figure GDA0003387467260000171
As can be seen from the analysis of table 1, the extraction rates of the antarctic krill oils obtained in examples 1 to 7 provided by the present invention are all above 3.3%, while the extraction rates of the antarctic krill oils are almost all below 3% in the existing process production, and although the extraction rates are not greatly increased from the data, the extraction process difficulty itself is relatively large because the limited content of the krill oil contained in the antarctic krill is low, and even the increase of the extraction rate of 0.01 percent is a great leap. Compared with the extraction rate of the comparative example 2 and the comparative example 3 is obviously lower than that of the example 4, the extraction rate of the antarctic krill oil can be obviously improved by homogenizing the shrimp meal and the ethanol in a homogenizer, and the extraction rate of the antarctic krill oil can be improved by adopting a centrifugal liquid removal method compared with the existing press dehydration method.
The total arsenic content in the euphausia superba oil prepared in the embodiments 1-7 of the invention is below 1 ppm. The total arsenic content of the krill oil in the existing market is 7-10 ppm, and the total arsenic content of the Antarctic krill oil prepared by the method is obviously much lower than that of the Euphausia krill oil in the market. The total arsenic content of the antarctic krill oil prepared in the comparative example 1 is greatly higher than that of the krill oil prepared in the examples 1 to 7, so that the method can be seen that in the extraction process of the antarctic krill oil, the organic solvent is adopted for extracting money, ethyl acetate is adopted for pretreatment and primary extraction, and after primary extraction, the ultrafiltration membrane is adopted for filtering and recovering phospholipid, so that the micromolecular organic arsenic is removed, and the effect of effectively reducing the total arsenic content is achieved.
In conclusion, in the method for preparing the antarctic krill oil and the protein powder by using the antarctic krill, the organic arsenic and other small molecular impurities are removed by filtering with the ultrafiltration membrane after the mixture of the ethyl acetate and the cooked antarctic krill meat paste is soaked for a proper time in the preparation process, so that the total arsenic content in the prepared antarctic krill oil is reduced; the shrimp meal and the mixed oil machine solvent of ethanol and petroleum ether with a reasonable proportion are uniformly mixed in the homogenizer, so that the krill oil contained in the shrimp meal is fully contacted with the organic solvent and enters the organic solvent no matter the polarity is strong or weak, and the extraction rate of the antarctic krill is effectively improved; the water in the euphausia superba meat is removed in a centrifugal mode in the liquid removing process, so that the subsequent extraction is facilitated, and compared with the existing squeezing and dewatering mode, the liquid removing process is not easy to cause the oil of the euphausia superba in the euphausia superba to be lost; and the subsequent two times of evaporation and concentration after the liquid removal are finished ensure that the ethanol, the petroleum ether and partial water are completely evaporated under proper evaporation conditions, so that the purity of the Antarctic krill oil is ensured, meanwhile, the shrimp paste produced in the extraction is dried to obtain the protein powder, so that the raw material waste is avoided, and the protein powder is defatted protein powder and has higher nutritional value.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. A method for preparing antarctic krill oil and protein powder by using antarctic krill is characterized by comprising the following steps:
mixing and soaking the cooked euphausia superba meat paste with ethyl acetate for 5-70 min, filtering to obtain an ethyl acetate mixed solution and euphausia superba meat paste filter residue, recovering the ethyl acetate mixed solution, centrifuging the euphausia superba meat paste filter residue to obtain a liquid-removed shrimp meat paste and a centrifugal liquid, and mixing the centrifugal liquid with the ethyl acetate mixed solution to obtain a mixed solution;
enabling the mixed solution to pass through an ultrafiltration membrane with the aperture of 200-300 daltons to obtain a intercepted mixed ester solution;
drying and grinding the deliquored shrimp meat paste to obtain shrimp powder;
adding the shrimp meal and a mixed organic solvent into a homogenizer, homogenizing for 10-60 min under the pressure of 10.8-20.6 MPa to obtain a homogenized mixed shrimp liquid, filtering the homogenized mixed shrimp liquid to obtain a filtrate and shrimp meat paste, wherein the dosage ratio of the shrimp meal to the mixed organic solvent is 1g: 1-7 mL of the mixed organic solvent, wherein the mixed organic solvent comprises petroleum ether and an ethanol solution with the mass concentration of more than 95% in a volume ratio of 1.5-3: 1;
mixing the filtrate and the mixed ester solution, carrying out primary purification at the temperature of 30-70 ℃, the pressure of 0.01-0.1 MPa and the extraction time of 60-180 min to obtain a concentrated solution and a steam condensate, and filtering the concentrated solution through 400-500-mesh filter cloth to obtain first antarctic krill oil;
carrying out secondary purification on the steam condensate under the conditions of 55-85 ℃, 0.01-0.08 MPa of pressure and 30-120 min of extraction time to obtain second Antarctic krill oil, and mixing the first Antarctic krill oil and the second Antarctic krill oil to obtain Antarctic krill oil;
and drying the shrimp paste to obtain protein powder.
2. The method for preparing the antarctic krill oil and protein powder from the antarctic krill according to claim 1, wherein the method further comprises a clear water cleaning step after the antarctic krill meat emulsion is mixed with the ethyl acetate and soaked and before centrifugation, wherein the filter residue of the antarctic krill meat emulsion is cleaned by clear water, and the mass ratio of the clear water to the filter residue of the antarctic krill meat emulsion is 2.5-3.5: 1 during cleaning.
3. The method for preparing the antarctic krill oil and protein powder from the antarctic krill according to claim 1, further comprising, before mixing the meat emulsion of the antarctic krill with the ethyl acetate: the antarctic krill is cooked, hulled and pulverized.
4. The method for preparing the antarctic krill oil and protein powder from the antarctic krill according to claim 3, wherein the cooking is performed by heating the antarctic krill at a temperature of 70-100 ℃ for 5-20 min.
5. The method for preparing the antarctic krill oil and protein powder from the antarctic krill according to claim 1, wherein the using amount ratio of the meat emulsion of the antarctic krill to the ethyl acetate is 1g: 5-17 ml.
6. The method for preparing the antarctic krill oil and protein powder from the antarctic krill as claimed in claim 1, wherein the de-liquefied minced shrimp is dried for 5-60 min at a temperature of 60-100 ℃.
7. The method for preparing the antarctic krill oil and protein powder from the antarctic krill as claimed in claim 1, wherein the shrimp meat paste is mixed with the mixed organic solvent again, homogenized under the same conditions and filtered, and the extraction is repeated at least 2 times.
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