CN107964453B - Method for preparing grease from degreased dried euphausia superba residues - Google Patents
Method for preparing grease from degreased dried euphausia superba residues Download PDFInfo
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- CN107964453B CN107964453B CN201711397160.4A CN201711397160A CN107964453B CN 107964453 B CN107964453 B CN 107964453B CN 201711397160 A CN201711397160 A CN 201711397160A CN 107964453 B CN107964453 B CN 107964453B
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- residues
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- ethanol
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- antarctic krill
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
Abstract
The invention belongs to the fields of food, chemistry and medicine, and particularly relates to a method for preparing grease from degreased dried shrimp residues of Antarctic krill. The method comprises the steps of firstly carrying out superfine grinding on dry shrimp residues, then extracting by using a mixed solvent of normal hexane and ethanol, and carrying out rotary evaporation on filtrate of an extracting solution to obtain oil, wherein the oil yield is 4.67-5.9%.
Description
Technical Field
The invention belongs to the fields of food, chemistry and medicine, and particularly relates to a method for preparing grease from degreased dried shrimp residues of Antarctic krill.
Background
Antarctic krill is a huge biomass living in Antarctic oceans (about 5-50 million tons, with differences in different estimation methods). The antarctic krill is rich in oil, and the oil content is different due to factors such as season, age, sex, abundance degree of food, environment and the like. The oil and fat is rich in unsaturated fatty acids (such as EPA, DHA, DPA, etc.), astaxanthin and its lipid, phospholipid, vitamin E, etc. At present, the antarctic krill oil is a high value-added product widely sold in the world, and the antarctic krill oil product is mainly produced in Canada, Japan, Norway and America. After 2000 years, a plurality of manufacturers in China began to produce the euphausia superba oil which meets the international standard.
Chinese patent (CN201210412979.4) discloses a process for extracting shrimp sauce with low cholesterol content from Antarctic krill, which comprises the following steps: (1) adding dried Euphausia superba into acetone, and extracting dried Euphausia superba for 3 times, wherein each time for 1 h; mixing the extractive solutions, and rotary evaporating to remove acetone to obtain shrimp sauce; (2) filtering to obtain shrimp residues after the last extraction in the step (1), adding n-hexane into the shrimp residues, and extracting for 3 times, wherein each extraction time is 1 hour; mixing the extractive solutions, and rotary evaporating to remove n-hexane to obtain shrimp sauce; (3) and (3) combining the shrimp sauce obtained in the step (1) and the step (2), adding ethanol, stirring to dissolve, freezing, naturally layering the mixed solution, pouring out the supernatant, and performing rotary evaporation to obtain the shrimp sauce with low cholesterol content.
Chinese patent (CN201210411171.4) discloses a process for extracting fluorine-free shrimp sauce from Antarctic krill, which is characterized in that: the method comprises the following steps: (1) taking dried euphausia superba, adding acetone, extracting for 3 times, combining extracting solutions, and performing rotary evaporation to obtain shrimp sauce; (2) filtering the last extraction in the step (1) to obtain shrimp residues, adding ethanol into the shrimp residues, extracting for 3 times, combining the extracting solutions, and performing rotary evaporation to obtain a concentrate; (3) adding acetone into the concentrate, stirring and extracting for 0.5-1h, extracting twice, filtering, combining the filtrates of the two times, and performing rotary evaporation to obtain shrimp sauce; (4) and (3) combining the shrimp sauce obtained in the step (1) and the shrimp sauce obtained in the step (3), adding ethanol, cooling, removing the precipitate to obtain a supernatant, freezing, removing the precipitate to obtain a supernatant, and performing rotary evaporation to obtain the fluorine-free shrimp sauce.
The euphausia superba residue after the shrimp sauce is extracted in production still has a certain amount of grease which is not extracted, and the grease yield is improved on the basis of equal amount of raw materials by preparing the grease, so that the cost is reduced, and the product competitiveness is improved. However, the properties of the shrimp residues are different from that of the shrimp powder of the Antarctic krill before oil extraction, the oil components are also different, and the oil in the shrimp residues cannot be effectively extracted by the conventional oil extraction method, so that a method for extracting the oil from the shrimp residues of the Antarctic krill is needed.
Disclosure of Invention
The invention mainly aims to provide a method for re-extracting grease from euphausia superba residues.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for preparing grease from degreased dried shrimp residues of Antarctic krill comprises the following steps: mixing the shrimp residue powder obtained by carrying out superfine crushing on degreased dry shrimp residues of Antarctic krill with a mixed solvent of n-hexane and ethanol, stirring and extracting for 0.5-1h, filtering, collecting filter residues, repeatedly extracting for 2 times, combining filtrates, and carrying out rotary evaporation on the solvent at 68-72 ℃ to obtain the euphausia superba residue powder.
In the preferred technical scheme of the invention, the superfine grinding process of the dry shrimp residues comprises the following steps: pulverizing defatted dried residue of Euphausia superba 0.6-1kg with vibration type medicinal micronizer, micronizing with stainless steel vibrating rod phi 20 × 174mm and amplitude 3-5mm for 0.5-1 h.
In the preferable technical scheme of the invention, the mixed solvent consists of n-hexane and ethanol in a ratio of 1-3: 1.
In a further preferable technical scheme of the invention, the mixed solvent is composed of n-hexane and ethanol according to the volume ratio of 2: 1.
In the preferred technical scheme of the invention, the obtained shrimp residue powder is mixed with a mixed solvent of n-hexane and ethanol according to the mass volume ratio of 1: 4-8.
Residual oil and fat components contained in shrimp residues obtained after the Antarctic krill is degreased are difficult to be obtained by leaching with a conventional organic solvent, and technicians extract the oil and fat in the shrimp residues by adopting a Folch method, so that only 0.8g of oil and fat is extracted from 100g of shrimp residues, and the extraction effect is not ideal; extracting by adopting a mixed system of three solutions of acetone, dichloromethane and ethanol to obtain 0.53g of grease, and the extraction effect is worse; extracting with acetone and ethanol to obtain 0.71g oil. After a large number of experiments, technicians of the invention unexpectedly find that when the shrimp residues are extracted with the mixed solution of n-hexane and ethanol, the extraction amount of the oil is greatly improved, and particularly when the n-hexane and the ethanol in the mixed solution are mixed according to the volume of 2:1, 2.7g of the oil can be extracted from every 100g of the shrimp residues, so that the yield of the oil in the shrimp residues is greatly improved.
The organic solvent can be extracted to obtain intracellular oil by destroying Antarctic phosphorus cells under the action of osmotic pressure difference, however, the penetration distance of the organic solvent in the cells is limited. The ultramicro breaking technology can fully dissolve out the grease in the cells. In the superfine pulverizing equipment, the efficiency of the vibration mill is 10-20 times higher than that of the common mill, the milling speed is faster than that of the conventional ball mill, and the energy consumption is lower than that of the common ball mill. The technical personnel of the invention find through experiments that the vibration type drug ultrafine pulverizer with the parameters of the stainless steel vibrating rod phi 20 multiplied by 174mm and the amplitude of 3-5mm can play a good crushing effect on the degreased dried shrimp residues of the antarctic krill; when the shrimp residue powder is crushed for 0.5 to 1 hour, not only can the grease component in the shrimp residue powder be fully dissolved out, but also wall sticking and overhigh material temperature caused by over-grinding can be effectively avoided.
According to the invention, after the degreased dry shrimp residue of the Antarctic krill is subjected to crushing pretreatment for 0.5-1h by using a vibrating mill with specific parameters, the degreased dry shrimp residue is extracted by using a mixed solution of n-hexane and ethanol, and the oil yield can reach 4.67-5.9%; therefore, the yield of the antarctic krill oil is effectively improved, the method is simple to operate, low in production cost and easy for large-scale production of the antarctic krill oil.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, elements, and/or combinations thereof, unless the context clearly indicates otherwise.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
The degreased dry shrimp residue of the Antarctic krill is purchased from Shandong Luhua Biotech Co.
Example 1 method for re-extracting grease from degreased dried shrimp residues of Antarctic krill
The method comprises the following steps: pulverizing defatted dried residue of Euphausia superba 0.6-1kg with vibration type medicinal micronizer, micronizing with stainless steel vibrating rod (phi 20 × 174mm, amplitude 3-5 mm) for 1 hr, and pouring out residue powder. Adding 500ml of mixed solution of n-hexane and ethanol (n-hexane: ethanol 1:1) into 100g of superfine pulverized shrimp residue powder, stirring and extracting for 45 minutes, and filtering to obtain filtrate. Extracting the residue for 3 times again by the same method for 2 times, mixing filtrates, and rotary evaporating at 70 deg.C to remove solvent to obtain 5.5g oil with oil content of 5.5%.
Example 2 method for re-extracting grease from degreased dried shrimp residues of Antarctic krill
The method comprises the following steps: pulverizing defatted dried residue of Euphausia superba 0.6-1kg with vibration type medicinal micronizer, micronizing with stainless steel vibrating rod of phi 20 × 174mm and amplitude 3-5mm for 0.5 hr, and pouring out residue powder. Adding 400ml of mixed solution of n-hexane and ethanol (n-hexane: ethanol is 3:1) into 100g of superfine pulverized shrimp residue powder, stirring and extracting for 1h, and filtering to obtain filtrate. Extracting the residue for 2 times in the same manner as above, extracting for 3 times, mixing the filtrates, and rotary evaporating at 68 deg.C to remove solvent to obtain 4.67g oil with oil content of 4.67%.
Example 3 method for re-extracting grease from degreased dried shrimp residues of Antarctic krill
The method comprises the following steps: pulverizing defatted dried residue of Euphausia superba 0.6-1kg with vibration type medicinal micronizer, micronizing with stainless steel vibrating rod (phi 20 × 174mm, amplitude 3-5 mm) for 1 hr, and pouring out residue powder. Adding 800ml mixed solution of n-hexane and ethanol (n-hexane: ethanol 2:1) into 100g of superfine pulverized shrimp residue powder, stirring and extracting for 0.5h, and filtering to obtain filtrate. Extracting the residue for 3 times again by the same method for 2 times, mixing filtrates, and rotary evaporating at 72 deg.C to remove solvent to obtain 5.9g oil with oil content of 5.9%.
Comparative example 1
Adding 800ml of mixed solution of n-hexane and ethanol (n-hexane: ethanol is 2:1) into 100g of degreased dried euphausia superba residue, stirring and extracting for 0.5h, and filtering to obtain filtrate. Extracting the residue for 3 times again by the same method for 2 times, mixing filtrates, and rotary evaporating at 72 deg.C to remove solvent to obtain 1.2g oil with oil content of 1.2%.
Comparative example 2
Pulverizing defatted dried residue of Euphausia superba 0.6-1kg with vibration type medicinal micronizer, micronizing with stainless steel vibrating rod (phi 20 × 174mm, amplitude 3-5 mm) for 1 hr, and pouring out residue powder. Collecting 100g of superfine pulverized shrimp residue powder, adding 800ml of mixed solution of acetone and ethanol (acetone: ethanol: 2:1), stirring and extracting for 0.5h, and filtering to obtain filtrate. Extracting the residue for 3 times again by the same method for 2 times, mixing filtrates, and rotary evaporating at 72 deg.C to remove solvent to obtain 2.6g oil with oil content of 2.6%.
Comparative example 3
Putting 0.6-1Kg of non-degreased euphausia superba powder into a vibration type medicine superfine pulverizer for pulverizing, carrying out superfine pulverization for 1h by a stainless steel vibrating rod phi of 20X 174mm and the amplitude of 3-5mm, and pouring out the shrimp residue powder. Collecting 100g of superfine pulverized shrimp residue powder, adding 800ml of mixed solution of n-hexane and ethanol (n-hexane: ethanol: 2:1), stirring and extracting for 45 min, filtering to obtain filtrate, repeatedly extracting the residue for 2 times, mixing the filtrates, and rotary evaporating to remove solvent to obtain 16.1g of oil with oil yield of 16.1%.
Comparative example 4
Adding 8000ml of mixed solution of normal hexane and ethanol (normal hexane: ethanol is 2:1) into 1Kg of non-degreased euphausia superba powder, stirring and extracting for 45 minutes, filtering to obtain filtrate, repeatedly extracting filter residues for 2 times, combining 3 times of filtrates, and performing rotary evaporation to remove the solvent to obtain 160g of oil, wherein the oil yield is 16.0%. Drying the residue, pulverizing with vibrating ultrafine pulverizer, micronizing with stainless steel vibrating rod (phi 20 × 174mm, amplitude 3-5 mm) for 1 hr, and pouring out the residue powder. Collecting 100g of superfine pulverized shrimp residue powder, adding 800ml of mixed solution of n-hexane and ethanol (n-hexane: ethanol: 2:1), stirring and extracting for 45 min, filtering to obtain filtrate, repeatedly extracting the residue for 2 times, mixing the filtrates, and rotary evaporating to remove solvent to obtain 5.4g of oil with oil yield of 5.4%.
Claims (4)
1. A method for preparing grease from dry degreased shrimp residues of Antarctic krill is characterized in that shrimp residue powder obtained by carrying out superfine crushing on the dry degreased shrimp residues of Antarctic krill is mixed with a mixed solvent of n-hexane and ethanol, the mixture is stirred and extracted for 0.5 to 1 hour and then filtered, filter residues are collected and extracted for 2 times, filtrate is combined, and the solvent is subjected to rotary evaporation at 68 to 72 ℃ to obtain the grease;
the superfine grinding process of the dried shrimp residues comprises the following steps: pulverizing defatted dried residue of Euphausia superba 0.6-1kg with vibration type medicinal micronizer, micronizing with stainless steel vibrating rod phi 20 × 174mm and amplitude 3-5mm for 0.5-1 h.
2. The method for preparing grease from antarctic krill residues according to claim 1, wherein the mixed solvent consists of n-hexane and ethanol in a volume ratio of 1-3: 1.
3. The method for preparing grease from antarctic krill residues according to claim 1, wherein the mixed solvent consists of n-hexane and ethanol in a volume ratio of 2: 1.
4. The method for preparing grease from antarctic krill residues according to claim 1, wherein the obtained shrimp residue powder is mixed with a mixed solvent of n-hexane and ethanol according to a mass-to-volume ratio of 1: 4-8.
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| CN102766530A (en) * | 2012-08-08 | 2012-11-07 | 辽宁省大连海洋渔业集团公司 | Method for extracting phospholipid-rich krill oil from Antarctic krill |
| CN102899163A (en) * | 2012-10-25 | 2013-01-30 | 山东师范大学 | Process for extracting fluoride-free shrimp oil from dried antarctic krill |
| CN102925284A (en) * | 2012-10-25 | 2013-02-13 | 山东师范大学 | Technique for extracting low-cholesterol-content krill oil from Antarctic krill |
| CN104152263A (en) * | 2014-08-18 | 2014-11-19 | 安徽中盛食用油科技有限公司 | Tea-seed oil extraction method with high oil yield |
| CN106010783A (en) * | 2016-05-24 | 2016-10-12 | 青岛南极维康生物科技有限公司 | Method for producing krill oil, protein peptide powder and chitosan by full utilization of Antarctic krill powder |
| CN106720466A (en) * | 2016-12-30 | 2017-05-31 | 徐霞 | It is a kind of while the method for extracting high phospholipid krill oil and astaxanthin ester krill oil high |
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102766530A (en) * | 2012-08-08 | 2012-11-07 | 辽宁省大连海洋渔业集团公司 | Method for extracting phospholipid-rich krill oil from Antarctic krill |
| CN102899163A (en) * | 2012-10-25 | 2013-01-30 | 山东师范大学 | Process for extracting fluoride-free shrimp oil from dried antarctic krill |
| CN102925284A (en) * | 2012-10-25 | 2013-02-13 | 山东师范大学 | Technique for extracting low-cholesterol-content krill oil from Antarctic krill |
| CN104152263A (en) * | 2014-08-18 | 2014-11-19 | 安徽中盛食用油科技有限公司 | Tea-seed oil extraction method with high oil yield |
| CN106010783A (en) * | 2016-05-24 | 2016-10-12 | 青岛南极维康生物科技有限公司 | Method for producing krill oil, protein peptide powder and chitosan by full utilization of Antarctic krill powder |
| CN106720466A (en) * | 2016-12-30 | 2017-05-31 | 徐霞 | It is a kind of while the method for extracting high phospholipid krill oil and astaxanthin ester krill oil high |
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