CN107904009B - Method for re-extracting grease from euphausia superba residues - Google Patents

Method for re-extracting grease from euphausia superba residues Download PDF

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CN107904009B
CN107904009B CN201711396238.0A CN201711396238A CN107904009B CN 107904009 B CN107904009 B CN 107904009B CN 201711396238 A CN201711396238 A CN 201711396238A CN 107904009 B CN107904009 B CN 107904009B
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extracting
ethanol
residue
euphausia superba
shrimp
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CN107904009A (en
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刘代成
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Shandong Normal University
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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
    • C11B1/10Production 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/108Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
    • 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
    • C11B3/12Refining fats or fatty oils by distillation

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

Abstract

The invention belongs to the technical field of food processing, and particularly relates to a method for re-extracting grease from euphausia superba residues. The extraction method comprises the following steps: mixing the shrimp residue with mixed solvent, stirring and extracting for 1-1.5h, filtering, collecting the residue, extracting for 2 times, mixing filtrates, and rotary evaporating solvent at 68-73 deg.C to obtain the final product. Wherein the mixed solvent consists of n-hexane and ethanol according to the volume ratio of 1-3: 1. The method can effectively extract the oil from the shrimp residues, and compared with a Folch method, the extraction amount of the oil is improved by 2.4 times; the extraction method of the invention adopts mixed extraction of ethanol and n-hexane, the toxicity of the ethanol is low, and the n-hexane is also a common solvent in the industry, so the extraction method of the invention is safe, low in cost and easy to popularize and apply.

Description

Method for re-extracting grease from euphausia superba residues
Technical Field
The invention belongs to the technical field of food, chemistry and medicine, and particularly relates to a method for re-extracting grease from euphausia superba residues.
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 0.5-1 h, 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 re-extracting grease from euphausia superba residues comprises the following steps: mixing the shrimp residue with mixed solvent of n-hexane and ethanol, stirring for 1-1.5 hr, filtering, collecting residue, extracting for 2 times, mixing filtrates, and rotary evaporating solvent at 68-73 deg.C to obtain the final product.
In the early period, technicians extract the grease in the shrimp residues by adopting a Folch method, and only 0.8g of grease is extracted from 100g of shrimp residues, so 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 mixed and extracted with the mixed solution of n-hexane and ethanol according to the mass-to-volume ratio of 1:5, 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.
Therefore, compared with the prior art, the invention has the following technical advantages:
(1) the method can effectively extract the oil from the shrimp residues, and compared with a Folch method, the extraction amount of the oil is improved by 2.4 times;
(2) the extraction method of the invention adopts mixed extraction of ethanol and n-hexane, the toxicity of the ethanol is low, and the n-hexane is also a common solvent in the industry, so the extraction method of the invention is safe, low in cost and easy to popularize and apply.
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 more effectively extract grease from the shrimp residue, the invention provides a method for re-extracting grease from the shrimp residue of Antarctic krill, which comprises the following steps: mixing the shrimp residue with mixed solvent, stirring and extracting for 1-1.5h, filtering, collecting the residue, extracting for 2 times, mixing filtrates, and rotary evaporating solvent at 68-73 deg.C to obtain the final product.
In a preferred technical scheme of the invention, the mixed solvent consists of n-hexane and ethanol according to the volume ratio of 1-3: 1.
In the best technical scheme of the invention, the mixed solvent consists of n-hexane and ethanol according to the volume ratio of 2: 1.
In the preferred technical scheme of the invention, the shrimp residue and the mixed solvent are mixed according to the mass-to-volume ratio of 1: 5.
In the preferable technical scheme of the invention, the shrimp residue is obtained by ultrasonic extraction and drying of Antarctic krill by taking ethanol as a solvent.
In the preferred technical scheme of the invention, the temperature of the rotary evaporation solvent is 68-73 ℃.
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 oil from euphausia superba residue
The extraction method comprises the following steps: weighing 100g of euphausia superba residues obtained by ultrasonic extraction and drying of euphausia superba by using ethanol as a solvent, mixing 500mL of mixed solvent, stirring and extracting for 1.5h, filtering, collecting filter residues, repeatedly extracting for 2 times, combining filtrates, and performing rotary evaporation of the solvent at 68 ℃ to obtain the euphausia superba extract.
The mixed solvent consists of n-hexane and ethanol according to the volume ratio of 2: 1.
Example 2 method for re-extracting oil from euphausia superba residue
The extraction method comprises the following steps: weighing 100g of euphausia superba residue obtained by performing ultrasonic extraction and drying on euphausia superba by using ethanol as a solvent, mixing 500mL of mixed solvent, stirring and extracting for 1h, filtering, collecting filter residue, repeatedly extracting for 2 times, combining filtrate, and performing rotary evaporation on the solvent at 70 ℃ to obtain the euphausia superba extract.
The mixed solvent consists of n-hexane and ethanol according to the volume ratio of 1: 1.
Example 3 method for re-extracting oil from euphausia superba residue
The extraction method comprises the following steps: weighing 100g of euphausia superba dregs obtained by performing ultrasonic extraction and drying on euphausia superba by using ethanol as a solvent, mixing 500mL of mixed solvent, stirring and extracting for 1.5h, filtering, collecting filter residues, repeatedly extracting for 2 times, combining filtrate, and performing rotary evaporation on the solvent at 73 ℃ to obtain the euphausia superba extract.
The mixed solvent consists of n-hexane and ethanol according to the volume ratio of 3: 1.
Comparative example 1 method for re-extracting grease from euphausia superba residues
The difference from example 1 is that the mixed solvent used consists of 1, 2-dichloroethane and ethanol in a volume ratio of 2:1, and the rest is similar to example 1.
Comparative example 2 method for re-extracting grease from euphausia superba residues
The difference from example 1 is that the mixed solvent used consists of 1, 4-dichlorobutane and ethanol in a volume ratio of 2:1, and the rest is similar to example 1.
Comparative example 3 method for re-extracting grease from euphausia superba residues
The difference from example 1 is that the mixed solvent used consists of 1, 4-dichlorobutane and methanol in a volume ratio of 2:1, and the rest is similar to example 1.
Comparative example 4 method for re-extracting grease from euphausia superba residues
The difference from example 1 is that the mixed solvent used consists of 1, 2-dichloroethane and methanol in a volume ratio of 2:1, and the rest is similar to example 1.
Comparative example 5 method for re-extracting grease from euphausia superba residue
The difference from example 1 is that the mixed solvent used consists of 1, 2-dichloroethane and ethanol in a volume ratio of 2:1, and the rest is similar to example 1.
Comparative example 6 method for re-extracting grease from euphausia superba residue
The difference from example 1 is that the mixed solvent used consists of methanol and ethyl acetate in a volume ratio of 2:1, and the rest is similar to example 1.
Comparative example 7 method for re-extracting grease from euphausia superba residues
The difference from example 1 is that the mixed solvent used consists of acetone, methanol and ethyl acetate in a volume ratio of 4:2:1, and the rest is similar to example 1.
Comparative example 8 method for re-extracting grease from euphausia superba residue
The difference from example 1 is that the mixed solvent used consists of acetone, dichloromethane and methanol in a volume ratio of 2:1:1, and the rest is similar to example 1.
Comparative example 9 method for re-extracting grease from euphausia superba residue
The difference from example 1 is that the mixed solvent used consists of acetone, dichloromethane and ethanol in a volume ratio of 2:1:1, and the rest is similar to example 1.
Comparative example 10 method for re-extracting grease from euphausia superba residue
The difference from example 1 is that the mixed solvent used consists of acetone and methanol in a volume ratio of 2:1, and the rest is similar to example 1.
Comparative example 11 method for re-extracting grease from euphausia superba residue
The difference from example 1 is that the mixed solvent used consists of acetone and ethanol in a volume ratio of 2:1, and the rest is similar to example 1.
Comparative example 12 method for re-extracting grease from euphausia superba residue
The difference from example 1 is that the mixed solvent used consists of acetone, dichloromethane and ethanol in a volume ratio of 2:1:1, and the rest is similar to example 1.
Comparative example 13 method for re-extracting grease from euphausia superba residue
The difference from example 1 is that the mixed solvent used consists of dichloromethane and ethanol in a volume ratio of 2:1, and the rest is similar to example 1.
Comparative example 14 method for re-extracting oil from euphausia superba residue
The difference from example 1 is that the mixed solvent used consists of dichloromethane and methanol in a volume ratio of 2:1, and the rest is similar to example 1.
Comparative example 15 method for re-extracting grease from euphausia superba residue
The difference from example 1 is that the mixed solvent used consists of chloroform and methanol in a volume ratio of 2:1, and the rest is similar to example 1.
Comparative example 16 method for re-extracting grease from euphausia superba residue
The difference from example 1 is that the mixed solvent used consists of chloroform and ethanol in a volume ratio of 2:1, and the rest is similar to example 1.
Comparative example 17 method for re-extracting grease from euphausia superba residue
The difference from the embodiment 1 is that firstly, 2 times of ethanol extraction is carried out, the total dosage of 2 times of ethanol is 3/4 of the dosage of the mixed solvent in the embodiment 1, the filtration is carried out, the filter residue is extracted by normal hexane, the dosage of normal hexane is 1/4 of the dosage of the mixed solvent, the filtration is carried out, and the two filtrates are combined; the rest is similar to example 1.
Comparative example 18 method for re-extracting grease from euphausia superba residue
The difference from the embodiment 1 is that firstly, 2 times of ethanol extraction is carried out, the total dosage of 2 times of ethanol is 3/4 of the dosage of the mixed solvent in the embodiment 1, the filtration is carried out, the filter residue is extracted by dichloromethane, the dosage of dichloromethane is 1/4 of the dosage of the mixed solvent in the embodiment 1, the filtration is combined, and two filtrates are obtained; the rest is similar to example 1.
Comparative example 19 method for re-extracting grease from euphausia superba residue
The difference from example 1 is that the mixed solvent used consists of n-hexane and ethanol in a volume ratio of 1:2, and the rest is similar to example 1.
Comparative example 20 method for re-extracting grease from euphausia superba residue
The difference from example 1 is that the mixed solvent used consists of n-hexane and ethanol in a volume ratio of 1:3, and the rest is similar to example 1.
Comparative example 21 method for re-extracting grease from euphausia superba residue
The difference from example 1 is that the amount of shrimp residues was 105g, and the rest was similar to example 1.
Test example-measurement of extracted oil content
The fats and oils obtained by the extraction methods of examples 1 to 3 and comparative examples 1 to 21 were weighed, respectively, and the results are shown in Table 1.
TABLE 1 weight of oil extracted by different extraction methods
Figure BDA0001518565580000061
As is clear from Table 1, the amount of the fat extracted in example 1 was 2.7g at the maximum in example 1, and thus example 1 was the most suitable example. Example 1 the amount of extracted oil was higher than that of comparative examples 1-20, wherein the amount of extracted oil was increased by 2.4 times in example 1 compared to comparative example 14; the effect of extracting the oil in the shrimp residue by using the extraction method in the embodiment 1 is much higher than that of a conventional oil extraction method, namely a folch method; example 1, with higher extraction than comparative examples 7-9, illustrates the use of n-hexane from example 1: the effect of extracting the oil in the shrimp residue after the ethanol is mixed 2:1 is better than that of extracting three different solvents; example 1 the extraction yield was higher than in comparative examples 17-18, indicating that better results were obtained only after first mixing n-hexane with ethanol at a ratio of 2: 1; example 1 has a higher extraction amount than comparative examples 19 to 20, which shows that the extraction of oil from shrimp residue has a greater effect when the mixing ratio of n-hexane and ethanol is 2:1, and the best effect is obtained when the volume ratio of n-hexane and ethanol is 2:1, and further, when the mass volume ratio of shrimp residue to mixed solvent is 1.05:5, compared with comparative example 21, the content of oil obtained by extraction is 1.75g, therefore, the invention adopts n-hexane and ethanol mixed solution (n-hexane: ethanol: 2:1) to extract the shrimp residue after ultrasonic extraction and drying of Antarctic krill by using ethanol as solvent, and only the mixed solution of shrimp residue and the mixed solution has the best effect when the volume ratio of shrimp residue to the mixed solution is 1: 5.

Claims (1)

1. A method for re-extracting grease from euphausia superba shrimp residues is characterized in that 100g of euphausia superba shrimp residues are weighed, are subjected to ultrasonic extraction and drying by taking ethanol as a solvent, are mixed with 500mL of a mixed solvent, are stirred and extracted for 1.5h, are filtered, are collected and are repeatedly extracted for 2 times, are combined with filtrates, and are subjected to rotary evaporation at 68 ℃ to obtain the grease;
the mixed solvent consists of n-hexane and ethanol according to the volume ratio of 2: 1.
CN201711396238.0A 2017-12-21 2017-12-21 Method for re-extracting grease from euphausia superba residues Expired - Fee Related CN107904009B (en)

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KR20100038029A (en) * 2008-10-02 2010-04-12 인성실업(주) Method of producing krill oil using supercritical extraction and krill oil composition with high contents of omega-3 fatty acids
CN102492545B (en) * 2011-12-28 2013-10-02 中国水产科学研究院黄海水产研究所 Methods for extracting high-quality shrimp oil from Antarctic krill and for preparing defatted krill protein powder
CN102746205B (en) * 2012-07-18 2014-07-23 山东师范大学 Method for extracting astaxanthin monoester from antarctic krill
CN102899161B (en) * 2012-10-25 2014-04-09 山东师范大学 Process for extracting shrimp oil crude product from dried antarctic krill and treating foam
CN102925284B (en) * 2012-10-25 2014-01-08 山东师范大学 Technique for extracting low-cholesterol-content krill oil from Antarctic krill
CN102899163B (en) * 2012-10-25 2015-03-25 山东师范大学 Process for extracting fluoride-free shrimp oil from antarctic krill
CN102911786B (en) * 2012-10-25 2014-01-08 山东师范大学 Technology for extracting shrimp oil with low fluoride from euphausia superba
CN102899165B (en) * 2012-10-25 2014-03-12 山东师范大学 Technology for extracting bright red shrimp oil crude product from euphausia superba
CN102899164B (en) * 2012-10-25 2015-12-02 山东师范大学 A kind of technique preparing fluoride-free euphausia superba oil
CN102899162B (en) * 2012-10-25 2013-12-04 山东师范大学 Technology for preparing euphausia superba oil in low fluorine content
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