CN113073004B - Enrichment and purification method for euphausia superba oil phospholipids - Google Patents
Enrichment and purification method for euphausia superba oil phospholipids Download PDFInfo
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- 150000003904 phospholipids Chemical class 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000000746 purification Methods 0.000 title claims abstract description 17
- 241000239370 Euphausia superba Species 0.000 title description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 115
- 229940106134 krill oil Drugs 0.000 claims abstract description 69
- 229920005989 resin Polymers 0.000 claims abstract description 46
- 239000011347 resin Substances 0.000 claims abstract description 46
- 238000001179 sorption measurement Methods 0.000 claims abstract description 40
- 238000001704 evaporation Methods 0.000 claims abstract description 12
- 239000003480 eluent Substances 0.000 claims abstract description 8
- 235000019441 ethanol Nutrition 0.000 claims description 33
- 239000003463 adsorbent Substances 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 abstract description 16
- 231100000331 toxic Toxicity 0.000 abstract description 5
- 230000002588 toxic effect Effects 0.000 abstract description 5
- 230000007935 neutral effect Effects 0.000 abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 15
- 238000004587 chromatography analysis Methods 0.000 description 7
- 238000001514 detection method Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 239000012528 membrane Substances 0.000 description 5
- 230000018109 developmental process Effects 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000002632 lipids Chemical class 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 235000020660 omega-3 fatty acid Nutrition 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 229930182558 Sterol Natural products 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 2
- 238000004440 column chromatography Methods 0.000 description 2
- CYQFCXCEBYINGO-IAGOWNOFSA-N delta1-THC Chemical compound C1=C(C)CC[C@H]2C(C)(C)OC3=CC(CCCCC)=CC(O)=C3[C@@H]21 CYQFCXCEBYINGO-IAGOWNOFSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 235000021588 free fatty acids Nutrition 0.000 description 2
- 231100000086 high toxicity Toxicity 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229940012843 omega-3 fatty acid Drugs 0.000 description 2
- 210000000056 organ Anatomy 0.000 description 2
- 238000010898 silica gel chromatography Methods 0.000 description 2
- 150000003432 sterols Chemical class 0.000 description 2
- 235000003702 sterols Nutrition 0.000 description 2
- 208000031226 Hyperlipidaemia Diseases 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- UEDUENGHJMELGK-HYDKPPNVSA-N Stevioside Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@]12C(=C)C[C@@]3(C1)CC[C@@H]1[C@@](C)(CCC[C@]1([C@@H]3CC2)C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O1)O)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O UEDUENGHJMELGK-HYDKPPNVSA-N 0.000 description 1
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- WORJEOGGNQDSOE-UHFFFAOYSA-N chloroform;methanol Chemical compound OC.ClC(Cl)Cl WORJEOGGNQDSOE-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920006037 cross link polymer Polymers 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000012156 elution solvent Substances 0.000 description 1
- 235000019197 fats Nutrition 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002212 flavone derivatives Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229940013618 stevioside Drugs 0.000 description 1
- OHHNJQXIOPOJSC-UHFFFAOYSA-N stevioside Natural products CC1(CCCC2(C)C3(C)CCC4(CC3(CCC12C)CC4=C)OC5OC(CO)C(O)C(O)C5OC6OC(CO)C(O)C(O)C6O)C(=O)OC7OC(CO)C(O)C(O)C7O OHHNJQXIOPOJSC-UHFFFAOYSA-N 0.000 description 1
- 235000019202 steviosides Nutrition 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides an enrichment and purification method of antarctic krill oil phospholipid, which comprises the following steps: a) Dissolving antarctic krill oil, and then adsorbing by adopting a pretreated nonpolar macroporous adsorption resin chromatographic column; b) And A), eluting the chromatographic column obtained in the step A) by adopting ethanol, and evaporating and concentrating the obtained eluent to obtain the antarctic krill oil rich in phospholipids. According to the invention, neutral fat in krill oil is subjected to specific adsorption by utilizing macroporous adsorption resin, so that enrichment of phospholipid in krill oil is realized, and ethanol is used as an eluting solvent without interference of other toxic solvents; furthermore, the macroporous adsorption resin can be recycled, so that the phospholipid can be produced in a large scale, and basic data is provided for development and utilization of the antarctic krill oil.
Description
The present application claims priority from the chinese patent office, application number 202110307309.5, entitled "method for enriching and purifying antarctic krill oil phospholipids" filed 23 in 2021, the entire contents of which are incorporated herein by reference.
Technical Field
The invention relates to the technical field of purification, in particular to an enrichment and purification method of euphausia superba oil phosphatide.
Background
The antarctic krill oil is rich in Omega-3 polyunsaturated fatty acids, which are mainly in the form of phospholipids. The phospholipid Omega-3 fatty acid is easier to be utilized by cells than the triglyceride Omega-3 fatty acid, and constructs cell membranes or is combined to the membrane structures of all tissues and organs to be utilized by the tissues and organs, so that EPA and DHA can be better absorbed by human bodies. Thus, phospholipids in antarctic krill oil have unique functional and nutritional characteristics that are different from other marine source lipids.
At present, the phospholipid content of the krill oil in the market is generally about 40-50%, the krill oil is mainly used in the field of foods (common foods and health foods), the krill oil with the phospholipid content of more than 90% is little, and the krill oil with the high-purity phospholipid can also be applied to the field of medicine development, such as the aspect of treating hyperlipidemia, so that the phospholipid in the selectively separated and purified krill oil is particularly important for the development and utilization of the antarctic krill oil.
The purifying technology of the phospholipid mainly adopts column chromatography, acetone deoiling method, membrane filtration method and the like. Column chromatography is more often performed by using silica gel column chromatography; the silica gel has low price, good repeatability of the adsorption separation process and reproducibility, and is the most commonly used adsorbent for purifying phospholipid; however, the common eluent contains chloroform and methanol, has high toxicity, and has the risk of influencing the food safety due to residual solvent. The acetone deoiling method has the problem of acetone residue at the same time, and affects the safety of products. Membrane technology for separating phospholipids is an emerging technology that has been valued in recent decades; although the membrane technology does not use chemical reagents and saves energy, the problems of permeation quantity, membrane life and the like are not better solved, so the industrial development of the membrane technology is limited.
At present, few reports are reported on the separation and purification of krill oil phospholipids. The method has been reported in the literature that the phospholipid in krill oil is separated and purified by adopting a silica gel column chromatography method and chloroform-methanol as an eluent, and the content of the phospholipid is increased to 86% after purification. Chinese patent publication No. CN 109097190A discloses a method for enriching phospholipids from krill oil; the krill oil is used as a purifying material, acetone is firstly used for extraction to obtain an acetone extracting solution and an insoluble substance, the acetone extracting solution also contains a part of phospholipids, the phospholipids in the acetone extracting solution are extracted by using a polar solvent and are combined with the acetone insoluble substance, and the solvent is removed to obtain purified phospholipids, wherein the content of the phospholipids can reach 50-95%.
Although both methods described above can achieve the purpose of phospholipid purification, organic solvents with greater toxicity are used, and the residue of the toxic solvents can pose a great threat to food safety.
Disclosure of Invention
The invention solves the technical problem of providing an enrichment and purification method for the phospholipid of the antarctic krill oil, which can effectively enrich the phospholipid and avoid introducing toxic solvents.
The application also provides an enrichment and purification method of the antarctic krill oil phospholipid, which comprises the following steps:
a) Dissolving antarctic krill oil, and then adsorbing by adopting a pretreated nonpolar macroporous adsorption resin chromatographic column;
b) And A), eluting the chromatographic column obtained in the step A) by adopting ethanol, and evaporating and concentrating the obtained eluent to obtain the antarctic krill oil rich in phospholipids.
Preferably, the pretreated nonpolar macroporous adsorption resin chromatographic column is a pretreated HP-20 macroporous adsorption resin chromatographic column or a pretreated HP-50 macroporous adsorption resin chromatographic column.
Preferably, in step a), the dissolved organic solvent is ethanol.
Preferably, the pretreatment method specifically comprises the following steps:
adding the nonpolar macroporous adsorption resin chromatographic column into absolute ethyl alcohol for soaking, vacuumizing until the air in the nonpolar macroporous adsorption resin is completely extracted, discharging absolute ethyl alcohol completely, and repeating for a plurality of times until the absolute ethyl alcohol is colorless;
soaking the obtained nonpolar macroporous adsorption resin chromatographic column in absolute ethanol for 24h.
Preferably, in the step B), the purity of the ethanol is 95.0-99.9%, and the volume of the ethanol is 4-6 times of that of the chromatographic column obtained in the step A).
Preferably, in the step B), the flow rate of the elution is 3-6 mL/min.
Preferably, in the step A), the content of the phospholipid in the antarctic krill oil is 40-50 wt%, and in the step B), the content of the phospholipid in the antarctic krill oil containing the phospholipid is 90-98 wt%.
The application provides an enrichment and purification method of euphausia superba oil phospholipid, which comprises the steps of dissolving euphausia superba oil, adsorbing by a pretreated nonpolar macroporous adsorption resin chromatographic column, eluting the obtained chromatographic column by ethanol, and evaporating and concentrating the obtained eluent to obtain the euphausia superba oil rich in phospholipid. According to the invention, neutral fat in krill oil is subjected to specific adsorption by utilizing macroporous adsorption resin, so that enrichment of phospholipid in krill oil is realized, and ethanol is used as an eluting solvent without interference of other toxic solvents; furthermore, the macroporous adsorption resin can be recycled, so that the phospholipid can be produced in a large scale, and basic data is provided for development and utilization of the antarctic krill oil.
Detailed Description
For a further understanding of the present invention, preferred embodiments of the invention are described below in conjunction with the examples, but it should be understood that these descriptions are merely intended to illustrate further features and advantages of the invention, and are not limiting of the claims of the invention.
In view of the problem that organic solvents with high toxicity are selected for purifying phospholipids in the krill oil in the prior art, the application utilizes macroporous adsorption resin to specifically adsorb neutral lipids in the krill oil, so that enrichment of phospholipids in the krill oil is realized, meanwhile, ethanol is used as an eluting solvent in the process of separating and purifying the phospholipids, no other toxic solvents interfere, and the macroporous adsorption resin can be reused. Specifically, the embodiment of the invention discloses an enrichment and purification method of euphausia superba oil phospholipid, which comprises the following steps:
a) Dissolving antarctic krill oil, and then adsorbing by adopting a pretreated nonpolar macroporous adsorption resin chromatographic column;
b) And A), eluting the chromatographic column obtained in the step A) by adopting ethanol, and evaporating and concentrating the obtained eluent to obtain the antarctic krill oil rich in phospholipids.
In the process, the antarctic krill oil is firstly dissolved, ethanol is specifically adopted to dissolve the antarctic krill oil in the application, and then the antarctic krill oil is adsorbed by a pretreated nonpolar macroporous adsorption resin chromatographic column; the nonpolar macroporous adsorption resin chromatographic column is specifically an HP-20 macroporous adsorption resin chromatographic column or an HP-50 macroporous adsorption resin chromatographic column, the macroporous adsorption resin is also called as full porous resin and polymer adsorbent, is a macromolecular adsorbent which does not contain ion exchange groups and has a macroporous network structure, belongs to porous crosslinked polymers, and has the effects of separating and enriching organic matters. The macroporous adsorption resin has the characteristics of good selectivity, high mechanical strength, convenient regeneration treatment and high adsorption speed. The HP-20 and HP-50 resins used in the patent are high-porosity styrene macroporous adsorption resins, are divided according to polarity, belong to nonpolar resins, can adsorb nonpolar compounds, are mainly applied to extraction and separation of stevioside, flavone, alkaloid and other components, and have not been reported in the literature for separating and purifying phospholipids. The krill oil mainly comprises phospholipids, triglyceride, sterol, esters, free fatty acid and derivatives thereof; because the polarity of substances such as triglyceride, sterol, esters, free fatty acid and the like is lower, the phospholipid in the antarctic krill oil is separated and purified by adopting the low-polarity adsorption material HP-20 macroporous adsorption resin for removal. The nonpolar macroporous adsorption resin chromatographic column has better adsorption effect after pretreatment, and the specific pretreatment method is as follows:
adding the nonpolar macroporous adsorption resin chromatographic column into absolute ethyl alcohol for soaking, vacuumizing until the air in the nonpolar macroporous adsorption resin is completely extracted, discharging absolute ethyl alcohol completely, and repeating for a plurality of times until the absolute ethyl alcohol is colorless;
soaking the obtained nonpolar macroporous adsorption resin chromatographic column in absolute ethanol for 24h.
The application then uses ethanol to elute the adsorbed chromatographic column, and the obtained eluent is evaporated and concentrated to obtain the antarctic krill oil rich in phospholipids. In the elution process, the purity of the ethanol is 95.0-99.9%, the volume of the ethanol is 4-6 times of the volume of the chromatographic column, and the flow rate of the elution is 3-6 mL/min; in specific embodiments, the purity of the ethanol is 96wt%, 97wt%, 98wt%, or 99wt%, the volume of the ethanol is 4 times, 5 times, or 6 times the volume of the chromatographic column, and the flow rate of the elution is 3mL/min, 4mL/min, 5mL/min, or 6mL/min.
In the application, the content of the phospholipid in the antarctic krill oil is 40-50wt%, and after enrichment and purification, the content of the phospholipid in the antarctic krill oil is 90-98wt%.
The application preferably uses HP-20 or HP-50 macroporous adsorption resin as an adsorption medium and ethanol as an elution solvent to adsorb triglyceride and other low-polarity lipid in the krill oil, so that the phospholipid content in the krill oil is improved to more than 90.0 percent from 40 to 50 percent, and the highest to 96.6 percent, and the selective enrichment of the phospholipid is realized.
In order to further understand the present invention, the following examples are provided to illustrate the enrichment and purification method of antarctic krill oil phospholipids, and the scope of the present invention is not limited by the following examples.
Example 1
About 3g of antarctic krill oil (phospholipid content 48.7%) was dissolved in 6mL of ethanol and added to a pretreated HP-20 macroporous adsorbent resin (about 120 g) chromatography column (27 mm x 400 mm); eluting with 4 times of 96% ethanol at a flow rate of about 3mL/min, collecting eluate, evaporating, concentrating to remove solvent to obtain antarctic krill oil rich in phospholipids; the content of the phospholipid in the obtained krill oil is 93.1 percent through detection.
Example 2
About 3g of antarctic krill oil (phospholipid content 48.7%) was dissolved in 6mL of ethanol and added to a pretreated HP-20 macroporous adsorbent resin (about 120 g) chromatography column (27 mm x 400 mm); eluting with 6 times of 99% ethanol at a flow rate of about 3mL/min, collecting eluate, evaporating, concentrating to remove solvent to obtain antarctic krill oil rich in phospholipids; the content of the phospholipid in the obtained krill oil is 96.6 percent through detection.
Example 3
About 3g of antarctic krill oil (phospholipid content 48.7%) was dissolved in 6mL of ethanol and added to a pretreated HP-20 macroporous adsorbent resin (about 120 g) chromatography column (27 mm x 400 mm); eluting with 6 times of 99% ethanol at a flow rate of about 6mL/min, collecting eluate, evaporating, concentrating to remove solvent to obtain antarctic krill oil rich in phospholipids; through detection, the phospholipid content of the obtained krill oil is 95.2%.
Example 4
About 3g of antarctic krill oil (phospholipid content 48.7%) was dissolved in 6mL of ethanol and added to a pretreated HP-50 macroporous adsorbent resin (about 120 g) chromatography column (27 mm x 400 mm); eluting with 5 times of 98% ethanol at a flow rate of about 3mL/min, collecting eluate, evaporating, concentrating to remove solvent to obtain antarctic krill oil rich in phospholipids; the content of phospholipid in the obtained krill oil is 92.7 percent through detection.
Comparative example 1
About 3g of antarctic krill oil (phospholipid content 48.7%) was dissolved in 6mL of ethanol and added to a pretreated LX-28 methacrylic acid macroporous resin (about 120 g) chromatography column (27 mm. Times.400 mm); eluting with 96% ethanol with volume of 4 times of column at flow rate of about 3mL/min, collecting eluate, evaporating, concentrating, and removing solvent to obtain Euphausia superba oil; the content of phospholipid in the obtained krill oil is 57.7 percent through detection.
Comparative example 2
About 3g of antarctic krill oil (phospholipid content 48.7%) was dissolved in 6mL of ethanol and added to a pretreated HP-20 macroporous adsorbent resin (about 120 g) chromatography column (27 mm x 400 mm); eluting with 6 times of column volume 80% ethanol at a flow rate of about 3mL/min, collecting eluate, evaporating and concentrating to remove solvent to obtain phospholipid-rich antarctic krill oil; the content of the phospholipid in the obtained krill oil is 82.0 percent through detection.
Comparative example 3
About 3g of antarctic krill oil (phospholipid content 48.7%) was dissolved in 6mL of ethanol and added to a pretreated HP-20 macroporous adsorbent resin (about 120 g) chromatography column (27 mm x 400 mm); eluting with 6 times of 99% ethanol at a flow rate of about 20mL/min, collecting eluate, evaporating, concentrating to remove solvent to obtain antarctic krill oil rich in phospholipids; the content of phospholipid in the obtained krill oil is 76.2 percent through detection.
The above description of the embodiments is only for aiding in the understanding of the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (3)
1. The enrichment and purification method of the antarctic krill oil phospholipids comprises the following steps:
a) Dissolving antarctic krill oil, and then adsorbing by adopting a pretreated nonpolar macroporous adsorption resin chromatographic column;
b) Eluting the chromatographic column obtained in the step A) by adopting ethanol, and evaporating and concentrating the obtained eluent to obtain the antarctic krill oil rich in phospholipids;
in the step B), the purity of the ethanol is 95.0-99.9%, and the volume of the ethanol is 4-6 times of that of the chromatographic column obtained in the step A);
in the step B), the flow rate of the elution is 3-6 mL/min;
the pretreatment method specifically comprises the following steps:
adding the nonpolar macroporous adsorption resin chromatographic column into absolute ethyl alcohol for soaking, vacuumizing until the air in the nonpolar macroporous adsorption resin is completely extracted, discharging absolute ethyl alcohol completely, and repeating for a plurality of times until the absolute ethyl alcohol is colorless;
soaking the obtained nonpolar macroporous adsorption resin chromatographic column in absolute ethyl alcohol for 24 hours;
in the step A), the content of the phospholipid in the antarctic krill oil is 40-50 wt%, and the content of the phospholipid in the antarctic krill oil containing the phospholipid in the step B) is 90-98 wt%.
2. The enrichment purification method according to claim 1, wherein the pretreated nonpolar macroporous adsorbent resin chromatographic column is a pretreated HP-20 macroporous adsorbent resin chromatographic column or a pretreated HP-50 macroporous adsorbent resin chromatographic column.
3. The enrichment purification method according to claim 1, wherein in step a), the dissolved organic solvent is ethanol.
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| CN101033236A (en) * | 2007-04-13 | 2007-09-12 | 江南大学 | Method of separating and purifying phosphatidyl choline from phospholipid by resin chromatography method |
| WO2009063500A2 (en) * | 2007-09-19 | 2009-05-22 | V.B.Medicare Pvt. Ltd. | Novel methods of isolation of poly unsaturated fatty acids |
| CN108913352A (en) * | 2018-07-27 | 2018-11-30 | 山东鲁华海洋生物科技有限公司 | Low raw meat krill oil of a kind of de- amine and preparation method thereof |
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| US9556116B2 (en) * | 2015-02-11 | 2017-01-31 | Orochem Technologies, Inc. | Krill oil refinery for purification of krill oil extract |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101033236A (en) * | 2007-04-13 | 2007-09-12 | 江南大学 | Method of separating and purifying phosphatidyl choline from phospholipid by resin chromatography method |
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