CN111100752A - Method for extracting EPA-rich fatty acid from garlic algae - Google Patents
Method for extracting EPA-rich fatty acid from garlic algae Download PDFInfo
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- CN111100752A CN111100752A CN201811265380.6A CN201811265380A CN111100752A CN 111100752 A CN111100752 A CN 111100752A CN 201811265380 A CN201811265380 A CN 201811265380A CN 111100752 A CN111100752 A CN 111100752A
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- fatty acid
- epa
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- purified oil
- algae
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- 235000014113 dietary fatty acids Nutrition 0.000 title claims abstract description 20
- 229930195729 fatty acid Natural products 0.000 title claims abstract description 20
- 239000000194 fatty acid Substances 0.000 title claims abstract description 20
- 150000004665 fatty acids Chemical class 0.000 title claims abstract description 20
- 241000195493 Cryptophyta Species 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 12
- 235000004611 garlic Nutrition 0.000 title claims abstract description 11
- 244000245420 ail Species 0.000 title claims abstract 3
- 238000000605 extraction Methods 0.000 claims abstract description 17
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000000746 purification Methods 0.000 claims abstract description 10
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 8
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 8
- 239000003921 oil Substances 0.000 claims description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 18
- 238000001914 filtration Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 239000010779 crude oil Substances 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 10
- 238000004042 decolorization Methods 0.000 claims description 8
- 238000004332 deodorization Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 6
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000003957 anion exchange resin Substances 0.000 claims description 5
- 239000003729 cation exchange resin Substances 0.000 claims description 5
- 230000018044 dehydration Effects 0.000 claims description 5
- 238000006297 dehydration reaction Methods 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000005342 ion exchange Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 230000001877 deodorizing effect Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 230000009965 odorless effect Effects 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 230000009967 tasteless effect Effects 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 2
- 102000004169 proteins and genes Human genes 0.000 abstract description 2
- 108090000623 proteins and genes Proteins 0.000 abstract description 2
- 235000013619 trace mineral Nutrition 0.000 abstract description 2
- 239000011573 trace mineral Substances 0.000 abstract description 2
- 235000019198 oils Nutrition 0.000 description 21
- 240000002234 Allium sativum Species 0.000 description 8
- 235000021323 fish oil Nutrition 0.000 description 5
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 235000012000 cholesterol Nutrition 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 208000024827 Alzheimer disease Diseases 0.000 description 1
- 201000001320 Atherosclerosis Diseases 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 206010039966 Senile dementia Diseases 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 1
- 239000003403 water pollutant Substances 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- 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
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
-
- 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
Landscapes
- 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)
- Fats And Perfumes (AREA)
Abstract
A method for extracting EPA-rich fatty acid from garlic algae adopts supercritical carbon dioxide for extraction, does not generate chemical reaction in the extraction process, is tasteless, odorless and nontoxic, can be repeatedly utilized in production, saves energy, effectively prevents effective components from being damaged, has no solvent residue after extraction, prevents harmful substances from being generated, and performs secondary purification treatment to effectively and comprehensively remove trace elements, sugar, protein and other impurities to obtain pure EPA fatty acid.
Description
Technical Field
The invention belongs to the technical field of fatty acid oil preparation, and particularly relates to a method for extracting EPA-rich fatty acid from garlic algae.
Background
EPA is an eicosapentaenoic acid-series polyunsaturated fatty acid and contains a special structure of five unsaturated bonds, so that EPA has special effects and influences on human health. EPA has effects of reducing cholesterol, reducing blood lipid, preventing and improving atherosclerosis, and has good curative effect in preventing and treating cardiovascular disease and cerebrovascular disease, diabetes and senile dementia. The deep sea fish oil and algae are main sources of EPA, the EPA extracted from the fish oil has high cholesterol content and fishy smell, the quality of the product is greatly influenced, the EPA composition and content in the fish oil are changed along with different factors such as the variety, the season and the like of fish, and a large amount of water pollutants are accumulated in the fish oil fat, so the fish oil has the defect of instability when being used as a raw material. The search for safe and reliable raw material sources becomes a main development trend for researching EPA, at present, people tend to extract EPA by using microalgae, fungi and the like, and the existing EPA preparation process by microalgae extraction is relatively backward, has low production efficiency and low yield, and cannot efficiently realize large-scale industrial production preparation.
Disclosure of Invention
Aiming at the problems in the prior art, the method for extracting EPA-rich fatty acid from garlic algae adopts supercritical carbon dioxide for extraction, does not generate chemical reaction in the extraction process, is tasteless, odorless and nontoxic, can be repeatedly used in production, saves energy, effectively prevents effective components from being damaged, has no solvent residue in the extract, and prevents harmful substances from being generated.
A method for extracting EPA-rich fatty acid from garlic algae comprises the following steps:
(1) pretreating, namely crushing the algae raw material, adding different acid-base salts for ultrasonic wall breaking, and filtering to obtain filtrate;
(2) fatty acid extraction: extracting the filtrate with supercritical carbon dioxide extraction at 30-50 deg.C for 30-80min under 25-40Mpa with carbon dioxide flow rate of 50-300 ml/min to obtain extract, and separating to obtain crude oil;
(3) primary purification: performing ion exchange treatment on the crude oil through an anion exchange resin column and a cation exchange resin column in sequence to obtain primary purified oil;
(4) secondary purification: carrying out secondary distillation dehydration on the primary purified oil to obtain secondary purified oil;
(5) and (3) decoloring: adding 1 weight percent of activated carbon into the secondary purified oil for decolorization, heating under the protection of nitrogen, stirring, and cooling to room temperature;
(6) deodorizing: removing the active carbon, performing steam stripping deodorization, and cooling to room temperature;
(7) fine filtering: and (4) circularly filtering the deodorized second-stage purified oil by using a filter to obtain a finished product.
A method for extracting EPA-rich fatty acid from garlic algae adopts supercritical carbon dioxide for extraction, does not generate chemical reaction in the extraction process, is tasteless, odorless and nontoxic, can be repeatedly utilized in production, saves energy, effectively prevents effective components from being damaged, has no solvent residue after extraction, prevents harmful substances from being generated, and performs secondary purification treatment to effectively and comprehensively remove trace elements, sugar, protein and other impurities to obtain pure EPA fatty acid.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1: a method for extracting EPA-rich fatty acid from garlic algae comprises the following steps:
(1) pretreating, namely crushing the algae raw material, adding different acid-base salts for ultrasonic wall breaking, and filtering to obtain filtrate;
(2) fatty acid extraction: extracting the filtrate with supercritical carbon dioxide extraction at 30 deg.C for 10min under 25Mpa for 50mL/min to obtain extract, and separating to obtain crude oil;
(3) performing primary purification, namely sequentially passing the crude oil through an anion exchange resin column and a cation exchange resin column to perform ion exchange treatment to obtain primary purified oil;
(4) and (2) performing secondary distillation and dehydration on the primary purified oil to obtain secondary purified oil decolorization, adding activated carbon with the weight percentage of one into the secondary purified oil for decolorization, heating under the protection of nitrogen, stirring, cooling to room temperature for deodorization, removing the activated carbon, performing steam gas stripping deodorization, cooling to room temperature, performing fine filtration, and performing circulating filtration on the deodorized secondary purified oil by using a filter to obtain a finished product.
Example 2: a method for extracting EPA-rich fatty acid from garlic algae comprises the following steps:
(1) pretreating, namely crushing the algae raw material, adding different acid-base salts for ultrasonic wall breaking, and filtering to obtain filtrate;
(2) fatty acid extraction: extracting the filtrate with supercritical carbon dioxide extraction at 40 deg.C for 60min under 30Mpa and carbon dioxide flow of 200 mL/min to obtain extract, and separating to obtain crude oil;
(3) performing primary purification, namely sequentially passing the crude oil through an anion exchange resin column and a cation exchange resin column to perform ion exchange treatment to obtain primary purified oil;
(4) and (2) performing secondary distillation and dehydration on the primary purified oil to obtain secondary purified oil decolorization, adding activated carbon with the weight percentage of one into the secondary purified oil for decolorization, heating under the protection of nitrogen, stirring, cooling to room temperature for deodorization, removing the activated carbon, performing steam gas stripping deodorization, cooling to room temperature, performing fine filtration, and performing circulating filtration on the deodorized secondary purified oil by using a filter to obtain a finished product.
Example 2 enables higher yields of EPA to be obtained than example 1.
Example 3: a method for extracting EPA-rich fatty acid from garlic algae comprises the following steps:
(1) pretreating, namely crushing the algae raw material, adding different acid-base salts for ultrasonic wall breaking, and filtering to obtain filtrate;
(2) fatty acid extraction: extracting the filtrate with supercritical carbon dioxide extraction at 50 deg.C for 80min under 40Mpa at carbon dioxide flow rate of 300 mL/min to obtain extract, and separating to obtain crude oil;
(3) performing primary purification, namely sequentially passing the crude oil through an anion exchange resin column and a cation exchange resin column to perform ion exchange treatment to obtain primary purified oil;
(4) and (2) performing secondary distillation and dehydration on the primary purified oil to obtain secondary purified oil decolorization, adding activated carbon with the weight percentage of one into the secondary purified oil for decolorization, heating under the protection of nitrogen, stirring, cooling to room temperature for deodorization, removing the activated carbon, performing steam gas stripping deodorization, cooling to room temperature, performing fine filtration, and performing circulating filtration on the deodorized secondary purified oil by using a filter to obtain a finished product.
The total amount of fatty acids extracted and the EPA content in the three examples are shown in the table above.
The extraction rate of EPA under different conditions of temperature, pressure, etc. for the three sets of examples is shown in the table above.
The yield of EPA was improved compared to example 1. In contrast, the EPA yields were similar and not much improved in example 3 compared to example 2.
The extraction conditions of example 2 are more suitable for purification of EPA, considering that further increases in temperature, pressure, time and carbon dioxide flow rate for EPA extraction would lead to further increases in cost.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (1)
1. A method for extracting EPA-rich fatty acid from garlic algae is characterized in that: the method comprises the following specific steps:
(1) pretreating, namely crushing the algae raw material, adding different acid-base salts for ultrasonic wall breaking, and filtering to obtain filtrate;
(2) fatty acid extraction: extracting the filtrate with supercritical carbon dioxide extraction at 30-50 deg.C for 10-80min under 25-40Mpa with carbon dioxide flow rate of 50-300 ml/min to obtain extract, and separating to obtain crude oil;
(3) primary purification: performing ion exchange treatment on the crude oil through an anion exchange resin column and a cation exchange resin column in sequence to obtain primary purified oil;
(4) secondary purification: carrying out secondary distillation dehydration on the primary purified oil to obtain secondary purified oil;
(5) and (3) decoloring: adding 1 weight percent of activated carbon into the secondary purified oil for decolorization, heating under the protection of nitrogen, stirring, and cooling to room temperature;
(6) deodorizing: removing the active carbon, performing steam stripping deodorization, and cooling to room temperature;
(7) fine filtering: and (4) circularly filtering the deodorized second-stage purified oil by using a filter to obtain a finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811265380.6A CN111100752A (en) | 2018-10-29 | 2018-10-29 | Method for extracting EPA-rich fatty acid from garlic algae |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811265380.6A CN111100752A (en) | 2018-10-29 | 2018-10-29 | Method for extracting EPA-rich fatty acid from garlic algae |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111100752A true CN111100752A (en) | 2020-05-05 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811265380.6A Pending CN111100752A (en) | 2018-10-29 | 2018-10-29 | Method for extracting EPA-rich fatty acid from garlic algae |
Country Status (1)
| Country | Link |
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| CN (1) | CN111100752A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6087798A (en) * | 1983-10-21 | 1985-05-17 | Meiji Milk Prod Co Ltd | Production of eicosapentaenoic acid by algae |
| CN101260344A (en) * | 2008-04-22 | 2008-09-10 | 天津大学 | Method for producing docosapentaenoic acid and docosahexaenoic acid mixed fatty acid from micro-algae oil |
| CN102618592A (en) * | 2012-04-13 | 2012-08-01 | 暨南大学 | Method for producing EPA (Eicosapentaenoic Acid) by using eustigmatoa cf. polyphem |
| US20150159116A1 (en) * | 2012-05-29 | 2015-06-11 | Roquette Freres | Method for continuously enriching an oil produced by microalgae with ethyl esters of dha |
| CN108004013A (en) * | 2017-12-20 | 2018-05-08 | 海南三元星生物科技股份有限公司 | A kind of method extracted from algae and be rich in DHA aliphatic acid |
-
2018
- 2018-10-29 CN CN201811265380.6A patent/CN111100752A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6087798A (en) * | 1983-10-21 | 1985-05-17 | Meiji Milk Prod Co Ltd | Production of eicosapentaenoic acid by algae |
| CN101260344A (en) * | 2008-04-22 | 2008-09-10 | 天津大学 | Method for producing docosapentaenoic acid and docosahexaenoic acid mixed fatty acid from micro-algae oil |
| CN102618592A (en) * | 2012-04-13 | 2012-08-01 | 暨南大学 | Method for producing EPA (Eicosapentaenoic Acid) by using eustigmatoa cf. polyphem |
| US20150159116A1 (en) * | 2012-05-29 | 2015-06-11 | Roquette Freres | Method for continuously enriching an oil produced by microalgae with ethyl esters of dha |
| CN108004013A (en) * | 2017-12-20 | 2018-05-08 | 海南三元星生物科技股份有限公司 | A kind of method extracted from algae and be rich in DHA aliphatic acid |
Non-Patent Citations (2)
| Title |
|---|
| 刘玉田等: "《藻类食品新工艺与新配方》", 30 June 2002, 山东科学技术出版社 * |
| 张荣灿等: "海藻多不饱和脂肪酸研究进展", 《食品研究与开发》 * |
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Application publication date: 20200505 |
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