CN1034730C - Method of dunaliella collecting and beta-carotene extracting - Google Patents
Method of dunaliella collecting and beta-carotene extracting Download PDFInfo
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- CN1034730C CN1034730C CN92107782A CN92107782A CN1034730C CN 1034730 C CN1034730 C CN 1034730C CN 92107782 A CN92107782 A CN 92107782A CN 92107782 A CN92107782 A CN 92107782A CN 1034730 C CN1034730 C CN 1034730C
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- 238000000034 method Methods 0.000 title claims abstract description 15
- OENHQHLEOONYIE-UKMVMLAPSA-N all-trans beta-carotene Natural products CC=1CCCC(C)(C)C=1/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C OENHQHLEOONYIE-UKMVMLAPSA-N 0.000 title claims abstract description 10
- 239000011648 beta-carotene Substances 0.000 title claims abstract description 10
- 235000013734 beta-carotene Nutrition 0.000 title claims abstract description 10
- TUPZEYHYWIEDIH-WAIFQNFQSA-N beta-carotene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1=C(C)CCCC1(C)C)C=CC=C(/C)C=CC2=CCCCC2(C)C TUPZEYHYWIEDIH-WAIFQNFQSA-N 0.000 title claims abstract description 10
- 229960002747 betacarotene Drugs 0.000 title claims abstract description 10
- OENHQHLEOONYIE-JLTXGRSLSA-N β-Carotene Chemical compound CC=1CCCC(C)(C)C=1\C=C\C(\C)=C\C=C\C(\C)=C\C=C\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C OENHQHLEOONYIE-JLTXGRSLSA-N 0.000 title claims abstract description 10
- 241000195634 Dunaliella Species 0.000 title description 2
- 241000195493 Cryptophyta Species 0.000 claims abstract description 61
- 150000003839 salts Chemical class 0.000 claims abstract description 36
- 238000000605 extraction Methods 0.000 claims abstract description 35
- 239000007788 liquid Substances 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000002360 preparation method Methods 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000004062 sedimentation Methods 0.000 claims abstract description 6
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 17
- 239000003921 oil Substances 0.000 claims description 17
- 235000019198 oils Nutrition 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 14
- 240000008415 Lactuca sativa Species 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 235000012045 salad Nutrition 0.000 claims description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
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- 238000005406 washing Methods 0.000 claims description 3
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 235000010469 Glycine max Nutrition 0.000 claims description 2
- 244000068988 Glycine max Species 0.000 claims description 2
- UPYKUZBSLRQECL-UKMVMLAPSA-N Lycopene Natural products CC(=C/C=C/C=C(C)/C=C/C=C(C)/C=C/C1C(=C)CCCC1(C)C)C=CC=C(/C)C=CC2C(=C)CCCC2(C)C UPYKUZBSLRQECL-UKMVMLAPSA-N 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 150000001746 carotenes Chemical class 0.000 claims description 2
- 235000005473 carotenes Nutrition 0.000 claims description 2
- 235000012343 cottonseed oil Nutrition 0.000 claims description 2
- 239000008157 edible vegetable oil Substances 0.000 claims description 2
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 239000010499 rapseed oil Substances 0.000 claims description 2
- 235000013311 vegetables Nutrition 0.000 claims description 2
- NCYCYZXNIZJOKI-UHFFFAOYSA-N vitamin A aldehyde Natural products O=CC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C NCYCYZXNIZJOKI-UHFFFAOYSA-N 0.000 claims description 2
- 241000206572 Rhodophyta Species 0.000 claims 1
- 235000014666 liquid concentrate Nutrition 0.000 claims 1
- 239000002994 raw material Substances 0.000 claims 1
- 235000015112 vegetable and seed oil Nutrition 0.000 abstract description 2
- 239000008158 vegetable oil Substances 0.000 abstract description 2
- 239000012141 concentrate Substances 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 239000002778 food additive Substances 0.000 abstract 1
- 235000013373 food additive Nutrition 0.000 abstract 1
- 239000012528 membrane Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 description 4
- 239000013543 active substance Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000005189 flocculation Methods 0.000 description 3
- 230000016615 flocculation Effects 0.000 description 3
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- ANVAOWXLWRTKGA-XHGAXZNDSA-N all-trans-alpha-carotene Chemical compound CC=1CCCC(C)(C)C=1/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=CC1C(C)=CCCC1(C)C ANVAOWXLWRTKGA-XHGAXZNDSA-N 0.000 description 2
- 159000000013 aluminium salts Chemical class 0.000 description 2
- 229910000329 aluminium sulfate Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002674 ointment Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 210000002377 thylakoid Anatomy 0.000 description 2
- FPIPGXGPPPQFEQ-UHFFFAOYSA-N 13-cis retinol Natural products OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- FPIPGXGPPPQFEQ-BOOMUCAASA-N Vitamin A Natural products OC/C=C(/C)\C=C\C=C(\C)/C=C/C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-BOOMUCAASA-N 0.000 description 1
- 229930003427 Vitamin E Natural products 0.000 description 1
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 description 1
- 239000011795 alpha-carotene Substances 0.000 description 1
- 235000003903 alpha-carotene Nutrition 0.000 description 1
- ANVAOWXLWRTKGA-HLLMEWEMSA-N alpha-carotene Natural products C(=C\C=C\C=C(/C=C/C=C(\C=C\C=1C(C)(C)CCCC=1C)/C)\C)(\C=C\C=C(/C=C/[C@H]1C(C)=CCCC1(C)C)\C)/C ANVAOWXLWRTKGA-HLLMEWEMSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 210000000038 chest Anatomy 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
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- 239000000049 pigment Substances 0.000 description 1
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- 238000000638 solvent extraction Methods 0.000 description 1
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- 229930003231 vitamin Natural products 0.000 description 1
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- 150000003722 vitamin derivatives Chemical class 0.000 description 1
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Landscapes
- Extraction Or Liquid Replacement (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention relates to a method for collecting salt algae and extracting beta carotene, which is characterized in that salt algae liquid is diluted by water to lower the density of the solution, and salt algae is collected by stagnant sedimentation or centrifugal sedimentation. Obtained salt algae concentrate is further ruptured under expansion by the use of low permeation, and cell liquid is expelled. An obtained algae membrane preparation is suspended in water, and extraction liquid which is extracted by vegetable oil or organic solvent in the state of low permeation is a final product; beta carotene can also be separated out through crystalization by the use of low grade alcohol for sedimentation or concentration. The beta carotene is used for health care and food additives.
Description
The invention belongs to a kind of extracting method of salt algae β-Hu Luobusu.
Before the present invention realizes, add flocculation agent such as molysite, aluminium salt etc. in the salt algae liquid that people normally will gather, make described salt algae flocculation, make the floating collection of salt algae with the air supporting method again, obtain wet algae enriched material, use citric acid complex flocculation agent such as aluminium salt, molysite etc. then.The concentration method complex process of this salt algae, cost is higher.The method of extracting β-Hu Luobusu from the wet algae enriched material of collecting has: (1) directly adopts vegetable oil extraction β-Hu Luobusu wherein, but solid-liquid separation is difficult, and inconvenience preparation crystal; (2) will wet and extract after the algae enriched material drying, but increase drying plant, and easily cause the oxidational losses of β-Hu Luobusu; (3) the algae enriched material washing desalination of will wetting, the dehydration enrichment carries out freezing heat then and melts, make cell rupture discharge enchylema after, use solvent extraction again, melt equipment but increased freezing heat, time-consuming taking a lot of work; (4) in the extraction agent edible oil, add tensio-active agent so that membranolysis helps the extraction of β-Hu Luobusu, but increased cost, and the removal of tensio-active agent is relatively more difficult.
The objective of the invention is to overcome the problem that exists in the prior art, a kind of extracting method of simple and easy effective salt algae β-Hu Luobusu is provided.
The extracting method of salt algae β-Hu Luobusu of the present invention at first be the salt algae liquid of will gather in 1: (algae liquid: ratio water water) dilutes salt algae liquid (degree Beaume 15-28 °) to 1-10, carry out solid-liquid separation with subsider or commercially available whizzer then, obtain wet algae enriched material, algae liquid is concentrated, salinity reduces, smaller volume is in order to further pre-treatment.
With above-mentioned wet algae enriched material in 1: (algae liquid: ratio water) adds water to 1-10, thermal agitation in basin, make that the salt frustule is hypotonic to be burst, examine under a microscope almost all that the thin chests of algae break, discharge enchylema, carry out solid-liquid separation with subsider or whizzer then, obtain the thick film preparation of the cytolemma, thylakoid membrane etc. of salt algae, wash film again with water for several times, further remove water soluble component, gained algae film preparation is a red-purple, for further extraction usefulness.
With described algae film preparation in 1: (algae film preparation: water: ratio extraction agent) adds water and one or more extraction agents to 1-5: 1-10.The effect of water is to keep hypotonic condition makes frustule be in state of rupture, and helps mixing and fully contacting of algae film and extraction agent.Extraction can be carried out in common extractor, and the extraction liquid layer that the upper strata contains β-Hu Luobusu is collected in room temperature or heated and stirred extraction 10-120 minute, and lower floor's algae-residue and aqueous phase layer are abandoned it.
Described extraction agent mainly adopts the good salad oil of low temperature current downflow or other vegetables oil such as soya-bean oil, rape oil, cottonseed wet goods, also can adopt ether, sherwood oil, hexanaphthene, hexane, acetone, dithiocarbonic anhydride or their volatile organic solvents such as mixture.When using salad oil to make extraction agent, the collected salad oil reservoir that contains β-Hu Luobusu is a finished product, it is brown xanchromatic oily liquids, its content beta-carotene is less than 20%, and its composition comprises carotenoid, fat-soluble pigment, liposoluble vitamin (as vitamin A and vitamin-E) and other fat-soluble cpds.When with an organic solvent making extraction agent, after the extraction liquid heating evaporation can being concentrated, add or do not add ethanol or methyl alcohol, 0-10 ℃ leaves standstill and separates out the red-purple crystal, and content beta-carotene is greater than 90%; Also can directly in extraction liquid, add ethanol or methyl alcohol (extraction liquid: ethanol or methyl alcohol=1: 1-10), the β-Hu Luobusu precipitation is separated out, content beta-carotene is greater than 50%, its composition is β-Hu Luobusu stereoisomer mixture and a small amount of alpha-carotene etc., and product is red-purple ointment shape.
Because described salt algae liquid solution proportion through diluting after descends, the salt algae is very easily by sedimentation or centrifuging collection, can make that salt algae thickening equipment is corresponding to dwindle, simplify technology, reduces cost.Salt algae enriched material bursts through water is hypotonic, and after the washing for several times, resulting salt algae film preparation has been removed the enchylema composition, has saved drying or freeze thawing equipment, also needn't add tensio-active agent, helps later extraction and separating technology.Extraction process carries out under hypotonic condition, and extraction is abundant, convenient, solid-liquid separation is simple, can make more than the extraction rate reached to 90% of β-Hu Luobusu in the described salt algae.As≤the 3ppm of products obtained therefrom, Pb≤10ppm.
Embodiment 1: the salt algae is diluted mixing with isopyknic water in basin, separate solid-liquid with commercially available whizzer, obtain wet algae enriched material.Wet algae enriched material is burst with 10 times water is hypotonic, enchylema in the frustule is flowed out, centrifuge dehydration then, make the thylakoid membrane that is rich in β-Hu Luobusu of salt algae and cytolemma etc. be deposited in the bottom, get salt algae film preparation, (algae film: water: ratio sherwood oil) added entry and sherwood oil in 1: 5: 5 with described salt algae film preparation then, the stirring at room extraction is after 30 minutes, carrying out two in extractor is separated, the upper layer of extraction liquid layer adds 2 times of ethanol, carotene is separated out, then can obtain containing the brown xanchromatic ointment shape throw out of β-Hu Luobusu more than 50%.
Embodiment 2: the preparation of described salt algae film preparation such as embodiment 1, (algae film: water: ratio salad oil) added entry and salad oil in 1: 1: 2 then, in extractor, stir and extracted 2 hours, centrifugally then carry out two and be separated, then can obtain containing the pale brown look oily liquids of β-Hu Luobusu more than 1%.
Embodiment 3: salt algae liquid is diluted sedimentation in the rearmounted subsider with 10 times water, obtain wet algae enriched material.Press embodiment 1, water is hypotonic burst, wash after, the algae film preparation.Pack in the extractor, then in 1: 1: 1 (algae film: water: ratio adding sherwood oil sherwood oil), 50 ℃ were stirred after 30 minutes, leave standstill and carry out two and be separated, upper layer of extraction liquid is taken out rearmounted commercially available evaporator evaporation and is concentrated, put then under the 0-10 ℃ of condition and separate out the red-purple crystallization, contain β-Hu Luobusu more than 90%.
Claims (4)
1. the extracting method of salt algae β-Hu Luobusu, it is characterized in that raw material salt algae liquid in 1: 1-10 (salt algae liquid: ratio dilute with water water), reduce the density of solution, method by standing sedimentation or centrifugal settling, reclaim the salt algae, make that algae liquid concentrates, salinity reduces, smaller volume, obtain salt algae enriched material.Water is hypotonic again bursts for described salt algae enriched material, promptly in 1: (salt algae enriched material: ratio water) is mixed salt algae enriched material and water to 1-10, and carry out thermal agitation, the salt frustule is broken, discharge enchylema, after water washing, make red algae film preparation, described algae film preparation need suspend in water to keep the hypotonic state that bursts, extract with common extraction agent, the gained extraction liquid can be used as finished product, and also available lower alcohol is heavy separates out or concentrated post crystallization is separated out β-Hu Luobusu.
2. method according to claim 1, when it is characterized in that the algae film preparation being extracted with extraction agent, needing the water existence makes frustule be in state of rupture to keep hypotonic condition, by 1: 1-5: 1-10 (algae film preparation: water: extraction agent) algae film and water, extraction agent are mixed, extract by room temperature or heating.
3. method according to claim 1, it is characterized in that the extraction agent that uses can be salad oil, soya-bean oil, rape oil, cottonseed wet goods edible vegetable oil, can be organic solvents such as ether, sherwood oil, hexanaphthene, normal hexane, acetone, dithiocarbonic anhydride also, also can be their mixture.
4. method according to claim 1 is characterized in that extraction liquid is the product that contains less than 20% β-Hu Luobusu when using vegetables oil to make extraction agent; When with an organic solvent making extraction agent, can be in 1: (extraction agent: ratio lower alcohol) adds ethanol or methyl alcohol to 1-10, and the β-Hu Luobusu precipitation is separated out, and is the violet oil paste, and content beta-carotene is greater than 50%; Also can be directly with the extraction liquid evaporation concentration, add or do not add ethanol or methyl alcohol, the carotene crystallization is separated out under 0-10 ℃, its content beta-carotene is greater than 90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92107782A CN1034730C (en) | 1992-09-29 | 1992-09-29 | Method of dunaliella collecting and beta-carotene extracting |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92107782A CN1034730C (en) | 1992-09-29 | 1992-09-29 | Method of dunaliella collecting and beta-carotene extracting |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1084848A CN1084848A (en) | 1994-04-06 |
| CN1034730C true CN1034730C (en) | 1997-04-30 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN92107782A Expired - Fee Related CN1034730C (en) | 1992-09-29 | 1992-09-29 | Method of dunaliella collecting and beta-carotene extracting |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| UA67742C2 (en) * | 1997-05-02 | 2004-07-15 | Дсм Іп Ассетс Б.В. | A process for isolation of carotenoid crystals from microbial biomass |
| CN103951600A (en) * | 2014-05-15 | 2014-07-30 | 中盐工程技术研究院有限公司 | Method for extracting beta-carotene from dunaliella salina |
| CN106261059A (en) * | 2015-06-12 | 2017-01-04 | 胡培芹 | A kind of preparation method of salt alga powder |
| CN105017115A (en) * | 2015-06-18 | 2015-11-04 | 中山鼎晟生物科技有限公司 | Ultrasonic extraction method for beta-carotene in Dunaliella salina powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044277A (en) * | 1990-01-25 | 1990-08-01 | 轻工业部制盐工业科学研究所 | The extracting method of carotene and extract in the salt algae |
| JP4095066B2 (en) * | 2002-12-04 | 2008-06-04 | エムコア・コーポレイション | Semiconductor structure of gallium nitride based semiconductor |
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1992
- 1992-09-29 CN CN92107782A patent/CN1034730C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044277A (en) * | 1990-01-25 | 1990-08-01 | 轻工业部制盐工业科学研究所 | The extracting method of carotene and extract in the salt algae |
| JP4095066B2 (en) * | 2002-12-04 | 2008-06-04 | エムコア・コーポレイション | Semiconductor structure of gallium nitride based semiconductor |
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| CN1084848A (en) | 1994-04-06 |
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