CN1067404C - Method for extraction water soluble polyose of spirulina - Google Patents
Method for extraction water soluble polyose of spirulina Download PDFInfo
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- CN1067404C CN1067404C CN97110608A CN97110608A CN1067404C CN 1067404 C CN1067404 C CN 1067404C CN 97110608 A CN97110608 A CN 97110608A CN 97110608 A CN97110608 A CN 97110608A CN 1067404 C CN1067404 C CN 1067404C
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- Prior art keywords
- acid
- extracting
- water
- spirulina
- extracting method
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- 235000016425 Arthrospira platensis Nutrition 0.000 title claims abstract description 25
- 240000002900 Arthrospira platensis Species 0.000 title claims abstract description 25
- 229940082787 spirulina Drugs 0.000 title claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 238000000605 extraction Methods 0.000 title description 4
- 238000000034 method Methods 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 11
- 239000001110 calcium chloride Substances 0.000 claims abstract description 11
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 11
- 239000000284 extract Substances 0.000 claims abstract description 9
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 5
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 238000001556 precipitation Methods 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 150000007524 organic acids Chemical class 0.000 claims description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 3
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 2
- 238000011001 backwashing Methods 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims description 2
- 238000003672 processing method Methods 0.000 claims description 2
- 150000004676 glycans Chemical class 0.000 abstract description 9
- 229920001282 polysaccharide Polymers 0.000 abstract description 9
- 239000005017 polysaccharide Substances 0.000 abstract description 9
- 238000005406 washing Methods 0.000 abstract description 3
- 239000003729 cation exchange resin Substances 0.000 abstract description 2
- 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 abstract 1
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 abstract 1
- 239000003957 anion exchange resin Substances 0.000 abstract 1
- 150000001450 anions Chemical class 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 238000011084 recovery Methods 0.000 description 8
- 238000001914 filtration Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003053 immunization Effects 0.000 description 1
- 238000002649 immunization Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000004223 radioprotective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000003724 spirulina extract Nutrition 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The present invention relates to a method for extracting water soluble spirulina polysaccharide. Calcium chloride is used as an extracting agent, and calcium hypochlorite is used as a precipitating agent. Obtained extract solution is concentrated to obtain a Baume degree of 4 to 5, and then one of the following technological methods is adopted, wherein the first technological method comprises: acid is added for neutralization, and ethanol is added for washing; the second technological method comprises: acid is not added, and ethanol is added for washing for multiple times; the third technological method comprises: the extract solution is directly delivered to an anion and cation exchange resin bed and is finally dried to obtain the neutral water soluble spirulina polysaccharide. The yield reaches 5 to 10%. The method has the characteristics of short extracting time, high yield, convenience, easy operation and obvious economic and social benefit.
Description
The present invention relates to a kind of preparation method's of spirulina extract, particularly a kind of water-soluble spirulina polyose extracting method, prepared water-soluble polysaccharide can be used for making medicine, food, healthcare products and makeup etc.
Spirulina is owing to itself contain multiple to the significant composition of human body, as amino acid, protein, water-soluble polysaccharide and trace element etc., wherein water-soluble polysaccharide and protein are its major ingredient, spirulina has stronger immunization and cytothesis effect, therefore, it is anticancer that it is had, the pharmacologically active characteristics of radioprotective etc., it is reported, train the spirulina of growing in the world and have 35 kinds approximately, from spirulina, extract various effective ingredients and be developed to the medicine of various series, healthcare products, food etc. have become people's research focus, at present, from spirulina, extract the method for water capacity polysaccharide except the warm water soaking extraction method, also retrieving the disclosed number of patent application of China on November 22 nineteen ninety-five " application for a patent for invention communique specification sheets " is the application for a patent for invention of 94105389.x, name is called " extracting method of water-soluble spirulina polyose " this method system and adopts alkali lye to make extractant, with in the organic acid and extract, the extract that obtains with organic solvent deposit at last, this method has advantages such as the recovery rate of raising than existing warm water soaking method, yet, it is longer that this method still exists extraction time, recovery rate is still lower, have only about 1.9%, so the higher weak point of cost.
Purpose of the present invention aims to provide different extractant of a kind of usefulness and precipitation agent, extracts the method for water-soluble polysaccharide from spirulina, and the polysaccharides recovery rate that this method obtained is significantly improved.
The object of the present invention is achieved like this: a kind of extracting method of water-soluble spirulina polyose, adopt the extractant extracting, the organic acid neutralization, the precipitation agent precipitation, it is characterized in that: extracting method comprises that water is carried and extractant extracts two stages, the condition that water is carried is temperature 70-100 ℃, time is 2-6 hour, extractive process adopts calcium chloride to make extractant, Losantin is made precipitation agent, the consumption of calcium chloride is the 0.005%-0.02% of spirulina powder weight (kilogram), the consumption of Losantin is the 40%-50% of concentrated solution weight (kilogram), extractive condition is: temperature 70-100 ℃, time 1-3 hour, the extracting solution of acquisition concentrated the back and handled by one of following processing method: (1) adds acid neutralization back washing with alcohol, or (2) do not add acid, repeatedly wash with ethanol, or (3) extracting solution directly feeds the moon, Zeo-karb finally obtains the neutral water-soluble spirulina polyose.
In the leaching process, the concentrated degree Beaume 4-5 degree that can be controlled in of extracting solution.
Adding in the acid and the acid of indication can be organic acid, as 36% formic acid or acetate etc., also can be mineral acid, as the sulfuric acid of 0.5%-3%, or the hydrochloric acid of 3%-8% etc.
Above-mentioned used extractant and precipitation agent can directly use commercially available calcium chloride and Losantin.
The ethanol consumption of washing usefulness is 2-4 a times of concentrated solution weight (kilogram), can reclaim, to reuse.
The present invention except that having suitability for industrialized production, the raw material of use, the reagent that can form scale advantage nontoxic and free from environmental pollution, still has following characteristics compared with prior art:
1. extraction time is short;
2. recovery rate significantly improves, and reaches 5%-10%.
For a more detailed description below in conjunction with embodiment to the present invention.
Embodiment 1
Get 50 kilograms of spirulina powders, add 650 kilograms in water, place extractor, be heated to 85 ℃, the time is 3 hours, adds 7.5 gram calcium chloride then, and 2 hours postcooling of insulation filter time extracting solution of winning to normal temperature under 85 ℃ temperature condition, and are standby; Filter residue adds 350 kilograms in water again, is heated to 85 ℃, is incubated 2 hours, be cooled to normal temperature, filter extracting solution for the second time, merge extracted twice liquid, be concentrated into degree Beaume 4 degree, add 45% the precipitation Losantin that consumption is about concentrated solution then, left standstill after the stirring 4 hours, produce throw out, filtration back gained filter thing consumption is that the industrial alcohol of 3 times of concentrated solutions repeatedly washs, and makes PH=5, reclaim ethanol, dry sediment gets 4 kilograms of polysaccharides, therefore, recovery rate is 8%.
Embodiment 2
Get 50 kilograms of spirulina powders, add 500 kilograms in water, place extractor, heat temperature raising to 70 ℃ keeps adding after 4 hours 5 gram calcium chloride, continues insulation 2 hours, is cooled to normal temperature, filters time extracting solution of winning, and is standby; Filter residue adds 300 kilograms in water again, is heated to 70 ℃, keeps 1 hour, cold filtration gets extracting solution for the second time, merges extracted twice liquid, is concentrated into degree Beaume 4 degree, the Losantin that adds consumption then and be concentrated solution 40% stirs as precipitation agent, leaves standstill 2 hours, add 2% sulfuric acid again, make the throw out of generation be neutral, then, throw out washs with the industrial alcohol of 2 times of concentrated solutions again, reclaims ethanol, dry sediment, obtain 3 kilograms of water-soluble spirulina polyoses, therefore, its recovery rate is 6%.
Embodiment 3
Get 50 kilograms of spirulina powders, add 750 kilograms in water, place extractor, be heated to 90 ℃, the time is 5 hours, adds 10 gram calcium chloride then, continue to keep 90 ℃ 2 hours, the cold filtration time extracting solution of winning, standby; Filter residue adds 400 kilograms in water again, be heated to 90 ℃ 2 hours, be cooled to the normal temperature after-filtration, get extracting solution for the second time, merge extracted twice liquid, be concentrated into degree Beaume 5 degree, the Losantin that adds consumption then and be concentrated solution 50% is made precipitation agent, stir, left standstill 4 hours, and produced precipitation, add the acetate of content 36% again, make PH=5, the industrial alcohol that three usefulness of throw out priority of filtration gained are equivalent to 3 times of concentrated liquid measures washs, and the final drying throw out obtains 5 kilograms water-soluble spirulina polyose, therefore, recovery rate is 10%.
Embodiment 4
Get 50 kilograms of spirulina powders, add 500 kilograms in water, place extractor, be heated to 75 ℃, 3 hours time, add calcium chloride 2.5 gram then, keeps 75 ℃ 2 hours, be cooled to normal temperature, filter the inferior extracting solution of winning, standby; Filter residue adds 300 kilograms in water again, is heated to 75 ℃, keeps 2 hours, cooled and filtered gets extracting solution for the second time, merges extracted twice liquid, is concentrated into degree Beaume 5 degree, adding consumption then is the precipitation agent Losantin of concentrated solution 50%, stir, left standstill 3 hours, feed the anion-cation exchange resin bed, with the gained drying precipitate, obtain 3 kilograms of water-soluble spirulina polyoses, therefore, recovery rate is 6%.
Claims (5)
1. the extracting method of a water-soluble spirulina polyose, adopt the extractant extracting, the organic acid neutralization, the precipitation agent precipitation, it is characterized in that: extracting method comprises that water is carried and extractant extracts two stages, the condition that water is carried is temperature 70-100 ℃, time is 2-6 hour, extractive process adopts calcium chloride to make extractant, Losantin is made precipitation agent, the consumption of calcium chloride is the 0.005%-0.02% of spirulina powder weight, the consumption of Losantin is the 40%-50% of concentrated solution weight, extractive condition is: temperature 70-100 ℃, time 1-3 hour, the extracting solution of acquisition concentrated the back and handled by one of following processing method: (1) adds acid neutralization back washing with alcohol, or (2) do not add acid, repeatedly wash with ethanol, or (3) extracting solution directly feeds the moon, Zeo-karb finally obtains the neutral water-soluble spirulina polyose.
2. extracting method according to claim 1 is characterized in that adding in the acid and the acid of indication can be formic acid, acetate, also can be sulfuric acid, hydrochloric acid.
3. extracting method according to claim 1 is characterized in that extractant and precipitation agent that leaching process is used, can use commercially available calcium chloride and Losantin respectively.
4. extracting method according to claim 1 is characterized in that the ethanol consumption that adopts conduct to wash usefulness is 2-4 a times of concentrated liquid measure.
5. extracting method according to claim 1 is characterized in that the degree of enrichment of extracting solution can be controlled in degree Beaume 4-5 degree.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97110608A CN1067404C (en) | 1997-05-26 | 1997-05-26 | Method for extraction water soluble polyose of spirulina |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN97110608A CN1067404C (en) | 1997-05-26 | 1997-05-26 | Method for extraction water soluble polyose of spirulina |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1200376A CN1200376A (en) | 1998-12-02 |
| CN1067404C true CN1067404C (en) | 2001-06-20 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN97110608A Expired - Fee Related CN1067404C (en) | 1997-05-26 | 1997-05-26 | Method for extraction water soluble polyose of spirulina |
Country Status (1)
| Country | Link |
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| CN (1) | CN1067404C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| AU2008291589A1 (en) * | 2007-08-30 | 2009-03-05 | Iogen Energy Corporation | Process of removing calcium and obtaining sulfate salts from an aqueous sugar solution |
| CN101168570B (en) * | 2007-11-15 | 2010-05-26 | 暨南大学 | Degradation method of kelp sulfated polysaccharide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6131095A (en) * | 1984-07-24 | 1986-02-13 | Kazutaka Shinohara | Mucilaginous polysaccharide and preparation thereof |
| JPS61167620A (en) * | 1985-01-19 | 1986-07-29 | Toa Nenryo Kogyo Kk | Carcinostatic agent containing polysaccharide |
| US4950749A (en) * | 1989-01-06 | 1990-08-21 | The Standard Oil Company | Recovery of glucan by employing a divalent cation at an alkaline pH |
| CN1112128A (en) * | 1994-05-16 | 1995-11-22 | 华南师范大学 | Method for extracting water-soluble spirulina polyose |
-
1997
- 1997-05-26 CN CN97110608A patent/CN1067404C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6131095A (en) * | 1984-07-24 | 1986-02-13 | Kazutaka Shinohara | Mucilaginous polysaccharide and preparation thereof |
| JPS61167620A (en) * | 1985-01-19 | 1986-07-29 | Toa Nenryo Kogyo Kk | Carcinostatic agent containing polysaccharide |
| US4950749A (en) * | 1989-01-06 | 1990-08-21 | The Standard Oil Company | Recovery of glucan by employing a divalent cation at an alkaline pH |
| CN1112128A (en) * | 1994-05-16 | 1995-11-22 | 华南师范大学 | Method for extracting water-soluble spirulina polyose |
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| Publication number | Publication date |
|---|---|
| CN1200376A (en) | 1998-12-02 |
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