CN1161368C - Production method of phycocolloid oligosaccharide - Google Patents
Production method of phycocolloid oligosaccharide Download PDFInfo
- Publication number
- CN1161368C CN1161368C CNB011079525A CN01107952A CN1161368C CN 1161368 C CN1161368 C CN 1161368C CN B011079525 A CNB011079525 A CN B011079525A CN 01107952 A CN01107952 A CN 01107952A CN 1161368 C CN1161368 C CN 1161368C
- Authority
- CN
- China
- Prior art keywords
- oligosaccharides
- algin
- manufacture method
- oligosaccharide
- oxidizing agent
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 229920001542 oligosaccharide Polymers 0.000 title claims abstract description 26
- 150000002482 oligosaccharides Chemical class 0.000 title claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 235000010443 alginic acid Nutrition 0.000 claims abstract description 20
- 229920000615 alginic acid Polymers 0.000 claims abstract description 20
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000005903 acid hydrolysis reaction Methods 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 9
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- FHVDTGUDJYJELY-UHFFFAOYSA-N 6-{[2-carboxy-4,5-dihydroxy-6-(phosphanyloxy)oxan-3-yl]oxy}-4,5-dihydroxy-3-phosphanyloxane-2-carboxylic acid Chemical compound O1C(C(O)=O)C(P)C(O)C(O)C1OC1C(C(O)=O)OC(OP)C(O)C1O FHVDTGUDJYJELY-UHFFFAOYSA-N 0.000 claims description 2
- 229920000936 Agarose Polymers 0.000 claims description 2
- 229920002307 Dextran Polymers 0.000 claims description 2
- 229940072056 alginate Drugs 0.000 claims description 2
- 229920002401 polyacrylamide Polymers 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 2
- 239000007800 oxidant agent Substances 0.000 abstract 3
- 239000005708 Sodium hypochlorite Substances 0.000 abstract 1
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 235000010408 potassium alginate Nutrition 0.000 abstract 1
- MZYRDLHIWXQJCQ-YZOKENDUSA-L potassium alginate Chemical compound [K+].[K+].O1[C@@H](C([O-])=O)[C@@H](OC)[C@H](O)[C@H](O)[C@@H]1O[C@@H]1[C@@H](C([O-])=O)O[C@@H](O)[C@@H](O)[C@H]1O MZYRDLHIWXQJCQ-YZOKENDUSA-L 0.000 abstract 1
- 239000000737 potassium alginate Substances 0.000 abstract 1
- -1 oligosaccharides calcium salt Chemical class 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 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 description 1
- WFIYPADYPQQLNN-UHFFFAOYSA-N 2-[2-(4-bromopyrazol-1-yl)ethyl]isoindole-1,3-dione Chemical compound C1=C(Br)C=NN1CCN1C(=O)C2=CC=CC=C2C1=O WFIYPADYPQQLNN-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- IAJILQKETJEXLJ-UHFFFAOYSA-N Galacturonsaeure Natural products O=CC(O)C(O)C(O)C(O)C(O)=O IAJILQKETJEXLJ-UHFFFAOYSA-N 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000012505 Superdex™ Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- AEMOLEFTQBMNLQ-UHFFFAOYSA-N beta-D-galactopyranuronic acid Natural products OC1OC(C(O)=O)C(O)C(O)C1O AEMOLEFTQBMNLQ-UHFFFAOYSA-N 0.000 description 1
- 230000031018 biological processes and functions Effects 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000005374 membrane filtration Methods 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
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
一种褐藻胶寡糖的制造方法，包括将褐藻胶分解成寡糖，并分离不同聚合度的寡糖，其特征是所述的分解为在氧化剂存在下的酸水解。所述的氧化剂为过氧化氢或次氯酸钠，其用量为褐藻酸钾水溶液的1-10%。所述的分离采用Bio-Gel-P6或Superdex30柱进行分离。本发明使用的氧化剂和酸的价格低廉，便于大规模生产，并且生产的速度快。A method for producing algin oligosaccharides, comprising decomposing algin into oligosaccharides and separating oligosaccharides with different degrees of polymerization, characterized in that the decomposition is acid hydrolysis in the presence of an oxidizing agent. The oxidizing agent is hydrogen peroxide or sodium hypochlorite, and its consumption is 1-10% of the potassium alginate aqueous solution. The separation is carried out with Bio-Gel-P6 or Superdex30 column. The oxidizing agent and acid used in the invention are cheap, convenient for large-scale production, and the production speed is fast.
Description
The present invention relates to a kind of manufacture method of algin oligosaccharide.
Algin is nontoxic, has obtained widespread use in food and medicine, but because the high molecular algin is not easy to be absorbed by human consumption, as reduces its molecular weight and obtain corresponding oligosaccharides, just can greatly improve its bioavailability, gives full play to its biological action.Preparation and application facet at algin oligosaccharide, there is a Japanese Patent (patent No. JP05304974) to disclose a kind of method that adopts the algin enzyme to prepare algin oligosaccharide, earlier 20 ℃ of pre-down algin degradation bacteria of cultivating, cultivated 24 hours down at 25 ℃ again, therefrom extract the algin enzyme again, following at 40 ℃ then with this enzymic hydrolysis Potassium polyalginate, obtain oligosaccharide mixture, adopt the Dowex50w ion exchange resin treatment to neutralize with calcium hydroxide, and with obtaining the oligosaccharides calcium salt after the separation of BioGel P-GDG column chromatography.This patent is applied to the oligosaccharides calcium salt to bring high blood pressure down.But it is long to be equipped with the required enzymolysis time of algin oligosaccharide (24 hours) with this legal system, agents useful for same price height, thereby be difficult for commercialization.
The purpose of this invention is to provide the method that a kind of oxidizing acid hydrolysis prepares algin oligosaccharide, but with its mass production algin oligosaccharide, can remedy the above-mentioned deficiency of prior art.
A kind of manufacture method of algin oligosaccharide comprises algin is hydrolyzed into oligosaccharides, and separates the oligosaccharides of different polymerization degree, it is characterized in that the described acid hydrolysis that is hydrolyzed in the presence of oxygenant.
The oxygenant that the present invention uses is cheap with acid, is convenient to scale operation, and the speed of producing is fast.
Below by embodiment the present invention is described.
It is 3 the aqueous solution that oligomeric Potassium polyalginate (molecular-weight average 10000) is made into concentration expressed in percentage by weight, be that the hydrochloric acid of 2mol/L is adjusted to pH4 with concentration then, add oxygenant and carry out oxidation, making its concentration expressed in percentage by weight is 2, in autoclave, be hydrolyzed 3 hours at 105 ℃, the cooling back is adjusted to pH7 with potassium hydroxide, behind 0.45 μ m membrane filtration, rotary evaporation concentrates, adopt polyacrylamide gel P6 (Bio-Gel-P6) or dextran to separate with agarose cross linked gel 30 (Superdex30) post, carry out wash-out with 0.1mol/L (pH7) phosphoric acid buffer, obtain the oligosaccharides that the polymerization degree is 2-12, after sephadex G 10 (Superdex G10) desalination, lyophilize obtains white powder and is oligosaccharides product of the present invention.This oligosaccharides has mannuronic acid oligosaccharide (being called for short M) and guluronic acid oligosaccharides (being called for short G), and the part by weight of the two is 2/1 to 3/1.Oxygenant is hydrogen peroxide or inferior hydracid sodium, and its consumption is the 1%-10% (by weight) of alginate aqueous solution.Hydrolysis is carried out in autoclave in the present embodiment, and temperature is 100-120 ℃, and the time is 2-4 hour.
Claims (4)
1, a kind of manufacture method of algin oligosaccharide comprises algin is hydrolyzed into oligosaccharides, and separates the oligosaccharides of different polymerization degree, it is characterized in that the described acid hydrolysis that is hydrolyzed in the presence of oxygenant.
2, manufacture method as claimed in claim 1, its feature is hydrogen peroxide or clorox with regard to described oxygenant, consumption is the 1%-10% of alginate aqueous solution weight.
3, manufacture method as claimed in claim 1 is characterized in that described separation adopts polyacrylamide gel P6 or dextran to separate with agarose cross linked gel 30 posts.
4, manufacture method as claimed in claim 1 is characterized in that described hydrolysis carries out in autoclave, temperature is 100-120 ℃, and the time is 2-4 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011079525A CN1161368C (en) | 2001-04-07 | 2001-04-07 | Production method of phycocolloid oligosaccharide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011079525A CN1161368C (en) | 2001-04-07 | 2001-04-07 | Production method of phycocolloid oligosaccharide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1380342A CN1380342A (en) | 2002-11-20 |
| CN1161368C true CN1161368C (en) | 2004-08-11 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011079525A Expired - Fee Related CN1161368C (en) | 2001-04-07 | 2001-04-07 | Production method of phycocolloid oligosaccharide |
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| CN (1) | CN1161368C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1562050A (en) | 2004-03-24 | 2005-01-12 | 中国海洋大学 | Use of oligose alginate in anti-dementia and anti-diabetes |
| CN100372542C (en) * | 2004-04-16 | 2008-03-05 | 中国海洋大学 | Application of algin oligosaccharides as prebiotics |
| CN1321139C (en) * | 2004-11-22 | 2007-06-13 | 青岛明月海藻集团有限公司 | Production process of algin oligose |
| CN1920002B (en) * | 2005-08-22 | 2011-06-08 | 中国海洋大学 | Novel vibrionaceae vibrio bacterial strain and application thereof |
| CN101037456B (en) * | 2007-04-24 | 2010-05-26 | 宁波大学 | Preparation method of algin oligosaccharide |
| CN101889027B (en) * | 2007-12-29 | 2013-05-01 | 于传兴 | Alginic acid with low molecular weight, its salts, uses, preparative methods, pharmaceutical compositions and foods |
| CN102391317A (en) * | 2011-08-05 | 2012-03-28 | 宁夏万胜生物工程有限公司 | Method for separating alginate-derived oligosaccharides from alginate-derived oligosaccharide fermentation liquor |
-
2001
- 2001-04-07 CN CNB011079525A patent/CN1161368C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1380342A (en) | 2002-11-20 |
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Owner name: QINGDAO OCEAN UNIVERSITY OF CHINA HOLDINGS CO., LT Free format text: FORMER OWNER: QINGDAO OCEANOLOGY UNIV. Effective date: 20130427 |
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Free format text: CORRECT: ADDRESS; FROM: 266003 QINGDAO, SHANDONG PROVINCE TO: 266071 QINGDAO, SHANDONG PROVINCE |
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Effective date of registration: 20130427 Address after: 266071 Hongkong East Road, Laoshan District, Shandong, China, No. 23, No. Patentee after: Qingdao Ocean University of China Holdings Limited Address before: 266003 No. 5 fish Hill Road, Shandong, Qingdao Patentee before: Qingdao Oceanology Univ. |
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Owner name: QINGDAO HAIDA HAITANG BIOTECHNOLOGY CO., LTD. Free format text: FORMER OWNER: QINGDAO OCEAN UNIVERSITY OF CHINA HOLDINGS CO., LTD. Effective date: 20130927 |
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Free format text: CORRECT: ADDRESS; FROM: 266071 QINGDAO, SHANDONG PROVINCE TO: 266061 QINGDAO, SHANDONG PROVINCE |
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Effective date of registration: 20130927 Address after: 1704 room 182-6, Fortune Tower, No. 266061 Haier Road, Laoshan District, Shandong, Qingdao Patentee after: Qingdao haidahai sugar Biotechnology Co. Ltd. Address before: 266071 Hongkong East Road, Laoshan District, Shandong, China, No. 23, No. Patentee before: Qingdao Ocean University of China Holdings Limited |
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| EE01 | Entry into force of recordation of patent licensing contract |
Application publication date: 20021120 Assignee: QINGDAO BZ OLIGO BIOTECH CO., LTD. Assignor: Qingdao haidahai sugar Biotechnology Co. Ltd. Contract record no.: 2014370000031 Denomination of invention: Production method of phycocolloid oligosaccharide Granted publication date: 20040811 License type: Exclusive License Record date: 20140324 |
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