CN1380342A - 一种褐藻胶寡糖的制造方法 - Google Patents
一种褐藻胶寡糖的制造方法 Download PDFInfo
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- CN1380342A CN1380342A CN 01107952 CN01107952A CN1380342A CN 1380342 A CN1380342 A CN 1380342A CN 01107952 CN01107952 CN 01107952 CN 01107952 A CN01107952 A CN 01107952A CN 1380342 A CN1380342 A CN 1380342A
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- Prior art keywords
- oligosaccharides
- algin
- oxidizing agent
- manufacture method
- aqueous solution
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- 229920001542 oligosaccharide Polymers 0.000 title claims abstract description 23
- 150000002482 oligosaccharides Chemical class 0.000 title claims abstract description 21
- 235000010443 alginic acid Nutrition 0.000 title claims abstract description 16
- 229920000615 alginic acid Polymers 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 5
- 238000005903 acid hydrolysis reaction Methods 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims abstract 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000007800 oxidant agent Substances 0.000 abstract description 7
- 235000010408 potassium alginate Nutrition 0.000 abstract description 3
- 239000000737 potassium alginate Substances 0.000 abstract description 3
- 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 description 3
- 239000005708 Sodium hypochlorite Substances 0.000 abstract description 2
- 239000002253 acid Substances 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 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 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 229940072056 alginate Drugs 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- -1 oligosaccharide calcium salt Chemical class 0.000 description 2
- 108010004131 poly(beta-D-mannuronate) lyase Proteins 0.000 description 2
- 238000002360 preparation method Methods 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
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000036772 blood pressure Effects 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
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 230000007071 enzymatic hydrolysis Effects 0.000 description 1
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000012528 membrane Substances 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
- 239000008363 phosphate buffer Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
- Preparation Of Compounds By Using Micro-Organisms (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。
Description
本发明涉及一种褐藻胶寡糖的制造方法。
褐藻胶无毒，在食品和医药中得到了广泛应用，但由于高分子量褐藻胶不容易被人体消化吸收，如降低其分子量得到相应寡糖，就可以极大地提高其生物利用度，充分发挥其生物学作用。在褐藻胶寡糖的制备与应用方面，有一日本专利(专利号JP05304974)披露了一种采用褐藻胶酶制备褐藻胶寡糖的方法，先在20℃下预培养褐藻胶降解菌，再在25℃下培养24小时，再从中提取褐藻胶酶，然后在40℃下用此酶水解褐藻酸钾，得到寡糖混合物，采用Dowex50w离子交换树脂处理用氢氧化钙中和，并用BioGel P-GDG柱色谱分离后得到寡糖钙盐。该专利将寡糖钙盐应用于降低血压。但用该法制备褐藻胶寡糖所需酶解时间(24小时)长，所用试剂价格高，因而不易商业化。
本发明的目的是提供一种氧化酸水解制备褐藻胶寡糖的方法，用它可大量生产褐藻胶寡糖，能弥补现有技术的上述不足。
一种褐藻胶寡糖的制造方法，包括将褐藻胶水解成寡糖，并分离不同聚合度的寡糖，其特征是所述的水解为在氧化剂存在下的酸水解。
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。
下面通过实施例说明本发明。
将低聚褐藻酸钾(平均分子量10000)配成重量百分浓度为3的水溶液，然后用浓度为2mol/L的盐酸调节至pH4，加入氧化剂进行氧化，使其重量百分浓度为2，在高压反应釜中在105℃进行水解3小时，冷却后用氢氧化钾调节至pH7，经0.45μm膜过滤后，旋转蒸发浓缩，采用Bio-Gel-P6或Superdex30柱进行分离，用0.1mol/L(pH7)磷酸缓冲液进行洗脱，得到聚合度为2-12的寡糖，经Sephadex G10脱盐后，冷冻干燥得到白色粉末即为本发明的寡糖产品。
本实施例中褐藻胶寡糖M和G的比例为2/1至3/1，M和G的聚合度均在2-12之间，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％(按重量)。本实施例中水解在高压釜中进行温度为100-120℃，时间为2-4小时。
Claims (4)
1、一种褐藻胶寡糖的制造方法，包括将褐藻胶水解成寡糖，并分离不同聚合度的寡糖，其特征是所述的水解为在氧化剂存在下的酸水解。
2、如权利要求1所述的制造方法，其特征就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％。
3、如权利要求1所述的制造方法，其特征是所述的分离采用Bio-Gel-P6或Superdex30柱进行分离。
4、如权利要求1所述的的制造方法，其特征是所述的水解在高压釜中进行，温度为100-120℃，时间为2-4小时。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011079525A CN1161368C (zh) | 2001-04-07 | 2001-04-07 | 一种褐藻胶寡糖的制造方法 |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011079525A CN1161368C (zh) | 2001-04-07 | 2001-04-07 | 一种褐藻胶寡糖的制造方法 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1380342A true CN1380342A (zh) | 2002-11-20 |
| CN1161368C CN1161368C (zh) | 2004-08-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011079525A Expired - Fee Related CN1161368C (zh) | 2001-04-07 | 2001-04-07 | 一种褐藻胶寡糖的制造方法 |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2005089776A1 (fr) * | 2004-03-24 | 2005-09-29 | Ocean University Of China | Oligosaccharides d'algine et derives de ceux-ci ainsi que leur fabrication et leur utilisation |
| CN1321139C (zh) * | 2004-11-22 | 2007-06-13 | 青岛明月海藻集团有限公司 | 褐藻胶低聚糖的生产工艺 |
| CN100372542C (zh) * | 2004-04-16 | 2008-03-05 | 中国海洋大学 | 褐藻胶低聚糖作为益生元的应用 |
| CN100508985C (zh) * | 2004-03-24 | 2009-07-08 | 中国海洋大学 | 褐藻胶寡糖及其衍生物及其制备方法和用途 |
| WO2009086685A1 (zh) * | 2007-12-29 | 2009-07-16 | Dalian Yaweite Bioengineering Co., Ltd. | 低分子量海藻酸及其盐、应用、制法及药物组合物、食品 |
| CN100543028C (zh) * | 2006-09-21 | 2009-09-23 | 寻山集团有限公司 | 一种褐藻胶寡糖的制备方法 |
| CN101037456B (zh) * | 2007-04-24 | 2010-05-26 | 宁波大学 | 褐藻胶寡糖的制备方法 |
| CN1920002B (zh) * | 2005-08-22 | 2011-06-08 | 中国海洋大学 | 一种新的弧菌科弧菌属菌株及其应用 |
| CN102391317A (zh) * | 2011-08-05 | 2012-03-28 | 宁夏万胜生物工程有限公司 | 一种从褐藻寡糖发酵液中分离褐藻寡糖的方法 |
| CN117326932A (zh) * | 2023-09-28 | 2024-01-02 | 青岛明月海藻集团有限公司 | 一种氧化海藻酸钠寡糖的制备方法和应用 |
-
2001
- 2001-04-07 CN CNB011079525A patent/CN1161368C/zh not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8835403B2 (en) | 2004-03-24 | 2014-09-16 | Meiyu Geng | Algin oligosaccharides and the derivatives thereof as well as the manufacture and the use of the same |
| EA011417B1 (ru) * | 2004-03-24 | 2009-02-27 | Оушн Юниверсити Оф Чайна | Олигосахаридальгината и его производные, способ получения и применение |
| CN100508985C (zh) * | 2004-03-24 | 2009-07-08 | 中国海洋大学 | 褐藻胶寡糖及其衍生物及其制备方法和用途 |
| US10213456B2 (en) | 2004-03-24 | 2019-02-26 | Ocean University Of China | Alginate oligosaccharides and the derivatives thereof as well as the manufacture and the use of the same |
| WO2005089776A1 (fr) * | 2004-03-24 | 2005-09-29 | Ocean University Of China | Oligosaccharides d'algine et derives de ceux-ci ainsi que leur fabrication et leur utilisation |
| US9493496B2 (en) | 2004-03-24 | 2016-11-15 | Ocean University Of China | Algin oligosaccharides and the derivatives thereof as well as the manufacture and the use of the same |
| CN100372542C (zh) * | 2004-04-16 | 2008-03-05 | 中国海洋大学 | 褐藻胶低聚糖作为益生元的应用 |
| CN1321139C (zh) * | 2004-11-22 | 2007-06-13 | 青岛明月海藻集团有限公司 | 褐藻胶低聚糖的生产工艺 |
| CN1920002B (zh) * | 2005-08-22 | 2011-06-08 | 中国海洋大学 | 一种新的弧菌科弧菌属菌株及其应用 |
| CN100543028C (zh) * | 2006-09-21 | 2009-09-23 | 寻山集团有限公司 | 一种褐藻胶寡糖的制备方法 |
| CN101037456B (zh) * | 2007-04-24 | 2010-05-26 | 宁波大学 | 褐藻胶寡糖的制备方法 |
| WO2009086685A1 (zh) * | 2007-12-29 | 2009-07-16 | Dalian Yaweite Bioengineering Co., Ltd. | 低分子量海藻酸及其盐、应用、制法及药物组合物、食品 |
| CN102391317A (zh) * | 2011-08-05 | 2012-03-28 | 宁夏万胜生物工程有限公司 | 一种从褐藻寡糖发酵液中分离褐藻寡糖的方法 |
| CN117326932A (zh) * | 2023-09-28 | 2024-01-02 | 青岛明月海藻集团有限公司 | 一种氧化海藻酸钠寡糖的制备方法和应用 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1161368C (zh) | 2004-08-11 |
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