CN1587271A - Process for preparing morinda officinalis total oligosaccharide - Google Patents
Process for preparing morinda officinalis total oligosaccharide Download PDFInfo
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- CN1587271A CN1587271A CN 200410050872 CN200410050872A CN1587271A CN 1587271 A CN1587271 A CN 1587271A CN 200410050872 CN200410050872 CN 200410050872 CN 200410050872 A CN200410050872 A CN 200410050872A CN 1587271 A CN1587271 A CN 1587271A
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Abstract
The present invention relates to the technology of extracting oligosaccharide from Chinese medicinal materials, and is the preparation process of total morinda officinalis oligosaccharide. The present invention features that the preparation process includes reflux extraction of coarse morinda officinalis powder with 95 % concentration ethanol solution, reflux extraction of residue with water, precipitation with 80 % concentration ethanol solution, vacuum concentrating supernatant to form extractum, eliminating impurity ywi weak acid, weak alkali and weak acid successively, chromatographic decolorizing with active carbon, vacuum concentration, and freeze drying to obtain white total morinda officinalis oligosaccharide crystal. The said process has high yield, and is simple, low in cost and easy to use in industrial production.
Description
Affiliated technical field:
The present invention relates to technical field of traditional Chinese medicines, relate to from Chinese medicinal materials the method for extracting oligosaccharides, a kind of preparation method of morinda root oligosacchride specifically, the preparation method of the total oligosaccharides of particularly a kind of Root of Medicinal Indian mulberry.
Background technology:
As everyone knows, Root of Medicinal Indian mulberry has higher pharmaceutical use, is one of China's work bright " four Da Nan medicines ".Morinda root oligosacchride (Bajitian oligosaccharide) is to extract, make with extra care the mixture that obtains from the root of Root of Medicinal Indian mulberry.Modern Chinese herbal medicine is learned and be studies show that, morinda root oligosacchride has the spermatogenesis effect of promotion and antidepressant effect, thereby makes having a sudden rise in social status of Root of Medicinal Indian mulberry, and some businessmans do not stint huge fund and this developed research in the industry, but still are in the starting stage at present.About the morinda root oligosacchride extracting method, Chinese Military Medical Science Institute utilizes sephadex column to separate and has obtained the 4-7 oligosaccharides, but content is lower, and sephadex column is more expensive; In addition, this method is had to the monomer of a Root of Medicinal Indian mulberry 4-7 monose, has lost the monomer oligosaccharide that other series has very high pharmaceutical use equally; Especially this method only is in experimental stage, and real industrialization is still difficult.
Summary of the invention:
The present invention's technical problem to be solved by this invention is to improve the extraction yield of morinda root oligosacchride, simplifies extraction process simultaneously, reduces production costs, and is beneficial to suitability for industrialized production.
The technical solution that the present invention solves the problems of the technologies described above is:
The preparation method of the total oligosaccharides of a kind of Root of Medicinal Indian mulberry is a raw material with the Root of Medicinal Indian mulberry root, and technological process is extraction, impurity elimination and refining three steps, and concrete preparation method is as described below:
1) extract: the Root of Medicinal Indian mulberry medicinal material coarse powder is used alcohol reflux earlier, and the residue that discards fat capacitive impurity is the water refluxing extraction again, and the water extract of gained adds ethanol sedimentation, gets supernatant liquid filtering then and is concentrated into flowing soaking paste;
2) resin removal of impurities: the fluid extract of gained is removed alkaline impurities with weakly acidic cation-exchange resin earlier, removes acidic impurities with weak base anion-exchange resin again, uses the removal of impurities of slightly acidic exchange resin at last, must remove OH
-The ionic neutral oligosaccharides aqueous solution;
3) decolorizing and refining: the neutral oligosaccharides aqueous solution that will obtain through step 2 is through decolorizing with activated carbon, vacuum concentration, and lyophilize promptly obtains the white crystals of the total oligosaccharides of Root of Medicinal Indian mulberry.
Because the water liquid-extracting amount of gained is big behind the extracting in water, in order to reduce next step treatment capacity, first important additional technical feature of the present invention is water extract elder generation evaporation concentration to 80% is added ethanol sedimentation again.
Removal of impurities process of the present invention is very crucial, directly the quality of finished product and and yield, therefore the working medium of used weak acid and weak base will be controlled its ratio and select the optimum handling order.Second important additional technical feature of the present invention is that resin removal of impurities process is: remove alkaline impurities with the weakly acidic cation-exchange resin of 3 times of fluid extracts earlier, remove acidic impurities with the weak base anion-exchange resin of 3 times of fluid extracts again, use the removal of impurities of 1/2 times of slightly acidic exchange resin at last.
The 3rd additional technical feature of the present invention is to add 30-40 80% ethanol sedimentation doubly after the Root of Medicinal Indian mulberry aqueous extract evaporation concentration, to improve the yield of fluid extract.
Therefore activated carbon decolorizing is important step of purified, is related to the quality of finished product, and the 4th the additional technical feature of the present invention activated carbon consumption that is to decolour is 10 times of fluid extract.
The total oligose preparing process of Root of Medicinal Indian mulberry of the present invention has following outstanding advantage than prior art:
1) higher yield is arranged, what obtain is the total oligosaccharides of Root of Medicinal Indian mulberry, detects it through flight time mass spectrum and consists of the total oligosaccharides of series that 1-22 left and right sides monose is formed, and yield is about 5% of crude drug; 2) extraction, removal of impurities, process for purification are simple, and the technological process time is short; 3) material is chosen conveniently, can use the different weak acid and weak base resins of producing the different model of family's production to remove impurity; 4) low cost, used industrial media ethanol, weak acid and weak base resin are all more cheap.5) simple to operate, security is higher, and agents useful for same is all fool proof.
Embodiment:
Description of drawings:
Figure of description is the preparation method's of the total oligosaccharides of a Root of Medicinal Indian mulberry of the present invention process flow sheet.
Embodiment:
Example 1:
Because morinda root oligosacchride is water-soluble stronger compound, therefore get meal 500 grams of Root of Medicinal Indian mulberry medicinal material fragmentation, earlier with 3 times 95% alcohol reflux 24 hours, the weeding of grease solubility impurity, use 10 times of hot water refluxing extraction 5 times again, extract the water-soluble substances in the Root of Medicinal Indian mulberry; With the water extract of gained elder generation evaporation concentration to 500 milliliter, 80% ethanol of using 40 times again is as sedimentary working medium, extract the less water-soluble substances of molecular weight in the aqueous solution, macromolecular substance in the precipitation aqueous solution, and then filtration, vacuum concentration be to flowing soaking paste, Root of Medicinal Indian mulberry fluid extract 50 grams; Next carry out the resin removal of impurity, in this process, for fear of the hydrolytic action of weakly alkaline material to morinda root oligosacchride, remove the weakly alkaline material so use 150 gram D152 weakly acidic cation-exchange resins earlier, to avoid interference, remove acidic impurities with fluid extract 150 gram D310R weak base anion-exchange resins again, with 26 gram D152 weakly acidic cation-exchange resin removal of impurities, obtain removing OH at last
-The total oligosaccharides aqueous solution of the neutral Root of Medicinal Indian mulberry of ionic; Will be through the total oligosaccharides aqueous solution of the Root of Medicinal Indian mulberry that said extracted, removal of impurities obtain earlier with 500 gram active carbon column chromatography decolourings, vacuum concentration, lyophilize promptly obtain white crystals 25.5 grams of the total oligosaccharides of Root of Medicinal Indian mulberry again, and yield is 5.1%.
Example 2:
Get meal 500 grams of Root of Medicinal Indian mulberry medicinal material fragmentation, earlier with 2 times 95% alcohol reflux 24 hours, the weeding of grease solubility impurity, use 10 times of hot water refluxing extraction 3 times again, extract the water-soluble substances in the Root of Medicinal Indian mulberry, then with the water extract elder generation evaporation concentration to 500 of gained milliliter, 80% ethanol of using 30 times again is as sedimentary working medium, extract the less water-soluble substances of molecular weight in the aqueous solution, macromolecular substance in the precipitation aqueous solution, and then filtration, vacuum concentration be to flowing soaking paste, Root of Medicinal Indian mulberry fluid extract 45 grams; Next carry out the resin removal of impurity, remove the weakly alkaline material with 135 gram CAD-50 weakly acidic cation-exchange resins earlier, remove acidic impurities with fluid extract 135 gram D380 weak base anion-exchange resins again, with 23 gram CAD-50 weakly acidic cation-exchange resin removal of impurities, obtain removing OH at last
-The total oligosaccharides aqueous solution of the neutral Root of Medicinal Indian mulberry of ionic; Will be through the total oligosaccharides aqueous solution of the Root of Medicinal Indian mulberry that said extracted, removal of impurities obtain earlier with 500 gram active carbon column chromatography decolourings, vacuum concentration, lyophilize promptly obtain white crystals 26.6 grams of the total oligosaccharides of Root of Medicinal Indian mulberry again, and yield is 5.32%.
Example 3:
Get meal 500 grams of Root of Medicinal Indian mulberry medicinal material fragmentation, earlier with 2.5 times 95% alcohol reflux 24 hours, the weeding of grease solubility impurity, use 10 times of hot water refluxing extraction 4 times again, extract the water-soluble substances in the Root of Medicinal Indian mulberry, then with the water extract elder generation evaporation concentration to 500 of gained milliliter, 80% ethanol of using 35 times again is as sedimentary working medium, extract the less water-soluble substances of molecular weight in the aqueous solution, macromolecular substance in the precipitation aqueous solution, and then filtration, vacuum concentration be to flowing soaking paste, Root of Medicinal Indian mulberry fluid extract 47 grams; Next carry out the resin removal of impurity, remove the weakly alkaline material with 140 gram D155 weakly acidic cation-exchange resins earlier, remove acidic impurities with fluid extract 140 gram D382 weak base anion-exchange resins again, with 23 gram D155 weakly acidic cation-exchange resin removal of impurities, obtain removing OH at last
-The total oligosaccharides aqueous solution of ionic neutral Root of Medicinal Indian mulberry; Will be through the total oligosaccharides aqueous solution of the Root of Medicinal Indian mulberry that said extracted, removal of impurities obtain earlier with 500 gram active carbon column chromatography decolourings, vacuum concentration, lyophilize promptly obtain white crystals 24.1 grams of the total oligosaccharides of Root of Medicinal Indian mulberry again, and yield is 4.82%.
Claims (5)
1, the preparation method of the total oligosaccharides of a kind of Root of Medicinal Indian mulberry is characterized in that its preparation process is:
1) extract: the Root of Medicinal Indian mulberry meal is used alcohol reflux earlier, and the residue that discards fat capacitive impurity is the water refluxing extraction again, and the water extract of gained adds ethanol sedimentation, gets supernatant liquid filtering then and is concentrated into flowing soaking paste;
2) resin removal of impurities: the fluid extract of gained is removed alkaline impurities with weakly acidic cation-exchange resin earlier, removes acidic impurities with weak base anion-exchange resin again, uses the removal of impurities of slightly acidic exchange resin at last, must remove OH
-The ionic neutral oligosaccharides aqueous solution;
3) decolorizing and refining: the neutral oligosaccharides aqueous solution that will obtain through step 2 is through decolorizing with activated carbon, vacuum concentration, and lyophilize promptly obtains the white crystals of the total oligosaccharides of Root of Medicinal Indian mulberry.
2, the preparation method of the total oligosaccharides of a kind of Root of Medicinal Indian mulberry according to claim 1 is characterized in that water extract elder generation evaporation concentration to 80% is added ethanol sedimentation again.
3, the preparation method of the total oligosaccharides of a kind of Root of Medicinal Indian mulberry according to claim 1 and 2, the consumption that it is characterized in that the removal of impurities resin is: remove alkaline impurities with the weakly acidic cation-exchange resin of 3 times of fluid extracts earlier, remove acidic impurities with the weak base anion-exchange resin of 3 times of fluid extracts again, use 1/2 times of slightly acidic OH at last
-The ion exchange resin removal of impurities.
4, the preparation method of the total oligosaccharides of a kind of Root of Medicinal Indian mulberry according to claim 3 is characterized in that the Root of Medicinal Indian mulberry aqueous extract adds 30-40 80% ethanol sedimentation doubly.
5, the preparation method of the total oligosaccharides of a kind of Root of Medicinal Indian mulberry according to claim 3, the activated carbon consumption that it is characterized in that decolouring is 10 times of fluid extract.
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| CN 200410050872 CN1253462C (en) | 2004-07-30 | 2004-07-30 | Process for preparing morinda officinalis total oligosaccharide |
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| CN 200410050872 CN1253462C (en) | 2004-07-30 | 2004-07-30 | Process for preparing morinda officinalis total oligosaccharide |
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| CN1253462C CN1253462C (en) | 2006-04-26 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009155757A1 (en) * | 2008-06-26 | 2009-12-30 | 北京同仁堂股份有限公司 | A pharmaceutical composition containing oligosaccharide obtained from morinda root and the procedure thereof |
| CN103665180A (en) * | 2013-11-29 | 2014-03-26 | 郑州大学 | Application of Morindae officinalis oligosaccharide 6 glycan in preparation of myocardial ischemia and reperfusion injury resistance medicines |
| CN105267356A (en) * | 2014-06-27 | 2016-01-27 | 广州万正药业有限公司 | Morinda officinalis oligosaccharides and preparation method therefor |
| CN107056851A (en) * | 2017-06-05 | 2017-08-18 | 广东省微生物研究所（广东省微生物分析检测中心） | A kind of preparation method of the total oligosaccharide of Morinda officinalis |
| CN114163486A (en) * | 2021-12-22 | 2022-03-11 | 云南三七科技有限公司 | Method for preparing oligosaccharide from pseudo-ginseng |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101334390B (en) * | 2008-06-26 | 2011-06-22 | 北京同仁堂股份有限公司 | Determination method for morinda root oligosacchride of morinda root Chinese herb or its extract |
-
2004
- 2004-07-30 CN CN 200410050872 patent/CN1253462C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009155757A1 (en) * | 2008-06-26 | 2009-12-30 | 北京同仁堂股份有限公司 | A pharmaceutical composition containing oligosaccharide obtained from morinda root and the procedure thereof |
| CN103665180A (en) * | 2013-11-29 | 2014-03-26 | 郑州大学 | Application of Morindae officinalis oligosaccharide 6 glycan in preparation of myocardial ischemia and reperfusion injury resistance medicines |
| CN103665180B (en) * | 2013-11-29 | 2017-08-01 | 郑州大学 | A kind of glycan of morinda root oligosacchride 6 prepare resist myocardial ischemia and reperfusion injury medicine in application |
| CN105267356A (en) * | 2014-06-27 | 2016-01-27 | 广州万正药业有限公司 | Morinda officinalis oligosaccharides and preparation method therefor |
| CN105267356B (en) * | 2014-06-27 | 2019-08-20 | 广州万正药业有限公司 | A kind of morinda root oligosacchride and preparation method thereof |
| CN107056851A (en) * | 2017-06-05 | 2017-08-18 | 广东省微生物研究所（广东省微生物分析检测中心） | A kind of preparation method of the total oligosaccharide of Morinda officinalis |
| CN114163486A (en) * | 2021-12-22 | 2022-03-11 | 云南三七科技有限公司 | Method for preparing oligosaccharide from pseudo-ginseng |
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| CN1253462C (en) | 2006-04-26 |
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