CN102321124A - Novel preparation method of glucosamine sulfate - Google Patents
Novel preparation method of glucosamine sulfate Download PDFInfo
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- CN102321124A CN102321124A CN201110263694A CN201110263694A CN102321124A CN 102321124 A CN102321124 A CN 102321124A CN 201110263694 A CN201110263694 A CN 201110263694A CN 201110263694 A CN201110263694 A CN 201110263694A CN 102321124 A CN102321124 A CN 102321124A
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- glucosamine
- aqueous solution
- glucosamine sulphate
- glucosamine sulfate
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Abstract
The invention discloses a novel preparation method of glucosamine sulfate, and belongs to the field of monosaccharide preparation methods. The novel preparation method adopts glucosamine hydrochloride as a raw material and comprises the following steps of treating a glucosamine hydrochloride aqueous solution by a strongly basic anion exchange resin to remove chloridions to obtain glucosamine; neutralizing the glucosamine by a sulfuric acid solution to obtain glucosamine sulfate; and drying the glucosamine sulfate to obtain a glucosamine sulfate preparation without sodium chloride. Specifically, the steps comprises 1) treating 1-25% (W/V) of the glucosamine hydrochloride aqueous solution by the pre-washed strongly basic anion exchange resin column to remove chloridions, 2) collecting effluent liquid obtained from the step 1), 3) adding 20-90% (W/W) of a sulfuric acid solution into the effluent liquid to obtain a glucosamine sulfate aqueous solution by neutralization, wherein a pH value of the glucosamine sulfate aqueous solution is in a range of 3.5 to 5.0; and 4) carrying out a freeze drying process on the glucosamine sulfate aqueous solution, or precipitating the glucosamine sulfate aqueous solution by an organic solvent and then carrying out vacuum drying to obtain a glucosamine sulfate preparation without sodium chloride. The novel preparation method has the advantages of simple process, low cost, less three-waste, and no pollution in production.
Description
Technical field
A kind of novel method for preparing Glucosamine Sulphate of the present invention belongs to monose preparation method field.
Background technology
GS is a kind of natural amino monose; Exist in the human body and be that human body is concluded the essential a kind of materials of structure such as tissue and cytolemma; It all has material impact to generating nail, muscle tendon, skin, eyes, synovial fluid, bone, ligament, heart valve and Digestive tract, respiratory system and urinary system being produced mucus secretion, is the specific substrates that in human body, generates glycosaminoglycan and proteoglycan.
GS is to be raw material with the chitin, prepares with hydrochloric acid or sulphuric acid hydrolysis.GS its vitriol commonly used and hydrochloride.Gondola company is just studied Glucosamine Sulphate as far back as the eighties, finds that it is the specifics of treatment osteoarthritis.The research of the pharmacological action and the mechanism of action shows that Glucosamine Sulphate is the necessary important component of synthetic proteins glycan in the human articular cartilage matrix.To the using sulfated GS of osteo-arthritis patient, can replenish stromatin glycan synthetic material, promote proteoglycan synthetic; The pathologic process of blocking-up osteoarthritis, the progress that wards off disease is improved function of joint and alleviating pain; And be free from side effects, can take for a long time.Therefore, the production of Glucosamine Sulphate brings glad tidings for numerous osteoarthritis patients, for they provide a kind of good medicine of curing the disease.
Existing commodity Glucosamine Sulphate is to adopt glucosamine hydrochloride and sodium sulfate equilibrated product; Directly glucosamine hydrochloride and sodium sulfate are mixed; Or drying then soluble in water obtains its double salt earlier; Sodium chloride-containing reaches about 20% in the product, and cardiovascular diseases and nephrotic all should not take.
Summary of the invention
The purpose of this invention is to provide a kind of novel method for preparing Glucosamine Sulphate; A kind of Glucosamine Sulphate preparation of not sodium chloride-containing is provided; Make it to be adapted to especially suffer from simultaneously senile osteoarthritis patient's use of cardiovascular diseases and ephrosis, to avoid existing Glucosamine Sulphate preparation institute sodium chloride-containing issuable negative impact when above-mentioned crowd uses.
The novel method that the present invention prepares Glucosamine Sulphate is: use glucosamine hydrochloride to be raw material; Its aqueous solution is handled to remove its cl ions through strongly basic anion exchange resin; Obtain GS; Again with obtaining Glucosamine Sulphate with GS in the sulfuric acid, dry then this aqueous solution and obtain the not Glucosamine Sulphate preparation of sodium chloride-containing.Its concrete technology is: the glucosamine hydrochloride aqueous solution of 1-25% (W/V) is handled through the strongly basic anion exchange resin post of prewashing removed its cl ions; Collect effluent; And add 20-90% (W/W) sulfuric acid neutralize the Glucosamine Sulphate aqueous solution; The Glucosamine Sulphate pH value of aqueous solution is 3.5～5.0; Then with this Glucosamine Sulphate aqueous solution through lyophilize or dry with the organic solvent deposit final vacuum, obtain the not Glucosamine Sulphate preparation of sodium chloride-containing.
The prewashing step of the strongly basic anion exchange resin that present method adopts is: earlier with this strongly basic anion exchange resin with the salt soak of 5% (W/W) 2 hours; Be washed till neutrality with deionized water; Use the soaking with sodium hydroxide 2 hours of 4% (W/W) again, be washed till neutral subsequent use with deionized water.
Present method technology is simple, and cost is low, and " three wastes " are few, have the advantage of process for cleanly preparing.
Embodiment
Below in conjunction with specific embodiment the present invention is further described.
Embodiment 1
3kg anionite-exchange resin is washed till neutrality with the salt soak of 5% (W/W) 2 hours with deionized water, uses the soaking with sodium hydroxide 2 hours of 4% (W/W) again, is washed till neutrality with deionized water.Glucosamine hydrochloride 50g is dissolved in the 2000ml water; Making it through the strongly basic anion exchange resin post, collect effluent, is 3.5～5.0 with the pH of 50% (W/W) sulfuric acid regulation solution; With this solution lyophilize, obtain the not Glucosamine Sulphate preparation of sodium chloride-containing again.
Embodiment 2
3kg anionite-exchange resin is washed till neutrality with the salt soak of 5% (W/W) 2 hours with deionized water, uses the soaking with sodium hydroxide 2 hours of 4% (W/W) again, is washed till neutrality with deionized water.Glucosamine hydrochloride 100g is dissolved in the 1000ml water, through anion-exchange resin column, collects effluent; PH with 60% (W/W) sulfuric acid regulation solution is 3.5～5.0; In this solution, add acetone again, deposition is spent the night, and filters to obtain throw out; Vacuum-drying obtains the not Glucosamine Sulphate preparation of sodium chloride-containing.
Embodiment 3
3kg anionite-exchange resin is washed till neutrality with the salt soak of 5% (W/W) 2 hours with deionized water, uses the soaking with sodium hydroxide 2 hours of 4% (W/W) again, is washed till neutrality with deionized water.Glucosamine hydrochloride 200g is dissolved in the 1000ml water, through anion-exchange resin column, collects effluent, is 3.5～5.0 with the pH of 50% (W/W) sulfuric acid regulation solution, again with this solution lyophilize, obtains the not Glucosamine Sulphate preparation of sodium chloride-containing.
Claims (4)
1. novel method for preparing Glucosamine Sulphate; It is characterized in that using glucosamine hydrochloride to be raw material; Its aqueous solution is handled to remove its cl ions through strongly basic anion exchange resin; Obtain GS, again with obtaining Glucosamine Sulphate with GS in the sulfuric acid, dry then this aqueous solution obtains the not Glucosamine Sulphate preparation of sodium chloride-containing.
2. a kind of technology for preparing the novel method of Glucosamine Sulphate according to claim 1; It is characterized in that the glucosamine hydrochloride aqueous solution of 1-25% (W/V) is handled its cl ions of removal through the strongly basic anion exchange resin post of prewashing; Collect effluent; And add 20-90% (W/W) sulfuric acid neutralize the Glucosamine Sulphate aqueous solution, the Glucosamine Sulphate pH value of aqueous solution is 3.5～5.0.Then this Glucosamine Sulphate aqueous solution is passed through drying, obtain the not Glucosamine Sulphate preparation of sodium chloride-containing.
3. a kind of technology for preparing the Glucosamine Sulphate novel method according to claim 2, the drying process that it is characterized in that the Glucosamine Sulphate aqueous solution is lyophilize.
4. a kind of technology for preparing the Glucosamine Sulphate novel method according to claim 2, the drying process that it is characterized in that the Glucosamine Sulphate aqueous solution are to add acetone, ethanol or Virahol organic reagent, filter its throw out and vacuum-drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110263694A CN102321124A (en) | 2011-09-07 | 2011-09-07 | Novel preparation method of glucosamine sulfate |
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| CN201110263694A CN102321124A (en) | 2011-09-07 | 2011-09-07 | Novel preparation method of glucosamine sulfate |
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| CN102321124A true CN102321124A (en) | 2012-01-18 |
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| CN201110263694A Pending CN102321124A (en) | 2011-09-07 | 2011-09-07 | Novel preparation method of glucosamine sulfate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710483A (en) * | 2014-09-11 | 2015-06-17 | 迪沙药业集团有限公司 | Preparation method for glucosamine sulfate |
| CN106008614A (en) * | 2016-05-24 | 2016-10-12 | 天津青松华药医药有限公司 | Preparation method of high-purity aminosaccharides |
| CN106967131A (en) * | 2017-05-17 | 2017-07-21 | 山西同达药业有限公司 | A kind of Glucosamine Sulphate product and preparation method thereof |
| CN110193006A (en) * | 2019-05-22 | 2019-09-03 | 四川农业大学 | Aminoglucose hydrochloride Bones and joints intelligent aqueous gel and its preparation method and application |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3683076A (en) * | 1968-10-26 | 1972-08-08 | Luigi Rovati | Pharmaceutically active glucosamine salts useful in the treatment of osteoarthritis and rheumatoid arthritis |
| WO2003053448A1 (en) * | 2001-12-21 | 2003-07-03 | Bioiberica, S.A. | Process for the preparation of glucosamine salts |
| JP2010059090A (en) * | 2008-09-03 | 2010-03-18 | Masao Kikuchi | Method for producing glucosamine derivative |
| CN101830939A (en) * | 2010-05-19 | 2010-09-15 | 王松叶 | Preparation method of high-purity D-glucosamine sulfate |
| CN102167714A (en) * | 2011-03-02 | 2011-08-31 | 中国药科大学 | Quick and efficient method for preparing glucosamine sulfate potassium chloride compound salt |
-
2011
- 2011-09-07 CN CN201110263694A patent/CN102321124A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3683076A (en) * | 1968-10-26 | 1972-08-08 | Luigi Rovati | Pharmaceutically active glucosamine salts useful in the treatment of osteoarthritis and rheumatoid arthritis |
| WO2003053448A1 (en) * | 2001-12-21 | 2003-07-03 | Bioiberica, S.A. | Process for the preparation of glucosamine salts |
| JP2010059090A (en) * | 2008-09-03 | 2010-03-18 | Masao Kikuchi | Method for producing glucosamine derivative |
| CN101830939A (en) * | 2010-05-19 | 2010-09-15 | 王松叶 | Preparation method of high-purity D-glucosamine sulfate |
| CN102167714A (en) * | 2011-03-02 | 2011-08-31 | 中国药科大学 | Quick and efficient method for preparing glucosamine sulfate potassium chloride compound salt |
Non-Patent Citations (1)
| Title |
|---|
| 周培根，等: "氨基葡萄糖硫酸盐的制备及其性质", 《上海水产大学学报》, vol. 11, no. 2, 30 June 2002 (2002-06-30), pages 145 - 148 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710483A (en) * | 2014-09-11 | 2015-06-17 | 迪沙药业集团有限公司 | Preparation method for glucosamine sulfate |
| CN106008614A (en) * | 2016-05-24 | 2016-10-12 | 天津青松华药医药有限公司 | Preparation method of high-purity aminosaccharides |
| CN106967131A (en) * | 2017-05-17 | 2017-07-21 | 山西同达药业有限公司 | A kind of Glucosamine Sulphate product and preparation method thereof |
| CN106967131B (en) * | 2017-05-17 | 2019-10-22 | 山西同达药业有限公司 | A kind of Glucosamine Sulphate product and preparation method thereof |
| CN110193006A (en) * | 2019-05-22 | 2019-09-03 | 四川农业大学 | Aminoglucose hydrochloride Bones and joints intelligent aqueous gel and its preparation method and application |
| CN110193006B (en) * | 2019-05-22 | 2022-11-25 | 四川农业大学 | Glucosamine hydrochloride bone joint intelligent hydrogel and preparation method and application thereof |
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Application publication date: 20120118 |