CN104610385A - Refining method of D-glucosamine hydrochloride - Google Patents
Refining method of D-glucosamine hydrochloride Download PDFInfo
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- CN104610385A CN104610385A CN201510025039.3A CN201510025039A CN104610385A CN 104610385 A CN104610385 A CN 104610385A CN 201510025039 A CN201510025039 A CN 201510025039A CN 104610385 A CN104610385 A CN 104610385A
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- glucosamine hydrochloride
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Abstract
The invention discloses a refining method of D-glucosamine hydrochloride, belongs to the technical field of D-glucosamine hydrochloride. The refining method comprises the specific steps as follows: (1), a crude D-glucosamine hydrochloride product is added to water in a mass ratio of 1: (2-6); (2), activated carbon is added to a feed liquid, the mixture is heated, subjected to backflow and filtered, filter residues are washed with water, filtrate and a cleaning solution are combined; (3), a mixed solution is pressed into a clean zone concentration tank and evaporated until solids are precipitated, a mixed solvent accounting for 2-5 times of the volume of the mixed solution is added to the concentration tank, the mixture is stirred uniformly, cooled and left to stand until crystal is precipitated, and the mixed solvent is prepared by mixing ethanol and isopropanol in a volume ratio of 1: (1-5); (4), filtering is performed to obtain the crystal, and the crystal is washed with a 75% mixed solvent aqueous solution and dried to obtain sterile D-glucosamine hydrochloride crystal. The method adopts the mixed solvent to crystallize the D-glucosamine hydrochloride feed liquid, the product yield is increased, and the production cost is reduced.
Description
Technical field
The present invention relates to the preparing technical field of glucosamine hydrochloride.
Background technology
Glucosamine hydrochloride, also known as D-Glucosamine Hydrochloride, chemical formula is C6H14O5NCl, and relative molecular mass is 215.63, is a kind of natural mucopolysaccharide, and containing a large amount of cellulosic, certified products is white crystalline powder, soluble in water, is insoluble to ethanol.
Glucosamine hydrochloride has been widely used at pharmaceutically tool, can be used for treatment rheumatism joint inflammation and gastric ulcer disease; Also can do nutritious subsidy agent for diabetic subject; If with microbiotic with the use of, microbiotic absorption in blood can be impelled, reduce side reaction; Simultaneously also can the growth of anticancer, be the main raw material of synthesizing new anticarcinogen NSC-178248.
Traditional glucosamine hydrochloride crystallization processes uses alcohol crystal, and product yield is low, and crystallization too increases production cost to the recovery of mother liquor after filtering.
Summary of the invention
The technical problem to be solved in the present invention is for above-mentioned the deficiencies in the prior art, provides a kind of process for purification of glucosamine hydrochloride, and production technique is simple, improves product yield, reduces production cost.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of process for purification of glucosamine hydrochloride, comprises the following steps:
(1) by soluble in water for glucosamine hydrochloride crude product, the mass ratio of described crude product and water is 1:2 ~ 6;
(2) add the gac that quality is crude product quality 1.5 ~ 3%, reflux is also filtered, and washes filter residue with water, merging filtrate and washings;
(3) mixed solution press-in clean area concentration tank step (2) obtained, be evaporated to precipitation solid, the mixed solvent that volume is mixeding liquid volume 2 ~ 5 times is added in concentration tank, stir, then cool and leave standstill until there is crystallization, described mixed solvent is that the ethanol of 1:1 ~ 5 and Virahol are mixed by volume ratio;
(4) cross leaching crystallization, and with 75% the crystallization of mixed solvent solution washing, namely obtain aseptic glucosamine hydrochloride crystal after drying.
As preferably, crude product is dissolved in the water of 30 ~ 50 DEG C in (1) by step.
As preferably, described in step (2), the fineness of gac is 20 ~ 60 orders.
As preferably, the return time in step (2) is 20 ~ 60 minutes.
As preferably, with the water washing filter residue of 30 ~ 50 DEG C in step (2).
As preferably, the vaporization temperature in step (3) is 70 ~ 80 DEG C.
As preferably, the churning time in step (3) is 0.5 ~ 1.5 hour.
As preferably, the time of repose in step (3) is 1 ~ 3 hour.
As preferably, the consumption of the mixed solvent aqueous solution described in step (4) is 1 times of crude product quality.
Whole material treating process all completes in closed environment, and sterility, visible foreign matters all meet States Pharmacopoeia specifications.
The beneficial effect adopting technique scheme to produce is: the ethanol that the inventive method use volume ratio is 1:1 ~ 5 and the mixed solvent of Virahol carry out crystallization to glucosamine hydrochloride feed liquid, improve product yield, crystallization remains mother liquor straight run distillation after filtering and reclaims solvent, reduces production cost.
Embodiment
Embodiment 1
Ethanol is used to carry out crystallization to glucosamine hydrochloride feed liquid in the present embodiment.
Be dissolved in by glucosamine hydrochloride crude product in the water of 40 DEG C, the mass ratio of crude product and water is 1:3.Add that quality is crude product quality 3%, fineness is 20 ~ 60 object gacs, reflux 50 minutes, filtered while hot, and with volume be filtrate volume 1 times, water washing filter residue, merging filtrate and the washings of 40 DEG C.By above-mentioned mixed solution press-in clean area concentration tank, be evaporated to precipitation solid in 75 DEG C, in concentration tank, add the ethanol that volume is mixeding liquid volume 4 times, stir 1 hour, then cool, leave standstill 2.5 hours, in process of cooling, have crystal to separate out.Cross leaching crystallization, and be the washing with alcohol crystallization of crude product quality 1 times by quality, after drying, obtain aseptic glucosamine hydrochloride white crystal.Product content is 98.57%, and yield is 50%.
Whole treating process all completes in closed environment, and sterility, visible foreign matters all meet States Pharmacopoeia specifications.
Embodiment 2
Be dissolved in by glucosamine hydrochloride crude product in the water of 50 DEG C, the mass ratio of crude product and water is 1:6.Add that quality is crude product quality 3%, fineness is 20 ~ 60 object gacs, reflux 60 minutes, filtered while hot, and with volume be filtrate volume 1 times, water washing filter residue, merging filtrate and the washings of 50 DEG C.By above-mentioned mixed solution press-in clean area concentration tank, be evaporated to precipitation solid, add the mixed solvent that volume is mixeding liquid volume 5 times in concentration tank in 80 DEG C, mixed solvent is that the ethanol of 1:5 and Virahol are mixed by volume ratio.Stir 1.5 hours, then cool, leave standstill 3 hours, in process of cooling, have crystal to separate out.Cross leaching crystallization, above-mentioned mixed solvent thin up is become massfraction be 75% the aqueous solution, and be the mixed solvent solution washing crystallization of crude product quality 1 times by quality, residual filtrate and washings can reclaim ethanol and Virahol by straight run distillation.Aseptic glucosamine hydrochloride white crystal is obtained after crystallizing and drying.Product content is 98.12%, and yield is 85%, and other test items are qualified.
Whole treating process all completes in closed environment, and sterility, visible foreign matters all meet States Pharmacopoeia specifications.
Embodiment 3
Be dissolved in by glucosamine hydrochloride crude product in the water of 45 DEG C, the mass ratio of crude product and water is 1:4.Add that quality is crude product quality 2%, fineness is 20 ~ 60 object gacs, reflux 40 minutes, filtered while hot, and with volume be filtrate volume 1 times, water washing filter residue, merging filtrate and the washings of 45 DEG C.By above-mentioned mixed solution press-in clean area concentration tank, be evaporated to precipitation solid, add the mixed solvent that volume is mixeding liquid volume 3 times in concentration tank in 76 DEG C, mixed solvent is that the ethanol of 1:4 and Virahol are mixed by volume ratio.Stir 1 hour, then cool, leave standstill 2 hours, in process of cooling, have crystal to separate out.Cross leaching crystallization, above-mentioned mixed solvent thin up is become massfraction be 75% the aqueous solution, and be the mixed solvent solution washing crystallization of crude product quality 1 times by quality, residual filtrate and washings can reclaim ethanol and Virahol by straight run distillation.Aseptic glucosamine hydrochloride white crystal is obtained after crystallizing and drying.Product content is 99.64%, and yield is 90%, and other test items are qualified.
Whole treating process all completes in closed environment, and sterility, visible foreign matters all meet States Pharmacopoeia specifications.
Embodiment 4
Be dissolved in by glucosamine hydrochloride crude product in the water of 40 DEG C, the mass ratio of crude product and water is 1:3.Add that quality is crude product quality 3%, fineness is 20 ~ 60 object gacs, reflux 50 minutes, filtered while hot, and with volume be filtrate volume 1 times, water washing filter residue, merging filtrate and the washings of 40 DEG C.By above-mentioned mixed solution press-in clean area concentration tank, be evaporated to precipitation solid, add the mixed solvent that volume is mixeding liquid volume 4 times in concentration tank in 75 DEG C, mixed solvent is that the ethanol of 1:3 and Virahol are mixed by volume ratio.Stir 1 hour, then cool, leave standstill 2.5 hours, in process of cooling, have crystal to separate out.Cross leaching crystallization, above-mentioned mixed solvent thin up is become massfraction be 75% the aqueous solution, and be the mixed solvent solution washing crystallization of crude product quality 1 times by quality, residual filtrate and washings can reclaim ethanol and Virahol by straight run distillation.Aseptic glucosamine hydrochloride white crystal is obtained after crystallizing and drying.Product content is 99.35%, and yield is 98%, and other test items are qualified.
Whole treating process all completes in closed environment, and sterility, visible foreign matters all meet States Pharmacopoeia specifications.
Embodiment 5
Be dissolved in by glucosamine hydrochloride crude product in the water of 30 DEG C, the mass ratio of crude product and water is 1:2.Add that quality is crude product quality 1.5%, fineness is 20 ~ 60 object gacs, reflux 20 minutes, filtered while hot, and with volume be filtrate volume 1 times, water washing filter residue, merging filtrate and the washings of 30 DEG C.By above-mentioned mixed solution press-in clean area concentration tank, be evaporated to precipitation solid, add the mixed solvent that volume is mixeding liquid volume 2 times in concentration tank in 70 DEG C, mixed solvent is that the ethanol of 1:1 and Virahol are mixed by volume ratio.Stir 0.5 hour, then cool, leave standstill 1 hour, in process of cooling, have crystal to separate out.Cross leaching crystallization, above-mentioned mixed solvent thin up is become massfraction be 75% the aqueous solution, and be the mixed solvent solution washing crystallization of crude product quality 1 times by quality, residual filtrate and washings can reclaim ethanol and Virahol by straight run distillation.Aseptic glucosamine hydrochloride white crystal is obtained after crystallizing and drying.Product content is 99.54%, and yield is 97%, and other test items are qualified.
Whole treating process all completes in closed environment, and sterility, visible foreign matters all meet States Pharmacopoeia specifications.
The inventive method uses mixed solvent to carry out crystallization to glucosamine hydrochloride feed liquid, improves product yield, reduces production cost.
Claims (9)
1. a process for purification for glucosamine hydrochloride, is characterized in that: comprise the following steps:
(1) by soluble in water for glucosamine hydrochloride crude product, the mass ratio of described crude product and water is 1:2 ~ 6;
(2) add the gac that quality is crude product quality 1.5 ~ 3%, reflux is also filtered, and washes filter residue with water, merging filtrate and washings;
(3) mixed solution press-in clean area concentration tank step (2) obtained, be evaporated to precipitation solid, the mixed solvent that volume is mixeding liquid volume 2 ~ 5 times is added in concentration tank, stir, then cool and leave standstill until there is crystallization, described mixed solvent is that the ethanol of 1:1 ~ 5 and Virahol are mixed by volume ratio;
(4) cross leaching crystallization, and with 75% the crystallization of mixed solvent solution washing, namely obtain aseptic glucosamine hydrochloride crystal after drying.
2. the process for purification of a kind of glucosamine hydrochloride according to claim 1, is characterized in that being dissolved in the water of 30 ~ 50 DEG C by crude product in step (1).
3. the process for purification of a kind of glucosamine hydrochloride according to claim 1, is characterized in that the fineness of gac described in step (2) is 20 ~ 60 orders.
4. the process for purification of a kind of glucosamine hydrochloride according to claim 1, is characterized in that the return time in step (2) is 20 ~ 60 minutes.
5. the process for purification of a kind of glucosamine hydrochloride according to claim 1, is characterized in that the water washing filter residue with 30 ~ 50 DEG C in step (2).
6. the process for purification of a kind of glucosamine hydrochloride according to claim 1, is characterized in that the vaporization temperature in step (3) is 70 ~ 80 DEG C.
7. the process for purification of a kind of glucosamine hydrochloride according to claim 1, is characterized in that the churning time in step (3) is 0.5 ~ 1.5 hour.
8. the process for purification of a kind of glucosamine hydrochloride according to claim 1, is characterized in that the time of repose in step (3) is 1 ~ 3 hour.
9. the process for purification of a kind of glucosamine hydrochloride according to claim 1, is characterized in that the consumption of the mixed solvent aqueous solution described in step (4) is 1 times of crude product quality.
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| CN201510025039.3A CN104610385B (en) | 2015-01-19 | 2015-01-19 | A kind of process for purification of aminoglucose hydrochloride |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110028533A (en) * | 2019-04-10 | 2019-07-19 | 浙江中医药大学 | A kind of method and application of the refining amino glucosamine salt hydrochlorate from microbial fermentation solution |
| CN110305176A (en) * | 2019-06-28 | 2019-10-08 | 山东润德生物科技有限公司 | A kind of preparation method improving aminoglucose hydrochloride thermal stability |
| CN112457206A (en) * | 2020-12-12 | 2021-03-09 | 弘健制药(上海)有限公司 | Refining process of meglumine |
| CN118480076A (en) * | 2024-07-16 | 2024-08-13 | 德州汇洋生物科技有限公司 | Method for preparing glucosamine hydrochloride by anti-solvent crystallization |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101012251A (en) * | 2007-01-11 | 2007-08-08 | 庄建华 | Method of preparing aminoglucose composite sulphate |
| CN101628921A (en) * | 2009-07-30 | 2010-01-20 | 扬州日兴生物科技股份有限公司 | Preparation method of plant source D-glucosamine hydrochloride |
| CN102850412A (en) * | 2012-10-12 | 2013-01-02 | 江苏澳新生物工程有限公司 | Preparation method of D-glucosamine sulfate sodium chloride salt |
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2015
- 2015-01-19 CN CN201510025039.3A patent/CN104610385B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101012251A (en) * | 2007-01-11 | 2007-08-08 | 庄建华 | Method of preparing aminoglucose composite sulphate |
| CN101628921A (en) * | 2009-07-30 | 2010-01-20 | 扬州日兴生物科技股份有限公司 | Preparation method of plant source D-glucosamine hydrochloride |
| CN102850412A (en) * | 2012-10-12 | 2013-01-02 | 江苏澳新生物工程有限公司 | Preparation method of D-glucosamine sulfate sodium chloride salt |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110028533A (en) * | 2019-04-10 | 2019-07-19 | 浙江中医药大学 | A kind of method and application of the refining amino glucosamine salt hydrochlorate from microbial fermentation solution |
| CN110305176A (en) * | 2019-06-28 | 2019-10-08 | 山东润德生物科技有限公司 | A kind of preparation method improving aminoglucose hydrochloride thermal stability |
| CN112457206A (en) * | 2020-12-12 | 2021-03-09 | 弘健制药(上海)有限公司 | Refining process of meglumine |
| CN118480076A (en) * | 2024-07-16 | 2024-08-13 | 德州汇洋生物科技有限公司 | Method for preparing glucosamine hydrochloride by anti-solvent crystallization |
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