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Preparation method of high-purity aminosaccharides

An amino sugar, high-purity technology, applied in the field of glucosamine sulfate preparation, can solve the problems of high difficulty, low purity of glucosamine sulfate, complicated operation, etc., and achieve the effect of low product cost, high purity and simple process

Inactive Publication Date: 2016-10-12
TIANJIN GREENPINE PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The second is to use anhydrous methanol and sodium metal to prepare a sodium methoxide solution according to the U.S. patent, then add D-glucosamine hydrochloride to the solution, and stir vigorously to complete the reaction. The resulting suspension should be centrifuged quickly to remove oxidation Sodium, then slowly add oleum to the methanol solution containing glucosamine for reaction, then add acetone, wash the precipitate obtained by centrifugation with acetone and ether, and dry to obtain glucosamine sulfate, with a purity of 99% and a yield of 86.4% , the method is as follows: However, the purity of glucosamine sulfate obtained by the first method is not high; while the actual operation of the second method is too complicated and difficult, and needs to be very careful, and the final product may also contain impurities such as sodium sulfite

Method used

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  • Preparation method of high-purity aminosaccharides

Examples

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Embodiment 1

[0034] Dissolve 100 g of glucosamine hydrochloride in 400 mL of purified water to prepare a glucosamine hydrochloride solution with a mass fraction of 25% (W / V) for use. Pack 1500mL of pre-washed D202SC anion exchange resin into the column, rinse the prepared glucosamine hydrochloride solution on the anion exchange resin bed, let the glucosamine hydrochloride solution pass through the anion exchange resin column, rinse with purified water until neutral , Collect a total of 1.3 L of effluent containing free glucosamine.

Embodiment 2

[0036] Pack 400 mL of prewashed 732 type strongly acidic styrene-based cation-exchange resin into a column, and rinse the 1.3 L glucosamine solution obtained in Example 1 on the cation-exchange resin bed to make the glucosamine completely adsorb on the cation-exchange resin bed. After washing the resin bed with purified water to elute impurities, concentrated ammonia water (commercially available, with a concentration of 25%-28%) was used to elute glucosamine. After elution, a total of 1.5 L of a mixed solution of ammonia gas and glucosamine was obtained, which was freeze-dried at a temperature of -50° C. and a pressure of 20 Pa to obtain 70.9 g of glucosamine. Example 3

Embodiment 3

[0037] Dissolve 100 g of glucosamine hydrochloride in 400 mL of purified water to prepare a glucosamine hydrochloride solution with a mass fraction of 25% (W / V) for use. Pack 1300mL prewashed 711-type anion exchange resin into the column, rinse the prepared glucosamine hydrochloride solution on the anion exchange resin bed, make the glucosamine hydrochloride solution pass through the anion exchange resin column, and rinse with purified water until neutralized. 1.2 L of effluent containing free glucosamine was collected.

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Abstract

The invention provides a preparation method of high-purity aminosaccharides. The preparation method comprises the following steps: adding a glucosamine hydrochloride solvent into purified water or a water-containing organic solvent in the stirring state to prepare a glucosamine solution, treating the solution with a prewashed strong base anion exchange resin to remove chlorine ions to obtain a free glucosamine solution, adsorbing the solution through a prewashed strong acid cation exchange resin, eluting with purified water or a water-containing organic solvent to remove other impurities, dissociating amino glucose with ammonia water, eluting to obtain a product-ammonia gas mixed solution, evaporating the ammonia gas and water together, and drying to obtain the high-purity glucosamines. The method has the advantages of simple technique and low product cost, and the used resins can be regenerated and reused.

Description

technical field [0001] The invention relates to a preparation method of high-purity amino sugar compounds, in particular to a preparation of glucosamine sulfate. Background technique [0002] Serious imbalance of proteoglycan metabolism, increased expression of inflammatory factors and α tumor necrosis factor, stimulation of matrix metalloproteinases and nitrogen dioxide synthase, production of prostaglandin E2, etc., will lead to degenerative lesions of bone and articular cartilage, resulting in the destruction of joint structure And progressive regression of sexual function, commonly known as osteoarthritis. Osteoarthritis is a degenerative disease, which is caused by many factors such as aging, obesity, strain, trauma, congenital abnormalities of joints, joint deformities and other factors. Osteoarthritis, degenerative arthritis, senile arthritis, hypertrophic arthritis, etc. Clinical manifestations include slowly developing joint pain, tenderness, stiffness, joint swel...

Claims

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Application Information

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IPC IPC(8): C07H5/06C07H1/00
CPCC07H5/06C07H1/00
Inventor 沈载宽郑林海
Owner TIANJIN GREENPINE PHARMA