A kind of preparation method of glucosamine sulfate double salt

Abstract

The invention relates to glucosamine sulfate compound salt and a preparation method thereof. The X-ray diffraction of the compound salt shows that the compound salt has a strongest peak at the position of 27.080 degrees. The preparation method comprises the following steps: 1, enabling chitin and a basic carbonate solution to have a deacetylation reaction under the condition of microwave heating, and drying to obtain glucosamine; 2, preparing the obtained glucosamine into a glucosamine solution, adding an excessive acid sulfate solution into the glucosamine solution for neutralizing the glucosamine solution, and enabling the glucosamine solution to be sulfated; removing the generated ammonia by using chlorine; adding activated carbon for carrying out a decolorizing reaction, and filtering the reaction product while the product is hot; 3, adding chlorine-containing metal salt into the solution obtained in the step 2, heating for carrying out an ion exchange reaction, and then carrying out a reflux reaction; 4, adding alcohol as a precipitator into the solution obtained after the reactions of the step 3 are finished, filtering to obtain precipitate, and carrying out freeze drying on the precipitate to obtain glucosamine sulfate compound salt concentrate. The preparation method provided by the invention is simple in production technology, low in cost and high in product purity, enables the quality of the product to reach the pharmacopeia standards, and can be used for large-scale production.

Description

technical field [0001] The invention relates to the field of preparation of glucosamine double salt, in particular to a preparation method of glucosamine sulfate double salt. Background technique [0002] At present, the drugs for osteoarthritis are mainly non-steroidal anti-inflammatory drugs (NSAID) and glucosamine sulfate drugs. Compared with NSAID, glucosamine sulfate drugs have better tolerance and lower incidence of adverse reactions. It has Jiangqiang's curative effect and long-lasting drug effect, but due to the strong water absorption of glucosamine sulfate, the drug content is very easy to drop, and the general preparation is unstable. Therefore, most of the existing glucosamine sulfate drugs are double salts. Existing preparation main production method of glucosamine sulfate medicine and defect are as follows: 1. a kind of equilibrium product of glucosamine sulfate hydrochloride and sodium sulfate, wherein the content of sodium chloride is up to about 20%, easily ...

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Problems solved by technology

[0002] At present, the drugs for osteoarthritis are mainly non-steroidal anti-inflammatory drugs (NSAID) and glucosamine sulfate drugs. Compared with NSAID, glucosamine sulfate drugs have better tolerance and lower incidence of adverse reactions. It has Jiangqiang's curative effect and long-lasting drug effect, but because of the strong water absorption of glucosamine sulfate, the drug content is easy to drop, and the general preparation is unstable. Therefore, most of the existing glucosamine sulfate drugs are double salts

Existing preparation main production method of glucosamine sulfate medicine and defect are as follows: 1. a kind of equilibrium product of glucosamine sulfate hydrochloride and sodium sulfate, wherein the content of sodium chloride is up to about 20%, easily causes water sodium to be retained and Adverse reactions such as edema are produced, which seriously affect the health treatment of patients with hypertension, cardiovascular disease and kidney disease. 3. Lin Xiufen, Xiao Ling and Zhang Jianglin used chitin or chitosan as raw materials, used sulfuric acid to degrade and deacetylate, and used a large amount of organic solvents for extraction, which often caused severe corrosion of the reactor in industrial production , organic solvent toxicity residues and greatly increased production costs are not suitable for industrial production. 4. Patent CN101343294 B improves the method of the above researchers, using nanofiltration membranes (150 ~ 450Da) to remove excess sulfuric acid, but this method is harmful to The membrane has high requirements and is easily damaged, which brings inconvenience to the production process and increases the cost, and also cannot meet the needs of production.

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