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Glucosamine sulfate product and preparation method thereof

A technology of glucosamine sulfate and glucosamine hydrochloride, applied in the preparation of amino sugar and sugar derivatives, chemical instruments and methods, etc., can solve the problems of poor pH control, uneven dispersion, poor solubility, etc., and achieve good physical Morphological, Yield-enhancing, Ease of Crushing

Active Publication Date: 2017-07-21
SHANXI TONGDA PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that D-glucosamine hydrochloride has poor solubility in alcohol solvents, uneven dispersion, poor pH control during neutralization, and in the subsequent treatment process, sodium ions (or potassium ions) and chloride ions are removed by solvent washing. The effect is poor, and the prepared glucosamine sulfate still contains a large amount of metal ions and chloride ions

Method used

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  • Glucosamine sulfate product and preparation method thereof
  • Glucosamine sulfate product and preparation method thereof
  • Glucosamine sulfate product and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Follow the steps below to prepare high-purity glucosamine sulfate

[0042] 1. Soak the strongly basic anion exchange resin with 0.8 hydrochloric acid for 2.5 hours, wash with deionized water until neutral, then soak with 0.8 sodium hydroxide for 2.5 hours, and then wash with deionized water until neutral.

[0043] 2. Configure glucosamine hydrochloride into a 15% aqueous solution, use pre-washed strong basic anion exchange resin to remove chloride ions in the aqueous solution, repeat 2 times, use glucosamine sulfate hydrochloride each time Strongly basic anion exchange resin with light on.

[0044] 3. Wash the anion exchange resin twice, the solvent used is purified water.

[0045] 4. Collect the glucosamine solution, concentrate it with a nanofiltration membrane, the molecular weight cut-off is 100-150D, concentrate it to 10%, add sulfuric acid to react.

[0046] 5. Freeze-drying, first lower the temperature of the product to -20°C, after forming frozen crystals, the...

Embodiment 2

[0048] Follow the steps below to prepare high-purity glucosamine sulfate

[0049] 1. Soak the strongly basic anion exchange resin in 1.2M hydrochloric acid for 1.5 hours, wash it with deionized water until it is neutral, then soak it with 1.2M sodium hydroxide for 1.5 hours, then wash it with deionized water until it is neutral.

[0050] 2. Configure glucosamine hydrochloride into a 20% aqueous solution, use pre-washed strong basic anion exchange resin to remove chloride ions in the aqueous solution, repeat 3 times, use glucosamine sulfate hydrochloride each time Strongly basic anion exchange resin with light on.

[0051] 3. Washing the anion exchange resin for 3 times, the solvent used is 2% ethanol solution.

[0052] 4. Collect the glucosamine solution, use nanofiltration membrane to concentrate, the molecular weight cut off is 100-150D, concentrate to 20%, add sulfuric acid to react.

[0053] 5. Freeze-drying, first lower the temperature of the product to -5°C, after the ...

Embodiment 3

[0055] Follow the steps below to prepare high-purity glucosamine sulfate

[0056] 1. Soak the strongly basic anion exchange resin in 1M hydrochloric acid for 2 hours, wash it with deionized water until it is neutral, then soak it with 1M sodium hydroxide for 2 hours, and then wash it with deionized water until it is neutral.

[0057] 2. Configure glucosamine hydrochloride into a 20% aqueous solution, use pre-washed strong basic anion exchange resin to remove chloride ions in the aqueous solution, repeat 4 times, use glucosamine sulfate hydrochloride each time Strongly basic anion exchange resin with light on.

[0058] 3. Wash the anion exchange resin 4 times, the solvent used is purified water or 10% ethanol solution.

[0059] 4. Collect the glucosamine solution, use nanofiltration membrane to concentrate, the molecular weight cut off is 100-150D, concentrate to 25%, add sulfuric acid to react.

[0060] 5. Freeze-drying, first lower the temperature of the product to -10°C, a...

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Abstract

The invention provides a preparation method of glucosamine sulfate. The preparation method comprises the following steps: collocating glucosamine hydrochloride into an aqueous solution, removing chloride ions in the aqueous solution by using anion exchange resin, washing the anion exchange resin to obtain a glucosamine solution, concentrating, adding sulfuric acid, reacting with the glucosamine solution to obtain a glucosamine sulfate solution, and drying to obtain the glucosamine sulfate. The invention further provides a glucosamine sulfate product prepared by the preparation method. In the glucosamine sulfate product, the purity of the glucosamine sulfate is higher than 98%, the contents of degraded products 2,5-fructosazine and 2,5-deoxyfructosazine is lower than 0.5%, the chlorine ion content is lower than 0.1%, sodium ion content is lower than 0.01%, and the moisture content is lower than 1.0%.

Description

technical field [0001] The invention relates to the field of biopharmaceuticals, in particular to a glucosamine sulfate product and a preparation method thereof. Background technique [0002] Glucosamine is a substance synthesized in the human body, an important component necessary for the synthesis of proteoglycans in the cartilage matrix, an important nutrient for the formation of chondrocytes, and a natural tissue component of healthy articular cartilage. Glucosamine not only controls the health of human bones and joints, but also controls the metabolic balance of articular cartilage synovium. Glucosamine can generate and replenish a large amount of synovial fluid for the human body, thereby continuously lubricating the surface of articular cartilage, reducing wear and tear, and making joints flexible and free. Supplementing a sufficient amount of synovial fluid also provides sufficient material carriers for articular cartilage. By strongly stimulating chondrocytes, glu...

Claims

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Application Information

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IPC IPC(8): C07H5/06C07H1/00
Inventor 陈丽琼
Owner SHANXI TONGDA PHARM CO LTD
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