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Preparation method of chondroitin sulfate

A technology of chondroitin sulfate and cartilage, applied in the biological field, can solve problems such as dehydration, drying, crushing and other operational difficulties, affect product production efficiency, and fail to meet customer requirements, etc., to achieve fine particles, low production costs, and easy dehydration Effect

Active Publication Date: 2011-09-21
江苏麦德森制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Because the chondroitin sulfate solution is relatively viscous, the traditional method is to add alcohol to the chondroitin sulfate solution to precipitate the chondroitin sulfate crystals during alcohol precipitation. During the dehydration and drying process, the organic solvent contained in the crystal is not easy to volatilize due to its large particle shape and hard and dense particle shape, resulting in high solvent residue in the product, ≥ 2%, which affects product quality and cannot meet customer requirements
Secondly, due to the viscous sedimentation and agglomeration, operations such as dehydration, drying, and crushing become difficult and waste energy
An invention patent application submitted by the applicant previously disclosed a method for producing chondroitin sulfate by reverse precipitation. The chondroitin sulfate obtained by precipitation is crisp and loose, easy to dehydrate and dry, does not need to be crushed, and the color of the product is good , the quality is stable, the content of chondroitin sulfate is above 98%, and the residual organic solvent is less than 0.2%, but the precipitation time of this method is long, which affects the production efficiency of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1: prepare chondroitin sulfate according to the following steps

[0020] (1) Alkaline extraction and enzymatic hydrolysis: First, add 100Kg of cartilage raw material to immerse in water, adjust the pH to 8 with alkali, raise the temperature to 55°C, and keep warm for 6 hours; then, add 1Kg2709 alkaline protease, keep the pH at 8, keep warm at 55°C and stir for 8 hours. Heat up to boiling for 12 minutes, filter to obtain 500L of chondroitin sulfate solution;

[0021] (2) Alcohol precipitation: Cool the chondroitin sulfate solution obtained in step (1) to room temperature, add 5Kg sodium chloride to the solution under stirring, so that the solution contains 1% sodium chloride by weight, and then add the solution 1000L of alcohol with a weight concentration of 2 times the volume of more than 90%, let it stand for more than 6 hours, and filter to obtain the chondroitin sulfate precipitate;

[0022] (3) Oxidation: Dissolve the chondroitin sulfate precipitate obta...

Embodiment 2

[0025] Embodiment 2: Prepare chondroitin sulfate according to the following steps

[0026] (1) Alkaline extraction and enzymatic hydrolysis: First, add 100Kg of cartilage raw material to immerse in water, adjust the pH to 8.5 with alkali, raise the temperature to 58°C, and keep it warm for 5 hours; then, add 2Kg of 2709 alkaline protease to keep the pH at 8.5, keep it warm at 58°C and stir for 7 hours hour, be warming up to boiling for 15 minutes, filter to obtain chondroitin sulfate solution 500L;

[0027] (2) Alcohol precipitation: Cool the chondroitin sulfate solution obtained in step (1) to room temperature, and add 13Kg of sodium chloride to the solution under stirring to make the solution contain 2.5% sodium chloride by weight, and then add the solution 1250L of alcohol with a weight concentration of 2.5 times the volume of more than 90%, let it stand for more than 6 hours, and filter to obtain the chondroitin sulfate precipitate;

[0028] (3) Oxidation: Dissolve the ch...

Embodiment 3

[0031] Embodiment 3: prepare chondroitin sulfate according to the following steps

[0032] (1) Alkaline extraction and enzymatic hydrolysis: First, add 100Kg of cartilage raw material and submerge in water, adjust the pH to 9 with alkali, raise the temperature to 60°C, and keep warm for 4 hours; then, add 3Kg2709 alkaline protease, keep the pH at 9, keep warm at 60°C and stir for 6 hours. Heat up to boiling for 18 minutes, filter to obtain 500L of chondroitin sulfate solution;

[0033] (2) Alcohol precipitation: drop the chondroitin sulfate solution obtained in step (1) to room temperature, and add 22Kg of sodium chloride to the solution under stirring to make the solution contain 4% sodium chloride by weight, and then add the solution 1500L of alcohol with a weight concentration of 3 times the volume and a weight concentration of 90% or more, rested for more than 6 hours, and filtered to obtain chondroitin sulfate precipitation;

[0034] (3) Oxidation: Dissolve the chondroit...

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PUM

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Abstract

The invention discloses a preparation method of chondroitin sulfate, which comprises the following steps of: adding water until cartilage is immersed; adjusting the pH value to be 8-9 with alkali and preserving heat at a temperature of 55-60DEG C for 4-6h; adding 2709 alkali protease and stirring for 6-8h, raising the temperature to boiling and filtering to obtain a chondroitin sulfate solution; adding sodium chloride to the chondroitin sulfate solution; adding alcohol of which the volume is 2-3 times of that of the solution, standing for 6h and filtering to obtain chondroitin sulfate precipitate; adding the chondroitin sulfate precipitate into water and dissolving; meanwhile, adding sodium chloride to the water, adjusting the pH value to be 10-12, adding hydrogen peroxide which accounts for 1-3 percent of the weight of the solution, oxidizing for 6h and filtering to obtain filtrate; adjusting the pH value of the chondroitin sulfate filtrate to be 5-6, adding alcohol of which the volume is 4-6 times of filtrate for secondary precipitation to obtain the chondroitin sulfate precipitate; pouring the secondary chondroitin sulfate precipitate into a dehydration tank provided with an emulsifying machine; pumping alcohol of which the volume is 3-5 times that of the chondroitin sulfate precipitate into the dehydration tank; and carrying out suction filtering, collecting the precipitate and drying to obtain a chondroitin sulfate finished product. The chondroitin sulfate obtained by the preparation method disclosed by the invention has the advantages of loose texture, fine particles, easiness of dehydration and drying, low energy consumption, extremely-low residual organic solvent and short production period.

Description

technical field [0001] The invention belongs to the field of biotechnology, and in particular relates to a preparation method of chondroitin sulfate. Background technique [0002] Chondroitin sulfate, English name chondroitin sulfate, is a kind of polymeric acidic mucopolysaccharide made from the cartilage of animals (pigs, cattle, horses, sheep, chickens, sharks, etc.), and its molecular structure is β-D-glucuronic acid It is a polysaccharide chain composed of repeating disaccharide units formed by β1→3 glycosidic bonds with N-acetylgalactosamine. It is a white or slightly yellow powder with strong water absorption, easily soluble in water to form a viscous liquid, insoluble in organic solvents such as alcohol, acetone, ether and chloroform, and its salts are relatively stable to heat. [0003] At present, chondroitin sulfate is usually extracted by alkali-enzymatic hydrolysis, which mainly includes the following steps: [0004] 1) Alkaline extraction and enzymatic hydrol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/08
Inventor 刘榜惠
Owner 江苏麦德森制药有限公司
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