Method for preparing glucosamine hydrochloride

Abstract

The invention relates to the technical field of bioengineering, in particular to a method for preparing glucosamine hydrochloride. The method includes: subjecting N-acetylglucosamine fermentation broth to vacuum concentration at the temperature of 50-65 DEG C and vacuum degree of -0.1-0.09MPa to obtain N-acetylglucosamine fermentation broth concentrate; adding the obtained N-acetylglucosamine fermentation broth concentrate into concentrated hydrochloric acid to perform hydrolysis, performing plate and frame filtration after the hydrolysis to obtain crude glucosamine hydrochloride, performing alcohol washing, redissolving and decoloring, and concentrating and crystallizing to obtain refined glucosamine hydrochloride. The method has the advantages that the process directly concentrating the N-acetylglucosamine fermentation broth to perform hydrolysis is used, the production process is simplified, product process loss and influence on product quality are reduced, product yield and quality are increased, and production cost is lowered; the one-step yield of the refined glucosamine hydrochloride reaches above 65%, and the purity of the refined glucosamine hydrochloride is 99-102%.

Description

technical field

[0001] The invention relates to the technical field of bioengineering, in particular to a method for preparing glucosamine hydrochloride. Background technique

[0002] Glucosamine hydrochloride promotes the regeneration of human joint synovial fluid, can improve the metabolism of articular cartilage, has important physiological functions for the human body, and is regarded as a substance that can fundamentally treat bone and joint diseases in the medical field. Used in conjunction with chondroitin sulfate, it has the effect of relieving pain and promoting cartilage regeneration, which can fundamentally improve joint problems.

[0003] Traditional glucosamine hydrochloride is obtained by hydrolysis of shrimp and crab shells, but this process is restricted by factors such as seasonality of raw material harvest, complex hydrolysis process, large amount of acid and alkali, and environmental pollution. Therefore, microbial fermentation is used to produce N- Acety...

Examples

Embodiment 1

[0023] 950ml of N-acetylglucosamine fermentation liquid (N-acetylglucosamine concentration 120.71g / L) was directly vacuum-concentrated at 60°C and a vacuum of -0.095MPa, and concentrated 4 times; the concentrated solution was mixed with 32% concentrated hydrochloric acid at 90 Carry out hydrolysis at ℃ for 2.5 hours, the mass ratio of the amount of hydrochloric acid added to N-acetylglucosamine (120.71g / L*0.95L=114.67g) is 2:1; after hydrolysis is completed, glucosamine hydrochloride is obtained by plate and frame filtration Crude product; mix the crude product with ethanol solution at a mass ratio of 1:2, stir at 50°C for 1 h, and filter through a plate frame to obtain a solid; add distilled water to dissolve back, the mass ratio of the solid to the added distilled water is 1:3, add 0.3 % activated carbon, heated to 80°C and stirred for 1 hour, and filtered through a plate frame; the filtrate was vacuum-concentrated to Baume at 28° at 65°C and a vacuum of -0.095 MPa, cooled ov...

Embodiment 2

[0025] 1000ml of N-acetylglucosamine fermentation liquid (N-acetylglucosamine concentration 118.62g / L) is directly vacuum-concentrated at 65°C and vacuum degree -0.095MPa, and concentrated 5 times; the concentrated solution is mixed with 35% concentrated hydrochloric acid at 90 Perform hydrolysis at ℃ for 3 hours, the mass ratio of the amount of hydrochloric acid added to N-acetylglucosamine (118.62g / L*1L=118.62g) is 3:1; after the hydrolysis is completed, the crude product of glucosamine hydrochloride is obtained by plate and frame filtration; Mix the crude product and ethanol solution, the mass ratio is 1:2.5, stir at 50°C for 1.5h, and filter through a plate frame to obtain a solid; add distilled water to dissolve, the mass ratio of the solid to the added distilled water is 1:3, add 0.35% Activated carbon, heated to 80°C and stirred for 1.5h, filtered through a plate frame; the filtrate was concentrated in vacuum at 60°C, vacuum degree -0.095MPa to Baume degree 28°, cooled o...

Embodiment 3

[0027] 1000ml of N-acetylglucosamine fermentation liquid (N-acetylglucosamine concentration 122.06g / L) is directly vacuum-concentrated at 55°C and vacuum degree -0.095MPa, and concentrated 6 times; the concentrated solution is mixed with 36% concentrated hydrochloric acid at 90 Carry out hydrolysis at ℃ for 3.5 hours, the mass ratio of the amount of hydrochloric acid added to N-acetylglucosamine (122.06g / L*1L=122.06g) is 2.5:1; after the hydrolysis is completed, the crude product of glucosamine hydrochloride is obtained by plate and frame filtration ; Mix the crude product with the ethanol solution, the mass ratio is 1:3, stir at 60°C for 1.5h, and filter through a plate frame to obtain a solid; % activated carbon, heated to 80°C and stirred for 2 hours, and filtered through a plate frame; the filtrate was concentrated in vacuum at 65°C, vacuum degree -0.095MPa to Baume degree 28°, cooled and crystallized overnight, and the crystals were cooled at 60°C, vacuum degree- Dry at 0...

technical field

[0001] The invention relates to the technical field of bioengineering, in particular to a method for preparing glucosamine hydrochloride. Background technique

[0002] Glucosamine hydrochloride promotes the regeneration of human joint synovial fluid, can improve the metabolism of articular cartilage, has important physiological functions for the human body, and is regarded as a substance that can fundamentally treat bone and joint diseases in the medical field. Used in conjunction with chondroitin sulfate, it has the effect of relieving pain and promoting cartilage regeneration, which can fundamentally improve joint problems.

[0003] Traditional glucosamine hydrochloride is obtained by hydrolysis of shrimp and crab shells, but this process is restricted by factors such as seasonality of raw material harvest, complex hydrolysis process, large amount of acid and alkali, and environmental pollution. Therefore, microbial fermentation is used to produce N- Acety...

Examples

Embodiment 1

[0023] 950ml of N-acetylglucosamine fermentation liquid (N-acetylglucosamine concentration 120.71g / L) was directly vacuum-concentrated at 60°C and a vacuum of -0.095MPa, and concentrated 4 times; the concentrated solution was mixed with 32% concentrated hydrochloric acid at 90 Carry out hydrolysis at ℃ for 2.5 hours, the mass ratio of the amount of hydrochloric acid added to N-acetylglucosamine (120.71g / L*0.95L=114.67g) is 2:1; after hydrolysis is completed, glucosamine hydrochloride is obtained by plate and frame filtration Crude product; mix the crude product with ethanol solution at a mass ratio of 1:2, stir at 50°C for 1 h, and filter through a plate frame to obtain a solid; add distilled water to dissolve back, the mass ratio of the solid to the added distilled water is 1:3, add 0.3 % activated carbon, heated to 80°C and stirred for 1 hour, and filtered through a plate frame; the filtrate was vacuum-concentrated to Baume at 28° at 65°C and a vacuum of -0.095 MPa, cooled ov...

Embodiment 2

[0025] 1000ml of N-acetylglucosamine fermentation liquid (N-acetylglucosamine concentration 118.62g / L) is directly vacuum-concentrated at 65°C and vacuum degree -0.095MPa, and concentrated 5 times; the concentrated solution is mixed with 35% concentrated hydrochloric acid at 90 Perform hydrolysis at ℃ for 3 hours, the mass ratio of the amount of hydrochloric acid added to N-acetylglucosamine (118.62g / L*1L=118.62g) is 3:1; after the hydrolysis is completed, the crude product of glucosamine hydrochloride is obtained by plate and frame filtration; Mix the crude product and ethanol solution, the mass ratio is 1:2.5, stir at 50°C for 1.5h, and filter through a plate frame to obtain a solid; add distilled water to dissolve, the mass ratio of the solid to the added distilled water is 1:3, add 0.35% Activated carbon, heated to 80°C and stirred for 1.5h, filtered through a plate frame; the filtrate was concentrated in vacuum at 60°C, vacuum degree -0.095MPa to Baume degree 28°, cooled o...

Embodiment 3

[0027] 1000ml of N-acetylglucosamine fermentation liquid (N-acetylglucosamine concentration 122.06g / L) is directly vacuum-concentrated at 55°C and vacuum degree -0.095MPa, and concentrated 6 times; the concentrated solution is mixed with 36% concentrated hydrochloric acid at 90 Carry out hydrolysis at ℃ for 3.5 hours, the mass ratio of the amount of hydrochloric acid added to N-acetylglucosamine (122.06g / L*1L=122.06g) is 2.5:1; after the hydrolysis is completed, the crude product of glucosamine hydrochloride is obtained by plate and frame filtration ; Mix the crude product with the ethanol solution, the mass ratio is 1:3, stir at 60°C for 1.5h, and filter through a plate frame to obtain a solid; % activated carbon, heated to 80°C and stirred for 2 hours, and filtered through a plate frame; the filtrate was concentrated in vacuum at 65°C, vacuum degree -0.095MPa to Baume degree 28°, cooled and crystallized overnight, and the crystals were cooled at 60°C, vacuum degree- Dry at 0...