CN101550170A - Production technology hydrolytically separating glucosamine hydrochloride from mushrooms - Google Patents
Production technology hydrolytically separating glucosamine hydrochloride from mushrooms Download PDFInfo
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- CN101550170A CN101550170A CNA200810088878XA CN200810088878A CN101550170A CN 101550170 A CN101550170 A CN 101550170A CN A200810088878X A CNA200810088878X A CN A200810088878XA CN 200810088878 A CN200810088878 A CN 200810088878A CN 101550170 A CN101550170 A CN 101550170A
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Abstract
The invention discloses a production technology hydrolytically separating glucosamine hydrochloride from mushrooms, in particular to a production technology hydrolytically separating glucosamine hydrochloride from mushrooms, which has the following steps: dry mushrooms are sequentially hydrolyzed by hydrochloric acid, filtered, absorbed by resin, concentrated by vacuum, microfiltered, crystallized and centrifugated, and then are dried to obtain the glucosamine hydrochloride.
Description
Technical field
Present method belongs to the natural product extraction method, particularly a kind of from mushroom the production technique of hydrolytically separating glucosamine hydrochloride.
Background technology
D-glucosamine hydrochloride (D-Glucosamine Hydrochloride) has another name called Portugal's amine sugar hydrochloride, formal name used at school is 2-amino-2-deoxy-D-glucose hydrochloride, and molecular formula is: C6H13NO5HCl, molecular weight 215.63, CAS number: 66-84-2, structural formula is:
The raw material that is rich in chitin or chitosan can be made into the D-glucosamine hydrochloride through hydrochloric acid hydrolysis.The D-glucosamine hydrochloride is the white granular crystal, and is very easily water-soluble, is insoluble to ethanol.The D-glucosamine hydrochloride is widely used in medicine and synthesizes, and useful as antibacterial infects and immunological adjuvant, is the activator of human body resisiting influenza virus.Can promote the synthetic of chondrocyte's protein-polysaccharide, improve knuckle synovia viscosity, improve the joint cartilage metabolism, effectively treat rheumatic arthritis.The D-glucosamine hydrochloride is the main raw material of synthetic cancer therapy drug NSC-178248, still the additive of up-to-date third generation nourishing function food.
Chitin and chitosan are to pass through 1 by N-ethanoyl glucose, the linear polysaccharide polymkeric substance that the 4-glycosidic link is formed by connecting, and the whole world year biosynthesizing amount is prevalent in the shell of Crustacean, insect, mollusk and microorganism up to 10,000,000,000 tons.This technology with the glucosamine polymer in mushroom or mushroom root or the broken mushroom as raw material sources.
Glucosamine hydrochloride and series derivates thereof are a kind of biotechnological formulations, have the important physical meaning in human body: participate in the detoxifcation of liver kidney, have anti-inflammatory, protect effect such as liver; Can be used for treating rheumatic arthritis and gastric ulcer,, can promote the absorption of microbiotic in blood, reduce side effect if use with the microbiotic compatibility; Growth that also can anticancer simultaneously.In foodstuffs industry, glucosamine hydrochloride and series derivates thereof are a kind of micro-carbohydrate content that add in the infant formulas Ruzhong, are again synthetic VB
6Starting raw material with the riboflavin intermediate.Glucosamine hydrochloride and series derivates thereof also can be applicable in makeup and the fodder additives.Along with the develop rapidly of medical science and biochemical industry, glucosamine hydrochloride and series derivates thereof demand at home and abroad increases just day by day.
Industrial production glucosamine hydrochloride and the used raw material of series derivates thereof mainly are the chitins that extracts from the shell of crustacean at present, this raw material is confined to the coastland, and being subjected to the influence in season bigger, also there are many defectives such as supersensitivity and vegetarians crowd can not take in the product with shrimp and crab shells chitin raw material production glucosamine hydrochloride in addition.
Though, need the soda acid pre-treatment to cause occurring shortcomings such as large amount of sewage, hydrolysis time length, product ash height at present relevant for the research of hydrolytically separating glucosamine hydrochloride from non-shrimp and crab shells chitin.
The present invention has following advantage: (1) is raw material with the mushroom of plant origin, has avoided traditionally producing many defectives such as the seasonal restriction of product supersensitivity, raw material of glucosamine hydrochloride and vegetarians crowd can not take with the shrimp and crab shells chitin raw material; (2) need not the soda acid pre-treatment, dry citric acid waste raw material direct hydrolysis, the effluent problem of having avoided the soda acid pre-treatment to cause; (3) hydrolysis time is short, only needs 2.5-3 hour.
Summary of the invention
This patent is invented technical problem to be solved, provide a kind of from mushroom the production technique of hydrolytically separating glucosamine hydrochloride, it is that the drying mushroom is hydrolyzed and purifies and separates, and purpose is to obtain the higher glucosamine hydrochloride of yield by simple technology.
Term among the present invention " mushroom " refers to the glucosamine polymer in the tankage (mushroom root or broken mushroom) of cultivation edible mushrooms, flat mushroom and mushroom as raw material sources.
Technical scheme of the present invention is: the production technique of hydrolytically separating glucosamine hydrochloride from mushroom, and the step of its method is:
(1) raw material is prepared: is raw material to be rich in the glucosamine polymer through the exsiccant mushroom, and the weight loss on drying of raw material is less than 18%;
(2) hydrolysis: raw material adds enamel reaction still, adds raw material weight 2-5 hydrochloric acid doubly then, and concentration of hydrochloric acid is 25-37%; Logical steam in the enamel reaction still chuck heats up gradually and stirs, be warming up to 80-150 ℃ after, insulation hydrolysis 1-3.5 hour;
(3) filter: hydrolysis finishes logical water coolant in the enamel reaction still chuck of back, and material begins Plate Filtration after being cooled to below 70 ℃, and filter residue cleans with pure water, merging filtrate and scavenging solution;
(4) resin absorption: filtrate and scavenging solution pump into the pillar that macroporous adsorbent resin is housed, and macroporous adsorbent resin weight is 1/5-1 times of dry mushroom raw material weight.Receive effluent liquid, use residual glucosamine hydrochloride material on the weight resin 1-3 pure water drip washing resin doubly then, merge effluent liquid and leacheate;
(5) concentrate: vacuum concentration, control vacuum tightness be-0.060～-0.099Mpa, make temperature of charge remain on 50-80 ℃, mass crystallization appears and after, stop steam and vacuum, filtration is to remove mother liquor;
(6) micro-filtration: crystallization is dissolved with pure water, utilizes millipore filtration to remove water-insoluble impurity;
(7) crystallization: vacuum concentration, control vacuum tightness be-0.060～-0.099Mpa, make temperature of charge remain on 50-80 ℃, mass crystallization appears.
(8) centrifuge washing: centrifugal removal mother liquor, ethanol drip washing crystallization is centrifugal again, repeatedly several times till crystallization is pure white.
(9) drying: 60-85 ℃ of control drying temperature gets product.
The excellence that the present invention compared with prior art embodies is:
(1) easy, the good reproducibility of technological operation, the productive rate height is applicable to suitability for industrialized production.
(2) with the raw material production ammonia of plant origins such as mushroom sugar series product, avoided traditionally producing many defectives such as the seasonal restriction of product supersensitivity, raw material of glucosamine hydrochloride and vegetarians crowd can not take with the shrimp and crab shells chitin raw material.
(3) technological process is not used the poisonous and harmful solvent, and the pure water of whole health safe in utilization and food grade hydrochloric acid are solvent.
(4) the hydrolysis hydrolysis time only is 2.5-3 hour.
(5) adopt resin absorption to remove impurity such as pigment, avoid the pollution of gac workshop condition.
Embodiment
Come more detailed description the present invention below in conjunction with embodiment, but the present invention is not subjected to the restriction of these embodiment.
Embodiment 1:
Dry mushroom 1000g, 31% hydrochloric acid 3000ml hydrolysis, 95 ℃ of temperature, 3 hours time.Be cooled to below 70 ℃, filter, with 1000ml pure water filter wash slag, merging filtrate is transferred on the D101 type macroporous resin column then, dress 200ml resin in the adsorption column, flow rate control was used 600ml pure water washing resin post then at 200ml/ hour during absorption, merged effluent liquid and water lotion.Destainer vacuum concentration, vacuum degree control be at-0.80--0.99Mpa, and controlled temperature is below 80 ℃, is concentrated into mass crystallization to occur and cooling-sedimentation 24 hours occurs.Filter the coarse crystallization product, the coarse crystallization product is crossed 0.45 μ m millipore filtration then with the dissolving of 200ml pure water, the micro-filtrate vacuum concentration, vacuum degree control is at-0.80--0.99Mpa, and controlled temperature is below 80 ℃, be concentrated into and the mass crystallization appearance occurs, cooling-sedimentation 24 hours, centrifugal, crystallization is washed with 90% alcohol, centrifuge washing is till crystallization is pure white again, the crystallization oven dry, controlled temperature obtains dry glucosamine hydrochloride below 80 ℃.
Embodiment 2:
Dry mushroom 1000g, 25% hydrochloric acid 4000ml hydrolysis, 100 ℃ of temperature, 3.5 hours time.Be cooled to below 70 ℃, filter, with 500ml pure water filter wash slag, merging filtrate is transferred on the D138 type macroporous resin column then, dress 200ml resin in the adsorption column, flow rate control was used 600ml pure water washing resin post then at 200ml/ hour during absorption, merged effluent liquid and water lotion.Destainer vacuum concentration, vacuum degree control be at-0.80--0.99Mpa, and controlled temperature is below 80 ℃, is concentrated into mass crystallization to occur and cooling-sedimentation 24 hours occurs.Filter the coarse crystallization product, the coarse crystallization product is crossed 0.2 μ m millipore filtration then with the dissolving of 200ml pure water, the micro-filtrate vacuum concentration, vacuum degree control is at-0.80--0.99Mpa, and controlled temperature is below 80 ℃, be concentrated into and the mass crystallization appearance occurs, cooling-sedimentation 24 hours, centrifugal, crystallization is washed with 90% alcohol, centrifuge washing is till crystallization is pure white again, the crystallization oven dry, controlled temperature obtains dry glucosamine hydrochloride below 80 ℃.
The product quality indicator of embodiment 1 and embodiment 2: glucosamine hydrochloride content is more than 98%, specific rotation+71.0 °+73.0 °, heavy metal is less than 10ppm, iron is less than 10ppm, sulfate radical is less than 0.24%, and dissolvent residual (alcohol) is less than 0.5%, and ash is less than 0.1%, weight loss on drying is less than 0.2%, and other organic impuritys are less than 0.1%.Product goes out rate 3-6%.
Claims (7)
1, a kind of from mushroom the production technique of hydrolytically separating glucosamine hydrochloride, it is characterized in that: the exsiccant mushroom is used hydrochloric acid hydrolysis, filtration, resin absorption, vacuum concentration, micro-filtration, crystallization, centrifugal successively, dry then, obtain glucosamine hydrochloride.
2, according to claim 1 from mushroom the production technique of hydrolytically separating glucosamine hydrochloride, it is characterized in that: the step of aforesaid method is:
(1) raw material is prepared: is raw material to be rich in glucosamine polymeric through the exsiccant mushroom, and the weight loss on drying of raw material is less than 18%;
(2) hydrolysis: raw material adds enamel reaction still, adds raw material weight 2-5 hydrochloric acid doubly then, and concentration of hydrochloric acid is 25-37%; Logical steam in the enamel reaction still chuck heats up gradually and stirs, be warming up to 80-150 ℃ after, insulation hydrolysis 1-3.5 hour;
(3) filter: hydrolysis finishes logical water coolant in the enamel reaction still chuck of back, and material begins Plate Filtration after being cooled to below 70 ℃, and filter residue cleans with pure water, merging filtrate and scavenging solution;
(4) resin absorption: filtrate and scavenging solution pump into the pillar that macroporous adsorbent resin is housed, and macroporous adsorbent resin weight is 1/5-1 times of dry mushroom raw material weight.Receive effluent liquid, use residual glucosamine hydrochloride material on the weight resin 1-3 pure water drip washing resin doubly then, merge effluent liquid and leacheate;
(5) concentrate: vacuum concentration, control vacuum tightness be-0.060～-0.099Mpa, make temperature of charge remain on 50-80 ℃, mass crystallization appears and after, stop steam and vacuum, filtration is to remove mother liquor;
(6) micro-filtration: crystallization is dissolved with pure water, utilizes millipore filtration to remove water-insoluble impurity;
(7) crystallization: vacuum concentration, control vacuum tightness be-0.060～-0.099Mpa, make temperature of charge remain on 50-80 ℃, mass crystallization appears.
(8) centrifuge washing: centrifugal removal mother liquor, ethanol drip washing crystallization is centrifugal again, repeatedly several times till crystallization is pure white.
(9) drying: 60-85 ℃ of control drying temperature gets product.
3, can be mushroom remaining mushroom root of processing and broken mushroom according to claim 1,2 described mushrooms.
4, according to claim 1,2 described from mushroom the production technique of hydrolytically separating glucosamine hydrochloride, it is characterized in that the hydrolysis concentration of hydrochloric acid is 28-31%.
5, according to claim 1,2 described from mushroom the production technique of hydrolytically separating glucosamine hydrochloride, it is characterized in that hydrolysis temperature is 95-105 ℃.
6, according to claim 1,2 described from mushroom the production technique of hydrolytically separating glucosamine hydrochloride, it is characterized in that hydrolysis time is 3-3.5 hour.
7, according to claim 1,2 described from mushroom the production technique of hydrolytically separating glucosamine hydrochloride, it is characterized in that glucosamine hydrochloride content is more than 98%, specific rotation is+71.0 °-+73.0 °, heavy metal content is less than 10ppm, and iron level is less than 10ppm, and sulfate radical content is less than 0.24%, dissolvent residual is less than 0.5%, ash is less than 0.1%, and weight loss on drying is less than 0.2%, and other organic impuritys are less than 0.1%.
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| CNA200810088878XA CN101550170A (en) | 2008-04-02 | 2008-04-02 | Production technology hydrolytically separating glucosamine hydrochloride from mushrooms |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079762A (en) * | 2011-01-27 | 2011-06-01 | 廊坊师范学院 | Method for separating glucosamine hydrochloride from Lentinus edodes leftovers |
| CN109836463A (en) * | 2019-03-07 | 2019-06-04 | 扬州日兴生物科技股份有限公司 | A kind of energy-saving and environment-friendly high-efficiency ammonia sugar preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125892A (en) * | 2007-09-12 | 2008-02-20 | 扬州日兴生物化工制品有限公司 | Method for producing aminoglucose hydrochloride |
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- 2008-04-02 CN CNA200810088878XA patent/CN101550170A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101125892A (en) * | 2007-09-12 | 2008-02-20 | 扬州日兴生物化工制品有限公司 | Method for producing aminoglucose hydrochloride |
Non-Patent Citations (3)
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| 张立伟 等: "氨基葡萄糖盐酸盐制备及脱色研究", 《化学世界》 * |
| 樊文华: "甲壳素及其应用", 《广西化工》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079762A (en) * | 2011-01-27 | 2011-06-01 | 廊坊师范学院 | Method for separating glucosamine hydrochloride from Lentinus edodes leftovers |
| CN102079762B (en) * | 2011-01-27 | 2013-04-10 | 廊坊师范学院 | Method for separating glucosamine hydrochloride from Lentinus edodes leftovers |
| CN109836463A (en) * | 2019-03-07 | 2019-06-04 | 扬州日兴生物科技股份有限公司 | A kind of energy-saving and environment-friendly high-efficiency ammonia sugar preparation method |
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Application publication date: 20091007 |